Method and device for preparing mass spectrum level acetonitrile

A mass spectrometry, acetonitrile technology, applied in the purification/separation of carboxylic acid nitrile, organic chemistry and other directions, can solve the problems of many impurity interference peaks, the purity does not meet the detection requirements of pesticide residues, etc., achieves simple operation, wide market application prospects, cost saving effect

Inactive Publication Date: 2012-05-02
NAT INST OF METROLOGY CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In order to solve the problems in the prior art that high-purity solvents contain too many interference peaks of impurities and the purity cannot meet the requirements for detection of pesticide residues, the present invention provides a mass spectrometry-level acetonitrile purification preparation method, and the acetonitrile prepared by the method of the present invention is The impurity content of the product is less than 10 -12 , can meet the requirements of pesticide residue analysis, and the operation is simple, cost-saving, and has a wide range of application prospects

Method used

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  • Method and device for preparing mass spectrum level acetonitrile
  • Method and device for preparing mass spectrum level acetonitrile
  • Method and device for preparing mass spectrum level acetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] 1. Oxidation

[0069] 2. Chromatography or adding sulfuric acid (choose one of the two)

[0070] Pass the acetonitrile raw material through two columns equipped with acidic alumina and activated carbon to remove allyl alcohol, oxazole and a certain amount of water. Or adding sulfuric acid can also remove allyl alcohol and oxazole, and can also neutralize a small amount of lye in the oxidation process.

[0071] Part of the preceding liquid was discarded and the remaining solvent was collected for a rectification step.

[0072] 3. Distillation

[0073] By optimizing the distillation conditions, the desired product is finally obtained.

[0074] Device parameters

[0075] 1) Oxidation reaction tank: the volume is 2000 liters.

[0076] Oxidation reagent: potassium permanganate (Beijing Chemical Reagent Factory), the purity is 98%, and the consumption of high-efficiency oxidation reagent is 22% of raw material weight.

[0077] 2) Dehydrogenation tower: tower height 6m, ...

Embodiment 2

[0110] Device parameters

[0111] 1) Oxidation reaction tank: glass separatory funnel, volume 2.5 liters.

[0112] Oxidation reagent: potassium permanganate (Beijing Chemical Reagent Factory), the concentration is 98%; the consumption of potassium permanganate is 5% of raw material weight.

[0113]2) Dehydrogenation tower: the height of the glass tower is 1.3m, and the inner diameter of the tower is 10cm; packing: θ ring packing.

[0114] The condenser tube is a coiled glass condenser.

[0115] Dehydrogenation tower kettle: a 3-liter triangular round-bottom glass flask, heated by an electric heating pot.

[0116] 3) Distillation tower: the height of the glass tower is 1.5m, and the inner diameter of the tower is 10cm; packing: θ ring packing.

[0117] The condenser tube is a coiled glass condenser.

[0118] Rectification tower kettle: a 3-liter triangular round-bottom glass flask, heated by an electric heating pot.

[0119] 4) Filtration device: glass solvent filter, the ...

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Abstract

The invention relates to a method and a device for preparing mass spectrum level acetonitrile. The method comprises the following steps of: performing oxidation reaction on acetonitrile to remove impurities, rectifying, and filtering to obtain the mass spectrum level acetonitrile, wherein an oxidant used in the oxidation reaction is potassium permanganate, sodium hydroxide, potassium hydroxide, calcium hydroxide and the like; the impurities such as residual trace hydrocyanic acid and acrylonitrile and the like in industrial acetonitrile are mainly removed; the using amount of the oxidation reaction agent is 1 to 50 weight percent of that of the acetonitrile; and oxidation reaction time is 3 to 24 hours. The impurity content of the mass spectrum level acetonitrile product prepared by the method is lower than 10 to 12, the requirement of pesticide residue analysis can be met, the method and the device are easy to operate, cost is saved, and wide market application prospects are achieved.

Description

technical field [0001] The present invention relates to the field of high-purity chemical reagents, and furthermore, relates to an oxidation reaction agent, which can be used for chromatographic analysis, mass spectrometry analysis and pesticide residue detection by rectifying and purifying acetonitrile of industrial grade purity through oxidation reaction. Method and apparatus for mass spectrometry-grade acetonitrile. Background technique [0002] The molecular formula of acetonitrile is CH 3 CN, also known as methyl cyanide or methyl cyanide, has a relative molecular mass of 41.05. It is a colorless transparent liquid under 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 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/03C07C253/34
Inventor 全灿黄挺李红梅
Owner NAT INST OF METROLOGY CHINA
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