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Simultaneous preparation of 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol

A technology of dimethylbenzyl alcohol and epoxy cyclohexane, applied in the field of simultaneous preparation, can solve the problems of poor product quality, production process pollution, and high production costs, and achieve the advantages of good product quality, high product purity, and reduced acidity. Effect

Inactive Publication Date: 2011-12-28
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 , providing a new method for the simultaneous preparation of 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol

Method used

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  • Simultaneous preparation of 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol

Examples

Experimental program
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Effect test

Embodiment 1

[0018] With stirring at room temperature, 15.0 g hexadecylamine was added to 80 ml H 2 O. In a mixed solution of 60ml ethanol and 5ml (1mol / L) hydrochloric acid, stir until the solution is one phase. 65.0 g of ethyl orthosilicate dissolved in 30 ml of ethanol and 4.0 g of tetrabutyl titanate dissolved in 10 ml of ethanol were simultaneously added to the above mixed solution, stirred for 30 min and then crystallized for 24 h. The resulting solid was then filtered and washed with water. The washed material was dried at 110° C. for 12 hours, and then calcined at 600° C. for 4 hours to obtain the Ti-HMS catalyst precursor.

[0019]In a 100ml three-necked flask, add 50ml cumene solution containing 4.0g hexamethyldisilazane, add 10.0g of the catalyst precursor prepared above into the flask, and under rapid stirring and reflux, raise the temperature to 150 ℃, and reacted at this temperature for 4h. Then, at this temperature, the remaining hexamethyldisilazane and cumene solvents w...

Embodiment 2

[0021] Prepare the Ti-HMS catalyst precursor according to the method of [Example 1], and carry out silanization treatment to it, except that the silylating agent is 1,1,3,3-tetramethyldisilazane, and its consumption is 2.5g , wherein the weight content of titanium is 2.3%. XRD,N 2 The results of adsorption, FT-IR, UV-Vis characterization and elemental analysis show that the material has typical HMS structure characteristics and Ti has entered the framework to form four-coordinated active titanium.

Embodiment 3

[0023] The Ti-HMS catalyst precursor was prepared according to the method of [Example 1], except that it was not subjected to silanization treatment, wherein the weight content of titanium was 2.5%. XRD,N 2 The results of adsorption, FT-IR, UV-Vis characterization and elemental analysis show that the material has typical HMS structure characteristics and Ti has entered the framework to form four-coordinated active titanium.

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Abstract

The invention relates to a method for simultaneously preparing 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol, which mainly solves the problem of separately producing 1,2-epoxycyclohexane and α,α in the prior art -When dimethyl benzyl alcohol, there are the problems of serious pollution of the production process, poor product quality and high production cost. In the present invention, cyclohexene and cumene hydroperoxide are used as raw materials, and a non-polar organic compound that is inert to the reaction system is used as a solvent, under mild reaction conditions, on a titanium-containing porous silica catalyst A redox reaction between cumene hydroperoxide and cyclohexene, in which cumene hydroperoxide is reduced to α,α-dimethylbenzyl alcohol, while cyclohexene is oxidized to 1,2-epoxy The technical scheme of cyclohexane solves this problem well, and can be used in the industrial production of simultaneously preparing 1,2-epoxycyclohexane and α,α-dimethylbenzyl alcohol.

Description

technical field [0001] The invention relates to a method for simultaneously preparing 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 prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/04C07D301/19C07C33/20C07C29/132B01J31/38
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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