The preparation method of di-tert-butyl peroxide

A technology of peroxidizing di-tert-butyl and tert-butanol, which is applied in the preparation of peroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve waste liquid damage and environment, difficult yield, long reaction process, etc. problems, to achieve the effect of saving raw materials, avoiding damage to the environment and reducing costs

Active Publication Date: 2018-03-20
江苏强盛功能化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition to the long reaction process mentioned by the applicant and the difficult yield to meet the expectations of the industry, this patent solution also has the risk of damage to the environment due to the waste liquid generated during the preparation process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A) Preparation of tert-butyl hydrogen sulfate esterification liquid, the mass % specific concentration of 95% tert-butanol and mass % specific concentration of 60% sulfuric acid is added dropwise to the first reaction device to stir the reaction, tert-butanol The mol ratio to sulfuric acid is 1:0.5, and the temperature and time of the stirring reaction of the first reaction device are respectively controlled at 40° C. and 40 minutes to obtain a tert-butyl hydrogen sulfate esterification liquid;

[0028] B) to prepare the reaction product, first add the reclaimed mother liquor in the second reaction device, then add the thick tert-butyl hydrogen sulfate in the second reaction device and add the tert-butyl hydrogen sulfate esterification solution obtained by step A) in a dropwise manner, and control The temperature of the stirring reaction of the second reaction device is 50°C, and the reaction time is controlled to be 330min to obtain a reaction product, wherein the weigh...

Embodiment 2

[0032]A) Preparation of tert-butyl hydrogen sulfate esterification solution, the mass % specific concentration is 90% tert-butanol and the sulfuric acid of mass % specific concentration 75% is added dropwise in the first reaction device for stirring reaction, tert-butanol The mol ratio to sulfuric acid is 1:0.75, and the temperature and time of the stirring reaction of the first reaction device are respectively controlled at 25° C. and 120 min to obtain tert-butyl hydrogen sulfate esterification solution;

[0033] B) to prepare the reaction product, first add the reclaimed mother liquor in the second reaction device, then add the thick tert-butyl hydrogen sulfate in the second reaction device and add the tert-butyl hydrogen sulfate esterification solution obtained by step A) in a dropwise manner, and control The temperature of the stirring reaction of the second reaction device is 25°C, and the reaction time is controlled as 60min to obtain a reaction product, wherein the weigh...

Embodiment 3

[0037] A) Preparation of tert-butyl hydrogen sulfate esterification solution, the mass % specific concentration is 85% tert-butanol and the sulfuric acid of mass % specific concentration 95% is added dropwise in the first reaction device to stir and react, tert-butanol The mol ratio with sulfuric acid is 1:1, and the temperature and time of the stirring reaction of the first reaction device are respectively controlled at 10° C. and 240 min to obtain tert-butyl hydrogen sulfate esterification liquid;

[0038] B) to prepare the reaction product, first add the reclaimed mother liquor in the second reaction device, then add the thick tert-butyl hydrogen sulfate in the second reaction device and add the tert-butyl hydrogen sulfate esterification solution obtained by step A) in a dropwise manner, and control The temperature of the stirring reaction of the second reaction device is 10 DEG C, and the reaction time is controlled as 220min to obtain a reaction product, wherein the weight...

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Abstract

A method of preparing di-tert-butyl peroxide is disclosed and belongs to the technical field of organic synthesis. The method includes a step of adding tert-butyl alcohol and sulfuric acid into a first reaction device, reacting under stirring, and controlling the temperature and reaction time of the reaction under stirring in the first reaction device to obtain a tert-butyl hydrogen sulfate liquid, a step of adding a recovered mother liquor into a second reaction device, adding crude tert-butyl alcohol and the tert-butyl hydrogen sulfate liquid into the second reaction device, and controlling the temperature and reaction time of a reaction under stirring in the second reaction device to obtain a reaction product, a step of feeding the reaction product to a liquid separating tank, and performing liquid separating to obtain an upper oil phase that is the di-tert-butyl peroxide and a lower water phase that is a mother liquor adopted as a recovery mother liquor for a next turn of reactions. The method is simple and short in process steps, and can allow the content of the di-tert-butyl peroxide in the upper oil phase to be 97.5% or above, thus meeting requirements on industrial scaled-up production. The method avoids environment pollution, saves raw materials, reduces the cost and achieves circular economy.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of di-tert-butyl peroxide. Background technique [0002] The aforementioned di-tert-butyl peroxide is also called "di-tert-butyl peroxide", its English name is: Di-t-butylPeroxide (DTBP for short), and its chemical formula is C 8 h 18 o 2 , the molecular weight is 146.23, the density is D(20°C) 0.794, the melting point is -40°C, the flash point is 9°C, the self-accelerating decomposition temperature is 80°C, and the theoretical active oxygen content is 10.94%. Exploding yellowish transparent liquid. [0003] Di-tert-butyl peroxide is one of the most stable and commonly used varieties of organic peroxide initiators. As a crosslinking agent, it can be used in silicone rubber, synthetic rubber and natural rubber, polyethylene, EVA and EPT, etc. As a polymerization initiator, it can be used for polystyrene and polyethylene. It is also ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C407/00C07C409/04C07C409/16
CPCC07C303/24C07C407/00C07C409/04C07C409/16C07C305/06
Inventor 应志耀陈丹应立顾屹立
Owner 江苏强盛功能化学股份有限公司
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