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Method for synthesizing cyclohexylbenzene by hydroalkylation

A cyclohexylbenzene, chemical synthesis technology, applied in the directions of hydrocarbons, hydrocarbons, chemical instruments and methods, can solve the problems of poor cyclohexylbenzene selectivity, low catalyst activity, etc., to reduce the oligomerization reaction and improve the reaction. The effect of stability and inhibition of carbon deposition

Active Publication Date: 2019-06-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is the problem of low catalyst activity and poor selectivity of cyclohexylbenzene in the prior art, and a new method for synthesizing cyclohexylbenzene by hydroalkylation is provided

Method used

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  • Method for synthesizing cyclohexylbenzene by hydroalkylation
  • Method for synthesizing cyclohexylbenzene by hydroalkylation
  • Method for synthesizing cyclohexylbenzene by hydroalkylation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Dissolve 3.0g of aluminum oxide in 450g of water, add 16.0g of sodium hydroxide to dissolve it, then add 34.7g of hexamethyleneimine while stirring, then add 60g of solid silicon oxide, dimethyldiethoxy Silane 5.9g, the material ratio (mol ratio) of reactant is:

[0035] SiO 2 / Al 2 o 3 =30

[0036] NaOH / SiO 2 =0.2

[0037] Dimethyldiethoxysilane / SiO 2 =0.04

[0038] Hexamethyleneimine / SiO 2 =0.35

[0039] h 2 O / SiO 2 =25

[0040] After the reaction mixture was evenly stirred, it was transferred to a stainless steel reaction kettle, and crystallized at 145° C. for 70 hours while stirring. After taking out, it is filtered, washed and dried. SiO was obtained by chemical analysis 2 / Al 2 o 3 The molar ratio was 30.1.

[0041] After drying the sample was determined, its Si 29 The NMR solid-state nuclear magnetic spectrum peak appears at -18.9ppm. Its X-ray diffraction data are shown in Table 1.

[0042] Table 1

[0043]

[0044] Prepare the mixed sol...

Embodiment 2

[0046] The organosilicon microporous zeolite was prepared according to the method of [Example 1]. Prepare the mixed solution of 40ml ruthenium chloride and ferric nitrate, the content of Ru is 0.25g in the solution, Fe(NO 3 ) 3 The content is 0.30g, and the molar ratio of Ru and Fe is 2. Take 32.50 g of organosilicon microporous zeolite powder samples, and spray the prepared mixed solution on the powder, stirring the organosilicon microporous zeolite continuously during the spraying process. After drying at normal temperature and pressure for 10 hours, dry at 120° C. for 10 hours, and grind into powder. Add 17.50g of alumina for mixing, and add dilute nitric acid solution for kneading and extruding into strips of φ1.6×2mm. After drying, it was calcined at 550° C. for 5 hours, then exchanged 5 times with 1M ammonium nitrate, filtered, and dried. Dry at 120°C for 12 hours and calcined at 480°C for 6 hours to prepare the desired catalyst and name it Ru-Fe / MP. Wherein, by wei...

Embodiment 3

[0048] The organosilicon microporous zeolite was prepared according to the method of [Example 1]. Prepare the mixed solution of 40ml ruthenium chloride and copper nitrate, the content of Ru is 0.25g in the solution, Cu(NO 3 ) 2 The content of is 0.23g, and the molar ratio of Ru and Cu is 2. Take 32.50 g of organosilicon microporous zeolite powder samples, and spray the prepared mixed solution on the powder, stirring the organosilicon microporous zeolite continuously during the spraying process. After drying at normal temperature and pressure for 10 hours, dry at 120° C. for 10 hours, and grind into powder. Add 17.50g of alumina for mixing, and add dilute nitric acid solution for kneading and extruding into strips of φ1.6×2mm. After drying, it was calcined at 550° C. for 5 hours, then exchanged 5 times with 1M ammonium nitrate, filtered, and dried. Dry at 120°C for 12 hours and calcined at 480°C for 6 hours to prepare the desired catalyst and name it Ru-Cu / MP. Wherein, by ...

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Abstract

The invention relates to a method for compounding phenylcyclohexane through hydroalkylation. The problems of low catalyst activity and poor phenylcyclohexane selectivity which are existing in the prior art are mainly solved. The method comprises the steps that benzene and hydrogen make contact with a catalyst for compounding the phenylcyclohexane under effective reaction conditions; and the catalyst comprises, by weight, 0.05-5% of precious metal active component, 0.05-10% of transition metal auxiliary active component, 40-85% of organic silicon micropore zeolite and 10-50% of binding agent. Through the technical scheme adopting the method, the problems are well solved, and the method for compounding the phenylcyclohexane through hydroalkylation can be applied to industrial production of the phenylcyclohexane.

Description

technical field [0001] The invention relates to a method for synthesizing cyclohexylbenzene by hydroalkylation. Background technique [0002] Cyclohexylbenzene is an important fine chemical intermediate. It has a high boiling point and a freezing point near room temperature, and has special physical and chemical properties. As an additive in lithium-ion battery electrolyte, cyclohexylbenzene has anti-overcharge performance and can improve the safety performance of the battery, so it has been widely used in the battery industry. In addition, cyclohexylbenzene can also be used to synthesize liquid crystal materials. [0003] The peroxidation reaction of cyclohexylbenzene can produce phenol and cyclohexanone. Phenol plays an important role as an important product in the chemical industry. At present, industrial production mainly adopts the peroxidation reaction of cumene to prepare phenol, but a large amount of acetone is by-produced in the reaction process. Compared with ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C13/28C07C2/66B01J29/068B01J29/072
CPCY02P20/52
Inventor 王高伟魏一伦方华顾瑞芳高焕新
Owner CHINA PETROLEUM & CHEM CORP