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Method for co-producing 1,2-epoxycyclohexane, α,α-dimethylbenzyl 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: 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

[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 co-producing 1,2-epoxycyclohexane, α,α-dimethylbenzyl alcohol and cyclohexane
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Embodiment 1

[0029] 30.0 kg of fumed silica was added to 48.0 kg of 25 wt% tetramethylammonium hydroxide aqueous solution, and continuously stirred for 30 minutes to form a solution. Subsequently, the above solution was added to a 120.0L aqueous solution containing 46.0kg of cetyltrimethylammonium bromide under stirring to form a transparent solution. Transfer the above mixed solution into a crystallization kettle, add 0.1kg MCM-41 as a seed crystal, and statically crystallize at 100°C for 3 days. The crystallized product is washed and filtered, dried at 100°C for 24 hours, and calcined at 550°C for 6 hours to obtain a catalyst carrier with MCM-41 structural characteristics. The powdered MCM-41 catalyst carrier prepared above is processed into strips with a diameter of 1.5 mm by using traditional extrusion molding technology, and then dried at 120°C for 12 hours and calcined at 550°C for 4 hours to obtain a shaped MCM-41 carrier.

[0030] Add 8.0kg TiCl in the reactor 4 Add the catalyst carr...

Embodiment 2

[0033] 30.0Kg of fumed silica was added to 48.0kg of 25wt% tetramethylammonium hydroxide aqueous solution, and continuously stirred for 30min to form a solution. Subsequently, the above solution was added to a 120.0L aqueous solution containing 46.0kg of cetyltrimethylammonium bromide under stirring to form a transparent solution. Under rapid stirring, slowly drop 4.8Kg of tetrabutyl titanate into the above mixed solution and continue stirring for 30 minutes. The above-mentioned mixed solution containing silicon and titanium was transferred into a crystallization kettle, 0.1kg Ti-MCM-41 was added as a seed crystal, and static crystallization was carried out at 100°C for 3 days to obtain a Ti-MCM-41 catalyst precursor.

[0034] Add 100L cumene solution containing 3.0kg 1,1,3,3-tetramethyldisilazane to another reactor, add 20.0kg of the catalyst precursor prepared above into the reactor, stir and reflux rapidly Then, the temperature was raised to 150°C and reacted at this temperat...

Embodiment 3

[0036] The Ti-MCM-41 catalyst was prepared according to the method of [Example 1], but the catalyst was not subjected to silanization treatment. XRD, N 2 The adsorption, FT-IR and UV-Vis characterization and analysis results show that the material has typical MCM-41 structural characteristics and Ti has entered the framework to form four-coordinate 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 organic synthesis intermediate. Because the epoxy group on its molecular structure is very active, it can react with amines, phenols, alcohols, carboxylic acids, etc. to form a series of derivatives. It can be widely used in medicine, pesticide, curing agent, plasticizer, diluent, surfactant and other fields. The pesticide Kemitte synthesized with 1,2-epoxycyclohexane is a high-efficiency and low-toxic pesticide which is very popular among farmers. Adipaldehyde synthesized from 1,2-epoxycyclohexane is widely used in petroleum exploration and leather making. In addition, as an epoxy resin reactive diluent, 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...

Claims

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Application Information

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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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