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Method for synthesizing tricyclodecanedimethanol

A technology of decanedimethanol and dicyclopentadiene is applied in the field of synthesizing tricyclodecanedimethanol and achieves the effects of easy separation, simple preparation process and short reaction time

Inactive Publication Date: 2015-03-04
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem is that a considerable part of DCPD is converted to monoalcohols

Method used

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  • Method for synthesizing tricyclodecanedimethanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of silica-supported cobalt-rhodium-copper trimetallic catalyst:

[0023] a. Dissolve 20ml of tetraethyl orthosilicate in 14ml of ethanol, and heat to a temperature of 60°C under stirring to obtain a mixed solution;

[0024] b. Dissolve 3g of copper nitrate, 0.3g of cobalt chloride and 0.3g of rhodium trichloride in 10ml of distilled water, add the mixed solution obtained in step a, then add the mixed solution of 5ml of concentrated nitric acid and 5ml of water, and age at a temperature of 60°C 24 hours, then baked at 400°C for 6 hours in an air atmosphere in a muffle furnace to obtain silica-supported cobalt-rhodium copper oxides; then the obtained silica-supported cobalt-rhodium copper oxides in hydrogen Reduction at a temperature of 400°C for 4 hours, cooling to room temperature, calcination at a temperature of 400°C in air for 6 hours, and reduction at a temperature of 400°C in hydrogen for 4 hours to obtain a silica-supported cobalt-rhodium-copper cataly...

Embodiment 2

[0030] Preparation of silica-supported cobalt-rhodium-copper trimetallic catalyst:

[0031] a. Dissolve 20ml of ethyl orthosilicate in 14ml of ethanol, and heat to a temperature of 80°C under stirring to obtain a mixed solution;

[0032] b. Dissolve 3g of copper nitrate, 0.3g of cobalt chloride and 0.3g of rhodium trichloride in 10ml of distilled water, add the mixed solution obtained in step a, then add the mixed solution of 5ml of concentrated nitric acid and 5ml of water, and age at a temperature of 80°C 72 hours, then baked at 600°C for 3 hours in an air atmosphere in a muffle furnace to obtain silica-supported cobalt-rhodium copper oxides; then the obtained silica-supported cobalt-rhodium copper oxides in hydrogen Reduction at 600°C for 2 hours, cooling to room temperature, calcination at 600°C in air for 3 hours, reduction at 600°C in hydrogen for 2 hours, to obtain a silica-supported cobalt-rhodium-copper catalyst;

[0033] Phosphine ligand-modified silica-supported co...

Embodiment 3

[0038] Preparation of silica-supported cobalt-rhodium-copper trimetallic catalyst:

[0039] a. Dissolve 20ml of tetraethyl orthosilicate in 14ml of ethanol, and heat to a temperature of 70°C under stirring conditions to obtain a mixed solution;

[0040] b. Dissolve 3g of copper nitrate, 0.3g of cobalt chloride and 0.3g of rhodium trichloride in 10ml of distilled water, add the mixed solution obtained in step a, then add the mixed solution of 5ml of concentrated nitric acid and 5ml of water, and age at a temperature of 70°C 48 hours, then baked at 500° C. for 4 hours in an air atmosphere in a muffle furnace to obtain silica-supported cobalt-rhodium copper oxides, and then the obtained silica-supported cobalt-rhodium copper oxides in hydrogen Reduction at a temperature of 500°C for 3 hours, cooling to room temperature, calcination at a temperature of 500°C in air for 4 hours, and reduction at a temperature of 500°C in hydrogen for 3 hours to obtain a silica-supported cobalt-rhod...

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Abstract

The invention relates to a method for synthesizing tricyclodecanedimethanol. The method is capable of synthesizing the tricyclodecanedimethanol by virtue of one-step hydroformylation of dicyclopentadiene in the presence of a catalyst, wherein the catalyst is a phosphine ligand modified cobalt-rhodium-copper trimetallic catalyst and prepared by use of a sol-gel method; besides, the catalyst is mainly a supported solid catalyst, and is relatively simple in preparation process, relatively low in catalyst price, relatively mild in reaction condition, high in catalytic activity and reaction selectivity, relatively short in reaction time, convenient to separate from the reaction system, reusable, and convenient for enlarged and industrial application. In the presence of the catalyst obtained by use of the method, the conversion rate of the dicyclopentadiene can be above 99% and the selectivity of the tricyclodecanedimethanol can be above 90%.

Description

Technical field: [0001] The invention relates to a method for synthesizing tricyclodecane dimethanol. Background technique: [0002] Tricyclodecane dimethanol is an important chemical raw material, which has been widely used in water-based dispersions, coating compositions, lubricating oils, etc. And the important method of synthesizing tricyclodecane dimethanol mainly contains: 1) two-step method: promptly dicyclopentadiene (DCPD) hydroformylation synthesizes tricyclodecane dicarbaldehyde, then hydrogenation; 2) one-step method: namely One-step hydroformylation of dicyclopentadiene to tricyclodecane dimethanol. [0003] The main problem of the two-step method is that the operation is complicated, two-step reaction is required, and two different gases need to be used. The one-step protocol is relatively simple and requires only one class of reactive gases. [0004] In one-step synthesis of tricyclodecane dimethanol, U.S. Patent 4,300,002 uses cobalt compounds and phosphin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/27C07C29/16B01J31/24
CPCB01J23/8926B01J31/24B01J2523/17B01J2523/822B01J2523/845C07C29/16C07C2603/68C07C35/37
Inventor 高志贤马昱博庆绍军尹铎
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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