Production method of di(tert-butylperoxy)ketal

A technology of tert-butyl peroxyl and tert-butyl hydroperoxide, which is applied in the field of bisketal production, can solve the problems of low product content, unsafe production, severe side reactions, etc., and achieve high product content and safe production High performance and smooth response

Active Publication Date: 2012-02-01
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is that there are severe side reactions in the prior art, resulting in low product content, low yield, dark color, and unsafe production. A new bis(tert-butyl peroxy) ketal is provided production method

Method used

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  • Production method of di(tert-butylperoxy)ketal

Examples

Experimental program
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Effect test

Embodiment 1～17

[0014] Preparation of 1,1-bis(tert-butylperoxy)cyclohexane (BPC)

[0015] Under normal pressure, add the solvent, cyclohexanone R1 and tert-butyl hydroperoxide R2 into a reaction kettle equipped with an electric stirrer, a thermometer, and a reflux condenser. Start the stirring, add the catalyst, and react for 4 hours to obtain the BPC reaction solution. After alkali washing and water washing, a neutral reaction solution is obtained, and a colorless liquid is obtained by vacuum distillation, which is the BPC product. The proportioning of each raw material, the composition, content, adding method of catalyst, the kind of solvent, consumption, reaction temperature, reaction time and content, yield of product, see Table 1 specifically.

Embodiment 18～34

[0019] Preparation of 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane (BPMC)

[0020] Under normal pressure, add the solvent, 3,3,5-trimethylcyclohexanone R1 and tert-butyl hydroperoxide R2 into a reaction kettle equipped with an electric stirrer, a thermometer and a reflux condenser. Start stirring, add the catalyst, and react for 4 hours to obtain the BPMC reaction liquid. After alkali washing and water washing, a neutral reaction solution is obtained, and a colorless liquid is obtained through vacuum distillation, which is the BPMC product. The proportioning of each raw material, the composition, content, adding method of the catalyst, the type and amount of the solvent, the reaction temperature and the reaction time are specifically shown in Table 2.

Embodiment 35～51

[0024] Preparation of n-butyl 4,4-bis(tert-butylperoxy)valerate (BBPV)

[0025]Under normal pressure, add the solvent, butyl levulinate R1 and tert-butyl hydroperoxide R2 into a reaction kettle equipped with an electric stirrer, a thermometer, and a reflux condenser. Start the stirring, add the catalyst, and react for 4 hours to obtain the BBPV reaction solution. After alkali washing and water washing, a neutral reaction solution is obtained, and a colorless liquid is obtained by vacuum distillation, which is the BBPV product. The proportioning of each raw material, the composition, content and adding method of the catalyst, the type and amount of the solvent, the reaction temperature and the reaction time are specifically shown in Table 3.

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Abstract

The invention relates to a production method of di(tert-butylperoxy)ketal, and mainly solves the problems of low product content, low yield, deep color and low production safety caused by violent side reaction in the previous technique. In the invention, R1 selected from cyclohexanone, 3,3,5-trimethylcyclohexanone or butyl levulinate and R2 tert-butyl hydroperoxide, which are used as raw materials, react in the presence of solvent at -20-40 DEG C under normal pressure for 0.5-10 hours to obtain the corresponding product 1,1-di(tert-butylperoxy)cyclohexane, 1,1-di(tert-butylperoxy)-3,3,5-trimethylcyclohexanone or 4,4,-di(tert-butylperoxy)-n-butyl valerate, wherein the mol ratio of R2 to R1 is (2-10):1, the weight ratio of solvent to R1 is (0.01-0.50):1, and the amount of the solvent accounts for 20-80% of the total weight of the reactants R1 and R2; and the catalyst is selected from at least one of sulfuric acid, phosphoric acid, hydrochloric acid, perchloric acid, p-methylbenzenesulfonic acid, nitric acid or acetic acid. The technical scheme provided by the invention solves the problems in the previous technique, and can be used for industrial production of di(tert-butylperoxy)ketal.

Description

technical field [0001] The invention relates to a production method of bis(tert-butyl peroxy) ketal. Background technique [0002] Organic peroxide crosslinking agent is an important auxiliary agent for organic polymers, which can convert linear or slightly branched organic polymer chains into three-dimensional network structures to limit the gap between polymer chains. And the relative movement between the internal segments of the polymer chain, thereby improving some properties of the organic polymer. Some organic high molecular polymers can significantly improve heat resistance, oil resistance, wear resistance, mechanical strength and other properties after cross-linking; and some organic high molecular polymers, such as rubber, must be cross-linked to have practical use value. [0003] The commonly used organic peroxide crosslinking agent is dicumyl peroxide (DCP for short), but when using this peroxide as a crosslinking agent, acetophenone with an unpleasant smell will...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/22C07C407/00
Inventor 谭永生崔敏华徐裕陆乔年万浥尘徐卫民冯娟利
Owner CHINA PETROCHEMICAL CORP
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