A method for removing impurities in acetonitrile prepared by ammoniation of acetic acid

A technology for ammoniation of acetic acid and acetonitrile, applied in the purification/separation of carboxylic acid nitrile, organic chemistry, etc., can solve the problems of high energy consumption, time and labor costs, long material cycle, long process flow, etc., and achieve low cost and high energy efficiency. Reduced consumption and simple process

Active Publication Date: 2021-11-02
WEIFANG ZHONGHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] (2) To solve the targeted impurity removal steps set up in the prior art to remove the above-mentioned impurities, it often requires a lot of energy consumption, time, and labor costs, and the required process flow is long and the material cycle is long, and There is a problem of material loss

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  • A method for removing impurities in acetonitrile prepared by ammoniation of acetic acid
  • A method for removing impurities in acetonitrile prepared by ammoniation of acetic acid
  • A method for removing impurities in acetonitrile prepared by ammoniation of acetic acid

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Embodiment 1

[0047] A method for removing impurities in acetonitrile prepared by ammoniation of acetic acid, comprising: reduction treatment, rectification, sewage decomposition treatment, molecular sieve multi-stage adsorption, and molecular sieve regeneration.

[0048] For the reduction treatment, the acetonitrile synthesis liquid prepared by the acetic acid ammonification method enters the reduction reaction kettle 1, then puts 0.1%wt sodium bisulfite into it, and starts the circulating water of the condenser connected to the reaction kettle (the temperature of the circulating water is 30°C), Turn on the reaction kettle to stir, feed steam into the coil of the reaction kettle to raise the temperature of the reduction reaction kettle 1 to 50°C, keep the temperature for 2 hours, and complete the reduction treatment until the acetone content in the acetonitrile synthesis liquid is less than or equal to 0.001%; ​​open the reduction reaction kettle 1 and put Material valve, after the material...

Embodiment 2

[0078] A method for removing impurities in acetonitrile prepared by ammoniation of acetic acid, comprising: reduction treatment, rectification, sewage decomposition treatment, molecular sieve multi-stage adsorption, and molecular sieve regeneration.

[0079] For the reduction treatment, the acetonitrile synthesis liquid prepared by the acetic acid ammonification method enters the reduction reaction kettle 1, and then puts 0.3%wt sodium bisulfite into it, and turns on the circulating water of the condenser connected to the reaction kettle (the temperature of the circulating water is 35°C), Turn on the reaction kettle to stir, feed steam into the reaction kettle coil to raise the temperature of the reduction reaction kettle 1 to 70°C, and keep it warm for 2 hours until the acetone content in the acetonitrile synthesis liquid is less than or equal to 0.001%, and the reduction treatment is completed; open the reduction reaction kettle 1 and put Material valve, after the material en...

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Abstract

The invention provides a method for removing impurities in acetonitrile prepared by ammoniation of acetic acid, said method comprising: reduction treatment, rectification, molecular sieve multi-stage adsorption; said reduction treatment, 0.1%-0.5%wt of sodium bisulfite Contact with acetonitrile synthesis solution until the acetone content in the acetonitrile synthesis solution is ≤0.001%. Beneficial effects of the present invention: Compared with the prior art, the cost is low, the process is simple, the steam consumption is about 1-2 tons of steam / ton of water, and the energy consumption is reduced by about 30 compared with atmospheric distillation and pervaporation membrane treatment. ‑50%, high impurity removal efficiency, the water content in the prepared acetonitrile is ≤10ppm, the acetone content is ≤2ppm, the propionitrile content is ≤2ppm, the acetonitrile content is ≥99.99%, and the light transmittance reaches the level of preparation grade acetonitrile, 193nm, 200nm, 240nm Respectively greater than 63%, 94%, 99%.

Description

technical field [0001] The invention relates to the field of acetonitrile synthesis, in particular to a method for removing impurities in acetonitrile prepared by ammoniation of acetic acid. Background technique [0002] Acetonitrile, English name: Acetonitrile; molecular formula: C 2 h 3 N; molecular weight: 41.05; appearance: colorless liquid with pungent odor; melting point: -45°C; boiling point: 81-82°C; water solubility: miscible with water, soluble in most organic solvents such as ethanol and ether. [0003] The role and use of acetonitrile: in the petroleum industry, it is used as a solvent for removing tar, phenol and other substances from petroleum hydrocarbons; in the oil industry, it is used as a solvent for extracting fatty acids from animal and vegetable oils; in medicine, it is used for steroid drugs The recrystallization reaction medium; when a polar solvent with a high dielectric constant is required, a binary azeotropic mixture of acetonitrile and water is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/34C07C255/03
CPCC07C253/34C07C255/03
Inventor 朱宝仁袁宏李艳萍王占明王丽娜刘卿李国明
Owner WEIFANG ZHONGHUI CHEM
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