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High-purity acetonitrile and method and device for preparing high-purity acetonitrile

A pure acetonitrile and acetonitrile technology, applied in the field of high-purity chemical reagents, can solve the problems of high impurity content of acetonitrile solvent, unsatisfactory purity, complicated preparation process, etc., and achieve the effects of low cost, simple operation, and simple device operation

Inactive Publication Date: 2014-09-24
NAT INST OF METROLOGY CHINA
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  • Abstract
  • Description
  • Claims
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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.

Method used

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Embodiment 1

[0060] Embodiment 1 Preparation of mass spectrometry 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 high-purity acetonitrile and a method and device for preparing the high-purity acetonitrile. The preparing method includes the steps that acetonitrile raw materials to be purified are adsorbed, an oxidizing reaction is carried out, and then the high-purity acetonitrile is prepared through rectification. A set of continuous preparing equipment is built with the method. Adsorbents used in the adsorption process are aluminum oxide and are mainly used for removing impurities, such as a little number of physical impurities, salt and water, in the acetonitrile raw materials. Oxidizing agents used in the oxidizing reaction are potassium permanganate and are mainly used for removing impurities such as a trace amount of hydrocyanic acid and acrylonitrile. Rectification is mainly used for removing impurities, such as a trace amount of homolog, in the acetonitrile. The high-purity acetonitrile product manufactured with the method is low in impurity content, the quality index can meet the analysis requirements of a high-resolution mass spectrometer, discharging of the three wastes is avoided in the purification process, the industrial-grade raw materials are directly used, cost is saved, and the wide market application and popularization prospects are achieved.

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 Applications(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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