Di-tert-butyl peroxide synthesis method

A technology of di-tert-butyl peroxide and synthesis method, which is applied to the preparation of peroxide compounds, chemical instruments and methods, and the preparation of organic compounds, which can solve the problems of increased side reactions, etc., to solve the problem of temperature out of control and reduce the risk of reaction performance, to achieve the effect of segmented temperature control

Active Publication Date: 2019-09-06
LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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  • Abstract
  • Description
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Problems solved by technology

[0007] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a synthesis method of di-tert-butyl peroxide. Compared with the traditional tank reactor, the heat and mass transfer efficiency of the present invention is extremely high, and the staged temperature control is realized. , accurately control the temperature of different reaction sections, realize the optimal heat exchange control scheme, solve the problem of product decomposition caused by temperature out of control and increase in side reactions, reduce energy cost and risk factor at the same time; adopt the synthesis method described in the present invention , the reaction conversion rate is above 99.3%, and the selectivity is above 99.0%.

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  • Di-tert-butyl peroxide synthesis method

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Embodiment 1

[0033] A kind of synthetic method of di-tert-butyl peroxide, comprises the following steps:

[0034] (1) tert-butanol and concentration are 98% vitriol oil mixed in the first microchannel continuous flow reactor, the internal diameter size of the first microchannel continuous flow reactor is 1mm, and length is 5m, and temperature is 20 ℃, reaction time 1min;

[0035] (2) the material that step (1) obtains and concentration are the hydrogen peroxide mixed reaction of 50% in the second microchannel continuous flow reactor, and the time of mixed reaction is 4min; Tertiary butanol, the vitriol oil, hydrogen peroxide The molar ratio is: 1:1.05:0.55, the inner diameter of the second microchannel continuous flow reactor is 1mm, and it is composed of 10 microchannel mixer substrates connected, and the length of each microchannel mixer substrate is 4m , where the temperature of the first three pieces is controlled at 50°C, the temperature of the last one is controlled at 55°C, and the...

Embodiment 2

[0038] A kind of synthetic method of di-tert-butyl peroxide, comprises the following steps:

[0039] (1) the vitriol oil that tert-butanol and concentration are 98% is mixed in the first microchannel continuous flow reactor, and the internal diameter size of the first microchannel continuous flow reactor is 2mm, and length is 3m, and temperature is 15 ℃, reaction time 1min;

[0040] (2) the material that step (1) obtains and concentration are the hydrogen peroxide mixed reaction of 40% in the second microchannel continuous flow reactor, and the time of mixed reaction is 3min; Tertiary butanol, the vitriol oil, hydrogen peroxide The molar ratio is: 1:1.1:0.57, the inner diameter of the second microchannel continuous flow reactor is 2mm, and it is composed of 8 microchannel mixer substrates connected, and the length of each microchannel mixer substrate is 5m , where the temperature of the first two pieces is controlled at 48°C, the temperature of the last one is controlled at 5...

Embodiment 3

[0043] A kind of synthetic method of di-tert-butyl peroxide, comprises the following steps:

[0044] (1) the vitriol oil that tert-butanol and concentration are 90% is mixed in the first microchannel continuous flow reactor, and the internal diameter size of the first microchannel continuous flow reactor is 0.5mm, and length is 5m, and temperature is 25 ℃, reacts The time is 0.8min;

[0045] (2) the material that step (1) obtains and concentration are the hydrogen peroxide mixed reaction of 60% in the second microchannel continuous flow reactor, and the time of mixed reaction is 5min; Tertiary butanol, the vitriol oil, hydrogen peroxide The molar ratio is: 1:0.95:0.48, the inner diameter of the second microchannel continuous flow reactor is 0.5mm, and is composed of 12 microchannel mixer substrates connected, and the length of each microchannel mixer substrate is 3m, where the temperature of the first two pieces is controlled at 48°C, the temperature of the last one is contro...

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Abstract

The invention belongs to the technical field of chemistry and chemical industry, and particularly relates to a di-tert-butyl peroxide synthesis method, which comprises: mixing tert-butanol and concentrated sulfuric acid in a first micro-channel continuous flow reactor, and carrying out a mixing reaction on the obtained product and hydrogen peroxide in a second micro-channel continuous flow reactor, wherein the temperature of the first micro-channel continuous flow reactor is 10-25 DEG C, the second micro-channel continuous flow reactor is formed by connecting 8-12 micro-channel mixer substrates, and the temperature of the second micro-channel continuous flow reactor is controlled at 45-65 DEG C. According to the present invention, the method has characteristics of extremely high heat transfer and mass transfer efficiency, segmental temperature control, energy consumption cost reducing and risk coefficient reducing, and can solve the product decomposition problem caused by temperature control loss and side reaction increasing; and by using the synthesis method, the reaction conversion rate is more than 99.3%, and the selectivity is more than 99.0%.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a synthesis method of di-tert-butyl peroxide. Background technique [0002] Di-tert-butyl peroxide, also known as initiator A, vulcanizing agent DTBP, is a colorless to slightly yellow transparent liquid, insoluble in water, miscible with benzene, toluene, acetone and other organic solvents, and has strong oxidizing properties. Flammable, relatively stable at room temperature, not sensitive to impact, and one of the most stable organic peroxides. At room temperature, its properties do not change for a long time, and its vapor forms explosive mixtures with air. [0003] The traditional production process is mostly batch reaction, using tert-butanol as raw material, reacting with hydrogen peroxide under the action of sulfuric acid to generate tert-butyl hydroperoxide, which can be obtained by further reacting with tert-butanol. The existing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/16C07C407/00B01J19/00
CPCB01J19/0093C07C407/00C07C409/16
Inventor 陈唐建翟志强崔黎明
Owner LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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