Preparation method of tert-butyl peroxide

A technology of tert-butyl peroxide and tert-butanol, which is applied in the direction of preparation of peroxy compounds, preparation of organic compounds, chemical instruments and methods, etc., can solve problems such as good recovery effect, many times of recovery, and easy separation of catalysts, etc. Achieve high economic value, less equipment corrosion, and easy separation

Inactive Publication Date: 2015-04-29
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of method that adopts new solid catalyst to prepare TBHP and DTBP for the problem that catalyst in traditional preparation TBHP and DTBP brings, makes The catalyst is easy to separate, the number of recovery times is high, and the recovery effect is good

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] At room temperature, add 7.4g of tert-butanol and 22.7g of 30wt% hydrogen peroxide into a two-neck flask, mix well, add 0.5g of Amberlyst-15, heat to 83°C, stir and reflux for 3h, cool, and transfer to a separating funnel , let stand for 30min, the reaction mixture was divided into two layers, liquid separation, and weighed the quality of oil phase and water phase, respectively 6.0g and 18.2g.

[0012] After chromatographic analysis, it was detected that the content of tert-butyl peroxide in the oil phase was 82.0%, the content of di-tert-butyl peroxide was 10.8%, and the content of tert-butyl peroxide in the water phase was 10.3%.

[0013] After the oil phase was washed with alkali and water, a colorless and transparent oily DTBP solution with a mass fraction of 97.0% was obtained.

Embodiment 2

[0015] At room temperature, add 7.4g of tert-butanol and 16.2g of 30wt% hydrogen peroxide into a two-neck flask, mix well, then add 0.35g of Amberlyst-15, heat to 83°C, stir and reflux for 3h, cool, and transfer to a separating funnel , standing still for 30min, the reaction mixture was divided into two layers, liquid separation, and the quality of the oil phase and the water phase was weighed, which were 5.8g and 14.5g respectively.

[0016] Through chromatographic analysis, it is detected that the content of tert-butyl hydroperoxide in the oil phase is 82.8%, and the content of di-tert-butyl peroxide is 7.8%. The content of tert-butyl hydroperoxide in the aqueous phase is 10.5%.

[0017] After the oil phase was washed with alkali and water, a colorless and transparent oily DTBP solution with a mass fraction of 97.0% was obtained.

Embodiment 3

[0019] At room temperature, add 7.4g of tert-butanol and 16.2g of 30wt% hydrogen peroxide into a two-neck flask, mix well, then add 0.5g of Amberlyst-15, heat the above raw materials to 83°C, stir and reflux for 5h, cool, turn Put it into a separating funnel, let it stand for 30min, the reaction mixture is divided into two layers, separate liquid, weigh the quality of oil phase and water phase, it is 6.2g and 14.8g respectively.

[0020] Through chromatographic analysis, it is detected that the content of tert-butyl peroxide in the oil phase is 80.1%, the content of di-tert-butyl peroxide is 13.0%, and the content of tert-butyl peroxide in the water phase is 10.2%.

[0021] After the oil phase was washed with alkali and water, a colorless and transparent oily DTBP solution with a mass fraction of 97.0% was obtained.

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PUM

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Abstract

The invention provides a method for preparing tert-butyl peroxide by using a heterogeneous catalyst. The method comprises the following steps: by using tert-butyl alcohol and oxydol as raw materials and an acidic ion exchange resin as a catalyst, reacting under reflux, cooling, standing, and separating to obtain an oil phase and a water phase; and washing the oil phase with alkali and water to obtain a di-tert-butyl peroxide solution (DTBP), wherein the oil phase water washing solution and water phase are the tert-butyl hydroperoxide water solution (TBHP). Since the ion exchange resin has the advantages of large pore structure, high acidity and high catalysis efficiency and the large pore structure can not be destroyed in reaction, the catalyst can be easily separated from the reaction product and can be recycled repeatedly, thereby having higher economic value. Besides, no sulfuric acid or any other strong acid is used in the production process, so the method has the advantages of low corrosion to equipment and no environment pollution, and has higher environmental benefit.

Description

technical field [0001] The invention relates to a method for preparing tert-butyl peroxide, in particular to a method for preparing tert-butyl peroxide with a heterogeneous catalyst. Background technique [0002] Organic peroxides can be divided into hydrocarbyl peroxides, percarboxylic acids, acyl peroxides, ester peroxides, ketone peroxides, etc. according to the different functional groups of the substituents. Among them, tert-butyl hydroperoxide ( TBHP) and di-tert-butyl peroxide (DTBP) are the main raw materials and important intermediates in the chemical industry, and are widely used as oxidants, initiators and crosslinking agents. [0003] In the process of producing DTBP and TBHP, scholars at home and abroad have used tert-butanol (TBA) and hydrogen peroxide to prepare under the catalysis of sulfuric acid, phosphoric acid, zeolite, heteropolyacids, etc. The corrosion of equipment is serious, and the cost of waste acid treatment is very high; the catalyst is dissolve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/16C07C409/04C07C407/00
Inventor 査飞王蕊
Owner NORTHWEST NORMAL UNIVERSITY
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