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Method of synthesizing tricyclic decane dimethyl carbinol

A technology of decanedimethanol and dicyclopentadiene is applied in the field of synthesizing tricyclodecanedimethanol, which can solve problems such as high pressure and increase pressure, and achieve the effects of short reaction time, easy separation, easy amplification and industrial application.

Inactive Publication Date: 2013-11-20
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 method described in this patent is relatively simple for the synthesis of tricyclodecane dimethanol, and the catalyst mainly exists in the organic phase, but the pressure of the reaction is too high, which will add a lot of pressure to the industrial scale-up. Another problem is that there are considerable A part of DCPD is converted into monoalcohols

Method used

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  • Method of synthesizing tricyclic decane dimethyl carbinol

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Effect test

Embodiment 1

[0024] Preparation of nano-gold catalyst supported by tricobalt tetroxide:

[0025] a. Under vigorous stirring, dissolve 28g of cobalt nitrate and 1g of chloroauric acid in 250mL of distilled water, then add dropwise to 660mL (0.47mol / L) of the precipitating agent as Na 2 CO 3 In the aqueous solution, the precipitation temperature is 20°C, and the whole process takes about 1 hour. The precipitate is vacuum filtered and centrifuged, and the precipitate is washed with distilled water to neutrality. °C drying for 16 hours to obtain a purple solid;

[0026] b. roasting the purple solid in step a at a temperature of 400° C., the roasting time is 4 hours, and the roasting atmosphere is air, so as to obtain gold nanoparticles supported by tricobalt tetroxide in a black solid;

[0027] Preparation of nano-gold catalyst supported by cobalt tetroxide modified by phosphine ligand:

[0028] c. Add the nano-gold and phosphine ligand supported by cobalt tetroxide in step b into tetrahydr...

Embodiment 2

[0032] Preparation of nano-gold catalyst supported by tricobalt tetroxide:

[0033] a. Under strong stirring, dissolve 28g of cobalt nitrate and 0.2g of chloroauric acid in 100mL of distilled water, and then add dropwise to 660mL (0.47mol / L) of NaOH aqueous solution as the precipitating agent. The precipitation temperature is 40°C. The whole process is about It takes 1 hour to vacuum filter and centrifuge the precipitate, wash the precipitate with distilled water to neutrality, and dry the nano-gold supported by cobalt hydroxide formed by precipitation at a temperature of 80 ° C for 6 hours. A purple solid was obtained;

[0034] b. Roasting the purple solid in step a at a temperature of 200° C., the roasting time is 3 hours, and the roasting atmosphere is air, so as to obtain gold nanoparticles supported by tricobalt tetroxide in a black solid;

[0035] Preparation of nano-gold catalyst supported by cobalt tetroxide modified by phosphine ligand:

[0036] c. Add the nano-gold...

Embodiment 3

[0040] Preparation of nano-gold catalyst supported by tricobalt tetroxide:

[0041] a. Under strong stirring, dissolve 14g of cobalt nitrate and 2g of chloroauric acid in 100mL of distilled water, and then add dropwise to 330mL (0.47mol / L) of ammonia solution as the precipitating agent. The precipitation temperature is 20°C. The whole process takes about For 1 hour, vacuum filter and centrifuge the precipitate, wash the precipitate with distilled water to neutrality, and dry the nano-gold supported by cobalt hydroxide formed by precipitation at a temperature of 30 ° C for 2 hours to obtain purple solid;

[0042] b. roasting the purple solid in step a at a temperature of 300° C., the roasting time is 6 hours, and the roasting atmosphere is air; obtain nano-gold supported by tricobalt tetroxide in a black solid;

[0043] Preparation of nano-gold catalyst supported by cobalt tetroxide modified by phosphine ligand:

[0044] c. Add the nano-gold and phosphine ligand supported by ...

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Abstract

The invention relates to a method of synthesizing tricyclic decane dimethyl carbinol. The method comprises the following steps of: preparing a cobaltosic oxide-supported nanogold catalyst, and modifying the obtained catalyst by a phosphine ligand; and catalyzing dicyclopentadiene to synthesize tricyclic decane dimethyl carbinol by a one-step method under the relatively low temperature and pressure, wherein the conversion rate of the dicyclopentadiene (DCPD) by the method is 99% or higher, and the selectivity of the tricyclic decane dimethyl carbinol can reach 80% or higher.

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. The unsaturated amorphous polyester resin composite material without benzene and formaldehyde developed from tricyclodecane dimethanol has the characteristics of anti-yellowing and low viscosity. Water-based dispersions, coating compositions, lubricating oils, etc. have been widely used. The important methods for the synthesis of tricyclodecane dimethanol mainly include: 1) hydroformylation of dicyclopentadiene (DCPD) to synthesize tricyclodecane dicarbaldehyde, and then hydrogenation; 2) one-step hydroformylation of dicyclopentadiene Synthesis of tricyclodecane dimethanol. [0003] In terms of two-step synthesis of tricyclodecane dimethanol, GB Patent 750144 discloses that tricyclodecanyl dialdehyde is synthesized first, and then tricyclodecane dimethanol is synthesized by hydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/37C07C29/16B01J31/24
Inventor 吾满江·艾力马昱博高志贤
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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