Method for preparing tert-butyl hydrogen peroxide and tert-butyl alcohol by oxidating isobutane

A technology of tert-butyl hydroperoxide and isobutane is applied in the preparation of oxidation reaction, chemical instruments and methods, preparation of peroxy compounds, etc. High performance, high conversion rate, the effect of reducing temperature and pressure

Inactive Publication Date: 2012-03-28
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, U.S. Patents US3478108, US3855314 and US3907202, etc. disclose the technology of increasing the yield of tert-butyl hydroperoxide by adding a small amount of water, peroxidized products or their corresponding alcohols, which can achieve certain results, but the reaction still needs to be carried out under high temperature and high pressure conditions. proceed next
[0004] It is now known that isobutane oxidation is a reaction process based on a free radical mechanism. The product tert-butyl hydroperoxide is in an unstable state above 75°C, and it will decompose violently when the temperature is higher than 90°C. There is a certain degree of safety. Hidden dangers in production
In addition, there is a long induction period in the early stage of the reaction, and the production capacity of the device is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 0.7690g of N-hydroxyphthalimide catalyst, 10mL of acetonitrile, 11.6g of isobutane into a 100mL passivation reaction kettle, feed 1.50MPa oxygen to react, the reaction temperature is 75°C, take out the reaction kettle after 5h and cool it down quickly , take out the reaction solution after depressurization, analyze with gas chromatograph, carry out quantification with ethyl acetate as internal standard, measure the isobutane conversion rate of 25.35%, the total selectivity of tert-butyl hydroperoxide and tert-butanol is 98.53% , the molar ratio of tert-butyl hydroperoxide to tert-butanol is 1.01.

Embodiment 2

[0024] Add 0.7660g of N-hydroxyphthalimide catalyst, 10mL of ethyl acetate, 11.8g of isobutane into a 100mL passivation reaction kettle, feed 2.30MPa oxygen to react, the reaction temperature is 75°C, take out the reaction kettle after 5h Cool rapidly, take out reaction solution after depressurization, analyze with gas chromatograph, carry out quantification with acetonitrile as internal standard, measure isobutane conversion rate 16.2%, the total selectivity of tert-butyl hydroperoxide and tert-butanol is 82.75% , the molar ratio of tert-butyl hydroperoxide to tert-butanol is 0.94.

Embodiment 3

[0026] Add 0.7662g of N-hydroxyphthalimide catalyst, 10mL of N,N-dimethylacetamide, 12.4g of isobutane into a 100mL passivation reaction kettle, and feed 2.30MPa oxygen to react at a reaction temperature of 75°C. After 5h, the reaction kettle was taken out to cool rapidly, and the reaction solution was taken out after depressurization, analyzed by a gas chromatograph, carried out quantitatively with ethyl acetate as an internal standard, and the conversion rate of isobutane was 11.8%, tert-butyl hydroperoxide and tert-butyl The total alcohol selectivity is 58.53%, and the molar ratio of tert-butyl hydroperoxide to tert-butanol is 2.06.

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PUM

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Abstract

The invention discloses a method for preparing tert-butyl hydrogen peroxide and tert-butyl alcohol by oxidating isobutene. Molecular oxygen is taken as an oxygen source; N-hydroxy phthalimide (NHPI) or a derivative thereof is taken as a catalyst; in the presence of a polar solvent, carrying out catalytic oxidation on the liquid phase of the isobutane to prepare the tert-butyl hydrogen peroxide and the tert-butyl alcohol; after finishing the reaction and rapidly cooling, the catalyst and the products are subjected to solid-liquid separation; and the catalyst is recycled through centrifugal sedimentation and washing. Compared with the existing process without catalytic optimization, the method disclosed by the invention has mild reaction conditions, the temperature and the pressure needed in the reaction can be remarkably lowered; and in addition, under the condition of having higher rate of conversion of the isobutane, the high selectivity of the tert-butyl hydrogen peroxide and the tert-butyl alcohol can be maintained.

Description

technical field [0001] The present invention relates to a method for preparing tert-butyl hydroperoxide and tert-butanol by oxidation of isobutane, and more particularly relates to a method for preparing tert-butyl hydroperoxide by oxidation of isobutane using non-metal as a catalyst and molecular oxygen as an oxygen source. Method for hydrogen peroxide and tert-butanol. Background technique [0002] Tert-butyl hydroperoxide is a main raw material and an important intermediate product in the chemical industry. It is widely used as an oxidant, an initiator of free radical reactions, and is also used as a raw material for the synthesis of other organic peroxides. A common oxygen source for oxypropane. [0003] Because tert-butyl hydroperoxide has a wide range of applications, its synthesis research has attracted widespread attention at home and abroad. According to the existing synthetic method of industry, it is mainly divided into four classes: (1) tert-butanol hydrogen pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/04C07C407/00C07C31/12C07C29/50
CPCY02P20/584
Inventor 吴剑冯倩袁霞罗和安
Owner XIANGTAN UNIV
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