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Method for purifying high-purity organic solvent acetonitrile for research

A purification method and organic solvent technology, which is applied in the field of purification of acetonitrile, a high-purity organic solvent for scientific research, can solve the problems of unsatisfactory detection of pesticide residues, liquid phase gradient elution, and low purification level, and achieve reduced dependence and easy operation , the effect of stable operation

Active Publication Date: 2009-11-04
天津市康科德科技有限公司
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Problems solved by technology

Wherein patent (patent No. is: 95102948.7, title is called: purification of acetonitrile by adsorption method) has announced the method for purifying acetonitrile with strong alkali and adsorbent, does not mention the grade of the acetonitrile of production in this patent, and its purification step is simple, and purification grade is relatively Low, unable to meet the needs of pesticide residue detection and liquid phase gradient elution

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  • Method for purifying high-purity organic solvent acetonitrile for research

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Embodiment Construction

[0018] Below in conjunction with the examples, the present invention is further described, the following examples are illustrative, not limiting, and the protection scope of the present invention cannot be limited by the following examples.

[0019] A kind of purification method of high-purity organic solvent acetonitrile for scientific research, its steps are as follows:

[0020] (1) 15 kg of raw material acetonitrile with a content of about 99.5% is injected into a 20L reactor, and 4.5 kg of solid sodium hydroxide is added according to 30% of the mass of the acetonitrile, stirred at room temperature after the addition, and the reaction time is controlled to be 6 hours. Then filter to obtain clear liquid.

[0021] The purpose of this step reaction is to remove unsaturated nitriles in the raw material acetonitrile, such as acrylonitrile, acetamide and the like.

[0022] (2) The clear liquid obtained by the above filtration is passed through an adsorption column equipped with ...

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Abstract

The invention relates to a method for purifying high-purity organic solvent acetonitrile for research, including the steps as below: acetonitrile which is used as a raw material reacts with solid alkali at low temperature so as to eliminate unsaturated nitrile; impurities absorbed by high waveband ultraviolet are removed by the adsorption of zeolite and polymeric adsorbent; and a 3A molecular sieve is used for drying and dehydration, and the operations of rectification, filtration and encapsulation are carried out to obtain the product of chromatographic grade, pesticide residue grade and gradient elution grade chromatographic acetonitrile. By the method, the product of chromatographic pure acetonitrile with purity of more than 99.9 percent can be obtained, and can meet the requirement of the pesticide residue grade and gradient elution grade chromatographic acetonitrile, thereby meeting the demand of customers on application of high efficiency liquid chromatography (HPLC) in pesticide residues, filling in the gap of domestic preparation of pesticide residue grade and gradient elution grade chromatographic reagents, reducing the dependency on abroad reagents, and providing the qualified reagents for the inspection of the pesticide residues and the separation and the nature determination of complex medicines.

Description

technical field [0001] The invention belongs to the field of chemical reagents, in particular to a method for purifying acetonitrile, a high-purity organic solvent for scientific research. Background technique [0002] Chromatographically pure acetonitrile is one of the commonly used liquid chromatographic mobile phases. In recent years, with the need for liquid chromatographic separation, the demand for reagents with low UV absorption, low impurities, low pH and low residue has increased. Among them, GC-ECD agricultural Residue detection and liquid chromatography gradient elution all require ultra-clean acetonitrile products with higher purity than chromatographic purity to meet the needs of scientific research. [0003] At present, there are few manufacturers producing chromatographic acetonitrile in my country. With the rapid development of analysis, synthesis, biochemical and other industries, the demand for high-purity acetonitrile is increasing, especially in scientifi...

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Application Information

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IPC IPC(8): C07C255/03C07C253/34
Inventor 宋金链张玉芝
Owner 天津市康科德科技有限公司
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