Catalyst for preparing 1,4-cyclohexanedimethanol and preparation method of catalyst

A cyclohexanedimethanol and catalyst technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, hydrogenation preparation, etc., can solve the problems of large energy and resource consumption, low conversion rate or selectivity, complex process routes, etc. problems, to achieve the effect of high reaction yield, small amount of precious metal and simple process

Inactive Publication Date: 2015-06-24
CHINA NAT OFFSHORE OIL CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current technology has complex process routes, large energy and resource consumption, and low conversion rate or selectivity of the reaction.

Method used

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  • Catalyst for preparing 1,4-cyclohexanedimethanol and preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 0.8g of [PtRu 5 (CO) 15 (μ-SnPh 2 )(μ 6 -C)] and 0.03gFe(NO 3 ) 3 Disperse in a mixed solution of 400ml of dichloromethane and ethanol, add it to 0.5g carrier SiC with a particle size of 40-80 mesh under an inert atmosphere, stir at room temperature for 12h, let it stand, remove the liquid, and dry it in vacuum at 60°C for 12h, after drying Baking in vacuum at 100°C for 8h, set aside.

Embodiment 2

[0020] 1.2g of [PtRu 5 (CO) 15 (μ-SnPh 2 )(μ 6 -C)] and 0.03gCo(NO 3 ) 2 Disperse in 500ml of a mixed solution of dichloromethane and ethanol, add it to 0.5g carrier SiC with a particle size of 40-80 mesh under an inert atmosphere, stir at room temperature for 12 hours, let it stand, remove the liquid, and dry it in vacuum at 60°C for 12 hours. Baking in vacuum at 300°C for 2h, set aside.

Embodiment 3

[0022] 1.6g of [PtRu 5 (CO) 15 (μ-SnPh 2 )(μ 6 -C)] and 0.03gNi(NO 3 ) 2 Disperse in a mixed solution of 600ml of dichloromethane and ethanol, add it to 0.5g of carrier SiC with a particle size of 40-80 mesh under an inert atmosphere, stir at room temperature for 12h, let it stand, remove the liquid, and dry it in vacuum at 60°C for 12h, after drying Baking in vacuum at 200°C for 6h, set aside.

[0023] The catalysts prepared in the above examples 1, 2, and 3 were applied to the reaction of preparing 1,4-cyclohexanedimethanol by one-step hydrogenation of dimethyl terephthalate. The specific reaction conditions were: 2.5 g of dimethyl terephthalate Dissolve the ester in 60g of ethanol and place it in a 150ml autoclave, add 0.5g of the catalyst prepared in Example 1, 2 or 3, and replace the air with nitrogen for three times after sealing the autoclave, then replace the nitrogen with hydrogen for three times; start heating at a hydrogen pressure of 3MPa Stir, raise the temp...

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Abstract

The invention belongs to the technical field of catalysis, and relates to a catalyst for preparing 1,4-cyclohexanedimethanol and a preparation method of the catalyst. The catalyst is characterized by being a load-type catalyst and mainly consisting of ruthenium, platinum and tin; the mass percent of the ruthenium in the catalyst is 0.3 to 3 percent, the mass percent of the platinum is 0.1 to 1 percent, and the mass percent of tin is 0.1 to 1 percent; an additive is one or more of ferric nitrate, cobalt nitrate and nickel nitrate, and the content of the additive is 0.1 to 20 percent; a carrier is silicon carbide. The preparation method adopts an immersion method and comprises the steps of dispersing 0.5g to 2g of active component precursor [PtRu5(CO)15(micro-SnPh2)(micro 6-C)] and 0.01g to 0.05g of additive in 200ml to 800ml of a mixed solution of dichloromethane and ethanol to obtain a mixture, placing the mixture into 0.2g to 1.0g of carrier SiC with granularity of 40 to 80 meshes under an inert atmosphere, stirring at the room temperature, vacuum drying, and vacuum roasting. According to the catalyst and the preparation method, only one hydrogenation catalyst and a single solvent are used, the one-step hydrogenation preparation is realized, the consumption of precious metal is small, the reaction yield is relatively high, the process is simple, the separation of middle products is avoided, and the consumption of resources and energy can be reduced.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, in particular to a catalyst for preparing 1,4-cyclohexanedimethanol by one-step hydrogenation conversion of dimethyl terephthalate and a preparation method thereof. Background technique [0002] 1,4-Cyclohexanedimethanol is an excellent monomer for the production of high value-added polyester materials. Compared with polyethylene terephthalate, the polyester fiber produced by substituting part or all of it for ethylene glycol not only has It has lower density, higher melting point and other characteristics, and its hydrolytic stability and insulation performance are also better. It is widely used in the production of films, resins for electronic products, and insulated wires. [0003] Most of the current methods for preparing 1,4-cyclohexanedimethanol are obtained by two-step hydrogenation of dimethyl terephthalate. The first step is to hydrogenate the benzene ring with precious met...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): B01J27/224C07C29/19C07C29/149C07C31/27
Inventor赵甲李孝国于海斌臧甲忠高鹏孙国方费亚南李佳郑修新刘有鹏
OwnerCHINA NAT OFFSHORE OIL CORP