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Method for preparing tricyclodecanedicarboxylic acid with dicyclopentadiene as raw material

A technology of cyclodecane dicarboxylic acid and dicyclopentadiene, which is applied in the field of carbonylation reaction to prepare carboxylic acids, can solve the problems that the production technology of tricyclodecane dicarboxylic acid is still in its infancy, and achieve easy scale-up and industrial application and preparation The effect of simple method and easy separation

Active Publication Date: 2021-09-28
重庆化工职业学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And the polyester based on tricyclodecane dicarboxylic acid has not yet seen relevant reports, mainly because the production technology of tricyclodecane dicarboxylic acid is still in its infancy

Method used

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  • Method for preparing tricyclodecanedicarboxylic acid with dicyclopentadiene as raw material
  • Method for preparing tricyclodecanedicarboxylic acid with dicyclopentadiene as raw material

Examples

Experimental program
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Effect test

Embodiment 1

[0059] The cobalt, rhodium and manganese trimetals supported by α-alumina modified by phosphine ligands are prepared, and the specific steps are as follows:

[0060] A: Dissolve 20ml of aluminum isopropoxide in 14ml of ethanol, and heat to 60°C with stirring to obtain an ethanol solution of aluminum isopropoxide;

[0061] B: 3g manganese nitrate, 0.3g cobalt chloride and 0.3g rhodium trichloride are dissolved in 10ml distilled water, join in the ethanolic solution of aluminum isopropoxide prepared in step A, then add 5ml concentrated nitric acid and 5ml water The mixed solution is aged at 60°C for 24h; then roasted at 400°C for 6h in an air atmosphere in a muffle furnace to obtain cobalt-rhodium-manganese oxide supported on α-alumina;

[0062] C: Reduce the α-alumina-supported cobalt-rhodium-manganese oxide prepared in step B at 400°C in hydrogen for 4 hours, cool to room temperature, then roast at 400°C in air for 6 hours, and finally reduce it again in hydrogen at 400°C 4 h...

Embodiment 2

[0065] The preparation of tricyclodecane dicarboxylic acid, concrete steps are:

[0066] Introduce 5 g of dicyclopentadiene (DCPD), 0.15 g of triphenylphosphine-modified α-alumina-supported cobalt-rhodium-manganese trimetal and 20 ml of tetrahydrofuran into a 200 ml autoclave, Airtight, filled with air and synthesis gas (volume ratio 1 / 1) to 5 MPa, the reaction temperature is 160 ° C, the reaction pressure is 8 MPa, and the reaction is 6 hours to obtain tricyclodecanedicarboxylic acid.

Embodiment 3

[0068] The cobalt, rhodium and manganese trimetals supported by α-alumina modified by phosphine ligands are prepared, and the specific steps are as follows:

[0069] A: Dissolve 28ml of aluminum isopropoxide in 14ml of ethanol, and heat to 80°C with stirring to obtain an ethanol solution of aluminum isopropoxide;

[0070] B: 3g manganese nitrate, 0.3g cobalt chloride and 0.3g rhodium trichloride are dissolved in 10ml distilled water, join in the ethanolic solution of aluminum isopropoxide prepared in step A, then add 5ml concentrated nitric acid and 5ml water The mixed solution was aged at 80°C for 72h, and then calcined at 600°C for 3h in an air atmosphere in a muffle furnace to obtain cobalt-rhodium-manganese oxide supported on α-alumina;

[0071] C: Reduce the α-alumina-supported cobalt rhodium manganese oxide prepared in step B at 600°C in hydrogen for 2h, cool to room temperature, then roast at 600°C in air for 3h, and finally reduce at 600°C in hydrogen for 2h , to obta...

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Abstract

The invention belongs to the technical field of preparing carboxylic acid by carbonylation reaction, and in particular relates to a preparation method of tricyclodecane dicarboxylic acid. The preparation method comprises the following steps: using dicyclopentadiene as a raw material, using phosphine ligand-modified α-alumina-supported cobalt-rhodium-manganese trimetal as a catalyst, and controlling the mixing of synthesis gas and air in the presence of an organic solvent The gas pressure is 4-7MPa, the reaction temperature is 150-170°C, the reaction pressure is 7-9MPa, and the reaction is 3-8h. By adopting the method to prepare tricyclodecane dicarboxylic acid, the conversion rate of dicyclopentadiene can reach more than 99%, and the selectivity of tricyclodecane dicarboxylic acid can reach more than 90%.

Description

technical field [0001] The invention belongs to the technical field of preparing carboxylic acid by carbonylation reaction, and in particular relates to a method for preparing tricyclodecanedicarboxylic acid by using dicyclopentadiene as a raw material. Background technique [0002] Dicyclopentadiene (DCPD for short), also known as dicyclopentadiene, is a by-product of petroleum cracking to acetylene and coal coking. Dicyclopentadiene is a dimer of cyclopentadiene, with a boiling point of 170°C, a melting point of 31.5°C, and a density of 0.9796g / cm 3 . Dicyclopentadiene has two isomers of bridging ring and hanging ring in the space structure (as shown below), at room temperature [0003] [0004] Cyclopentadiene dimerizes to form a bridged ring, and when heated to 150°C dimerizes to form a hanging ring. The bridged ring dicyclopentadiene is mainly used in industry. High-purity dicyclopentadiene is a colorless crystal at room temperature, and when it contains impuritie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/145B01J31/24B01J31/02C07C61/135
CPCB01J31/0269B01J31/24B01J31/2404B01J2231/321B01J2231/70C07C51/145C07C2603/68C07C61/135
Inventor 马昱博揭芳芳宋春雨狄宁何桅李小庆
Owner 重庆化工职业学院
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