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Industrial method for purifying tert-butyl peroxybenzoate

A technology of tert-butyl peroxybenzoate and an industrial method, which is applied in the field of purifying tert-butyl peroxybenzoate, can solve problems such as low conversion rate, influence conversion rate, excessive tert-butyl hydroperoxide, etc., so as to reduce the content , the effect of speeding up the reaction

Pending Publication Date: 2021-11-05
九江前发精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] And make in the tert-butyl peroxybenzoate again, there are many impurities and the conversion rate is low, in the preparation of tert-butyl peroxybenzoate, if the tert-butyl hydroperoxide consumption is too much, the tert-butyl peroxide of impurity can be caused Too much hydrogen, in the final purification, repeated washing is required, and during the reaction, the temperature affects the conversion rate

Method used

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  • Industrial method for purifying tert-butyl peroxybenzoate
  • Industrial method for purifying tert-butyl peroxybenzoate
  • Industrial method for purifying tert-butyl peroxybenzoate

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Embodiment 1

[0028] A kind of industrial method for purifying tert-butyl peroxybenzoate that the present invention proposes comprises the following steps:

[0029] S1. The temperature of the reaction kettle is 15°C, add tert-butyl hydroperoxide and active agent to the reaction kettle and stir for 5 minutes, then pour the sodium hydroxide solution into the reaction kettle and mix and stir, the active agent, tert-butyl hydroperoxide and The mass ratio of sodium hydroxide solution is 1:35:18, and the active agent includes styrene, sodium alkylbenzene sulfonate and saponin with a mass ratio of 1:0.5:1.5. After stirring, the first mixed solution is obtained, and the pH value of the first mixed solution is is 10, the mixing and stirring time is 35min, the first mixed solution is extracted to separate out the sodium salt, and the sodium salt and the filtrate are obtained, the extract is water, or other solutions insoluble in organic liquids, and the mass ratio of the extract to the mixed solution ...

Embodiment 2

[0034] An industrial method for purifying tert-butyl peroxybenzoate, comprising the following steps:

[0035] S1. The temperature of the reaction kettle is 17°C, add tert-butyl hydroperoxide and active agent to the reaction kettle and stir for 7 minutes, then pour the sodium hydroxide solution into the reaction kettle and mix and stir, the active agent, tert-butyl hydroperoxide and The mass ratio of sodium hydroxide solution is 1:42:21, and the active agent includes styrene, sodium alkylbenzene sulfonate and saponin with a mass ratio of 1:0.5:1.5. After stirring, the first mixed solution is obtained, and the pH value of the first mixed solution is is 12, the mixing and stirring time is 43min, the first mixed solution is extracted to separate out the sodium salt, and the sodium salt and the filtrate are obtained, the extract is water, or other solutions insoluble in organic liquids, and the mass ratio of the extract to the mixed solution is 1 :5;

[0036] S2. Add pure water at...

Embodiment 3

[0040] An industrial method for purifying tert-butyl peroxybenzoate, comprising the following steps:

[0041]S1. The temperature of the reaction kettle is 25°C, add tert-butyl hydroperoxide and active agent to the reaction kettle and stir for 9 minutes, then pour the sodium hydroxide solution into the reaction kettle and mix and stir, the active agent, tert-butyl hydroperoxide and The mass ratio of sodium hydroxide solution is 1:55:29, and the active agent includes styrene, sodium alkylbenzene sulfonate and saponin with a mass ratio of 1:0.5:1.5. After stirring, the first mixed solution is obtained, and the pH value of the first mixed solution is is 14, the mixing and stirring time is 55min, the first mixed solution is extracted and separated out sodium salt, and sodium salt and filtrate are obtained;

[0042] S2. Add pure water at -3°C to the sodium salt, and the pure water flows at a flow rate of 0.2cm 3 / h is stirred with sodium salt, and the stirring speed is 15 revolutio...

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Abstract

The invention discloses an industrial method for purifying tert-butyl peroxybenzoate. The industrial method comprises the following steps: S1, adding tert-butyl hydroperoxide and an active agent into a reaction kettle with a temperature of 15-25 DEG C, conducting stirring, pouring a sodium hydroxide solution into the reaction kettle, performing mixing and stirring to obtain a first mixed solution, and extracting the first mixed solution to separate out sodium salt so as to obtain the sodium salt and a filtrate, wherein an extraction solution is ethanol; S2, adding purified water with a temperature of -3 DEG C into the sodium salt, and conducting slow stirring to obtain a pasty mixture; S3, adding a catalyst into benzoyl chloride, conducting stirring to obtain a second mixed solution, dropwise adding the second mixed solution into the pasty mixture through a condensation pipe, and performing stirring to obtain a crude tert-butyl peroxybenzoate product; and S4, washing and separating the tert-butyl peroxybenzoate crude product with sodium carbonate, conducting washing once with a magnesium sulfate solution, and performing drying to obtain the tert-butyl peroxybenzoate. In the preparation of tert-butyl peroxybenzoate in the invention, the content of tert-butyl hydroperoxide is reduced, and the reaction of tert-butyl hydroperoxide and sodium hydroxide is accelerated.

Description

technical field [0001] The invention relates to the technical field of tert-butyl perbenzoate, in particular to an industrial method for purifying tert-butyl perbenzoate. Background technique [0002] Tert-butyl peroxybenzoate is an organic compound with molecular formula C11H14O3, colorless to slightly yellowish liquid. Slightly aromatic. Insoluble in water, soluble in organic solvents. Tert-butyl peroxybenzoate is widely used as an initiator in the polymerization of ethylene, styrene, propylene, vinyl acetate, diallyl phthalate and isobutylene. In the curing process of unsaturated polyester, it is widely used in molding processes such as SMC, BMC, DMC, etc. At the same time, it can also be used in two-component curing systems with higher activity such as MEPK, BPO or TBPO. . Store in a cool, ventilated warehouse. Keep away from fire, heat sources and direct sunlight. Storage temperature should not exceed 30°C. The package is sealed. It should be stored separately f...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/38
CPCC07C407/00C07C409/38
Inventor 茆金年徐立高德亮
Owner 九江前发精细化工有限公司
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