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Method for preparing 1,2-epoxycyclohexane and dicumyl peroxide

A technology for dicumyl peroxide and cumene hydrogen peroxide, which is applied in the preparation of peroxy compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor product quality, high production cost, and production process pollution. Serious problems, to achieve the effect of reducing adsorption, reducing acidity, and good product selectivity

Active Publication Date: 2011-12-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem to be solved by this invention is that prior art produces 1 independently, and when 2-epoxycyclohexane and the necessary raw material α of producing dicumyl peroxide separately, α-dimethyl benzyl alcohol, there is production The problem of serious process pollution, poor product quality and high production cost provides a new method for 1,2-epoxycyclohexane and dicumyl peroxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 30.0kg of fumed silica into 48.0kg of 25wt% tetramethylammonium hydroxide aqueous solution, and continuously stir for 30min to form a solution. Subsequently, the above solution was added to 120.0 L of aqueous solution containing 46.0 kg of cetyltrimethylammonium bromide under stirring to form a transparent solution. Transfer the above mixed solution into a crystallization kettle, add 0.1kg of MCM-41 as a species, and statically crystallize at 100°C for 3 days. The crystallized product was washed and filtered, dried at 100°C for 24 hours, and calcined at 550°C for 6 hours to obtain a catalyst carrier with the structural characteristics of MCM-41. The powder MCM-41 catalyst carrier prepared above was processed into strips with a diameter of 1.5 mm by traditional extrusion molding technology, then dried at 120°C for 12 hours, and calcined at 550°C for 4 hours to obtain the shaped MCM-41 carrier.

[0025] In the reactor, add 8.0kgTiCl 4 100L of cumene solution, the ab...

Embodiment 2

[0028] Add 30.0kg of fumed silica into 48.0kg of 25wt% tetramethylammonium hydroxide aqueous solution, and continuously stir for 30min to form a solution. Subsequently, the above solution was added to 120.0 L of aqueous solution containing 46.0 kg of cetyltrimethylammonium bromide under stirring to form a transparent solution. Slowly add 4.8Kg of tetrabutyl titanate dropwise into the above mixed solution under rapid stirring and continue stirring for 30 min. Transfer the above mixed solution containing silicon and titanium into a crystallization kettle, add 0.1kg Ti-MCM-41 as a seed crystal, and statically crystallize at 100°C for 3 days to obtain the Ti-MCM-41 catalyst precursor.

[0029] In another reaction kettle, add 100L cumene solution containing 5.0kg1,1,3,3-tetramethyldisilazane, add 20.0kg of the catalyst precursor prepared above into the reaction kettle, under stirring and reflux , raise the temperature to 150°C, and react at this temperature for 4h. Then, at this ...

Embodiment 3

[0031] Ti-MCM-41 catalyst was prepared according to the method of [Example 1], except that the catalyst was not silanized. XRD,N 2 Adsorption, FT-IR and UV-Vis characterization and analysis results show that the material has typical MCM-41 structure characteristics and Ti has entered the framework to form four-coordinated active titanium, in which the weight content of titanium is 3.7%.

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Abstract

The invention relates to a method for preparing 1,2-cyclohexene oxide and dicumyl peroxide, and mainly solves the problems that when the 1,2-cyclohexene oxide is independently produced and an essential raw material of the dicumyl peroxide, namely alpha, alpha-dimethyl benzyl alcohol is independently produced, the production processes pollute environment seriously, the quality of products is low, and production cost is high in the prior art. The method comprises the following steps of: a) performing contact reaction of cyclohexene serving as a raw material, dimethylbenzyl hydroperoxide dissolved in a solvent, and a catalyst in an oxidation-reduction reaction device to obtain a material flow I; b) allowing the material flow I to enter a separating column and rectifying and separating to obtain a material flow II on a column top and a material flow III containing alpha, alpha-dimethyl benzyl and dimethylbenzyl hydroperoxide; c) refining the material flow II to obtain a product 1,2-cyclohexene oxide; and d) allowing the material III to enter a condensation reactor, and performing condensation reaction of alpha, alpha-dimethyl benzyl and dimethylbenzyl hydroperoxide at the presence of a condensation agent to obtain a product dicumyl peroxide. The technical scheme solves the problem well and can be used for the industrial production of 1,2-cyclohexene oxide and dicumyl peroxide.

Description

technical field [0001] The invention relates to a method for preparing 1,2-epoxycyclohexane and dicumyl peroxide. Background technique [0002] 1,2-epoxycyclohexane is an important intermediate in organic synthesis, because the epoxy group on its molecular structure is very active, it can react with amines, phenols, alcohols, carboxylic acids, etc. to generate a series of derivatives, It can be widely used in medicine, pesticide, curing agent, plasticizer, diluent, surfactant and other fields. The pesticide clofenac synthesized with 1,2-epoxycyclohexane is a high-efficiency and low-toxicity pesticide and is very popular among farmers. Adipaldehyde synthesized from 1,2-epoxycyclohexane is widely used in oil extraction and tanning. In addition, as a reactive diluent for epoxy resin, it has more advantages in economy and performance. [0003] The main industrial production method of 1,2-epoxycyclohexane is the dichlorohydrin method. This method produces a large amount of ch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/04C07D301/19C07C409/16C07C407/00
Inventor 金国杰高焕新杨洪云陈璐丁琳康陈军
Owner CHINA PETROLEUM & CHEM CORP
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