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High-purity acetonitrile and its preparation method and device

An acetonitrile and purity technology, which is applied in the purification/separation of carboxylic acid nitrile, organic chemistry, etc., can solve the problems of high impurity content of acetonitrile solvent, complicated preparation process, unsatisfactory purity, etc., and achieves low cost, simple device operation, and simple operation. Effect

Inactive Publication Date: 2016-07-06
NAT INST OF METROLOGY CHINA
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Problems solved by technology

[0011] The above-mentioned methods for preparing mass spectrometry-grade acetonitrile disclosed in the prior art all have many problems such as high impurity content of acetonitrile solvent, purity that cannot meet mass spectrometry detection, complex preparation process, high cost, and serious pollution.

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Embodiment 1

[0060] The preparation of embodiment 1 mass spectrum grade acetonitrile product

[0061] A method for preparing mass spectrometry grade acetonitrile, said mass spectrometry grade acetonitrile is obtained by preparing and purifying industrial grade acetonitrile, said method comprising three steps of adsorption, oxidation and rectification:

[0062] (1) Adsorption

[0063] With 20 liters of industrial grade acetonitrile (Nanjing Nanshi Chemical Reagent Co., Ltd.) from the chromatographic column (200 orders, Shanghai Wusi Chemical Reagent Co., Ltd.) filled with 100-200 mesh 2.5kg alumina, after the adsorbent is activated, dry In the chromatographic column, no dead volume is left, and the raw material is pumped in from the top with a metering pump, the flow rate of the raw material is controlled, and the material is received at the bottom. The height of the chromatographic column is 1.8m, and the inner diameter is 8cm; Adsorb to remove trace physical impurities and a small amount...

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Abstract

The invention relates to a high-purity acetonitrile and its preparation method and device. The preparation method comprises the steps of absorbing the acetonitrile raw material to be purified, undergoing oxidation reaction, and then performing rectification to obtain high-purity acetonitrile, and using the method to establish a set of continuous preparation equipment. The adsorbent used in the adsorption process is aluminum oxide, which is mainly used to remove a small amount of physical impurities, salts, moisture and other impurities in the acetonitrile raw material. The oxidant used in the oxidation reaction is potassium permanganate, which is mainly used to remove impurities such as trace amounts of hydrocyanic acid and acrylonitrile. Rectification mainly removes impurities such as trace homologues in acetonitrile. The high-purity acetonitrile product prepared by the method of the present invention has low impurity content, and the quality index can meet the requirements of high-resolution mass spectrometer analysis, and the purification process does not discharge three wastes, directly uses industrial-grade raw materials, saves costs, and has a broad market Promote application prospects.

Description

technical field [0001] The invention relates to the field of high-purity chemical reagents, in particular to a method and a device for preparing industrial-grade acetonitrile into high-purity acetonitrile that can be used for mass spectrometry by using an adsorbent, an oxidant, and a rectification purification process. Background technique [0002] The molecular formula of acetonitrile is CH 3 CN, with a relative molecular mass of 41.05, is a colorless and transparent liquid at normal temperature and pressure. The melting point is -45.7°C, the boiling point is 81.1°C, the relative density is 0.79, the relative vapor density is 1.42, the flash point is 2°C, the ignition temperature is 524°C, and it is flammable. Acetonitrile is extremely volatile, miscible with water, soluble in most organic solvents such as alcohol, and is a polar solvent with a high insulation coefficient. It has excellent solvent properties and can dissolve various organic, inorganic and gaseous substanc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/03C07C253/34
Inventor 全灿韩强杜然戴新华
Owner NAT INST OF METROLOGY CHINA
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