A kind of preparation method of chromatographic grade methyl tertiary butyl ether

A technology of methyl tertiary butyl ether and chromatographic grade, applied in the field of preparation of chromatographic grade methyl tertiary butyl ether, can solve the problems of complicated operation steps and high cost, and achieve the effects of classic process, easy operation and cheap raw materials

Active Publication Date: 2021-08-03
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is prepared by alkali metal oxide treatment, modified activated carbon adsorption, alumina column treatment, rectification and other steps; the method has high cost and complicated operation steps

Method used

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  • A kind of preparation method of chromatographic grade methyl tertiary butyl ether

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Embodiment 1

[0024] (1) In a 5L three-neck flask with stirring, condensation and thermometer, under nitrogen protection, put 3 liters of industrial grade methyl tert-butyl ether (about 2220g) and 120g of sodium hypochlorite solution, heat, stir and reflux for 2 hours to generate chlorohydrins, And under alkaline hydrolysis to generate diol soluble in water;

[0025] (2) Cool the mixture of the reactants of industrial-grade methyl tert-butyl ether and sodium hypochlorite solution in step (1) to below 10°C, let it stand for 0.5 hours, and separate the phases; the water phase is used for wastewater treatment;

[0026] (3) Add 240g of anhydrous calcium oxide to the organic phase, and dry it under ultrasonic waves at room temperature for 1 hour;

[0027] (4) standing and microfiltration to obtain purified and dried methyl tert-butyl ether, wherein the methyl tert-butyl ether does not contain olefins and alcohols;

[0028] (5) Under the protection of nitrogen, add dry methyl tert-butyl ether in...

Embodiment 2

[0031] (1) In a 5L three-necked flask with stirring, condensation and thermometer, under the protection of nitrogen, put 3 liters of industrial grade methyl tert-butyl ether (about 2220g) and 200g of sodium hypochlorite solution, heat, stir and reflux for 1 hour to generate chlorohydrins, And under alkaline hydrolysis to generate diol soluble in water;

[0032] (2) Cool the mixture of the reactants of industrial-grade methyl tert-butyl ether and sodium hypochlorite solution in step (1) to below 10°C, let it stand for 0.5 hours, and separate the phases; the water phase is used for wastewater treatment;

[0033] (3) Add 180g of anhydrous calcium oxide to the organic phase, and dry it under ultrasonic wave at room temperature for 1 hour;

[0034] (4) standing and microfiltration to obtain purified and dried methyl tert-butyl ether, wherein the methyl tert-butyl ether does not contain olefins and alcohols;

[0035] (5) Distill the dried methyl tert-butyl ether through a rectifica...

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Abstract

The invention discloses a preparation method of chromatographic grade methyl tertiary butyl ether. The preparation method comprises the following steps: under nitrogen protection, sodium hypochlorite solution and technical grade methyl tertiary butyl ether are used for reflux reaction to generate high-boiling chlorohydrin, and then Diol is further generated; water and alcohol impurities are removed by drying with anhydrous calcium oxide; finally, chromatographic grade methyl tertiary butyl ether is obtained by rectification; It is suitable for large-scale operation, and the purity of the prepared product can reach more than 99.99%.

Description

technical field [0001] The invention belongs to the technical field of chemical purification, and in particular relates to a method for preparing chromatographic grade methyl tert-butyl ether. Background technique [0002] Methyl tert-butyl ether (MTBE for short) is a petrochemical bulk chemical, usually prepared from isobutene and methanol in the C4 fraction in the presence of an acidic catalyst; it is a colorless, transparent, high-octane High-value liquid with an ether-like odor. It is an ideal blending component for the production of unleaded, high-octane, and oxygen-containing gasoline. It has been widely used as a gasoline additive throughout the world; it can also be re-cracked into isobutylene and used as a rubber and other raw materials for chemical products. Good quality methyl tert-butyl ether can be used as pharmaceutical intermediates and solvents. [0003] According to the petrochemical industry standard SH / T 1550-2000, MTBE contains the following impurities:...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/34C07C41/42C07C41/44C07C43/04
CPCC07C41/34C07C41/42C07C41/44C07C43/046
Inventor 顾小焱郭建国郑琦顾金凤凌芳
Owner SINOPHARM CHEM REAGENT
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