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Novel method for producing nitromethane

A technology of nitromethane and sodium nitrite, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., to achieve the effect of improving product purity, mild rectification conditions, and reducing harmful gases

Active Publication Date: 2014-07-16
HUBEI YUANDA FUCHI PHARMA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In order to solve the above problems, we consider adding appropriate additives during the reaction to solve the above problems. Since soda ash is used in the reaction, we first consider organic amines

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Using N,N-dimethylaniline as a reaction auxiliary reagent

[0026] In a three-necked flask equipped with an electric stirrer, reflux condenser and thermometer, add 63 grams (0.5 mol) of dimethyl sulfate, 69 grams (1 mol) of sodium nitrite, and 1 gram of N,N-dimethylaniline. 4g of sodium carbonate and 30ml of water, start stirring and heating, control the temperature at 30-32°C, and finish the reaction after 3 hours. The sulfate and other solids were filtered out, and 24.7 g of nitromethane was obtained by distillation. The yield was 81%. Purity determination: 99.12%.

Embodiment 2

[0027] Example 2 Using N, N-dimethyl n-propylamine as a reaction auxiliary reagent

[0028] In a three-necked flask equipped with an electric stirrer, reflux condenser and thermometer, add 63 grams (0.5mol) of dimethyl sulfate, 69 grams (1mol) of sodium nitrite, and 1g of N,N-dimethyl-n-propylamine. , 4 grams of sodium carbonate and 30 milliliters of water. Start stirring and heating, and the temperature is controlled at 50-55°C. The reaction ends after 5 hours. The solids such as sulfate are filtered out, and 26 grams of nitromethane are obtained by distillation. The yield was 86%. Purity determination: 99.10%.

Embodiment 3

[0029] Example 3 Using N,N-diethylaniline as a reaction auxiliary reagent

[0030] In a 5000L reactor, add 630 kg of dimethyl sulfate, 690 kg of sodium nitrite, 10 kg of N,N-diethylaniline, 40 kg of sodium carbonate and 300 liters of water. Start stirring and heating, and the temperature is controlled at 35- At 40°C, the reaction was finished after 3 hours. After filtering out the sulfate and other solids, the filtrate is fed into a rectifying tower and rectified to obtain 250 kg of nitromethane with a yield of 83%. Purity determination: 99.33%.

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Abstract

The invention relates to a novel method for producing an important organic synthetic intermediate nitromethane. If a substitution reaction between dimethyl sulphate and sodium nitrite is performed to produce nitromethane, there exists factors which damage the environment and safety, such as a lot of harmful gases generated during the reaction and simple distillation processes and spark which is easy to generate during the rectification process. According to the novel method, soda ash is used to adjust pH of the reaction solution, a few organic amine is also added, and simultaneously the reaction temperature is controlled within 30-35 DEG C. Therefore, harmful gases during the reaction process are greatly minimized, spark generated during the rectification process is avoided, and the product having purity of 99.9% can be finally obtained.

Description

Technical field [0001] The invention belongs to the technical field of compound synthesis, and specifically relates to a new method for producing nitromethane. technical background [0002] Nitromethane is an important organic chemical product and organic synthesis intermediate. It is a colorless, transparent, aromatic and volatile oily liquid. It has a melting point of -28.5°C, a boiling point of 100.8°C, and a relative density of 1.1371 (20 / 4°C). ), refractive index 1.3817, flash point 35℃; partly miscible with water, its aqueous solution is acidic, soluble in ethanol, ether, dimethylformamide and caustic alkali solution; flammable, can be caused by strong impact or detonation Explosion. Its vapor and air can form an explosive mixture, the lower limit of explosion is 7.3% (V), the toxicity is very high, and it is irritating to the conjunctiva, respiratory tract and skin. The maximum allowable concentration in the air is 100 ppm. [0003] Nitromethane is miscible with most organ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/02C07C201/10
Inventor 杨尚金熊先胜石松华余登峰
Owner HUBEI YUANDA FUCHI PHARMA CHEM
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