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Preparation method of 1, 1-bis (tert-butylperoxy) cyclohexane

A technology of tert-butyl peroxy and tert-butyl hydroperoxide, which is applied in the field of synthesis and preparation of 1,1-bicyclohexane, can solve the problems of poor stability, potential safety hazards, yellowish color and the like, and achieves improved stability. , the effect of improving yield and fast reaction speed

Pending Publication Date: 2022-02-08
SHANDONG YANGGU HUATAI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the 1,1-bis(tert-butylperoxy)cyclohexane obtained by the above-mentioned traditional method has yellowish color, poor stability, easy decomposition, low yield, and certain potential safety hazards during production

Method used

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preparation example Construction

[0031] The application provides a method for preparing 1,1-bis(tert-butylperoxy)cyclohexane, comprising the following steps in sequence:

[0032] 1) Mix tert-butyl hydroperoxide aqueous solution, phlegmatizer, solid acid and phase transfer catalyst and use an emulsifier to disperse evenly, and obtain intermediate liquid A after mixing and dispersing evenly;

[0033] 2) Add cyclohexanone dropwise to the intermediate liquid A in the reaction kettle, and in the presence of solid acid, cyclohexanone and tert-butyl hydroperoxide chemically react to generate 1,1-bis(tert-butyl peroxy ) cyclohexane, obtain intermediate liquid B after reaction is completed;

[0034] 3) filtering the intermediate liquid B prepared in step 2), removing the solid acid by filtering, and leaving the filtrate;

[0035] 4) Transfer the filtrate obtained in step 3) to a separatory funnel, and use a separatory funnel to separate the liquid. After the liquid separation is completed, the upper layer obtained is...

Embodiment 1

[0055] A kind of preparation method of 1,1-bis(tert-butylperoxy)cyclohexane, comprises the following steps carried out in sequence:

[0056] 1) 578g (concentration is 70%) of tert-butyl hydroperoxide aqueous solution, 478g of liquid paraffin, 10g of strong acid type cation exchange resin D001 and 0.6g of sodium dodecylsulfonate are mixed and dispersed evenly using an emulsifier , the intermediate liquid A is obtained after mixing and dispersing evenly;

[0057] 2) 200g of cyclohexanone is added dropwise to the intermediate liquid A in the reactor at a rate of 5mL / min. In the presence of solid acid, cyclohexanone and tert-butyl hydroperoxide undergo a chemical reaction to generate 1,1 -bis(tert-butylperoxy)cyclohexane, the reaction temperature is controlled at 45-50°C, the reaction time is 45min, and intermediate liquid B is obtained after the reaction is completed;

[0058] 3) Filter the intermediate liquid B obtained in step 2), filter and remove the strong acid type cation ...

Embodiment 2

[0063] A kind of preparation method of 1,1-bis(tert-butylperoxy)cyclohexane, comprises the following steps carried out in sequence:

[0064] 1) 766g (concentration is 75%) of tert-butyl hydroperoxide aqueous solution, 597g of liquid paraffin, 15g of strong acid type cation exchange resin D001 and 1.25g of sodium dodecylsulfonate are mixed and dispersed evenly using an emulsifier , the intermediate liquid A is obtained after mixing and dispersing evenly;

[0065] 2) 250g of cyclohexanone is added dropwise to the intermediate liquid A in the reactor, the rate of addition is 7mL / min, and in the presence of solid acid, cyclohexanone and tert-butyl hydroperoxide undergo a chemical reaction to generate 1,1 -bis(tert-butylperoxy)cyclohexane, the reaction temperature is controlled at 55-60°C, the reaction time is 30min, and intermediate liquid B is obtained after the reaction is completed;

[0066] 3) Filter the intermediate liquid B obtained in step 2), filter and remove the strong ...

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Abstract

The invention provides a preparation method of 1, 1-bis (tert-butylperoxy) cyclohexane, which comprises the following steps: mixing tert-butyl hydroperoxide, a desensitizer, solid acid and a phase transfer catalyst, then adding cyclohexanone, in the presence of the solid acid, carrying out chemical reaction on the cyclohexanone and the tert-butyl hydroperoxide to generate the 1, 1-bis (tert-butylperoxy) cyclohexane, then filtering, and then carrying out liquid separation treatment on the filtrate, and then sequentially carrying out alkali washing, water washing and drying to obtain the finished product 1, 1-bis (tert-butylperoxy) cyclohexane after drying is completed. According to the method, the reaction time is short, the product yield is increased, the yield is 85%-95%, dangerous factors in the production process are reduced, the product stability is improved, the product is a colorless transparent solution, wastewater generated in the production process is easy to treat, and industrial production is easy.

Description

technical field [0001] The invention relates to the technical field of synthesis and preparation of 1,1-bis(tert-butylperoxy)cyclohexane, in particular to a preparation method of 1,1-bis(tert-butylperoxy)cyclohexane. Background technique [0002] 1,1-bis(tert-butylperoxy)cyclohexane, referred to as CH, is a ketal organic peroxide, which is mainly used in PS initiators, unsaturated resin curing agents, and polyethylene crosslinking agents. The preparation of organic peroxides has experienced a history of more than 100 years since benzoyl peroxide (BPO) was synthesized in 1858. At present, there are more than 70 varieties of organic peroxides that have been industrialized abroad. At present, due to various reasons such as the rapid development of the downstream polymer material industry and the support of national industrial policies, the demand for organic peroxides continues to increase. The development and research of new production processes for organic peroxides has beco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/18
CPCC07C407/00C07C407/003C07C2601/14C07C409/18
Inventor 李庆朝马振宇李元杰于磊王博玉陈庆兵
Owner SHANDONG YANGGU HUATAI CHEM
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