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Method for producing 1,2-epoxy cyclohexane and alpha, alpha-dimethyl benzyl alcohol

A technology of dimethyl benzyl alcohol and epoxycyclohexane, which is applied in the field of co-production of 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol, can solve the problem of high production cost and production process Pollution, poor product quality and other problems, to achieve the effect of good product quality, high product purity, and reduce adsorption

Active Publication Date: 2014-01-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The technical problem to be solved by the present invention is that in the prior art, when 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol are produced separately, there are problems of serious production process pollution, poor product quality and high production cost , to provide a new co-production method of 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol

Method used

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  • Method for producing 1,2-epoxy cyclohexane and alpha, alpha-dimethyl benzyl alcohol
  • Method for producing 1,2-epoxy cyclohexane and alpha, alpha-dimethyl benzyl alcohol

Examples

Experimental program
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Embodiment 1

[0030] 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 seed crystal, and conduct static crystallization 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.

[0031] In the reactor, add 8.0kgTiCl 4 100L of cumene solution, the above-prepared catalyst support was added into the reaction kettle, under stirring and reflux, the temperature was raised to 150°C, and the reaction was carried out at this temperature for 4h. Then at this temperature, the residual TiCl was ...

Embodiment 2

[0034] 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 4.8 kg of tetrabutyl titanate dropwise into the above mixed solution under rapid stirring and continue stirring for 30 min. Move 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.

[0035] According to the method of [Example 1], the prepared Ti-MCM-41 catalyst precursor is silanized, except that the silylating agent adopts 1,1,3,3-tetramethyldisilazane, and its consumption is 3.0kg , that is, the finished Ti-MCM-41 catalyst product treated with silane is obtained. XRD,N 2 Adso...

Embodiment 3

[0037] 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 4.5%.

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Abstract

The invention relates to a method for producing 1,2-epoxy cyclohexane and alpha, alpha-dimethyl benzyl alcohol. The method mainly solves the problems of serious production process pollution, poor product quality and high production cost when the 1,2-epoxy cyclohexane and the alpha, alpha-dimethyl benzyl alcohol are separately produced in the prior art. Isopropyl benzene hydroperoxide and cyclohexene undergo oxidation-reduction reaction on a titanium-containing porous silicon dioxide catalyst under the mild reaction condition, wherein the isopropyl benzene hydroperoxide is reduced into the alpha, alpha-dimethyl benzyl alcohol, and the cyclohexene is oxidized into the 1,2-epoxy cyclohexane; and meanwhile, by adjusting the molar ratio of the cyclohexene to the isopropyl benzene hydroperoxide in the raw materials, the cyclohexene is totally converted or has little residue in the reaction process. According to the technical scheme, the problems are well solved, and the method can be used for industrial production of producing the 1,2-epoxy cyclohexane and the alpha, alpha-dimethyl benzyl alcohol.

Description

technical field [0001] The invention relates to a co-production method of 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol. 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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/04C07D301/19C07C33/20C07C29/132
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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