May 2024 – Page 8 – Pu catalyst

Methyl magnesium bromide

Structural formula

Business number	01J3
Molecular formula	CH3MgBr
Molecular weight	119.24
label	Grignard reagent, format reagent

Numbering system

CAS number:75-16-1

MDL number:MFCD00000041

EINECS number:200-844-1

RTECS number:OM3700000

BRN number:3535220

PubChem number:24858252

Physical property data

1. Properties: Solid

2. Density (g/mL, 20℃): 1.035

3. Relative vapor density (g/mL, air=1): Undetermined

4. Melting point (ºC): Undetermined

5. Boiling point (ºC, normal pressure): Undetermined

6. Boiling point (ºC, 5.2kPa): Not determined

7. Refractive index: Not determined

8. Flash point (ºF): 77

9. Specific rotation (º ): Undetermined

10. Autoignition point or ignition temperature (ºC): 160

11. Vapor pressure (kPa, 25ºC): Undetermined

12. Saturated vapor pressure (kPa, 60ºC) not determined:

13. Heat of combustion (KJ/mol): not determined

14. Critical temperature (ºC): not determined

15. Critical pressure (KPa): Undetermined

16. Log value of oil-water (octanol/water) partition coefficient: Undetermined

17. Explosion Upper limit (%, V/V): Undetermined

18. Lower explosion limit (%, V/V): Undetermined

19. Solubility: Reacts strongly with water, producing Combustible gas

Toxicological data

None

Ecological data

None

Molecular structure data

None

Compute chemical data

1. Reference value for hydrophobic parameter calculation (XlogP): None

2. Number of hydrogen bond donors: 0

3. Number of hydrogen bond acceptors: 2

4. Number of rotatable chemical bonds: 0

5. Number of tautomers: none

6. Topological molecule polar surface area 0

7. Number of heavy atoms: 3

8. Surface charge: 0

9. Complexity: 4.8

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain number of atomic stereocenters: 0

13. Determine the number of chemical bond stereocenters: 0

14. Number of uncertain chemical bond stereocenters: 0

15. Number of covalent bond units: 3

Properties and stability

Reacts with water, oxides, acids, alkalis, and alcohols.

Sensitive to water, light and air.

Storage method

Store in a cool, dry, well-ventilated non-combustible warehouse. Keep away from fire and heat sources. The warehouse temperature should not exceed 28℃.The packaging must be sealed and must not come into contact with air. Keep away from light. Not suitable for large quantities or long-term storage. It should be stored separately from acids, flammables, combustibles, oxidants, oxygen, compressed air, etc. The lighting, ventilation and other facilities in the storage room should be explosion-proof, and the switches should be located outside the warehouse. Equipped with the appropriate variety and quantity of fire equipment. Fire and explosion prevention technical measures must be taken during tank storage. It is prohibited to use mechanical equipment and tools that are prone to sparks. When handling, load and unload with care to prevent damage to packaging and containers. Smoking, drinking, and eating are not allowed at the operation site.

Synthesis method

Use carbide tools to cut single crystal magnesium flakes with a purity of 99.999%, wash them several times with ether treated with lithium aluminum tetrahydride, and add a dry ice-acetone condenser tube. And in the reaction bottle directly connected to the ether distillation device. The device is repeatedly baked with gas lamps and filled with high-purity nitrogen several times. Add dry ice to the condenser tube, evaporate 50 mL of ether directly into the flask, and then introduce a small amount of ethyl bromide from the side tube installed near the bottom of the condenser tube. Bubbles are released and heat is released, proving that the reaction has begun. Thereafter, continue to pass in methyl bromide and steam into ether. Keep methyl bromide and ether at reflux without heating until the magnesium metal reacts completely. During this period, it is appropriate to keep the ether solution at about 300 mL. Remove the flask in the nitrogen flow and put it in the operating box with a stopper, filter it into the flask with a glass sand funnel, and cover it with a tetrafluoroethylene piston. A colorless and transparent methylmagnesium bromide solution was obtained. The ratio of the analytical values of C:Mg:Br is 1.00:1.03:0.99.

Purpose

for organic synthesis

5-nitrosalicylicaldehyde

Structural formula

Business number	02C8
Molecular formula	C7H5NO4
Molecular weight	167.12
label	2-hydroxy-5-nitrobenzoyl, 2-Hydroxy5-nitrobenzaldehyae

Numbering system

CAS number:97-51-8

MDL number:MFCD00007337

EINECS number:202-587-0

RTECS number:CU6675000

BRN number:512565

PubChem number:24856642

Physical property data

Appearance: light yellow or white powder.
Density (g/mL, 20℃): Undetermined
Relative vapor density (g/mL, air=1): Undetermined
Melting point ( ºC): 125-128
Boiling point (ºC, normal pressure): Undetermined
Boiling point (ºC, KPa): Undetermined
Refractive index: Undetermined Determined
Flash point (ºC): Not determined
Specific optical rotation (º): Not determined
Autoignition point or ignition temperature (ºC): Not determined Determined
Vapor pressure (mmHg, 20.2ºC): Undetermined
Saturation vapor pressure (kPa, ºC): Undetermined
Heat of combustion (KJ/mol ): Undetermined
Critical temperature (ºC): Undetermined
Critical pressure (KPa): Undetermined
Oil-water (octanol/water) partition coefficient Log value: Undetermined
Upper explosion limit (%, V/V): Undetermined
Lower explosion limit (%, V/V): Undetermined
Solubility: Not determined

Toxicological data

Acute toxicity: Rat oral LD50: 799mg/kg; Mouse oral LD50: 672mg/kg;

Ecological data

None

Molecular structure data

1. Molar refractive index: 41.43

2. Molar volume (cm³/mol): 111.3

3. Isotonic specific volume (90.2K ): 322.8

4. Surface tension (dyne/cm): 70.5

5. Polarizability (10-24cm3): 16.42

Compute chemical data

1. Reference value for hydrophobic parameter calculation (XlogP): None

2. Number of hydrogen bond donors: 1

3. Number of hydrogen bond acceptors: 4

4. Number of rotatable chemical bonds: 1

5. Number of tautomers: 4

6. Topological molecule polar surface area 83.1

7. Number of heavy atoms: 12

8. Surface charge: 0

9. Complexity: 188

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain number of atomic stereocenters: 0

13. Determine the number of chemical bond stereocenters: 0

14. Number of uncertain chemical bond stereocenters: 0

15. Number of covalent bond units: 1

Properties and stability

None

Storage method

None

Synthesis method

None

Purpose

Intermediates for organic synthesis of medicines, spices and dyes.

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carbon disulfide

Structural formula

Business number	01J2
Molecular formula	CS2
Molecular weight	76.14
label	carbon disulfide, Dithoicarbonic anhydride, Carbon bisulfide, Aliphatic sulfur compounds

Numbering system

CAS number:75-15-0

MDL number:MFCD00011321

EINECS number:200-843-6

RTECS number:FF6650000

BRN number:1098293

PubChem number:24860298

Physical property data

1. Properties: colorless or light yellow transparent liquid with pungent odor and easy to evaporate. ^[1]

2. Melting point (℃): -111.5^[2]

3. Boiling point (℃): 46.3^[3]

4. Relative density (water = 1): 1.26^[4]

5. Relative vapor Density (air=1): 2.63^[5]

6. Saturated vapor pressure (kPa): 40 (20℃)^[6]

7. Heat of combustion (kJ/mol): -1029.4^[7]

8. Critical temperature (℃): 280^[8]

9. Critical pressure (MPa): 7.39^[9]

10. Octanol/water partition coefficient: 1.94^[10]

11. Flash point (℃): -30 (CC) ^[11]

12. Ignition temperature ( ℃): 90^[12]

13. Explosion upper limit (%): 50.0^[13]

14. Explosion Lower limit (%): 1.3^[14]

15. Solubility: Insoluble in water, soluble in most organic solvents such as ethanol and ether. ^[15]

16. Refractive index (25ºC): 1.6241

17. Viscosity (mPa·s, 20ºC): 0.363

18. Ignition point (ºC): 100

19. Heat of evaporation (KJ/mol, 25ºC): 27.54

20. Heat of fusion (KJ/mol): 4.392

21. Heat of formation (KJ/mol): 89.47

22. Specific heat capacity (KJ/(kg·K), 25ºC, constant pressure): 1.00

23 .Conductivity (S/m, 25ºC): 3.7×10^-3

Toxicological data

1. Acute toxicity^[16] LD50: 3188mg/kg (rat oral)

2. Irritation No data yet

3. Subacute and chronic toxicity^[17] Rabbit inhalation 1.28g/m³, 5 months, causing chronic poisoning; 0.5~0.6g/m³, 6.5 months, causing an increase in serum cholesterol.

4. Mutagenicity ^[18] Microbial mutagenicity: Salmonella typhimurium 100μg/dish. Sister chromatid exchange: human lymphocytes 10200μg/L

5. Teratogenicity ^[19] Inhalation is the lowest in rats 1 to 22 days after pregnancy Toxic dose (TCLo) 10mg/m³ (8h) can cause eye and ear development malformations. Rats inhaled the lowest toxic dose (TCLo) 100 mg/m³ (8 hours) from 1 to 21 days after pregnancy, causing developmental malformations of the craniofacial region (including nose and tongue).

6. Others^[20] Minimum toxic concentration for male inhalation (TCLo): 40mg/m³ (91 weeks ), causing changes in sperm production. The lowest toxic concentration for inhalation in rats (TCLo): 100mg/m³ (8h) (administered from 1st to 21st day of pregnancy), �� Started with fetal death and abnormal craniofacial development.

Ecological data

1. Ecotoxicity^[21] LC50: 162~135mg/L (24~96h) (mosquito fish)

2. Biodegradability No data yet

3. Non-biodegradability^[22] In the air, when hydroxyl radicals When the concentration is 5.00×10⁵ pieces/cm³, the degradation half-life is 5.5d (theoretical).

4. Bioaccumulation ^[23] BCF: <6.1 (carp, contact concentration 50μg/L) <60 (carp, contact concentration 5μg/L)

Molecular structure data

1. Molar refractive index: 21.50

2. Molar volume (cm³/mol): 60.4

3. Isotonic specific volume (90.2K ): 143.8

4. Surface tension (dyne/cm): 32.0

5. Polarizability (10^-24cm³): 8.52

Compute chemical data

1. Reference value for hydrophobic parameter calculation (XlogP): 2.1

2. Number of hydrogen bond donors: 0

3. Number of hydrogen bond acceptors: 2

4. Number of rotatable chemical bonds: 0

5. Number of tautomers: none

6. Topological molecule polar surface area 64.2

7. Number of heavy atoms: 3

8. Surface charge: 0

9. Complexity: 18.3

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain number of atomic stereocenters: 0

13. Determine the number of chemical bond stereocenters: 0

14. Number of uncertain chemical bond stereocenters: 0

15. Number of covalent bond units: 1

Properties and stability

1. Extremely flammable and can easily burn and explode when exposed to heat, sparks, flames or oxidants. Decomposes when heated to produce toxic sulfide fumes. Reacts violently with aluminum, zinc, potassium, fluorine, chlorine, azide, etc., posing a risk of combustion and explosion. High-speed impact and friction can cause combustion and explosion due to static spark discharge.

2. Chemical properties: Stable to acids, and does not interact with concentrated sulfuric acid and concentrated nitric acid at room temperature. But it is unstable to alkali and reacts with potassium hydroxide to generate potassium thiosulfate and potassium carbonate. It reacts with sodium alcohol to form xanthate; it gradually oxidizes in the air, becoming yellow and smelly. It decomposes under the influence of sunlight; at low temperatures, it reacts with water to form crystals with the structure of 2CS2·H2O. It reacts with chlorine under appropriate conditions to produce carbon tetrachloride and sulfur chloride.

3. The high-concentration vapor of this product has an anesthetic effect. The concentration is 0.1% to 0.3%. Inhalation can cause death in 1 hour. Even if it is lower than the lethal dose, it will leave sequelae. Long-term inhalation (3 months) 160 When ×10-6 or more, neuritis will occur after 1 to 2 years. The maximum allowable concentration in the workplace is 60mg/m3. This product is toxic and irritating. Closed operation, local exhaust. Operators must undergo special training and strictly abide by operating procedures. It is recommended that operators wear self-priming filter gas masks (half masks), chemical safety glasses, anti-static overalls, and rubber oil-resistant gloves. Keep away from fire and heat sources. Smoking is strictly prohibited in the workplace. Use explosion-proof ventilation systems and equipment. Prevent vapors from leaking into the workplace air. Avoid contact with oxidants, amines, and alkali metals. The flow rate should be controlled during filling, and a grounding device should be installed to prevent the accumulation of static electricity. Equipped with corresponding varieties and quantities of fire-fighting equipment and leakage emergency treatment equipment. Empty containers may be harmful residues.

4. Due to its low boiling point, strong volatility and high toxicity, it is easily dispersed in the air during production and use, causing serious pollution and harm to the environment and human body. Carbon disulfide is a poison that damages nerves and blood vessels. When people are exposed to high concentrations of carbon disulfide, it has a paralyzing effect. If it lasts for a long time, the respiratory center may be paralyzed, resulting in loss of consciousness and death. At high concentrations, it can also be absorbed by human skin.

5. This product is a gas anesthetic. Its vapor has a strong irritating effect on the skin and eyes, and can easily cause dermatitis and burns. Acute poisoning begins to cause delirium, and later anesthesia, loss of consciousness, and even death from respiratory failure. Long-term inhalation of its vapor can cause symptoms such as weak stomach, insomnia, fatigue, loss of appetite, headache, dizziness, abnormal sensation, drop in blood pressure, trembling, stiffness of hands and feet, slow movement, salivation, sweating, memory loss and other symptoms. Mainly damages the nervous and cardiovascular systems. When the vapor concentration is 12440 mg/m3, death will occur in 30 to 60 minutes. TJ 36-79 stipulates that the maximum allowable concentration in workshop air is 10 mg/m3.

6. Stability^[24] Stable

7. Incompatible substances^[25] Strong oxidizing agent, aluminum

8. Conditions to avoid contact^[26] Heating

9. Polymerization hazard^[27] No polymerization

10. Decomposition products^[28] Hydrogen chloride

Storage method

1. Storage precautions^[29]It is easily volatile at room temperature, so the surface of the container can be covered with water. Store in a cool, ventilated warehouse. Keep away from fire and heat sources. The storage temperature should not exceed 29°C. Keep container tightly sealed. They should be stored separately from oxidants, amines, alkali metals, and food chemicals, and avoid mixed storage. Use explosion-proof lighting and ventilation facilities. It is prohibited to use mechanical equipment and tools that are prone to sparks. The storage area should be equipped with leakage emergency treatment equipmentequipment and suitable containment materials.

2. This product is packed in glass bottles and metal barrels (aluminum barrels, iron barrels, storage tanks) and protected by wooden boxes, and must be stored in In a warehouse constructed of non-combustible materials and with ground ventilation facilities, keep away from fire sources and avoid sunlight. In summer, cooling measures should be taken to keep storage below 17°C. There should be no electrical equipment or heating facilities near the warehouse, and lightning or static electricity must be prevented from igniting fires. The liquid level of the storage tank should be sealed with inert gas. Store and transport according to regulations for flammable materials.

Synthesis method

1. Methane sulfur method: solid sulfur is heated and melted into liquid, and then purified with activated clay. Natural gas purification treatment uses light diesel to adsorb fractions above C2 and separate pure methane gas. After the natural gas and sulfur vapor are heated, they can be fully mixed and heated to 650°C, and then sent to the reactor for reaction. The pressurized partial condensation method is used to separate carbon disulfide and hydrogen sulfide, and carbon disulfide is obtained after distillation. The reaction formula is as follows:

2. Charcoal sulfur method : According to different heating methods, it can be divided into two categories: external heating iron steamer method and internal heating electric furnace method. Generally, the three-phase electric furnace method is used. In the electric furnace method, charcoal is directly roasted at 800°C to remove moisture and organic matter and then added to the electric furnace intermittently. Molten sulfur is continuously added to the electric furnace to react with the red charcoal at about 1000°C. The generated carbon disulfide is desulfurized and condensed to obtain a crude product, which is then refined. Distillation and condensation to obtain carbon disulfide finished product. The reaction formula is as follows:

3. Commercially available Carbon disulfide is synthesized by heating charcoal and sulfur to 850 to 950°C. As a reagent, it can meet general requirements, but when the required purity is high, the following methods need to be used to remove the impurities contained in it. These impurities are hydrogen sulfide, sulfurous acid, sulfuric acid, organic sulfides, water and sulfur. Add 100 to 200 g of mercury and an appropriate amount of phosphorus pentoxide to 500 mL of commercially available carbon disulfide, shake for about 1 hour, filter, fractionate the filtrate away from light, discard the high and low fractions, and collect the middle fraction. The collected fractions are remixed with mercury and phosphorus pentoxide, shaken, and fractionated. Repeat this operation until the content of harmful impurities reaches the standard.

Refining method: Impurities contained include sulfur, sulfide and water. There are several refining methods: ① Distill 3 times with a glass still. ② Dry with calcium chloride and then fractionate multiple times. ③ Shake with mercury to remove sulfide, then dry and fractionate with phosphorus pentoxide. ④ Add 5g of crushed potassium permanganate to 1L of carbon disulfide and shake it thoroughly until the hydrogen sulfide is completely removed and then place it. After separation, add a small amount of mercury and shake it to remove the sulfur until the interface does not turn black further. Finally, add 5g of mercury sulfate to each 1L of carbon disulfide and shake to eliminate the odor. After separation, it is dried with calcium chloride and fractionated.

4. Use industrial carbon disulfide as raw material, add anhydrous copper sulfate (25-37.5g copper sulfate is required for each carbon disulfide), stir thoroughly until the black powder disappears and there is no unpleasant smell, immediately Filter to remove insoluble impurities, then add anhydrous copper sulfate to the filtrate, distill, and collect the fractions according to product specifications, which is the pure product.

Purpose

1. Used in the manufacture of viscose fiber, cellophane, xanthate, thiocyanate and carbon tetrachloride. Xanthate produced from carbon disulfide is used as an ore flotation agent in the metallurgical industry. Used in the production of agricultural pesticides. When vulcanized in the rubber industry, it can be used as a solvent for sulfur chloride. Use it to make anti-corrosion agents for equipment and pipelines in ammonia treatment systems. It is also a solvent used for testing primary amines, secondary amines and α-amino acids, measuring refractive index, and chromatographic analysis. It is also used to extract oil from linseed, olive fruit, animal bones, leather and wool. Used as an accelerator in aviation. It is also used as a solvent for grease, wax, paint, camphor, resin, rubber, sulfur, phosphorus, iodine, etc., as a degreaser for wool, as an agricultural pesticide, as a soil disinfectant, as a stain remover for clothes, etc. In analysis, it is used for the determination of primary amines, secondary amines and α-amino acids and as a solvent for infrared spectroscopy.

2. Carbon disulfide is widely used in metallurgy, pesticides, rubber, viscose fiber and other industrial fields. It has good penetrability and is generally used as a mixture with non-combustible ingredients when fumigating grain. Fumigation of dry seeds with carbon disulfide does not reduce seed viability. For grains such as wheat, barley, corn, rice, etc., fumigation at 250g/m3 for 24 hours will not affect germination. Gaseous carbon disulfide will seriously damage or kill growing plants or seedlings. Water-diluted carbon disulfide emulsion treats the soil around the roots of evergreen trees and deciduous seedlings, and can effectively control a variety of underground pests. Due to the flammable and explosive properties of carbon disulfide, this agent is used less and less in modern fumigations.

3. Mainly used as raw material for manufacturing viscose fiber and cellophane. Xanthate produced from carbon disulfide is used as an ore flotation agent in the metallurgical industry. Used in the production of agricultural pesticides. When vulcanized in the rubber industry, it can be used as a solvent for sulfur chloride. It is also a solvent used for testing primary amines, secondary amines and α-amino acids, measuring refractive index, and chromatographic analysis. It is also used to extract oil from linseed, olive fruit, animal bones, leather and wool. Used as aerospace accelerator.

4. Used as analytical reagents, solvents, viscose fibersVJ wool degreaser. Also used for refractive index determination.

5. Used in the manufacture of rayon, pesticides, accelerator M, accelerator D, and also used as solvents. ^[30]

5-Chloro-2,4-dimethoxyaniline

Structural formula

Business number	02C7
Molecular formula	C8H10ClNO2
Molecular weight	187.62
label	2,4-Dimethoxy-5-chloroaniline

Numbering system

CAS number:97-50-7

MDL number:MFCD00025752

EINECS number:202-586-5

RTECS number:None

BRN number:2211013

PubChem number:24862121

Physical property data

Characteristics: white to light gray crystal.
Density (g/mL, 20℃): Undetermined
Relative vapor density (g/mL, air=1): Undetermined
Melting point ( ºC): 89-92
Boiling point (ºC, normal pressure): Undetermined
Boiling point (ºC, KPa): Undetermined
Refractive index: Undetermined Determined
Flash point (ºC): Not determined
Specific optical rotation (º): Not determined
Autoignition point or ignition temperature (ºC): Not determined Determined
Vapor pressure (mmHg, 20.2ºC): Undetermined
Saturation vapor pressure (kPa, ºC): Undetermined
Heat of combustion (KJ/mol ): Undetermined
Critical temperature (ºC): Undetermined
Critical pressure (KPa): Undetermined
Oil-water (octanol/water) partition coefficient Log value: Undetermined
Upper explosion limit (%, V/V): Undetermined
Lower explosion limit (%, V/V): Undetermined
Solubility: Not determined

Toxicological data

None

Ecological data

None

Molecular structure data

1. Molar refractive index: 45.64

2. Molar volume (cm³/mol): 132.6

3. Isotonic specific volume (90.2K ): 359.2

4. Surface tension (dyne/cm): 53.7

5. Polarizability (10-24cm3): 18.09

Compute chemical data

1. Reference value for hydrophobic parameter calculation (XlogP): 1.8

2. Number of hydrogen bond donors: 1

3. Number of hydrogen bond acceptors: 3

4. Number of rotatable chemical bonds: 2

5. Number of tautomers: none

6. Topological molecule polar surface area 44.5

7. Number of heavy atoms: 12

8. Surface charge: 0

9. Complexity: 145

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain number of atomic stereocenters: 0

13. Determine the number of chemical bond stereocenters: 0

14. Number of uncertain chemical bond stereocenters: 0

15. Number of covalent bond units: 1

Properties and stability

None

Storage method

None

Synthesis method

None

Purpose

Used in the synthesis of naphthol AS-ITR, Pigment Red 5 and other dyes and their intermediates.

DL-glyceraldehyde

Structural formula

Business number	017X
Molecular formula	C3H6O3
Molecular weight	90.08
label	None

Numbering system

CAS number:56-82-6

MDL number:MFCD00064379

EINECS number:200-290-0

RTECS number:MA6475000

BRN number:635685

PubChem number:24895192

Physical property data

1. Properties: white crystal.

2. Density (g/mL, 25/4℃): 1.445

3. Relative vapor density (g/mL, air=1): Undetermined

4. Melting point (ºC): 145

5. Boiling point (ºC, normal pressure): Undetermined

6. Boiling point (ºC, 5.2kPa): Undetermined

7. Refractive index: Undetermined

8. Flash point (ºC): Undetermined

9. Specific rotation (º): Undetermined

7. p>

10. Autoignition point or ignition temperature (ºC): Undetermined

11. Vapor pressure (kPa, 25ºC): Undetermined

12. Saturated vapor pressure (kPa, 60ºC): Undetermined

13. Heat of combustion (KJ/mol): Undetermined

14. Critical temperature (ºC): Undetermined

15. Critical pressure (KPa): Undetermined

16. Log value of oil-water (octanol/water) partition coefficient: Undetermined

17. Explosion upper limit (%, V /V): Undetermined

18. Lower explosion limit (%, V/V): Undetermined

19. Solubility: Slightly soluble in water, insoluble in benzene and petroleum ether and pentane.

Toxicological data

1. Acute toxicity: rat abdominal LD50: 2mg/kg 2. Mutagenicity: mutation microorganismsTEST system: bacteria – Salmonella typhimurium: 100ug/plate

Ecological data

None

Molecular structure data

5. Molecular property data:

1. Molar refractive index: 19.16

2. Molar volume (cm³/mol): 70.7

3. Isotonic specific volume (90.2K): 191.2

4. Surface tension (dyne/cm): 53.3

5. Polarizability (10^-24cm³): 7.59

Compute chemical data

1. Reference value for calculation of hydrophobic parameters (XlogP): -1.6

2. Number of hydrogen bond donors: 2

3. Number of hydrogen bond acceptors: 3

4. Number of rotatable chemical bonds: 2

5. Number of tautomers: 3

6. Topological molecule polar surface area 57.5

7. Number of heavy atoms: 6

8. Surface charge: 0

9. Complexity: 43.3

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain number of atomic stereocenters: 1

13. Determine ��Number of stereocenters of chemical bonds: 0

14. Number of stereocenters of uncertain chemical bonds: 0

15. Number of covalent bond units: 1

Properties and stability

None

Storage method

This product should be stored in a sealed, cool place and away from light.

Synthesis method

1. Mix 50g (0.3mol) diethanol acetal DL-glyceraldehyde and 500ml 0.1mol/L sulfuric acid, and place at 20°C for 7 days. After adding 30ml of glacial acetic acid, neutralize with barium hydroxide solution, add 5g of activated carbon, stir and filter. The water in the filtrate was evaporated under reduced pressure, and an equal volume of absolute ethanol was added to the residue. The crystals were filtered out and dried to obtain 22g DL-glyceraldehyde, with a yield of 80%.

2. Preparation method:

Dietol-β-chloroacetaldehyde (3): In a 3L reaction bottle equipped with a stirrer and ventilation tube, add 253 mL of absolute ethanol, cool it to below 0°C in an ice-salt bath, and dry it of hydrogen chloride gas to saturation. While stirring, 112g (2.0 mol) of acrolein (2) cooled to 0°C was added dropwise, the reaction temperature was controlled to 0°C, and the addition was completed in about 1.5 hours. Let stand and separate the layers, separate the lower organic layer, add solid sodium bicarbonate powder in batches, neutralize and remove acid. Filter, wash the filtrate with ice water, and dry over anhydrous potassium carbonate for 10 hours. After filtration, distill under reduced pressure and collect the fractions at 58-62°C/1.06kPa to obtain 112g of diethanol-β-chloroacetaldehyde (3) with a yield of 34%. Diethanol acrolein (4): Add 340g (6mol) of dry powdered potassium hydroxide and 167g (1.0mol) of the above compound (3) into a distillation bottle. After shaking vigorously, install a fractionation device. Heat the distillation bottle in an oil bath at 210 to 220°C until no more distillate is distilled. The water in the distillate was separated, and the organic layer was dried with potassium carbonate, filtered and distilled. The fractions at 122-126°C were collected to obtain 98g of diethanol acrolein (4), with a yield of 75%. Diethylglyceraldehyde (5): In a reaction bottle equipped with a stirrer, thermometer, and dropping funnel, add 65g (0.5mol) of diethylglyceraldehyde (4) and 600mL of water, cool to 5°C, and stir Add dropwise a solution of 80g (0.5mol) water, control the dropping speed to about 25mL/min, and keep the temperature of the reaction solution at about 5°C. Stirring – stop, the reactants will become gel-like. After leaving it for 2 hours, heat it in a steam bath for 1 hour. Filter with suction, and wash the manganese dioxide with 150 mL of water. Combine the filtrate and washing liquid, and add 1200g anhydrous potassium carbonate while cooling. The organic layer was separated, and the aqueous layer was extracted 4 times with diethyl ether. The organic layers were combined and dried over anhydrous potassium carbonate. After recovering the diethyl ether, distill under reduced pressure and collect the fraction at 120-121°C/1.06kPa to obtain 55g of diethyl glyceraldehyde (5) with a yield of 67%. DL-Glyceraldehyde (1): Place 50g (0.3mol) of the above-mentioned diethanol glyceraldehyde (5) and 0.05mol/L sulfuric acid in a reaction bottle, and place it at 20°C for 1 week. Add 30 mL of glacial acetic acid. The reaction compound was carefully neutralized with barium hydroxide solution and decolorized with activated carbon. Filter, and the filtrate is concentrated at a pressure of 1.33kPa. Add an equal volume of absolute ethanol to the remainder and slowly crystallize. Filter the precipitated crystals and vacuum dry them in a vacuum dryer containing soda lime and calcium chloride desiccant to obtain 22g of DL-glyceraldehyde (1) with a yield of 80%. ^[1]

Purpose

Used in biochemical research, organic synthesis intermediates, and nutritional agents.

formamide

Structural formula

Business number	01J1
Molecular formula	CH3NO
Molecular weight	45.04
label	Aminoformaldehyde, Methanamide, Carbamaldehyde, Reagents for genetic engineering research, paper treatment agent, Softeners for the fiber industry, Softener for animal glue, Reaction solvents for organic synthesis

Numbering system

CAS number:75-12-7

MDL number:MFCD00007941

EINECS number:200-842-0

RTECS number:LQ0525000

BRN number:505995

PubChem number:24894985

Physical property data

1. Properties: Colorless and transparent viscous liquid with a slight ammonia smell and hygroscopicity.

2. Boiling point (ºC, 101.3kPa, partially decomposed): 220, 70.5ºC (133.3pa)

3. Melting point (ºC): 2.55~3

4. Relative density (g/mL, 20/4ºC): 1.13339

5. Relative density (g/mL, 25/4ºC): 1.134

6. Relative steam Density (g/mL, air=1): 1.55

7. Refractive index (20ºC): 1.447

8. Refractive index (25ºC): 1.44682

9. Viscosity (mPa·s, 20ºC): 3.764

10. Viscosity (mPa·s, 25ºC): 3.302

11. Flash point (ºC, closed): 175

12. Flash point (ºC, open): 150

13. Fire point (ºC): >500

14. Heat of vaporization (KJ/mol, 25ºC): 65.021

15. Heat of fusion (KJ/mol): 6.699

16. Heat of formation (KJ/mol, 25ºC, liquid): -254.1

17. Heat of combustion (KJ/mol, 25ºC, liquid): 568.6

18. Specific heat capacity (KJ/(kg·K), 25ºC, constant pressure): 2.39

19. Conductivity (S/m): <2×10^-1

20. Solubility: Can be dissolved with water, alcohol, ethylene glycol, acetone, acetic acid, dihydrogen Miscible with alkane, glycerin, phenol, etc. But it is almost insoluble in aliphatic hydrocarbons, aromatic hydrocarbons, ethers, chlorinated hydrocarbons, chlorobenzene, nitrobenzene, etc.

Toxicological data

Formamide has an irritating effect on the skin and mucous membranes, can occasionally cause allergies, and can be absorbed by the skin. The oral lethal dose LD for rats is 7500 mg/kg. Rat oral LD50>4000mg/kg. Dermal toxicity in guinea pigs is LD50<5mL/kg and LD50 is 2539mg/kg.

Ecological data

None

Molecular structure data

1. Molar refractive index: 10.40

2. Molar volume (cm³/mol): 46.0

3. Isotonic specific volume (90.2K): 109.8

4. Surface tension (dyne/cm): 32.4

5. Polarizability (10^-24cm³): 4.12 p>

Compute chemical data

1. Hydrophobic parameter calculation reference value (XlogP): -0.8

2. Number of hydrogen bond donors: 1

3. Number of hydrogen bond acceptors: 1

4. Number of rotatable chemical bonds: 0

5. Number of tautomers: 2

6. Topological molecular polar surface area (TPSA): 43.1

7. Number of heavy atoms: 3

8. Surface charge: 0

9. Complexity: 12.3

10. Isotopic atoms Quantity: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain number of atomic stereocenters: 0

13. Determine the chemical bond structure Number of stereocenters: 0

14, Number of uncertain chemical bond stereocenters: 0

15, Number of covalent bond units: 1

Properties and stability

1. Chemical properties: The alkalinity of formamide is very weak, so the salt formed with strong acid is very unstable. Formamide is easily hydrolyzed to ammonium formate in aqueous solution. Ammonium formate is heated and dehydrated to form formamide again:

The hydrolysis rate of formamide is very slow at room temperature, but it is actually relatively stable. However, the hydrolysis rate is relatively fast at high temperatures, especially in the presence of acids and alkalis. There are two ways to pyrolyze formamide: it decomposes into ammonia and carbon monoxide when boiled under normal pressure:

When gaseous formamide is pyrolyzed at 400~600°C in the presence of a dehydrating agent, hydrogen cyanide is obtained , yield 90%:

The adduct formed by formamide and strong acid is very reactive and can undergo the following reactions:

Formamide reacts with alcohol in the presence of hydrogen chloride to form formate. . It reacts with hypochlorous acid in a cold water bath to form N,N-dichloroformamide HCONCl2. This compound is explosive when pure. It reacts with metal potassium and sodium to form a metal compound such as diformamide (HCO)2NH. Photochemical reactions with alkenes produce fatty acid amides. Reacts with alkyl halides at 150°C to form formamide compounds and formic esters:

Formamide reacts with metal salts to form substitutions or adducts:

Formamide reacts with pentoxide Dehydration under the action of diphosphorus produces hydrogen cyanide.

2.This product has low toxicity. Temporarily irritating to skin and mucous membranes. The oral LC50 of mice is greater than 1000mg/kg. Wear protective equipment for long-term exposure.

3. Exist in smoke.
　

Storage method

1. This product should be kept sealed, cool and dry. Keep sealed, avoid contact with water, and store in a cool and ventilated place.

2. Formamide products can be stored and transported in stainless steel or aluminum tanks (tank trucks) or tank-type containers as well as 60kg and 220kg drums. The container material can be polyethylene or polyethylene-lined steel. Keep sealed, avoid contact with water, and store in a cool and ventilated place.

Synthesis method

1. Two-step method: The first step is to generate methyl formate from carbon monoxide and methanol under the action of sodium methoxide. In the second step, methyl formate is ammonolyzed to form formamide, and the reaction conditions are 80-100°C and 0.2-0.6MPa. This method has fewer problems.

2. Formic acid method Formic acid and methanol First, esterification reaction is performed to generate methyl formate, and then ammonolysis is performed to generate formamide, and then distillation is performed to separate methanol and impurities to obtain the finished product. This method has become obsolete due to its high cost.

3. One-step method consists of carbon monoxide and Ammonia is catalyzed by sodium methoxide to directly synthesize formamide through high pressure (10-30MPa) and temperature of 80-100℃

4. Formic acid and urea method.

5. The new method consists of sodium formate and Ammonium salt reacts under certain temperature and pressure to form formamide. This method is a domestic patent invention.

Refining method: Formamide is produced on a large scale from carbon monoxide and ammonia at 15~20MPa and 200℃. It can also be obtained by heating ammonium formate or the reaction between formate and ammonia. Therefore, it often contains water, ammonia, methanol, formate and ammonium formate. The purity of formamide can be improved by using fractional distillation under reduced pressure or fractional crystallization. Formamide used for determination of physical constants can be refined by adding a few drops of bromothymol blue to formamide. Neutralize with sodium hydroxide, heat the neutralized solution at 80 to 90°C under reduced pressure, and then neutralize. Repeat the operation several times until the solution remains neutral during heating. Then add sodium formate and distill under reduced pressure at 80~90°C. The distillate is neutralized and then distilled, and the next 4/5 fractions are collected to obtain formamide with a melting point of 2.2°C.

6.Ammonium formate is heated and decomposed to obtain formamide, which is then refined through distillation:

Purpose

1. Formamide has active reactivity and special solubility. It can be used as a raw material for organic synthesis, paper treatment agent, softener in the fiber industry, softener for animal glue, and also used to determine the amino acid content in rice. Analytical reagents. In organic synthesis, it is mostly used in medicine, and it also has many uses in pesticides, dyes, pigments, spices, and auxiliaries. It is also an excellent organic solvent and is mainly used in the spinning of acrylonitrile copolymers and ion exchange resins, as well as in the anti-static coating or conductive coating of plastic products. In addition, it is also used to separate chlorosilanes, purify oils, etc. Formamide can undergo a variety of reactions. In addition to the participation of three hydrogens in the reaction, it can also undergo dehydration, removal of CO, introduction of amino groups, introduction of acyl groups and cyclization reactions. Take Ringhe as an example. Diethyl malonate is cyclized with formamide to obtain the intermediate 4,6-dihydroxypyrimidine of vitamin B4. Anthranilic acid is cyclized with an amide to obtain the antiarrhythmic croroline intermediate quinazolone-4. 3-Amino-4-ethoxycarbonylpyrazole is cyclized with carboxamide to obtain the xanthine oxidase inhibitor allopurinol . The anticancer drug ethyleneimine is obtained by cyclizing ethylenediaminetetraacetic acid with formamide. Methyl ethyl methoxymalonate is cyclized with formamide to obtain disodium 5-methoxy-4,6-dihydroxypyrimidine, an intermediate of sulfonamide drugs.

2. Since formamide can dissolve inorganic salts and proteins with high dielectric constants, it can be used in the electrolysis and electroplating industries, as well as as reaction solvents and refining solvents for organic synthesis. In addition, formamide is also used as a raw material for medicines, dyes, spices, etc., as a treatment agent for paper, as a softener in the fiber industry, and as a softener for animal glue.

3.Used as raw material for organic synthesis. Polar solvent for organic reactions. Liquid chromatography solvents and eluents.

acetylsamine

Structural formula

Business number	02C6
Molecular formula	C8H10AsNO5
Molecular weight	275.09
label	acetapine, 3-acetamido-4-hydroxyphenylarsonic acid, acetylsamine, Acetaminophen Hydroxybenzoic Acid, Acetamide arsine, N-Acetyl-4-hydroxy-m-arsanilic acid, [3-(Acetylamino)-4-hydroxyphenyl)]arsonic acid, Acetphenarsine

Numbering system

CAS number:97-44-9

MDL number:MFCD00019936

EINECS number:202-582-3

RTECS number:CF8400000

BRN number:None

PubChem number:24890414

Physical property data

1. Properties: White prismatic crystals, odorless.

2. Density (g/mL, 20℃): Undetermined

3. Relative vapor density (g/mL, air=1): Undetermined

4. Melting point (ºC): 240-250℃ (decomposition)

5. Boiling point (ºC, normal pressure): Undetermined

6. Boiling point (ºC, KPa) : Undetermined

7. Refractive index: Undetermined

8. Flash point (ºC): Undetermined

9. Specific rotation (º): Not determined

10. Autoignition point or ignition temperature (ºC): Not determined

11. Vapor pressure (mmHg, 20.2ºC): Not determined

12. Saturated vapor pressure (kPa, ºC): Undetermined

13. Heat of combustion (KJ/mol): Undetermined

14. Critical temperature (ºC): Undetermined

15. Critical pressure (KPa): Undetermined

16. Log value of oil-water (octanol/water) partition coefficient: Undetermined

17. Explosion Upper limit (%, V/V): Undetermined

18. Lower explosion limit (%, V/V): Undetermined

19. Solubility: Slightly soluble in cold water and ethanol and dilute acids, soluble in boiling water, caustic alkali solutions or carbonic acid alkali solutions.

Toxicological data

Rat oral LD₅₀ is 4mg/kg

Ecological data

None

Molecular structure data

None

Compute chemical data

1. Reference value for hydrophobic parameter calculation (XlogP): None

2. Number of hydrogen bond donors: 4

3. Number of hydrogen bond acceptors: 5

4. Number of rotatable chemical bonds: 2

5. Number of tautomers: 10

6. Topological molecule polar surface area 107

7. Number of heavy atoms: 15

8. Surface charge: 0

9. Complexity: 289

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain.Number of ��stereocenters: 0

13. Determine the number of stereocenters of chemical bonds: 0

14. Uncertain number of stereocenters of chemical bonds: 0

15. Number of covalent bond units: 1

Properties and stability

1. Highly toxic.

Storage method

Stored sealed and protected from light.

Synthesis method

Originated from acetylation of 1.3-amino-4-hydroxyphenylarsonic acid. Add 3-amino-4-hydroxyphenylarsonic acid to 5% sodium hydroxide solution and stir until completely dissolved. Adjust pH to 8, heat to 30-35°C, add acetic anhydride under vigorous stirring to precipitate, continue stirring for 1 hour, add hydrochloric acid at 55-60°C to precipitate crystals, filter, and wash with water to obtain crude acetylsamine. Refining: Dissolve the crude product in 5% sodium hydroxide solution, add activated carbon, stir, filter, and slowly add 10% sulfuric acid to the filtrate to make the Congo red test paper turn blue and precipitate crystals. Filter and wash to obtain refined acetylsamine.

Purpose

1. Medicine. Disinfectant, has the effect of killing trichomoniasis, and is used to treat vaginal trichomoniasis. It is often made into Diweijing tablets, each tablet contains 0.25g of acetylsamine and 0.30g of boric acid.

Diiodomethane

Structural formula

Business number	01J0
Molecular formula	CH2I2
Molecular weight	267.84
label	methylene iodide, methine iodide, methylene diiodide, methylene iodide, Methylene iodide, Methylene diodide, Aliphatic halogenated derivatives

Numbering system

CAS number:75-11-6

MDL number:MFCD00001079

EINECS number:200-841-5

RTECS number:PA8575000

BRN number:1696892

PubChem number:24849735

Physical property data

1. Properties: colorless clear to light yellow liquid. ^[14]

2. Melting point (℃): 5~6^[15]

3. Boiling point (℃) : 181 (decomposition) ^[16]

4. Relative density (water = 1): 3.32^[17]

5. Relative vapor density (air = 1): 9.25^[18]

6. Heat of combustion (kJ/mol): -745.7^[19]

7. Critical pressure (MPa): 5.47^[20]

8. Octanol/water partition coefficient: 2.3^[21]

9. Flash point (℃): 110^[22]

10. Solubility: insoluble in water, soluble in ethanol, Most organic solvents such as ether, benzene, and chloroform. ^[23]

11. Refractive index at room temperature (n²⁰): 1.7411

12. Refractive index at room temperature (n²⁵): 1.7380

13. Solubility parameter (J·cm^-3)^0.5: 24.055

14.van der Waals area (cm²·mol^-1): 6.430×10⁹

15. van der Waals volume (cm³·mol^-1): 50.930

16. Viscosity (10ºC): 3.35mPa. s

17. Liquid phase standard claimed heat (enthalpy) (kJ·mol^-1): 67.8

18. Liquid phase standard hot melt (J ·mol^-1·K^-1): 135.5

19. The gas phase standard claims heat (enthalpy) (kJ·mol^-1): 118.7

20. Gas phase standard entropy (J·mol^-1·K^-1): 309.50

21. Gas phase standard formation free energy (kJ·mol^-1): 101.7

22. Gas phase standard hot melt (J·mol^-1 sup>·K^-1): 57.73

Toxicological data

1. Acute toxicity

Children’s oral LDLO: 2778 uL/kg

Rat abdominal LD50: 403mg/kg

Mouse abdominal LD50: 467mg /kg

Mouse subcutaneous LD50: 830mg/kg

2. Acute toxicity^[24] LD50: 403mg/kg (rat oral); 830mg/kg (rat transdermal)

3. Irritation No data available

4. Mutagenicity ^[25] Microbial mutagenicity: Escherichia coli 3mg/dish.

Ecological data

1. Ecotoxicity No data available

2. Biodegradability No data available

3. Non-biodegradability No information yet

4. Other harmful effects This substance is harmful to the environment and attention should be paid to atmospheric pollution. ^[26]

Molecular structure data

1. Molar refractive index: 32.62

2. Molar volume (cm³/mol): 82.6

3. Isotonic specific volume (90.2K ): 219.9

4. Surface tension (dyne/cm): 50.0

5. Polarizability (10^-24cm³): 12.93

Compute chemical data

1. Reference value for hydrophobic parameter calculation (XlogP): 2.3

2. Number of hydrogen bond donors: 0

3. Number of hydrogen bond acceptors: 0

4. Number of rotatable chemical bonds: 0

5. Number of tautomers:

6. Topological molecular polar surface area (TPSA): 0

7. Number of heavy atoms: 3

8. Surface charge: 0

9. Complexity: 2.8

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain number of atomic stereocenters: 0

13. Determine the number of chemical bond stereocenters Number: 0

14. Number of uncertain chemical bond stereocenters: 0

15. Number of covalent bond units: 1

Properties and stability

1. Toxic. Less anesthetic than methylene bromide.

2. Cause headache and difficulty breathing after smelling it. See Dibromomethane.

3. Storing it with copper powder can effectively prevent its decomposition; care should be taken to protect it from light; it cannot coexist with many metals (such as Al, Mg, Na, etc.) and strong alkali; there is certain corrosion safety; operate in a fume hood.

4. Stability^[27] Stable

5. Incompatible substances^[28] Strong oxidants, strong bases, alkali metals

6. Conditions to avoid contact^[29] Heat and light

7. Polymerization hazard^[30] No polymerization

8. Decomposition products^[31] Iodide

Storage method

Storage Precautions^[32] Store in a cool, ventilated warehouse. Keep away from fire and heat sources. Keep container tightly sealed. They should be stored separately from oxidants, alkalis, alkali metals, and food chemicals, and avoid mixed storage. Equipped with the appropriate variety and quantity of fire equipment. The storage area should be equipped with emergency release equipment and suitable containment materials.

Synthesis method

1. The iodoform and sodium arsenite method first uses arsenic trioxide and liquid alkali to react to prepare sodium arsenite, then mix the iodoform and sodium arsenite solutions, heat to 60~65°C with stirring, and then Add sodium hydroxide to produce diiodomethane in a one-step reaction. The reaction product is washed with water, distilled, decolorized, crystallized, separated and dried to obtain the finished product.

2. The effect of iodoform method and sodium acetate The reaction formula is as follows:

After the above reaction is completed, The finished product is obtained by distillation.

3. The phase transfer catalytic synthesis method uses triethylbenzyl ammonium chloride as the catalyst and is obtained by the reaction of dichloromethane and sodium iodide. The reaction formula is as follows:

Purpose

1. Organic synthetic raw materials, chemical reagents and pharmaceutical intermediates can be used to manufacture X-ray contrast agents, determine mineral density and refractive index, and separate minerals, etc.

2. Diiodomethane is a methylene transfer reagent that can react with different metals or alkyl metals to form carbenes, undergo cyclopropanation reactions with alkenes, and can also react with carbonyl groups to form methylene groups. chemical reaction. At the same time, nucleophiles such as ICH₂M and I₂CHM can also be prepared, and can also participate in free radical coupling reactions.

Methylene Many carbonyl methylation reagents use diiodomethane as the carbon source, which can be used as an alternative to the Wittig reaction; in the presence of ketones, diiodomethane The reaction of methane and magnesium amalgam can produce olefins (formula 1) in high yields^[1]. This reaction can occur with aldehydes and ketones of different structures.

The presence of Lewis acid can greatly Accelerate the reaction and improve the selectivity and yield of the reaction. Commonly used Lewis acids include trimethylaluminum, titanium tetraisopropoxide, titanium tetrachloride, di(cyclopentadienyl)zirconium dichloride, etc. Among them, CH₂I₂/Zn/ Me₃Al and CH₂Br₂/Zn/TiCl₄The two groups of reagents have the best effect. In the presence of ketones, aldehydes can selectively undergo methylation reactions (Formula 2)^[2].

Cyclopropanation In organic synthesis, diiodomethane is mainly used to carry out cyclopropanation reactions involving metals. The most important is zinc-involved cyclopropanation (Simmons-Smith reaction), a reagent that is widely used and capable of many variations. ZincThe source is crucial to the success or failure of the reaction. Zn/Cu, diethyl zinc, etc. can be used as sources of Zn for cyclopropanation reaction. Diiodomethane and samarium mercury or samarium iodide can be combined to obtain many different samarium-containing olefin cyclopropanation reagents, all of which can react with allyl alcohol and enol. α,β-unsaturated esters and α,β-unsaturated amides can also be combined with samarium catalysis Diiodomethane undergoes cyclopropanation reaction (Formula 3)^[3]. The cyclopropanation reactions of zinc-containing reagents and samarium-containing reagents are directly affected by hydroxyl groups ^[4]. Treating diiodomethane with trialkyl aluminum (such as triisobutylaluminum) will also give the corresponding cyclopropane, which is a good complement to the zinc and samarium system. This reaction tends to react with independent alkenes, while It does not react with allyl alcohol (Formula 4)^[5].

‘ICH_{Nucleophilic addition of 2}‘ Methyl iodide prepared from samarium metal ^[6] can react with aldehydes, ketones and enones, and magnesium reagents can also be used For this reaction (Equation 5)^[7]. The aluminum reagent can also be used to replace the allyl alcohol hydroxyl group with iodomethyl, Et₃Al, Et₂AlCl, Et₂AlOEt All can participate in this reaction (such as equation 6)^[8].

(+)-trans-(2S,3S)-bis(diphenylphosphine)bicyclo[2.2.1]hept-5-ene

Nucleophilic addition of ‘I₂CH’ CH₂I₂ deprotonates under the action of a base After oxidation, I₂CHM derivatives are obtained. These compounds are more stable than the corresponding ICH₂M and can react with many electrophiles^[9]. Commonly used bases include Cy₂NLi, NaHMDS, LiHMDS and LDA. Allyl iodide is synthesized using I₂CHLi. First treat diiodomethane with LiHMDS, then add sulfone, and evaporate the water to obtain allyl iodide, but the selectivity is relatively poor (Formula 7)^[9].

Free radical addition Addition of ICH₂ fragments to α,β-unsaturated ketones in the presence of triethylborane Reaction to obtainγ-iodoketone (formula 8)^[10]. The intermediate boron enolate can be either hydrolyzed or alkylated.

Alkylation reaction The application of diiodomethane in alkylation is limited. ClCH₂I and ClCH₂Br are more prone to alkylation reactions than diiodomethane, but , diiodomethane can be used in cycloalkylation reactions. Diamine can react with diiodomethane. Slowly adding diiodomethane solution to the diamine solution can obtain a higher yield (Formula 9)^[11]. In the reaction with Pt as a catalyst, diiodomethane reacts with thiol to obtain dithiane^[12]. In addition, the in-situ generation of iodomethyllithium in the presence of diiodomethane and alkyl lithium can easily and quickly convert many carbonyl compounds into epoxides (Formula 10)^[13].

3. Used in organic synthesis and Separation of mixed minerals. ^[33]

glycerin

Structural formula

Business number	017W
Molecular formula	C3H8O3
Molecular weight	92.09
label	Glycerol, glycol, trihydroxypropane, 1,2,3-propanetriol, Glycerol, Glycol alcohol, 1,2,3-Propanetriol, Trihydroxypropane, automobile and aircraft fuel, antifreeze, hygroscopic agent, lubricants, Solvents and co-solvents, Aquasorb, carrier solvent, thickener, plasticizer, vehicle, alcohol compounds

Numbering system

CAS number:56-81-5

MDL number:MFCD00004722

EINECS number:200-289-5

RTECS number:MA8050000

BRN number:635685

PubChem number:24895092

Physical property data

1. Properties: Colorless and odorless viscous liquid with sweet taste.

2. Boiling point (ºC, 101.3kPa): 290, 182 (2666pa)

3. Melting point (ºC, pouring point): 20

4. Relative density (g/mL, 15/15ºC): 1.26526

5. Relative density (g/mL, 20/20ºC): 1.2613

6. Relative density (g/mL, 25/25ºC): 1.26170

7. Relative vapor density (g/mL, air=1): 3.1

8. Refractive index (15ºC): 1.47547

9. Refractive index (n20ºC): 1.4746

10. Refractive index (n25ºC): 1.4730

11. Viscosity (mPa·s, 20ºC): 243

12. Viscosity (mPa·s, 25ºC): 56.0

13. Viscosity (mPa·s, 30ºC): 18

14. Viscosity (mPa·s, 50ºC): 18

15. Flash point (ºC, closed): 177

16. Flash point (ºC): 523 (on Pt); 429 (on glass)

17. Heat of evaporation (KJ/mol, 55ºC): 88.17

18. Heat of evaporation (KJ/mol, b.p.): 61.09

19.Heat of formation (KJ/mol, 15ºC, liquid): 669.05

20. Heat of combustion (KJ/mol, 25ºC, liquid): 1656.42

21. Specific heat capacity (KJ/(kg·K), 15ºC): 2.46

22. Conductivity (S/m, 20ºC): 1.0×10-8

23. Thermal conductivity (W/(m·K)): 0.29

24. Vapor pressure (kPa, 125.5ºC): 0.13

25. Body expansion coefficient (K-1): 0.000615

26. Solubility: able to absorb hydrogen sulfide, hydrocyanic acid, and sulfur dioxide. It is miscible with water and ethanol. One part of this product can be dissolved in 11 parts of ethyl acetate and about 500 parts of ether. It is insoluble in benzene, carbon disulfide, chloroform, carbon tetrachloride, petroleum ether, chloroform and oil. It is easily dehydrated and loses water to form diglycerol and polyglycerol. Oxidation produces glyceraldehyde and glyceric acid, etc. Solidifies at 0°C to form flashing rhombic crystals. Polymerization occurs at temperatures around 150°C. Incompatible with anhydrous acetic anhydride, potassium permanganate, strong acids, corrosives, fatty amines, isocyanates, and oxidants.

27. Relative density (20℃, 4℃): 1.2613

28. Relative density (25℃, 4℃): 1.255130

29. Critical temperature (ºC): 576.85

30. Critical pressure (MPa): 7.5

31. Eccentricity factor: 1.320

32. Solubility parameter (J·cm-3)0.5: 34.315

33. van der Waals area (cm2·mol-1): 7.650×1010

34. van der Waals volume (cm3·mol-1): 51.360

Toxicological data

Toxicity Classification Poisoning
Acute toxicity: Oral – rat LD50: 26000 mg/kg; Oral – mouse LC50: 4090 mg/kg.
Irritation data: Skin – Rabbit 500 mg/24 hours Mild; Eyes – Rabbit 126 mg Mild.
It is non-toxic to humans when consumed. When used as a solvent, it can be oxidized into acrolein and become irritating. The LC50 of intravenous injection in mice is 7.56g/kg, and the maximum allowable concentration in the workplace is 10mg/m3.
Rat oral LD50: 20ml/kg; intravenous LD50: 4.4ml/kg. Store in a cool, dry place.

Ecological data

Has certain harm to water bodies. No pollution to the environment.

Molecular structure data

1. Molar refractive index: 20.51

2. Molar volume (cm3/mol): 70.9

3. Isotonic specific volume (90.2K): 199.0

4. Surface tension (dyne/cm): 61.9

5. Polarizability (10-24cm3): 8.13

Compute chemical data

1. Hydrophobic parameter calculation reference value (XlogP): None

2. Number of hydrogen bond donors: 3

3. Number of hydrogen bond acceptors: 3

4. Number of rotatable chemical bonds: 2

5. Number of tautomers: None

6. Topological molecular polar surface area 60.7

7. Number of heavy atoms: 6

8. Surface charge: 0

9. Complexity: 25.2

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Number of uncertain atomic stereocenters: 0

13. Determine the number of stereocenters of chemical bonds: 0

14. Number of uncertain chemical bond stereocenters: 0

15. Number of covalent bond units: 1

Properties and stability

1. Colorless, transparent, odorless, viscous liquid with sweet taste and hygroscopicity. It is miscible with water, alcohols, amines and phenols in any proportion, and the aqueous solution is neutral. Soluble in 11 times of ethyl acetate and about 500 times of diethyl ether. Insoluble in benzene, chloroform, carbon tetrachloride, carbon disulfide, petroleum ether, oils, and long-chain fatty alcohols. It is flammable and can cause combustion and explosion when exposed to strong oxidants such as chromium dioxide and potassium chlorate. It is also a good solvent for many inorganic salts and gases. It is non-corrosive to metals and can be oxidized to acrolein when used as a solvent.

Chemical properties: esterification reaction with acid, such as esterification with phthalic acid to form alkyd resin. Transesterification occurs with esters. Reacts with hydrogen chloride to form chlorohydrins. There are two ways to dehydrate glycerol: intermolecular dehydration to obtain diglycerol and polyglycerol; intramolecular dehydration to obtain acrolein. Glycerol reacts with alkali to form alcoholate. Reacts with aldehydes and ketones to form acetals and ketals. Oxidation with dilute nitric acid produces glyceraldehyde and dihydroxyacetone; oxidation with periodic acid produces formic acid and formaldehyde. Contact with strong oxidants such as chromic anhydride, potassium chlorate or potassium permanganate can cause combustion or explosion. Glycerol can also play a role in nitration and acetylation.

2. Non-toxic. It is harmless even if the total amount of the dilute solution reaches 100g, and it is hydrolyzed and oxidized in the body to become a nutrient source. In animal experiments, it has the same anesthetic effect as alcohol when consumed in extremely large amounts.

3. Exists in flue-cured tobacco leaves, burley tobacco leaves, oriental tobacco leaves and smoke.

4. Naturally found in tobacco, beer, wine, and cocoa.

StorageHow to save

1. Store in a clean and dry place and pay attention to sealed storage. Pay attention to moisture, water and heat protection, and it is strictly forbidden to mix with strong oxidants. Can be stored in tin-plated or stainless steel containers.

2. Packed in aluminum drums or galvanized iron drums or stored in phenolic resin-lined storage tanks. During storage and transportation, it must be protected from moisture, heat and water. It is prohibited to put glycerol together with strong oxidants (such as nitric acid, potassium permanganate, etc.). Store and transport according to general regulations on flammable chemicals.

Synthesis method

The industrial production methods of glycerol can be divided into two categories: the method using natural oils as raw materials, and the resulting glycerin is commonly known as natural glycerin; the synthesis method using propylene as raw materials, the obtained glycerin Commonly known as synthetic glycerol.

1. Production of natural glycerin. Before 1984, glycerin was all recovered from the by-products of animal and vegetable fat soap making. Until now, natural oils and fats are still the main raw materials for the production of glycerol. About 42% of the natural glycerin in the base comes from soap by-products, and 58% comes from fatty acid production. Saponification reaction of fats and oils in soap making industry. The saponification reaction product is divided into two layers: the upper layer mainly contains sodium salts of fatty acids (soap) and a small amount of glycerol, and the lower layer is waste alkali liquid, which is a dilute glycerol solution containing salts and sodium hydroxide, generally containing 9-16% of glycerol and inorganic salts. 8-20%. Grease reaction. Glycerin water (also called sweet water) obtained by hydrolysis of oil and fat has a higher glycerin content than soapmaking waste liquid, about 14-20%, and inorganic salts of 0-0.2%. In recent years, continuous high-pressure hydrolysis has been widely used. The reaction does not use a catalyst. The resulting sweet water generally does not contain inorganic acid, and the purification method is simpler than that of spent alkali. Whether it is soap-making waste liquid or glycerol water obtained by hydrolysis of oil, the amount of glycerol is not high, and they all contain various impurities. The production process of natural glycerin includes purification and concentration to obtain crude glycerol, as well as distillation, decolorization, and Deodorization refining process. This process is described in detail in some books and periodicals.

2. Production of synthetic glycerol The various pathways for synthesizing glycerin from propylene can be summarized into two major categories, namely chlorination and oxidation. Propylene chlorination method and propylene irregular acetic acid oxidation method are still used in industry.

(1) Propylene chlorination method This is the most important production method in synthetic glycerol. It includes four steps, namely high-temperature chlorination of propylene, hypochlorous acidification of chloropropene, Saponification of dichloropropanol and hydrolysis of epichlorohydrin. The hydrolysis of epichlorohydrin to glycerin is carried out at 150°C and 1.37MPa carbon dioxide pressure in an aqueous solution of 10% hydrogen oxide and 1% sodium carbonate to generate a glycerin aqueous solution containing sodium chloride with a glycerol content of 5-20%. After concentration, desalination and distillation, glycerin with a purity of more than 98% is obtained.

(2) Propylene peracetic acid oxidation method Propylene and peracetic acid react to synthesize propylene oxide, and propylene oxide isomerizes into alkene and propanol. The latter reacts with peracetic acid to generate glycidol (glycidol), which is finally hydrolyzed to glycerol. The production of peracetic acid does not require a catalyst. Acetaldehyde is oxidized with oxygen in the gas phase. Under normal pressure, 150-160°C, and a contact time of 24 seconds, the acetaldehyde conversion rate is 11% and the peracetic acid selectivity is 83%. The above-mentioned last two steps of reaction are carried out continuously in the reactive distillation tower with special structure. After the raw materials allyl alcohol and ethyl acetate solution containing peracetic acid are sent into the tower, the tower still is controlled at 60-70°C and 13-20kPa. The ethyl acetate solvent and water are evaporated from the top of the tower, and a glycerol aqueous solution is obtained from the tower still. This method has high selectivity and yield, uses peracetic acid as the oxidant, does not require a catalyst, has a fast reaction speed, and simplifies the process. The production of 1 ton of glycerin consumes 1.001t of allyl alcohol, 1.184t of peracetic acid, and 0.947t of acetic acid as a by-product. At present, the output of natural glycerin and synthetic glycerin accounts for almost 50% each, while the propylene chlorination method accounts for about 80% of Hezhi’s glycerol output. my country’s natural glycerin accounts for more than 90% of the total output.

3. Dilute the industrial grade glycerin with 1/2 the amount of distilled water. After stirring thoroughly, add activated carbon and heat to 60~70℃ for decolorization, and then vacuum Filter to ensure the filtrate is clear and transparent. Control the dripping speed, and add the filtrate into the column of the pre-processed mixture of 732 strong acid cation resin and 717 strong alkali anion and cation resin to adsorb and remove electrolytes and non-electrolyte impurities such as aldehydes, pigments, and esters in glycerol.
The glycerin solution after removing impurities is distilled under reduced pressure, and the vacuum degree is controlled to be above 93326Pa. The kettle temperature is between 106 and 108°C. After steaming out most of the water, the kettle temperature is raised to 120°C for rapid dehydration. When no water comes out, the heating is stopped. The materials in the kettle are the finished products.

Purpose

1. Glycerol is an important organic chemical raw material and is widely used in many sectors of the national economy. It is an excellent hygroscopic agent, antifreeze, lubricant, solvent and co-solvent. It is an important raw material for the production of polyester, explosives, medicine, etc. In the food industry, it can be used as a water-retaining agent (for bread and cakes), a carrier solvent (for spices, pigments, and non-water-soluble preservatives), a thickener (for beverages, wine preparation, etc.), and a plasticizer. Agent(�(used in candies, desserts, meat products, etc.); can be used as a color carrier in colored foods. Glycerin is also used as a lubricant in food processing and packaging machinery. Commonly used as softeners, viscosity improvers and solvents in pharmaceutical and cosmetic manufacturing. Among polymer materials, glycerol is often used as a raw material for the production of polyurethane foam, polyether, etc. It is an important raw material for the production of alkyd resin and celluloid, and is especially used in large quantities in the manufacture of alkyd resin paint. It is also widely used in tobacco industry, ceramic industry, leather industry, wood industry and photography. and used as automobile and aircraft fuel and as antifreeze in oil fields.

2. Used as analytical reagent and gas chromatography stationary solution. Measure boron complexing agent. Used as solvents, lubricants, in the formulation of cosmetics and in the pharmaceutical industry.

3. Used as a toughening agent for polyvinyl alcohol and starch adhesives, and also used in the manufacture of unsaturated polyester resin, alkyd resin, polyester, glycerin epoxy resin, etc. As an important organic chemical raw material, it is widely used in military, food, pharmaceutical, daily chemical and other industries, with more than 1,700 uses. Defense industry: Nitroglycerin produced by the reaction of glycerin and nitric acid is an extremely sensitive explosive. Glycerin is also used as an antifreeze in aircraft fuel. Food industry: used as solvent, hygroscopic agent and color vehicle. In flavored and colored foods, glycerin helps shape the food due to its viscosity. In the rapid freezing of food, glycerin can be used as a heat transfer medium in direct contact with the food. Glycerin is also a lubricant for food processing and packaging machinery. In addition, the application of polyglycerol and polyglyceryl esters in the manufacture of crispy foods and margarine is increasing year by year. Pharmaceutical industry: used as softener, viscosity improver and solvent. Glycerol can be used as a sedative, nitroglycerin is a vasodilator in coronary spasm, etc. Daily chemical industry: additives for cosmetics, toothpaste, food flavors, anti-drying agent for tobacco. Plastic industry: used as starting agent in polyurethane foam production. Textile printing and dyeing industry: used as lubricant, moisture absorbent, anti-shrink and anti-wrinkle treatment agent, diffusing agent, penetrating agent, etc. In addition, glycerol is widely used in ceramics, photography, leather and wood industries.

4. This product is used in stainless steel polishing solution, trivalent chromium plating solution and chemical copper plating, etc.
In cyanide zinc plating, it can make the coating smooth and delicate, improve cathodic polarization, and also make the coating bright. Glycerol and triethanolamine can be used for bright nickel plating at room temperature in a certain proportion.

methylene chloride

Structural formula

Business number	01HZ
Molecular formula	CH2Cl2
Molecular weight	85
label	dichloromethylene, methylene chloride, Methylene dichloride, Methylene dichloride, DCM

Numbering system

CAS number:75-09-2

MDL number:MFCD00000881

EINECS number:200-838-9

RTECS number:PA8050000

BRN number:1730800

PubChem number:24856423

Physical property data

1. Properties: colorless and transparent liquid with aromatic odor. ^[1]

2. Melting point (℃): -95^[2]

3. Boiling point (℃): 39.8^[3]

4. Relative density (water = 1): 1.33^[4]

5. Relative vapor Density (air=1): 2.93^[5]

6. Saturated vapor pressure (kPa): 46.5 (20℃)^[6]

7. Heat of combustion (kJ/mol): -604.9^[7]

8. Critical temperature (℃): 237^[8]

9. Critical pressure (MPa): 6.08^[9]

10. Octanol/water partition coefficient: 1.25^[10]

11. Flash point (℃): -4^[11]

12. Ignition temperature (℃): 556^[12]

13. Explosion upper limit (%): 22^[13]

14. Explosion lower limit (% ): 14^[14]

15. Solubility: Slightly soluble in water, soluble in ethanol and ether. ^[15]

16. Viscosity (mPa·s, 20ºC): 0.425

17. Relative density (25℃, 4℃): 1.3162

18. Ignition point (ºC): 662

19. Heat of evaporation (KJ/mol, b.p.): 329.5

20. Heat of fusion (KJ/mol) : 4.187

21. Heat of formation (KJ/mol, 25ºC, liquid): 121.54

22. Heat of combustion (KJ/kg, 25ºC, liquid): 558.27

23. Specific heat capacity (KJ/(kg·K), 20ºC): 0.992

24. Electrical conductivity (S/m, 25ºC): 4.3×10^-11

25. Vapor pressure (kPa, 0ºC): 19.7

26. Vapor pressure (kPa, 10ºC): 30.6

27. Vapor pressure (kPa, 20ºC): 46.5

28. Vapor pressure (kPa, 30ºC): 68.2

29. Vapor pressure (kPa, 35ºC): 80.00

30. Body Expansion coefficient (K^-1, 10~40ºC, liquid): 0.00137

31. Refractive index at room temperature (n²⁵): 1.4213

32. Eccentricity factor: 0.192

33. Lennard-Jones parameter (A): 9.951

34. Lennard-Jones parameter (K): 150.5

35. Solubility parameter (J·cm^-3)^0.5: 20.378

36.van der Waals area (cm²·mol^-1): 4.990×10⁹

37. van der Waals volume (cm³ sup>·mol^-1): 34.710

38. The gas phase standard claims heat (enthalpy) (kJ·mol^-1): -95.4

39. Gas phase standard entropy (J·mol^-1·K^-1): 270.44

40. Gas phase standard generation Free energy (kJ·mol^-1): -68.8

41. Gas phase standard hot melt (J·mol^-1·K^-1): 50.88

42. Liquid phase standard claims heat (enthalpy) (kJ·mol^-1): -124.26

43. Liquid phase standard entropy (J·mol^-1·K^-1): 178.7

44. Liquid phase standard free energy of formation (kJ·mol^-1): -70.42

45. Liquid phase standard hot melt (J·mol^-1·K^-1): 100.0

Toxicological data

1. Acute toxicity^[16]

LD50: 1600~2000mg/kg (rat oral )

LC50: 88000mg/m³ (rat inhalation, 1/2h)

2. Irritation^[17]

Rabbit transdermal: 810mg (24h), severe stimulation.

Rabbit eye: 162mg, moderate irritation.

3. Subacute and chronic toxicity^[18]

Rat inhalation 4.69g /m³, 8 hours a day, 75 days in total, no pathological changes. As exposure time increased, there was mild liver atrophy, steatosis, and cellular infiltration.

4. Mutagenicity^[19] Microbial mutagenicity: Salmonella typhimurium 5700ppm. DNA inhibition: human fibroblasts 5000ppm (1h) (continuous). DNA damage: Hamster ovary 3000ppm. Sister chromatid exchange: hamster lung 5000ppm (1h) (continuous)

5. Teratogenicity^[20] Rats were given the lowest toxic dose (TCLo) of 1250ppm (7h) by inhalation 6 to 15 days after pregnancy, causing developmental malformations in the musculoskeletal system and genitourinary system.

6. Carcinogenicity^[21] IARC Carcinogenicity Comment: G2B, suspected human carcinogen.

7. Others^[22] The lowest inhalation toxic concentration for rats (TCLo): 1250ppm (7h) (pregnant 6~15 days), causing abnormal musculoskeletal development and abnormal development of the genitourinary system.

Ecological data

1. Ecotoxicity^[23]

LC50: 193mg/L (96h) (fathead minnow , dynamic); 310mg/L (96h) (fathead minnow, static); 200~250mg/L (96h) (bluegill, static); 224mg/L (48h) (water fleas); 256mg/L ( 96h) (sugar shrimp)

2. Biodegradability^[24]

Good Aerobic biodegradation (h): 168~672

Anaerobic biodegradation (h): 672~2688

3. Non-biodegradability^[25]

Photolysis maximum light absorption wavelength range (nm): 220~250

Photooxidation half-life in air – high (h): 458~4584

First-grade hydrolysis half-life (h): 704a

4. Other harmful effects^[26] This substance is harmful to the environment and has an accumulation effect in groundwater. Special attention should be paid to aquatic life. Attention should also be paid to atmospheric pollution.

Molecular structure data

1. Molar refractive index: 16.38

2. Molar volume (cm³/mol): 67.8

3. Isotonic specific volume (90.2K ): 148.8

4. Surface tension (dyne/cm): 23.1

5. Polarizability: 6.49

Compute chemical data

1. Reference value for hydrophobic parameter calculation (XlogP): 1.5

2. Number of hydrogen bond donors: 0

3. Number of hydrogen bond acceptors: 0

4. Number of rotatable chemical bonds: 0

5. Topological molecular polar surface area (TPSA): 0

6. Number of heavy atoms: 3

7. Surface charge: 0

8. Complexity: 2.8

9. Number of isotope atoms: 0

10. Determine the number of atomic stereocenters : 0

11. The number of uncertain atomic stereocenters: 0

12. The number of determined chemical bond stereocenters: 0

13. Uncertain chemical bond stereocenters Number of structural centers: 0

14. Number of covalent bond units: 1

Properties and stability

1. It has very little toxicity and recovers quickly after poisoning, so it can be used as an anesthetic. Irritating to skin and mucous membranes. Oral LD50 in young adult rats: 1.6mL/kg. The maximum allowable concentration in the air is 500×10^-6. Gas masks should be worn during operation. When poisoning is discovered, leave the scene immediately and receive symptomatic treatment. The smallest among the chlorides of methane. The vapor is highly anesthetic, and inhaling large amounts can cause acute poisoning, with symptoms such as nasal pain, headache, and vomiting. Chronic poisoning can cause dizziness, fatigue, loss of appetite, impaired hematopoietic function, and reduced red blood cells. Liquid methylene chloride can cause dermatitis when it comes into contact with the skin. Rats died after inhaling vapor with a concentration of 90.5g/m3 for 90 minutes. The olfactory threshold concentration is 522mg/m3, and the maximum allowable concentration in the workplace is 1740mg/m3.

2. Stability^[27] Stable

3. Incompatible substances^[28] Alkali metals, aluminum

4. Conditions to avoid contact ^[29] Light, humid air

5. Polymerization hazard^[30] No polymerization

6. Decomposition products^[31] Hydrogen chloride, phosgene

Storage method

Storage Precautions^[32]Stored in a cool, ventilated warehouse. Keep away from fire and heat sources. The storage temperature does not exceed 32°C and the relative humidity does not exceed 80%. Keep container tightly sealed. Should be stored separately from alkali metals and food chemicals, and avoidMixed storage. Equipped with the appropriate variety and quantity of fire equipment. The storage area should be equipped with emergency release equipment and suitable containment materials.

Synthesis method

1. Methane chlorination method: After mixing methane, chlorine and circulating gas, they are sent to the reactor for thermal chlorination reaction at 380~400°C. After the gas reaction product is cooled to 70-80°C by the cooler, it is sent to the hydrogen chloride absorption tower, where the hydrogen chloride in the gas product is absorbed and removed with water, and then sent to the alkali washing tower, where it is neutralized with alkali liquid to remove residual hydrochloric acid and free chlorine. The purified gas product is compressed, cooled, and condensed into crude chloride. The crude chloride is sent to the distillation process, and methyl chloride, methylene chloride and chloroform are steamed out through each distillation tower. Except for a part of the non-condensable gas that is vented, the rest is mixed with new materials for recycling. The controlled operating conditions are reaction temperature 400-420°C, ingredient ratio CH4:Cl2=4:1, and products based on methylene chloride can be obtained.

2. Methanol ammoniation method: After the methanol is gasified in the gasifier, it is mixed with the hydrogen chloride separated in the subsequent reaction, and then passed through the catalyst alumina or suboxone chloride or zinc chloride with activated carbon or pumice as the carrier. Phosphoric acid supported on the activated carbon can also be used as the catalyst. , react in a hydrochlorinator at 350°C to generate methyl chloride. The gaseous reaction product is washed with cold water and sodium hydroxide solution in a water washing tower or an alkali washing tower respectively. After removing unreacted methanol and hydrogen chloride, it is sent to the dehydrogenation tower and washed again with sulfuric acid to remove the dimethyl ether and dimethyl ether generated during the reaction. water to obtain methyl chloride. Methyl chloride reacts with chlorine at 410 to 420°C to produce dichloromethane and chloroform, as well as a small amount of carbon tetrachloride. After quenching, it is divided into a liquid phase containing dichloroethane and a gas phase containing uncondensed hydrogen chloride, unreacted methyl chloride, and chlorine. The gas phase is separated to separate hydrogen chloride, methyl chloride and chlorine for recycling. The liquid phase is first sent to the absorption tower and washed with dilute alkali and water to remove carbon tetrachloride, and then sent to the rectification tower to obtain dichloromethane and chloroform respectively through azeotropic distillation and rectification.

3. Methyl chloride chloride Methane chlorination has two processes: photochlorination and thermal chlorination.
Photochlorination is the reaction of methyl chloride and chlorine under 4000kW light. The reaction product is washed with alkali, compressed, condensed, dried and distilled to obtain the finished product.
Thermal chlorination is to mix methyl chloride and chlorine gas according to (2~2.5):1 (mass), and react at a reaction temperature of 400°C and a reaction pressure of 0.2MPa. The reaction product is washed with water, alkali washed, compressed, condensed, dried and distilled to obtain the finished product.

4. Use industrial methylene chloride as raw material , wash several times with concentrated sulfuric acid 1/8 to 1/10 of the raw material volume until the acid layer is colorless, then wash once with 5% sodium hydroxide solution, the dosage is 1/5 of the raw material volume, and wash twice with water. Then it is dried with anhydrous calcium chloride, the clear liquid is sucked out and then distilled, and the middle fraction is collected to obtain pure methylene chloride.

Purpose

1. In addition to being used in organic synthesis, this product is also widely used as a solvent in cellulose acetate film forming, cellulose triacetate spinning, petroleum dewaxing, aerosols and the production of antibiotics, vitamins and steroids. As well as cleaning, degreasing and release agents for metal surface paint layers.

2. Used for grain fumigation and refrigeration of low-pressure freezers and air-conditioning devices. It is used as an auxiliary blowing agent in the production of polyether urethane foam and as a blowing agent for extruded polysulfone foam.

3. Used as solvent, extraction agent and mutagen. For plant genetic research.

4. It has good dissolving power. It is a low-toxic, non-flammable and low-boiling point solvent among commonly used industrial solvents. It has good dissolving power for many resins, paraffin and fats. Mainly used as paint stripper, petroleum dewaxing solvent, extractant for thermally unstable substances, extractant for lanolin from wool and edible oil from coconut, and solvent for cellulose triacetate film film. It is also widely used in the manufacturing and processing of acetate fiber and vinyl chloride fiber, as well as the manufacturing of fire extinguishing agents, refrigerants, methenamine, etc.

5. Used in the electronics industry. Commonly used as a cleaning and degreasing agent.

6. Because it has an extremely low boiling point and is a flame-retardant solvent, it is widely used. In addition to being used as a cleaning solvent for aircraft engines, precision machinery, etc., it can also be used as a stripper for coatings. It can also be properly mixed with other solvents and used in various industrial cleanings.

7. It is also used as an ethyl fiber solvent, dental local anesthetic, refrigerant and fire extinguishing agent. It is a commonly used eluent for chromatographic separation and a common solvent for extraction separation.

8. Used as a solvent in the resin and plastic industry. ^[33]