Cyclohexane ionic liquid catalyst prepared from benzene and hydrogen and preparation method thereof

A technology of ionic liquid and catalyst, which is applied in the field of benzene hydrogenation to cyclohexane ionic liquid catalyst and its preparation, can solve the problems of hidden safety hazards in production and storage, increased operation difficulty, nitrogen oxide pollution, etc., to reduce temperature, Effects of reduced energy consumption and mild reaction conditions

Inactive Publication Date: 2009-12-16
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The production process of supported catalysts produces nitrogen oxides that pollute the air, are expensive, and must be reduced with hydrogen at 400-500°C and cooled before use.
Wastewater is generated during the preparation of Ziegler-Natta catalysts, and the wastewater needs to be purified, and aluminum alkyls are used in the production process of the catalysts, which increases the difficulty of operation and poses safety hazards during production and storage

Method used

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  • Cyclohexane ionic liquid catalyst prepared from benzene and hydrogen and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0020] 1) Take 655mgRuCl 3 ·3H 2 O was added to 50 mL of absolute ethanol, and hydrogen reduction was carried out at 30°C under normal pressure for 46 hours to obtain RuCl 2 ethanol solution, sealed for future use;

[0021] 2) Take 8.210g of N-methylimidazole and 10.183g of n-chlorobutane, add them into a three-necked flask filled with 10mL of ethylbenzene, put them in a constant temperature oil bath, and react for 24h at 106°C and normal pressure. The product was washed with toluene until there was no N-methylimidazole, the detergent was distilled off under reduced pressure, and dried in vacuum at 60°C for 10 h to obtain [BMIM]Cl (16.931 g, yield 96.93%);

[0022] 3) Take the 5mL RuCl prepared in step 1) 2 Ethanol solution and 578mg[BMIM]Cl were placed in a three-necked flask, under normal pressure, N 2 Protected, reacted at 70°C for 6h, distilled under reduced pressure, and dried in vacuo to remove absolute ethanol to obtain the ionic liquid catalyst [BMIM]Cl / [RuCl 2 ],...

Embodiment 2

[0025] 1) Take 65.5mgRuCl 3 ·3H 2 O and 10 mL of absolute ethanol were placed in a high-pressure reactor, and reduced for 30 min at 30 ° C and a hydrogen pressure of 1 Mpa to prepare RuCl 2 ethanol solution, sealed for future use;

[0026] 2) Take 8.210g of N-methylimidazole and 10.183g of n-chlorobutane, add them into a three-necked flask filled with 10mL of ethylbenzene, put them in a constant temperature oil bath, and react for 6h at 106°C and normal pressure. The product was washed with toluene until there was no N-methylimidazole, the detergent was distilled off under reduced pressure, and dried in vacuum at 40°C for 30 hours to obtain [BMIM]Cl (13.427g, yield 76.87%);

[0027] 3) Take the RuCl prepared in step 1) 2 Ethanol solution with 428mg [BMIM]Cl, 300mg ZnCl 2 and 10mL of absolute ethanol, placed in a three-necked flask, under normal pressure, N 2 After protecting and reacting at 78°C for 4 hours, distilling under reduced pressure, and drying in vacuo to remove...

Embodiment 3

[0030] 1) Take 52mgRuCl 3 and 10 mL of absolute ethanol were placed in a high-pressure reactor, and reduced for 20 min at 30 ° C and a hydrogen pressure of 1 Mpa to prepare RuCl 2 ethanol solution, sealed for future use;

[0031] 2) Take 8.210g of N-methylimidazole and 11.11g of n-chlorobutane, add them into a three-necked flask filled with 10mL of ethylbenzene, put them in a constant temperature oil bath, and react for 48h at 88°C and normal pressure. The product was washed with toluene until there was no N-methylimidazole, the detergent was distilled off under reduced pressure, and vacuum-dried at 50°C for 40 h to obtain [BMIM]Cl (13.539 g, yield 77.51%);

[0032] 3) Take the RuCl prepared in step 1) 2 Ethanol solution with 428mg [BMIM]Cl, 300mg ZnCl 2 and 10mL of absolute ethanol, placed in a three-necked flask, under normal pressure, N 2 After protecting and reacting at 78°C for 5.5h, the absolute ethanol was distilled off under reduced pressure to obtain the ionic liq...

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Abstract

The invention relates to a cyclohexane ionic liquid catalyst prepared from benzene and hydrogen and a preparation method thereof, belonging to the development field of industrial catalysts. The prior supported catalyst pollutes the environment during production and has a high price, and the Ziegler catalyst has hidden danger in the production and storage processes. The Cl in the ionic liquid catalyst Cl / is chlorine N-methyl-N-normal-butyl-imidazole and has a molar percentage of 75-99; and the is ruthenous chloride and has a molar percentage of 1-25. The preparation method comprises the following steps: (1), reducing RuCl3 into RuCl2; (2), using N-butyl-imidazole and chloro-normal butane as raw materials and using phenylethane as a solvent to prepare the Cl; and (3), using the Cl and the as raw materials to prepare the Cl / . The catalyst has the advantages of high activity, good selectivity, environment-friendly preparation process, no hidden danger, and the like.

Description

technical field [0001] The invention belongs to the field of industrial catalyst development, in particular to a catalyst for benzene hydrogenation to cyclohexane ionic liquid and a preparation method thereof. Background technique [0002] Cyclohexane is an important organic chemical raw material, which can be used to produce products such as cyclohexanol, cyclohexanone, polycaprolactam and polyhexamethylene adipamide. Excellent solvent, so the production of cyclohexane is becoming more and more important. Industrially, the production methods of cyclohexane are divided into benzene hydrogenation method and fractional distillation and refining method of petroleum hydrocarbon fractions. The benzene hydrogenation method is further divided into liquid phase method and gas phase method. It is widely used because of its high rate and yield. Catalyst is an important factor affecting the conversion rate of benzene hydrogenation to cyclohexane. At present, the commonly used cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/30C07C5/10C07C13/18
CPCY02P20/52
Inventor 王艳辉朱景利张金昌朱周静陆冬润
Owner BEIJING UNIV OF CHEM TECH
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