Preparation method of chromatographic-grade methyl tert-butyl ether

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

Active Publication Date: 2017-01-25
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Preparation method of chromatographic-grade methyl tert-butyl ether

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Comparison scheme
Effect test

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 tert-butyl ether. The preparation method includes subjecting a sodium hypochlorite solution and industrial-grade methyl tert-butyl ether to refluxing reaction to generate high-boiling-point chlorohydrin and then glycol under the protection of nitrogen; drying the glycol by anhydrous calcium chloride to remove moisture and alcohol impurities; rectifying to obtain the chromatographic-grade methyl tert-butyl ether. The preparation method of the chromatographic-grade methyl tert-butyl ether has the advantages of classical process, easiness in operation, stability, cheap raw materials, easy availability and suitability for large-scale operation, and the purity of the obtained chromatographic-grade methyl tert-butyl ether can be higher 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 Applications(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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