Method for preparing methyl cyclohexanecarboxylate from methyl benzoate through hydrogenation reaction

A technology of methyl benzoate and cyclohexanecarboxylic acid, which is applied in the field of producing methyl cyclohexanecarboxylate through the hydrogenation reaction of methyl benzoate, can solve the problems of catalyst loss, achieve reduced production costs, good loss resistance, and low price Effect

Inactive Publication Date: 2017-04-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

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Problems solved by technology

However, under this reaction condition, the corrosiveness of benzoic acid and cyclohexanecarboxylic acid is enhanced, and the device must be made of corrosion-resistant alloy steel, and the catalyst is easy to lose

Method used

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  • Method for preparing methyl cyclohexanecarboxylate from methyl benzoate through hydrogenation reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Embodiment 1 Catalyst preparation:

[0022] After the activated carbon carrier was ground and sieved to 100 meshes, it was placed in an oven at 120°C and dried overnight; an equal volume impregnation method was used to prepare a 1.5 mg / ml ruthenium trichloride precursor impregnating solution equivalent to the saturated water absorption of the carrier, and stirred The carrier was added to make it evenly mixed. After ultrasonic treatment, it was left to stand for 24 hours, and then dried overnight in an oven at 110°C. The loading amount of Ru is 5 wt.%.

Embodiment 2

[0023] The preparation of embodiment 2 methyl benzoate:

[0024] 0.25 g of the Ru / C catalyst prepared in Example 1 was weighed and placed in a tube furnace for hydrogen reduction at a reduction temperature of 350° C. and a reduction time of 3 h. Add the reduced catalyst, 4g of methyl benzoate, and 20ml of methanol into the reaction kettle, and stir to disperse evenly. Seal the reactor, replace the air with hydrogen gas and heat it to 120°C, then flush with 3MPa hydrogen gas and keep it warm for 3h. After the reaction, the reaction kettle was taken out, cooled to room temperature, opened after the pressure was reduced, and the liquid product was taken out and analyzed by chromatography. Analysis results showed that the conversion rate of methyl benzoate was 65%, and the product selectivity was 94%.

Embodiment 3

[0026] According to the method in Example 1, the activated carbon carrier is replaced by SiO 2 Support, preparation of Ru / SiO 2 . Then weigh 0.25g of the prepared Ru / SiO 2 The catalyst was reduced with hydrogen, the reduction temperature was 400°C, and the reduction time was 3h. Add the reduced catalyst, 4g of methyl benzoate, and 30ml of methanol into the reaction kettle, and stir to disperse evenly. Seal the reactor, replace the air with hydrogen gas and heat it to 120°C, then flush with 3MPa hydrogen gas and keep it warm for 2h. After the reaction, the reaction kettle was taken out, cooled to room temperature, opened after the pressure was reduced, and the liquid product was taken out and analyzed by chromatography. Analysis results show that the conversion rate of methyl benzoate is 96%, and the product selectivity is >95%.

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Abstract

The invention discloses a method for preparing methyl cyclohexanecarboxylate from methyl benzoate through hydrogenation reaction. The methyl cyclohexanecarboxylate is an important organic synthesis intermediate and medical intermediate. A loading ruthenium-based catalyst is used, a methyl benzoate methanol solution is used as a reaction material, the reaction temperature ranges from 50 DEG C to 150 DEG C, the reaction pressure ranges from 0.5 MPa to 5 MPa, the reaction time is between 0.5 h and 5 h, the methyl benzoate conversion rate can reach 95%, the methyl cyclohexanecarboxylate selectivity can reach 96%, the production separation purity is larger than 99%, and the catalyst can be circularly and repeatedly used.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing methyl cyclohexanecarboxylate through the hydrogenation reaction of methyl benzoate. Background technique [0002] Cyclohexanecarboxylic acid is an important organic chemical raw material and intermediate of synthetic drugs, and has good application value in the research and development of new materials and drugs. It is an important raw material for the synthesis of cyclohexanoyl chloride ring, and cyclohexanoyl chloride is an important synthetic intermediate of photoinitiator 184 and praziquantel. In addition, cyclohexanecarboxylic acid is an important intermediate for the preparation of caprolactam by the toluene method. Caprolactam (CPL) is one of the important organic chemical raw materials. It is mainly used in the production of nylon 6 engineering plastics and synthetic fibers (nylon), and has excellent thermal stability. properties, processability, ...

Claims

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Application Information

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IPC IPC(8): C07C69/75C07C67/303
CPCC07C67/303C07C69/75
Inventor 于维强徐杰黄倩倩孙志强高进苗虹路芳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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