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Purification method for acetonitrile

A technology of acetonitrile and calcium hydride, applied in the direction of carboxylic acid nitrile purification/separation, etc., can solve the problems of complicated operation steps, low purity of acetonitrile, long time, etc., and achieve the effect of safe and simple purification process, stable product quality and high yield.

Inactive Publication Date: 2012-10-24
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to provide a method for purifying acetonitrile, so as to overcome the disadvantages of low purity of acetonitrile purified products in the prior art, cumbersome operation steps, long time and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 1000ml of industrial acetonitrile into a 2000ml three-neck flask equipped with a rectification device, a thermometer and a heating device, add 10g of anhydrous aluminum trichloride into the acetonitrile, heat and reflux for 1 hour to distill out acetonitrile, add 5g of potassium permanganate to heat After reflux for 15 minutes, distill out acetonitrile, add 15ml of sulfuric acid with a mass fraction of 95% and heat to reflux for 30 minutes to distill out acetonitrile, add 5g of calcium hydride and heat to reflux for 1h, then add 30g of 4A molecular sieves for adsorption and purification for 20min, and finally rectify at a flow rate of 20mL / min Methods 887ml of purified acetonitrile was collected, the yield was 88.7%, and the purity was 99.83%.

Embodiment 2

[0021] Add 1000ml of industrial acetonitrile into a 2000ml three-necked flask equipped with a rectification device, a thermometer and a heating device, add 15g of anhydrous aluminum trichloride into the acetonitrile, heat and reflux for 1.5h, distill out the acetonitrile, and add 10g of potassium permanganate After heating to reflux for 20 minutes, distill acetonitrile, add 20ml of sulfuric acid with a mass fraction of 95% and heat to reflux for 40 minutes to distill acetonitrile, add 10g of calcium hydride and heat to reflux for 1.5h, then add 40g of 4A molecular sieves for adsorption and purification for 25min, and finally use a flow rate of 15mL / min 896ml of purified acetonitrile was collected by rectification, with a yield of 89.6% and a purity of 99.85%.

Embodiment 3

[0023] Add 1000ml of industrial acetonitrile into a 2000ml three-necked flask equipped with a rectification device, a thermometer and a heating device, add 20g of anhydrous aluminum trichloride into the acetonitrile, heat and reflux for 2 hours to distill out acetonitrile, add 15g of potassium permanganate to heat After reflux for 25 minutes, distill out acetonitrile, add 25ml of sulfuric acid with a mass fraction of 98% and heat to reflux for 50 minutes to distill out acetonitrile, add 15g of calcium hydride and heat to reflux for 2 hours, then add 50g of 4A molecular sieves for adsorption and purification for 30 minutes, and finally rectify at a flow rate of 10mL / min Methods 905ml of purified acetonitrile was collected, the yield was 90.5%, and the purity was 99.9%.

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PUM

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Abstract

The invention discloses a purification method for acetonitrile. The method comprises the steps of using industrial grade acetonitrile as raw material, successively adding anhydrous aluminum chloride, potassium permanganate and sulfuric acid and carrying refluxing and distilling respectively, adding calcium hydride for drying, adding a 4A molecular siev for adsorption and purification, and finally performing distillation method to obtain purified acetonitrile. The purity of the acetonitrile obtained by the purification method provided by the invention is greater than 99.8%. Compared with the existing technology, the purification process is safe, simple, energy-saving and emission-reducing. The added purifying agent can be recycled after treatment, and the requirements of green chemical industry and environmental protection are met. The acetonitrile product obtained by the purification method has the advantages of stable quality and high purity, and has prospect for industrial production.

Description

technical field [0001] The invention relates to a method for purifying acetonitrile, in particular to a method for purifying acetonitrile with anhydrous aluminum trichloride, potassium permanganate, sulfuric acid, calcium hydride and 4A molecular sieves. Background technique [0002] Acetonitrile, also known as methyl nitrile, is a colorless liquid, highly volatile, has a special odor similar to ether, has excellent solvent performance, and can dissolve various organic, inorganic and gaseous substances. It has certain toxicity and is infinitely miscible with water and alcohol. Acetonitrile can undergo typical nitrile reactions and is used to prepare many typical nitrogen-containing compounds. It is an important organic intermediate. Acetonitrile can be used as a solvent for the synthesis of vitamin A, cortisone, carbon amine drugs and their intermediates, and as an active medium solvent for the manufacture of vitamin B1 and amino acids. Can replace chlorinated solvents. I...

Claims

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Application Information

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IPC IPC(8): C07C255/03C07C253/34
Inventor 王伟顾小焱吕明王永旗
Owner TAICANG HUSHI REAGENT
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