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Preparation method for high-purity gradient acetonitrile

A pure acetonitrile, gradient grade technology, applied in the field of high-purity chemical reagent preparation, to achieve the effect of overcoming waste treatment and less pollution

Active Publication Date: 2015-06-17
WEIFANG ZHONGHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a preparation method of gradient grade high-purity acetonitrile, which purifies industrial acetonitrile through four processes of adsorption, drying, osmotic distillation and rectification, which are highly efficient, energy-saving, and will not bring Secondary pollution, thereby eliminating the defects in the above-mentioned background technology

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  • Preparation method for high-purity gradient acetonitrile

Examples

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Embodiment 1

[0032] A preparation method of gradient grade high-purity acetonitrile, the steps are as follows:

[0033] (1) Take a clean adsorption column, the column height is 1m, the inner diameter is 3cm, and the high-purity carbon fiber is installed inside, and the column volume is 4 / 5 of the column height; The carbon fiber adsorption column removes most of the impurities. The high-purity carbon fiber is made of asphalt, viscose fiber or acrylonitrile at a processing temperature of 1200°C and has a carbon content of 99.8%.

[0034] (2) Take a clean and dry column with a height of 1m and an inner diameter of 3cm, which contains a desiccant 3A molecular sieve and silica gel, and the amount of the column is 4 / 5 of the column height; pass the acetonitrile adsorbed by high-purity carbon fiber at a speed of 70ml / min A drying column filled with a desiccant to remove moisture;

[0035] (3) Pass the dried acetonitrile through the osmotic distillation device to further remove small molecular im...

Embodiment 2

[0043] A preparation method of gradient grade high-purity acetonitrile, the steps are as follows:

[0044] (1) Take a clean adsorption column with a column height of 1m and an inner diameter of 3cm, with high-purity carbon fiber inside, and the column volume is 4 / 5 of the column height; The carbon fiber adsorption column removes most of the impurities. The high-purity carbon fiber is made of asphalt, viscose fiber or acrylonitrile at a processing temperature of 1250°C and has a carbon content of 99.9%.

[0045] (2) Take a clean and dry column with a height of 1m and an inner diameter of 3cm, which contains desiccant 3A molecular sieve and silica gel, and the amount of the column is 4 / 5 of the column height; pass the acetonitrile adsorbed by high-purity carbon fiber at a speed of 60ml / min A drying column filled with a desiccant to remove moisture;

[0046] (3) Pass the dried acetonitrile through an osmotic distillation device to further remove small molecular impurities that c...

Embodiment 3

[0054] A preparation method of gradient grade high-purity acetonitrile, the steps are as follows:

[0055] (1) Take a clean adsorption column with a height of 1m and an inner diameter of 3cm, with high-purity carbon fiber inside, and the column volume is 4 / 5 of the column height; at room temperature, pass the raw material industrial acetonitrile through the high-purity The carbon fiber adsorption column removes most of the impurities. The high-purity carbon fiber is made of asphalt, viscose fiber or acrylonitrile, processed at a processing temperature of 3000°C, and has a carbon content of 99.6%.

[0056] (2) Take a clean and dry column with a height of 1m and an inner diameter of 3cm, which contains a desiccant 3A molecular sieve and silica gel, and the amount of the column is 4 / 5 of the column height; pass the acetonitrile adsorbed by high-purity carbon fiber at a speed of 50ml / min A drying column filled with a desiccant to remove moisture;

[0057] (3) Pass the dried aceto...

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Abstract

The invention relates to a preparing method for high-purity gradient acetonitrile. The preparation method comprises the steps as follows: (1) enabling the raw material of industrial acetonitrile to pass through an adsorption column filled with high-purity carbon fiber at a speed of 40-80 ml / min to remove most impurities; (2) enabling acetonitrile after being adsorbed by the high-purity carbon fiber to pass through a drying column filled with desiccants at a speed of 50-70 ml / min to remove moisture; (3) enabling acetonitrile after drying to pass through an osmotic distillation device to further remove small-molecule impurities failing to be adsorbed by the high-purity carbon fiber; (4) sending acetonitrile subjected to impurity removal by the osmotic distillation device into a rectification device for rectification processing to obtain the high-purity gradient acetonitrile. The yield of the high-purity gradient acetonitrile reaches more than 80%, and the detection indicators of the high-purity gradient acetonitrile can fully meet the product standards of the international high-purity acetonitrile manufacturers.

Description

technical field [0001] The invention relates to the technical field of preparation of high-purity chemical reagents, in particular to a method for preparing gradient grade high-purity acetonitrile by using industrial acetonitrile. Background technique [0002] At present, high-purity acetonitrile is one of the commonly used mobile phases in high-performance liquid chromatography, which has the characteristics of low UV absorption and high sensitivity. With the rapid development of chemical, pharmaceutical, and biological industries at home and abroad, the application of high-performance liquid chromatography is becoming more and more extensive, and the demand for high-purity acetonitrile is also increasing. At present, there are very few manufacturers in my country that can produce gradient-grade high-purity acetonitrile, and they mainly meet the demand through imports. In addition, the existing technology for preparing high-purity acetonitrile is that industrial acetonitri...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/34C07C255/03
Inventor 傅鹏远吴绍帅李华青
Owner WEIFANG ZHONGHUI CHEM