Acetonitrile purification method

A purification method and acetonitrile technology, applied in the direction of carboxylic acid nitrile purification/separation, etc., can solve the problems of long purification time, insufficient product yield and purity, and high equipment requirements

Inactive Publication Date: 2015-07-01
TAICANG HUSHI REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned prior art involves fractional distillation, which leads to long time-consuming purification, high requirements on equipment, and the yield and purity of the obtained products are not high enough.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 1000g of industrial grade acetonitrile (purity 98%) and 5g of sodium hydroxide solid (powder) into the reaction kettle and pretreat at 20°C for 6h under mechanical stirring. After completion, filter and collect the supernatant. Next, the supernatant was passed through a sulfonic acid-type ion exchange column at a flow rate of 50 mL / min. Then, 40 g of 4A molecular sieves with a mass of 40 g were dropped into the liquid passing through the sulfonic acid type ion exchange column for adsorption, and then the liquid was filtered out. Finally, the liquid is microfiltered with a microfiltration membrane with a pore size of 0.1 micron to obtain purified acetonitrile. In this example, 9010 g of acetonitrile was collected, the yield was 90.1%, and the tested purity was 99.50%.

Embodiment 2

[0023] Add 1000 g of industrial grade acetonitrile (purity 98%) and 25 g of sodium hydroxide solid (powder) into the reactor, pretreat at 40° C. for 3 h under mechanical stirring, filter after completion, and collect the supernatant. Next, the supernatant was passed through a sulfonic acid-type ion exchange column at a flow rate of 100 mL / min. Then, 80 g of 4A molecular sieves with a mass of 80 g were put into the liquid passing through the sulfonic acid type ion exchange column for adsorption, and then the liquid was filtered out. Finally, the liquid is microfiltered with a microfiltration membrane with a pore size of 0.3 micron to obtain purified acetonitrile. In this example, 9050 g of acetonitrile was collected, the yield was 90.5%, and the tested purity was 99.70%.

Embodiment 3

[0025] Add 1000g of industrial grade acetonitrile (purity 98%) and 75g of sodium hydroxide solid (powder) into the reaction kettle and pretreat at 30°C for 4.5h under mechanical stirring. After completion, filter and collect the supernatant. Next, the supernatant was passed through a sulfonic acid-type ion exchange column at a flow rate of 80 mL / min. Then, 60 g of 4A molecular sieves with a mass of 60 g were put into the liquid passing through the sulfonic acid type ion exchange column for adsorption, and then the liquid was filtered out. Finally, the liquid is microfiltered with a microfiltration membrane with a pore size of 0.2 microns to obtain purified acetonitrile. In this example, 9110 g of acetonitrile was collected, the yield was 91.1%, and the tested purity was 99.90%.

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Abstract

The invention discloses an acetonitrile purification method. The purification method comprises the following steps: (1) adding a strong alkali solid into crude acetonitrile to be treated to perform pretreatment; (2) passing through a strong-acid ion exchange resin; (3) passing through a 4A molecular sieve; and (4) microfiltering. The firstly added strong alkali solid can react with unsaturated nitrile and other impurities containing ultraviolet absorbance functional groups in the crude acetonitrile to generate the products with different physical properties from acetonitrile, thereby removing the unsaturated nitrile and other impurities; and the strong-acid ion exchange resin for adsorption is utilized to further remove impurities, the 4A molecular sieve for adsorption is utilized to remove water, and the microfiltration is utilized to remove the doped treating agents used in the three previous steps. Compared with the method comprising distillation, the method disclosed by the invention can save time, and the purified product has higher purity and higher yield.

Description

technical field [0001] The invention relates to the technical field of acetonitrile purification, in particular to a method for purifying acetonitrile. 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, carboamine drugs and their intermediates, and as an active medium solvent for the manufacture of vitamin B1 and amino acids. Can replace chlorinated solvents. It is also used as an extractant for fatty acid, alcohol denaturant, butadiene extractant and solvent for ...

Claims

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Application Information

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IPC IPC(8): C07C253/34C07C255/03
Inventor 王永旗王伟吕明李定发
Owner TAICANG HUSHI REAGENT
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