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Preparation method of high-purity acetonitrile

A technology of pure acetonitrile and acetonitrile, which is applied in the field of preparation of high-purity acetonitrile, can solve the problems of complex processing technology, low product purity, environmental pollution, etc., and achieve the effects of easy dissociation, simple operation, and energy saving

Inactive Publication Date: 2019-08-02
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the above-mentioned method of purifying and reclaiming a refined method of high-purity acetonitrile can generate and / or purify a refined method of high-purity acetonitrile, this method has low product purity, complicated treatment process, high energy consumption, and the existence of Certain environmental pollution problems and many other shortcomings

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The preparation method of the present embodiment high-purity acetonitrile comprises the steps:

[0027] (1) Adsorption: Adsorb and dehydrate the raw material—industrial grade acetonitrile through a chromatographic column equipped with a composite dehydration adsorbent to obtain crude acetonitrile; the composite dehydration adsorbent includes high-purity carbon fiber, magnetic iron oxide and sulfate ore. Ratio, high-purity carbon fiber: magnetic iron oxide: sulfate ore = 1:0.5:1.5; the amount of composite dehydration adsorbent is 0.5% of the weight of industrial-grade acetonitrile; the purity of industrial-grade acetonitrile is greater than 99%, and the water content is less than 300ppm; The high-purity carbon fiber in the dehydration adsorbent is made of pitch, viscose fiber or acrylonitrile as raw material and processed at 1200-3000°C, with a carbon content of >9.5%;

[0028] (2) Oxidation: Add an oxidant——potassium permanganate to the crude acetonitrile for oxidation ...

Embodiment 2

[0031] The preparation method of the present embodiment high-purity acetonitrile comprises the steps:

[0032] (1) Adsorption: Adsorb and dehydrate the raw material—industrial grade acetonitrile through a chromatographic column equipped with a composite dehydration adsorbent to obtain crude acetonitrile; the composite dehydration adsorbent includes high-purity carbon fiber, magnetic iron oxide and sulfate ore. Ratio, high-purity carbon fiber: magnetic iron oxide: sulfate ore = 1:1:2; the amount of composite dehydration adsorbent is 1.5% of the weight of industrial-grade acetonitrile; the purity of industrial-grade acetonitrile is greater than 99%, and the water content is less than 300ppm; The high-purity carbon fiber in the dehydration adsorbent is made of pitch, viscose fiber or acrylonitrile as raw material and processed at 1200-3000°C, with a carbon content of >9.5%;

[0033] (2) Oxidation: Add an oxidizing agent—potassium permanganate to the crude acetonitrile for oxidati...

Embodiment 3

[0036] The preparation method of the present embodiment high-purity acetonitrile comprises the steps:

[0037] (1) Adsorption: Adsorb and dehydrate the raw material—industrial grade acetonitrile through a chromatographic column equipped with a composite dehydration adsorbent to obtain crude acetonitrile; the composite dehydration adsorbent includes high-purity carbon fiber, magnetic iron oxide and sulfate ore. Ratio, high-purity carbon fiber: magnetic iron oxide: sulfate ore = 1:2:3; the amount of composite dehydration adsorbent is 3.5% of the weight of industrial-grade acetonitrile; the purity of industrial-grade acetonitrile is greater than 99%, and the water content is less than 300ppm; The high-purity carbon fiber in the dehydration adsorbent is made of pitch, viscose fiber or acrylonitrile as raw material and processed at 1200-3000°C, with a carbon content of >9.5%;

[0038] (2) Oxidation: Add an oxidant——potassium permanganate to the crude acetonitrile for oxidation reac...

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Abstract

The invention relates to a preparation method of high-purity acetonitrile. The method comprises steps as follows: (1) adsorption: a raw material industrial acetonitrile is subjected to adsorption dewatering through a chromatographic column containing a compound dewatering adsorbent, and crude acetonitrile is obtained, wherein the compound dewatering adsorbent comprises high-purity carbon fiber, magnetic iron oxide and sulfate ore in the mass ratio being 1:(0.5-2):(1.5-3); (2) oxidation: an oxidant or a mixture of the oxidant and a catalyst is added to crude acetonitrile for an oxidization reaction, and a rectification stock solution is obtained; (3) rectification: the rectification stock solution is sent into a rectification device for rectification, and high-purity acetonitrile is obtained. According to the preparation method, the high-purity acetonitrile is prepared in three steps including adsorption, oxidation and rectification, the impurity content of the product is reduced to 10-12, the requirement of the high-purity solvent for scientific research can be met, and the method is simple to operate, lower in cost and small in pollution and has broad market application prospects.

Description

technical field [0001] The invention relates to a method for preparing acetonitrile, in particular to a method for preparing high-purity acetonitrile. Background technique [0002] Acetonitrile (ACN) is an important industrial solvent widely used in chemical reactions, synthesis and purification of pharmaceutical intermediates, and as a mobile phase solvent for high performance liquid chromatography. With the expansion of market applications, acetonitrile is gradually used as a DNA synthesis and purification solvent, a solvent for the synthesis of organic EL materials, and a cleaning solvent for electronic components. [0003] Commercially available acetonitrile is mainly obtained by recovering and purifying the crude acetonitrile by-product obtained by the ammoxidation of propylene or isobutylene. Crude acetonitrile obtained as a by-product in the production of acrylonitrile or methacrylonitrile usually contains allyl alcohol, oxazole, water, acetone, hydrocyanic acid, acr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/34
CPCC07C253/34C07C255/03
Inventor 王永旗王伟吕明李定发
Owner TAICANG HUSHI REAGENT
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