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Composite oxidizer and method for preparing high efficiency liquid chromatography eluate acetonitrile by using same

A technology of high performance liquid chromatography and composite oxidant, which is applied in the field of purification of chemical products, can solve the problems of long oxidation time, violent reaction, residual manganese salt, etc., and achieve the effect of saving reaction time, good oxidation effect and stable operation

Active Publication Date: 2012-11-14
FTSCI HUBEI BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In these methods, most of them use oxidation as a purification method, but at present, sodium hydroxide, potassium permanganate, phosphorus pentoxide, etc. or ozone are used as oxidants to oxidize industrial acetonitrile, combined with distillation or adsorption. The method can obtain chromatographic grade acetonitrile, but its disadvantages are large amount of oxidant, long oxidation time, violent reaction, residual manganese salt, environmental pollution and low product yield

Method used

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  • Composite oxidizer and method for preparing high efficiency liquid chromatography eluate acetonitrile by using same
  • Composite oxidizer and method for preparing high efficiency liquid chromatography eluate acetonitrile by using same

Examples

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Embodiment 1

[0027] A preparation method of high performance liquid chromatography eluent acetonitrile, the steps are as follows:

[0028] (1) The raw material acetonitrile (99.9% purity) is injected into the three-layer adsorption bed. The three-layer adsorption bed is composed of activated alumina layer, activated carbon layer and 3A molecular sieve layer in series from top to bottom. The specifications of the three layers are: long 1 meter, 1 meter high, 1.2 meters wide;

[0029] The outlet channel of each layer of adsorption bed is equipped with an opening connected with a water pump to generate negative pressure to control the flow rate of acetonitrile;

[0030] Among them, the activated alumina layer, activated carbon layer, and 3A molecular sieve layer are respectively filled with activated alumina with a particle size of 0.2mm, activated carbon with a particle size of 0.2mm, and 3A molecular sieve. 1 / 2 of the height;

[0031] After acetonitrile is injected into the activated alum...

Embodiment 2

[0036] A preparation method of high performance liquid chromatography eluent acetonitrile, the steps are as follows:

[0037] (1) The raw material acetonitrile (99.5% purity) is injected into the three-layer adsorption bed. The three-layer adsorption bed is composed of activated alumina layer, activated carbon layer, and 3A molecular sieve layer in series from top to bottom. The specifications of the three layers are: long 0.5 meters, 0.5 meters high, 0.6 meters wide;

[0038] The outlet channel of each layer of adsorption bed is equipped with an opening connected with a water pump to generate negative pressure to control the flow rate of acetonitrile;

[0039] Among them, the activated alumina layer, activated carbon layer, and 3A molecular sieve layer are respectively filled with activated alumina with a particle size of 0.2mm, activated carbon with a particle size of 0.2mm, and 3A molecular sieve. 1 / 2 of

[0040] After acetonitrile is injected into the activated alumina l...

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Abstract

The invention belongs to the technical field of purification of chemical products, and particularly relates to a composite oxidizer and a method for preparing high efficiency liquid chromatography eluate acetonitrile by using the same. The composite oxidizer is composed of potassium superoxide, potassium hydroxide and sodium hydroxide. The method for preparing high efficiency liquid chromatography eluate acetonitrile by using the composite oxidizer comprises the following steps: adsorbing the raw material acetonitrile with the content of more than 99.5% with an active aluminum oxide-activated carbon-3A molecular sieve three-layer adsorption bed, oxidizing by the composite oxidizer, rectifying, and filtering to obtain the high efficiency liquid chromatography eluate acetonitrile. The composite oxidizer provided by the invention overcomes the defect of long oxidization time in the use of the single oxidizer, saves the reaction time, and has better oxidization effect; the preparation method has the advantage of simple and stable operation, and is suitable for large-scale production; and when the method is used for preparing the chromatography acetonitrile, the product yield can reach more than 95%, and the product quality achieves the quality level of like products abroad.

Description

technical field [0001] The invention relates to the technical field of purification of chemical products, in particular to a composite oxidizing agent and a method for preparing high-performance liquid chromatography eluent acetonitrile by using the compound oxidant. Background technique [0002] Acetonitrile, the eluent of high performance liquid chromatography, is one of the mobile phases commonly used in liquid chromatography. The purity of chromatographic grade acetonitrile is required to reach more than 99.9%, and the water content is lower than 1ppm. The main source of industrial grade acetonitrile is the by-product of the production of acrylonitrile. Products, so in the production of acetonitrile will inevitably produce or bring impurities. The impurities that may be contained in industrial acetonitrile mainly include hydrocyanic acid, acrylonitrile, acetaldehyde, acetone, propionitrile, methanol, acrolein, methacrylonitrile, cis- and trans-acrylonitrile, oxazole, all...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/34
Inventor 文胜覃彩芹周亚洲
Owner FTSCI HUBEI BIOTECH CO LTD
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