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Process for preparing tert-butyl hydroperoxide

A technology of tert-butyl hydroperoxide and hydrogen peroxide, which is applied in the preparation of peroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc., to achieve the effects of high stability, avoiding the difficulty of separation of the same phase, and high selectivity

Active Publication Date: 2005-11-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of this invention is to provide a kind of method of new synthetic tert-butyl hydroperoxide, to solve many problems that exist in the industrial process

Method used

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  • Process for preparing tert-butyl hydroperoxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 3.5g of titanium-silicon molecular sieves and put them in a 100ml three-neck glass bottle, then add 50.6ml of tert-butanol and 10ml of 30% hydrogen peroxide to the bottle in turn. At this time, the molar ratio of tert-butanol to hydrogen peroxide is 5.57 . Put the three-necked glass bottle on a temperature-controlled magnetic stirrer, use a condenser tube to condense and reflux the upper part of the three-necked glass bottle, start the magnetic stirring and heating control, and start the reaction. The reaction temperature is controlled at about 65°C. After 6 hours of reaction, the selectivity of tert-butyl hydroperoxide is 100%, the utilization rate of hydrogen peroxide reaches 83.6%, and the conversion rate of tert-butanol is 15.01%.

Embodiment 2

[0023] Weigh 4g of titanium-silicon molecular sieve and put it in a 100ml three-necked glass bottle, and then add 27.6ml of tert-butanol and 30ml of 30% hydrogen peroxide to the bottle in turn. At this time, the molar ratio of tert-butanol to hydrogen peroxide is 1.00. Put the three-necked glass bottle on a temperature-controlled magnetic stirrer, use a condenser tube to condense and reflux the upper part of the three-necked glass bottle, start the magnetic stirring and heating control, and start the reaction. The reaction temperature is controlled at about 70°C. After 10 hours of reaction, the selectivity of tert-butyl hydroperoxide is 100%, the utilization rate of hydrogen peroxide reaches 66.83%, and the conversion rate of tert-butanol is 66.83%.

Embodiment 3

[0025] Weigh 4g of titanium-silicon molecular sieve and put it in a 100ml three-necked glass bottle, and then add 41.4ml of tert-butanol and 15ml of 30% hydrogen peroxide to the bottle in turn. At this time, the molar ratio of tert-butanol to hydrogen peroxide is 3.01. Put the three-necked glass bottle on a temperature-controlled magnetic stirrer, use a condenser tube to condense and reflux the upper part of the three-necked glass bottle, start the magnetic stirring and heating control, and start the reaction. The reaction temperature is controlled at about 80°C. After 3 hours of reaction, the selectivity of tert-butyl hydroperoxide is 100%, the utilization rate of hydrogen peroxide reaches 65.78%, and the conversion rate of tert-butanol is 21.85%.

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Abstract

The invention provides a process for preparing tert-butyl hydroperoxide, which comprises contacting tert-butanol and hydrogen dioxide by the mol ratio of 0.5-10 for 0.5-10hours at 40-100 deg. C at the presence of titanium-silicon molecular screen, the content of titanium-silicon molecular screen is 0.005-0.1g molecular screen in each one ml of reaction liquid.

Description

technical field [0001] The present invention relates to the preparation method of tert-butyl hydroperoxide. More specifically, it is about the method for preparing tert-butyl hydroperoxide with titanium-silicon molecular sieve as catalyst and tert-butyl alcohol as raw material. Background technique [0002] Tertiary butyl hydroperoxide (tertiary butyl hydroperoxide, referred to as TBHP), mainly used in vinyl monomer polymerization initiator, thermosetting polyester resin curing agent, can also be used to manufacture di-tertiary butyl peroxide, later Or it can be used to improve the cetane number of diesel. [0003] According to literature reports, TBHP is made by isobutane and oxygen through liquid phase reaction, and the product that generates simultaneously also has tert-butanol (US2,845,461, US3,478,108, US3,816,540, US3,907,902, US4,404,406, US4,408,081, US5,196,597, etc.). [0004] According to the article "Development and Application of Tert-Butyl Alcohol" on the 33...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/04
Inventor 林民刘郁东朱斌郑金玉汝迎春焦永东
Owner CHINA PETROLEUM & CHEM CORP
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