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

A technology of epoxy cyclohexane and dimethyl benzyl alcohol, which is applied in the field of co-production 1, can solve the problems of affecting the normal progress of the reaction, pollution of the production process, and affecting the reaction efficiency, so as to reduce acidity, improve product quality, and enhance hydrophobicity. sexual effect

Active Publication Date: 2013-10-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] 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 serious pollution in the production process, poor product quality, high production cost, and The accumulation of cyclohexane in the raw material in the system affects the reaction efficiency and the normal progress of the reaction, and provides a new co-production of 1,2-epoxycyclohexane, α,α-dimethylbenzyl alcohol and cyclohexane Methods

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 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. 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.

[0030] In the reactor, add 8.0kgTiCl 4 100L of cumene sol...

Embodiment 2

[0033] 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 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.

[0034] In another reactor, add 100L cumene solution containing 3.0kg1,1,3,3-tetramethyldisilazane, add 20.0kg of the catalyst precursor prepared above into the reactor, stir and reflux , the temperature was raised to 150°C, and the reaction was carried out at this temperature for 4h. Then, at this temp...

Embodiment 3

[0036] 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 producing 1,2-epoxy cyclohexane, alpha, alpha-dimethyl benzyl alcohol and cyclohexane. 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 and the problems that the accumulated cyclohexane in the raw material affects the reaction efficiency and affects normal reaction. 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 isoxidized into the 1,2-epoxy cyclohexane; and meanwhile, the cyclohexane and the cyclohexene are efficiently separated by adopting an extractive rectification technology. 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, the alpha, alpha-dimethyl benzyl alcohol and the cyclohexane.

Description

technical field [0001] The invention relates to a method for co-producing 1,2-epoxycyclohexane, α,α-dimethylbenzyl alcohol and cyclohexane. 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 pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/04C07D301/19C07C33/20C07C29/132C07C13/18C07C7/08
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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