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A kind of purification technology of methyl tert-amyl ether purity standard substance raw material

A technology of methyl tert-amyl ether and standard substances, which is applied in the field of purity standard substances, can solve the problems of high raw material purity requirements, difficult separation, difficult removal, etc., and achieve good economic benefits, simple process, and stable product quality.

Active Publication Date: 2021-12-14
NAT INST OF METROLOGY CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The difficulty in the purification of raw materials for the purity standard substance of methyl tert-amyl ether is that the preparation of methyl tert-amyl ether mainly adopts the dehydration synthesis process of methanol and tert-amyl alcohol, which will produce a large amount of by-products of tert-amyl alcohol, of which methyl tert-amyl ether and tert-amyl alcohol have similar boiling points, so separation is difficult; raw material purity requirements are high, and industrial-grade products contain different types of trace impurities such as alcohols, ethers, alkanes, etc., which are difficult to remove by a single purification method, and may also cause Introduce new impurities, which will affect subsequent use
At present, there are few literatures on the purification of methyl tert-amyl ether in China

Method used

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  • A kind of purification technology of methyl tert-amyl ether purity standard substance raw material
  • A kind of purification technology of methyl tert-amyl ether purity standard substance raw material
  • A kind of purification technology of methyl tert-amyl ether purity standard substance raw material

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Embodiment 1

[0041] Example 1 Purification of technical-grade methyl tert-amyl ether by means of sophisticated rectification-adsorption coupling technology.

[0042] The raw material of industrial grade methyl tert-amyl ether is purchased from Sigma Company of the United States, the Lot number is BCBS3844V, and the purity of gas chromatography (GC) is 98.73%. According to the analysis of impurities by gas chromatography-mass spectrometry, it contains about 0.23% of various olefin impurities, Alkanes are about 0.21%, and tert-amyl alcohol impurities are about 0.83%.

[0043] The inner diameter of the rectification tower is 29mm, the outer diameter is 32mm, the height of the rectification tower is 1m, and the built-in 3mm×3mmθ ring packing, the packing height is 0.6m. The heating voltage of the kettle is 200V, the liquid is boiling and the reflux liquid at the top of the tower just flows down in a stream, and the total reflux is for 3 hours. The product is extracted at a reflux ratio of 10:1...

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Abstract

The invention provides a purification technology of methyl tert-amyl ether purity standard substance raw material, comprising steps: (1) precision rectification: under normal pressure, adding industrial-grade methyl tert-amyl ether into a rectification tower, the rectification tower Built-in packing, obtain the methyl tert-amyl ether product from the top of the rectification tower, discard the front fraction with more impurities to obtain the sample to be adsorbed; (2) adsorption: at normal temperature, transfer the sample to be adsorbed obtained in step (1) to Adsorption tower, the adsorption tower has a built-in adsorbent, and the methyl tert-amyl ether product is obtained from the bottom of the adsorption tower; (3) Filtration: at normal temperature, the methyl tert-amyl ether product obtained in step (2) is passed through an organic microporous membrane Filter to obtain high-purity methyl tert-amyl ether. The purification technology of the present invention can solve the difficulty in the prior art that various trace impurities are difficult to remove, and the obtained methyl tert-amyl ether has a purity higher than 99.9%, less impurities and can be used as a standard substance.

Description

technical field [0001] The present invention relates to the technical field of purifying purity standard material raw materials, in particular to a purification technology of methyl tert-amyl ether purity standard material raw materials, in particular to a precision rectification-adsorption coupling technology to convert industrial-grade purity The methyl tert-amyl ether was purified, and the obtained product was used as a purity standard substance. Background technique [0002] A reference material is a class of substances of sufficiently homogeneous and stable specific properties suitable for their intended use in measurement or checking of nominal properties. The characteristic value of purity standard substance is its purity. Unlike conventional chemical reagents, its purity value is known and obtained by high-accuracy determination technology. It is often used as the basis for quantitative analysis in the field of scientific research and analysis and detection. Standar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/04C07C41/42C07C41/36
CPCC07C41/36C07C41/42C07C43/046
Inventor 全灿杨菡孙永跃金君素李红梅
Owner NAT INST OF METROLOGY CHINA
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