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Application and preparation method of bimetallic catalyst for synthesizing dimethyl 1,2-cyclohexanedicarboxylate from dimethyl phthalate

A technology of dimethyl cyclohexanedicarboxylate and dimethyl phthalate, which is applied in the field of catalyst preparation, can solve the problems of decreased catalytic activity of the catalyst, uniform dispersion of active components, and inability to give full play to the mutual coordination effect, and the like, Achieving the effect of small mass transfer limit, simple and easy method, enhanced electron transport characteristics and chemical reactivity

Inactive Publication Date: 2021-11-23
RUNTAI CHEM TAIXING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Bimetallic catalysts are usually prepared by co-impregnation or co-precipitation, but these two methods cannot disperse the active components more uniformly, and will make part of the active components be covered inside, and cannot fully develop the bimetallic catalyst. The mutual coordination effect of the two metals in the catalyst leads to a relative decrease in the catalytic activity of the catalyst

Method used

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  • Application and preparation method of bimetallic catalyst for synthesizing dimethyl 1,2-cyclohexanedicarboxylate from dimethyl phthalate
  • Application and preparation method of bimetallic catalyst for synthesizing dimethyl 1,2-cyclohexanedicarboxylate from dimethyl phthalate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of nitrogen-doped carbon nanotube support

[0024] Grind and grind 4g of melamine salt into a porcelain boat, wrap 2g of Fe / SBA-15 molecular sieve catalyst on the melamine, pass in argon, the flow rate of argon is 80ml / min, heat to 650°C and keep it for 1 hour, A black powder was obtained. Then the black powder was soaked with 2mol / L hydrofluoric acid for 4 hours to remove the catalyst, and finally washed with deionized water until neutral, and dried at 70°C to obtain nitrogen-doped carbon nanotubes (N-CNTs).

[0025] (2) Preparation of bimetallic catalysts by galvanic displacement method

[0026] The nitrogen-doped carbon nanotubes prepared in step (1) were dispersed in the nickel chloride solution, and the nickel chloride consumption was calculated as 10% of the mass of the carrier based on nickel, stirred at room temperature for 3 hours, and then added dropwise with KBH under stirring 4 Aqueous solution (the molar ratio of KBH4 to nickel is 4:1), fi...

Embodiment 2

[0030] In embodiment 1, palladium chloride is changed to use ruthenium chloride.

[0031] Nitrogen-doped carbon nanotubes are dispersed in nickel chloride solution, the amount of nickel chloride is calculated as nickel accounts for 10% of the carrier mass, stirred at room temperature for 3 hours, and then KBH is added dropwise under stirring 4 Aqueous solution (KBH 4 The molar ratio to nickel is 4:1), filtered and washed until neutral, then dispersed in deionized water, heated to 100°C, and then added dropwise with ruthenium chloride aqueous solution (the amount of ruthenium chloride is based on the molar ratio of ruthenium to nickel being 2 : 1 calculation), and then stirred for 4 hours to ensure that all ruthenium ions were replaced. After the galvanic couple was replaced, after the slurry was cooled to normal temperature, 4 ml of hydrochloric acid (37% concentration) was added dropwise. Finally, the black solid was filtered out and washed with deionized water until neutra...

Embodiment 3

[0034]In Example 1, the amount of nickel chloride is calculated as nickel accounts for 13% of the mass of the carrier.

[0035] Other operations are the same as in Example 1.

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Abstract

The invention belongs to the field of catalyst preparation, and particularly relates to an application and a preparation method of a bimetallic catalyst for synthesizing dimethyl 1,2-cyclohexanedicarboxylate from dimethyl phthalate. An M-Ni / nitrogen-doped carbon nanotube (M=Ru, Pd) bimetallic catalyst is prepared by taking a nitrogen-doped carbon nanotube as a dispersing agent and a carrier and utilizing a couple replacement method. The catalyst prepared by the method has the advantages of large specific surface area, high mechanical strength, small mass transfer limit, more uniform dispersion of active components on the surface of the carrier and the like; the preparation method is simple and easy to implement, high in operability, available for batch preparation and small in environmental pollution, and the catalyst can be used in a reaction for hydrogenation synthesis of dimethyl 1,2-cyclohexanedicarboxylate from dimethyl phthalate; and the reaction activity of the catalyst and the selectivity of dimethyl 1,2-cyclohexanedicarboxylate are obviously improved.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to the application and preparation method of a bimetallic catalyst for synthesizing 1,2-cyclohexanedicarboxylate from dimethyl phthalate. Background technique [0002] Plasticizers are indispensable additives in the polymer processing industry, which can greatly improve the processability, softness, fluidity and other properties of polymers. At present, more than 80% of plasticizers in the world are phthalates Plasticizers, and recent studies have shown that phthalate plasticizers are difficult to degrade due to the benzene ring structure in their molecules, and are easy to accumulate in organisms, which are likely to cause cancer, obesity and reproductive problems, and are extremely harmful to human health . With the public's emphasis on environmental protection, countries around the world have actively carried out research and development of environmental...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C67/303C07C69/75
CPCB01J27/24C07C67/303C07C69/75
Inventor 韩伟卢小松张世元
Owner RUNTAI CHEM TAIXING CO LTD
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