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Preparation method of 3,3,5-trimethylcyclohexanone

A technology of trimethylcyclohexanone and hydrogenation catalyst, which is applied in the preparation of carbon-based compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the need to add heavy metal Cr and low selectivity of trimethylcyclohexanone. , unfavorable environmental protection and other problems, to achieve the effect of continuous preparation of saving subsequent separation energy consumption, high selectivity and high yield

Active Publication Date: 2020-04-07
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has low selectivity of trimethylcyclohexanone, and needs to add heavy metal Cr, which is not conducive to environmental protection and increases the cost of wastewater treatment

Method used

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  • Preparation method of 3,3,5-trimethylcyclohexanone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Using equal volume impregnation method, 38.9gNi(NO 3 ) 2 ·6H 2 O and 0.14g of sodium carbonate were added to water under stirring. After all the salt was dissolved, water was added until the volume of the solution was 100ml. Stirring was added in batches of 100g of alumina as a carrier, and it was soaked at room temperature for 24 hours to form a 2-3mm clover shape. Dry at 120°C for 2h; then calcinate at 600°C for 6h to obtain Catalyst 1. Calculated as NiO, the loading amount of Ni is 10wt% of the carrier, and the content of the modifying agent sodium carbonate calculated as Na element is 2% of the molar amount of Ni.

Embodiment 2

[0031] Using equal volume impregnation method, 77.8gNi(NO 3 ) 2 ·6H 2O and 1.14g of sodium carbonate were added to water under stirring. After all the salt was dissolved, water was added until the volume of the solution was 100ml. Stirring was added in batches of 100g of alumina as a carrier, and it was soaked at room temperature for 24h, and then formed into a 2-3mm clover shape. Dry at 120°C for 2h; then calcinate at 600°C for 6h to obtain catalyst 2. Calculated as NiO, the loading amount of Ni is 20wt% of the carrier, and the amount of modifier sodium carbonate calculated as Na element is 8% of the molar amount of Ni.

Embodiment 3

[0033] Using equal volume impregnation method, 58.4gNi(NO 3 ) 2 ·6H 2 O and 0.53g of sodium carbonate were added to water under stirring. After all the salt was dissolved, water was added until the volume of the solution was 100ml. Stirring was added in batches of 100g of alumina as a carrier, and it was soaked at room temperature for 24 hours, and then formed into a 2-3mm clover shape. Dry at 120°C for 2h; then calcinate at 600°C for 6h to obtain catalyst 3. Calculated as NiO, the loading amount of Ni is 15wt% of the carrier, and the amount of modifier sodium carbonate calculated as Na element is 5% of the molar amount of Ni.

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Abstract

The invention relates to a preparation method of 3,3,5-trimethylcyclohexanone. Isophorone undergoes a selective hydrogenation reaction in the presence of hydrogen and a hydrogenation catalyst to prepare 3,3,5-trimethylcyclohexanone. The hydrogenation catalyst is selected from supported nickel or supported cobalt modified with carbonate or bicarbonate of alkali metal. A certain amount of ammonium oxalate into a reaction liquid, and is slowly decomposed to slowly release ammonia and carbon monoxide at a hydrogenation reaction temperature, so the conversion rate of isophorone is increased, generation of byproducts can be inhibited, subsequent separation operation of TMC and the byproduct 3,3,5-trimethylcyclohexanol is avoided, and high-selectivity and high-yield continuous preparation of 3,3,5-trimethylcyclohexanone is achieved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and relates to a preparation method of 3,3,5-trimethylcyclohexanone. Background technique [0002] 3,3,5-Trimethylcyclohexanone (TMC), as an important high-boiling organic solvent and pharmaceutical synthesis intermediate, is mainly used in the fields of medicine, pesticides, fine chemicals, etc., and its downstream products can be used in industries such as rubber Vulcanizing agents and polymer monomers for the plastics industry. [0003] TMC is mainly prepared by hydrogenation of isophorone (IP). The molecular structure of isophorone contains a C=C double bond and a C=O double bond, and the product 3,3,5-trimethylcyclohexanone is obtained by hydrogenating the C=C double bond. Under the action of a general hydrogenation catalyst, not only the C=C double bond is hydrogenated, but also the C=O double bond is easily hydrogenated, thereby forming the by-product 3,3,5-trimethylcyclohexanol...

Claims

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Application Information

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IPC IPC(8): C07C45/62C07C49/403B01J23/78
CPCC07C45/62B01J23/78C07C2601/14C07C49/403
Inventor 丁可王磊刘运海安丽艳曾伟赵欣靳少华蒋玉鑫陈永宋延方杨洋黎源
Owner WANHUA CHEM GRP CO LTD
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