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Preparation method of 1, 1-bis (tert-butylperoxy)-3, 3, 5-trimethylcyclohexane

A technology of trimethylcyclohexane and tert-butyl peroxy, applied in the field of synthesis and preparation of 1,1-bis-3,3,5 trimethylcyclohexane, which can solve the yellowish color and potential safety hazards , poor stability and other issues, to achieve the effect of fast response, improved stability and reduced sensitivity

Pending Publication Date: 2022-01-04
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] But the color of 1,1-bis(tert-butylperoxy)-3,3,5 trimethylcyclohexane that above-mentioned this traditional method obtains is yellowish, poor in stability, easy to decompose, and yield is low, and There are certain 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)-3,3,5-trimethylcyclohexane, 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 3,3,5 trimethylcyclohexanone dropwise to the intermediate liquid A in the reactor, and in the presence of solid acid, 3,3,5 trimethylcyclohexanone and tert-butyl hydroperoxide A chemical reaction occurs to generate 1,1-bis(tert-butylperoxy)-3,3,5 trimethylcyclohexane, and intermediate liquid B is obtained after the 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 liq...

Embodiment 1

[0055] A preparation method of 1,1-bis(tert-butylperoxy)-3,3,5 trimethylcyclohexane, comprising the following steps carried out in sequence:

[0056] 1) 478g (concentration is 70%) of tert-butyl hydroperoxide aqueous solution, 389g 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) Add 200g of 3,3,5 trimethylcyclohexanone dropwise to the intermediate liquid A in the reactor at a rate of 5mL / min. In the presence of solid acid, 3,3,5 trimethylcyclohexanone The chemical reaction between hexanone and tert-butyl hydroperoxide produces 1,1-bis(tert-butylperoxy)-3,3,5 trimethylcyclohexane, the reaction temperature is controlled at 45-50°C, and the reaction time For 45min, intermediate liquid B was obtained after the reaction was completed;

[0058] 3) Filter the intermediate liquid B obtain...

Embodiment 2

[0063] A preparation method of 1,1-bis(tert-butylperoxy)-3,3,5 trimethylcyclohexane, comprising the following steps carried out in sequence:

[0064] 1) 600g (concentration is 75%) of tert-butyl hydroperoxide aqueous solution, 486g 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) Add 250g of 3,3,5 trimethylcyclohexanone dropwise to the intermediate liquid A in the reactor, the dropping rate is 7mL / min, in the presence of solid acid, 3,3,5 trimethylcyclohexanone Hexanone reacts with tert-butyl hydroperoxide to generate 1,1-bis(tert-butylperoxy)-3,3,5 trimethylcyclohexane, the reaction temperature is controlled at 55-60°C, and the reaction time For 30min, intermediate liquid B was obtained after the reaction was completed;

[0066] 3) Filter the intermediate liquid B obtained in ste...

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Abstract

The invention provides a preparation method of 1, 1-bis (tert-butylperoxy)-3, 3, 5-trimethylcyclohexane, which comprises the following steps of: mixing tert-butyl hydroperoxide, a desensitizer, solid acid and a phase transfer catalyst, then adding 3, 3, 5-trimethylcyclohexanone, carrying out a chemical reaction on 3, 3, 5-trimethylcyclohexanone and tert-butyl hydroperoxide in the presence of the solid acid to generate 1, 1-bis (tert-butylperoxy)-3, 3, 5-trimethylcyclohexane, then filtering, carrying out liquid separation treatment on a filtrate, and sequentially carrying out alkali washing, water washing and drying to obtain a finished product, namely, 1, 1-bis (tert-butylperoxy)-3, 3, 5-trimethylcyclohexane. 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, generated wastewater 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)-3,3,5-trimethylcyclohexane, in particular to a 1,1-bis(tert-butylperoxy) Base)-3,3,5 The preparation method of trimethylcyclohexane. Background technique [0002] 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane, referred to as TMCH, is a ketal organic peroxide, mainly used in PS initiators, unsaturated resins Curing agent, polyethylene crosslinking agent. 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 pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/22
CPCC07C407/00C07C2601/14C07C409/22
Inventor 马振宇李庆朝黄存影胡圣英任才泽刘希霖
Owner SHANDONG YANGGU HUATAI CHEM
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