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Preparation method of di-tert-butyl peroxide

A technology of di-tertiary peroxide and di-tert-butyl peroxide, which is applied in the field of preparation of di-tertiary peroxide, can solve the problems of high safety risk, long reaction time, strict requirements on feeding temperature, etc. High performance, short reaction time and easy control of reaction conditions

Active Publication Date: 2017-08-18
西安万德能源化学股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] This method has the disadvantages of demanding feeding temperature (-5°C to 0°C), long reaction time (about 4h), and high safety risks. At the same time, the product contains the first step intermediate mono-tert-butyl peroxide impurity, which needs to be separated in the later stage

Method used

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preparation example Construction

[0025] A kind of preparation method of di-tertiary base peroxide, tert-butanol, hydrogen peroxide, catalyzer are introduced in the micro-reaction device in continuous mode, and the total flow velocity that tert-butanol, hydrogen peroxide and catalyzer enters micro-reaction device is 5 ~30mL / min, that is, the sum of the flow rates of tert-butanol, hydrogen peroxide and catalyst is 5~30mL / min, so that tert-butanol and hydrogen peroxide undergo peroxidation reaction, the reaction temperature is 30~60℃, and the time is 26 ~218s, make the stream that comprises di-tert-butyl peroxide, then draw the stream that comprises di-tert-butyl peroxide from the micro-reaction device, separate, wash with water, dry to obtain di-tert-butyl peroxide, Wherein catalyzer is the sulfuric acid that mass concentration is 98%;

[0026] Wherein the molar ratio of tert-butanol to peroxide is 1:2~1:2.2, and the catalyst consumption accounts for 10~20% of the total mass of tert-butanol, hydrogen peroxide a...

Embodiment 1

[0029] Such as figure 1 As shown, tert-butanol, hydrogen peroxide, and sulfuric acid are transported into the micro-mixer B by the first micro-advection pump A1, the second micro-advection pump A2, and the third micro-advection pump A3 (T-shaped stainless steel tee, inner diameter 0.5 mm), uniform mixing reaction, the total feed rate is 5mL / min, the mol ratio of tert-butanol to hydrogen peroxide is 1:2, and the sulfuric acid consumption is 10% of the overall material quality. The length of microreactor C is 10m, placed in thermostat D (30°C), and the reaction residence time is 26s. The material enters the product collector E after fully reacting in the microreactor. After the crude product was separated, washed with water and dried, the peroxide components were analyzed by gas chromatography. The content of di-tert-butyl peroxide was 89.7%, and the content of mono-tert-butyl peroxide was 10.2%. The conversion rate of tert-butanol is 98.1%.

Embodiment 2

[0031] Such as figure 1 As shown, tert-butanol, hydrogen peroxide, and sulfuric acid are transported into the micro-mixer B by the first micro-advection pump A1, the second micro-advection pump A2, and the third micro-advection pump A3 (T-shaped stainless steel tee, inner diameter 0.5 mm), uniform mixing reaction, the total feed rate is 5mL / min, the mol ratio of tert-butanol to hydrogen peroxide is 1:2.02, and the sulfuric acid consumption is 10% of the overall material quality. The length of microreactor C is 10m, placed in thermostat D (30°C), and the reaction residence time is 26s. The material enters the product collector E after fully reacting in the microreactor. After the crude product was separated, washed with water and dried, the peroxide components were analyzed by gas chromatography. The content of di-tert-butyl peroxide was 91.6%, and the content of mono-tert-butyl peroxide was 8.2%. The conversion rate of tert-butanol is 99.3%.

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Abstract

The invention discloses a preparation method of di-tert-butyl peroxide. Tert-butyl alcohol, hydrogen peroxide and a catalyst are continuously introduced into a micro-reactor, so that tert-butyl alcohol and hydrogen peroxide are subjected to a peroxidation reaction, and a material flow containing a di-tert-butyl peroxide is prepared; the material flow containing the di-tert-butyl peroxide is led out from the micro-reactor, and the di-tert-butyl peroxide is obtained through separation, washing and drying, wherein the molar ratio of tert-butyl alcohol to hydrogen peroxide is 1:2-1:2.2, and the catalyst accounts for 10-20% of the total mass of tert-butyl alcohol, hydrogen peroxide and the catalyst. The process is simple, the micro-reactor good in safety is used for continuous production, the prepared di-tert-butyl peroxide is high in reaction selectivity and good in yield, the production procedures are reduced, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of di-tertiary peroxide. Background technique [0002] The O-O bond decomposition activation energy in di-tert-butyl peroxide is very low, and it is easy to decompose into oxygen-containing free radicals or oxygen-containing compounds. It is the initiator of the chain reaction during diesel combustion, which reduces the initial temperature of diesel combustion reaction, thereby It improves the ignition performance of diesel and can be used as an additive to increase the cetane number of diesel. The hydrogen peroxide reaction method is the main method for industrial production of tert-butyl hydroperoxide and di-tert-butyl peroxide, and currently domestic production enterprises all adopt this process for production. It uses 35% hydrogen peroxide mixed with tert-butanol, and uses 70% concentrated sulfuric acid as a catalyst. After several hours of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/16
CPCC07C407/00C07C409/16
Inventor 曹彬
Owner 西安万德能源化学股份有限公司
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