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Novel method for producing nitromethane

A technology of nitromethane and alkyl, which is applied in the field of compound synthesis to achieve the effects of improving product purity, reducing harmful gases, and mild distillation conditions

Active Publication Date: 2012-09-12
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] Embodiment 1 uses N, N-dimethylaniline as reaction auxiliary reagent

[0026] In the there-necked flask equipped with electric stirrer, reflux condenser and thermometer, add 63 grams (0.5mol) dimethyl sulfate, 69 grams (1mol) sodium nitrite, 1 gram N, N-dimethylaniline respectively, 4 grams of sodium carbonate and 30 milliliters of water, start stirring and heating, the temperature is controlled at 30~32 ℃, and the reaction ends after 3 hours. Solids such as sulfate were filtered off, and 24.7 g of nitromethane was obtained by rectification. Yield 81%. Purity assay: 99.12%.

Embodiment 2

[0027] Embodiment 2 uses N, N-dimethyl n-propylamine as reaction auxiliary reagent

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

Embodiment 3

[0029] Embodiment 3 uses N, N-diethylaniline as 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 control the temperature at 35- 40°C, the reaction ended after 3 hours. After filtering out solids such as sulfate, the filtrate was input into a rectification tower for rectification to obtain 250 kg of nitromethane with a yield of 83%. Purity assay: 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 in particular 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, oily liquid with aroma and certain volatility. ), a refractive index of 1.3817, and a flash point of 35°C; it is partially miscible with water, and its aqueous solution is acidic, soluble in ethanol, ether, dimethylformamide and caustic alkali solution; flammable, and can be ignited by strong impact or detonation Explosion. Its vapor and air can form an explosive mixture. The lower explosion limit is 7.3% (V). It is highly toxic and irritating to the conjunctiva, respiratory tract and skin. The maximum allowable concentration in the air is 100ppm. [0003] Nitromethane is miscible with most organic compounds and is an excellent solvent for aromatic hydrocarbons, alc...

Claims

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Application Information

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Patent Type & Authority Applications(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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