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Preparation method and application of N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine

A technology of trimethylcyclohexylamine and dimethyl, applied in the field of N, to achieve the effect of simple production process

Active Publication Date: 2012-12-12
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no effective utilization method for this product, and it can only be treated as waste.
There is no report on using N,N-dimethyl-3,3,5-trimethylcyclohexylamine as a catalyst for the synthesis of polyurethane foam

Method used

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  • Preparation method and application of N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine
  • Preparation method and application of N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine
  • Preparation method and application of N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] By-product 3,3,5-trimethylcyclohexylamine in the manufacture of IPDA:

[0057] The reaction is carried out on a fixed-bed reaction equipment, which is composed of two-stage trickle-bed reactors. The first stage is filled with 100ml of zeolite, and the second stage is filled with 100ml of cobalt as the active component and diatomaceous earth as the carrier. hydrogenation catalyst, the reaction raw materials pass through the first reactor and the second reactor sequentially from top to bottom. The hydrogenation catalyst was reduced with pure hydrogen at 400°C for 12 hours before running the test. The controlled temperature of the first-stage reactor is 50°C, and the controlled temperature of the second-stage reactor is 90°C. The reaction pressure is 20MPa. The feed rate of IPN is 80g / h, the feed rate of ammonia is 137g / h, and the feed rate of hydrogen is 110 standard L / h. When the device runs for 100h, the reaction discharge is analyzed by gas chromatography, wherein is...

Embodiment 2

[0063] Embodiment 2: in the autoclave of 1L, add 140g 3,3,5-trimethylcyclohexylamine (the obtaining route of 3,3,5-trimethylcyclohexylamine is the same as embodiment 1), the content of 324g is 37% formaldehyde in water. 0.7 g of a common commercially available Pd / C catalyst with a Pd content of 5% was added. Seal the reaction kettle, replace the air with nitrogen 3 times, and replace the nitrogen with hydrogen 3 times. Turn on stirring to 600 rpm, raise the temperature in the reactor to 50° C., and increase the pressure in the reactor to 2 MPa. React until the system no longer absorbs hydrogen, and the reaction time is about 3 hours. After the reaction is finished, the reactant and the catalyst are filtered, and the reaction product is divided into a water phase and an oil phase. The oily and aqueous phases were separated using a pear-shaped separatory funnel. The oil phase was taken for gas chromatography analysis, and the content of N,N-dimethyl-3,3,5-trimethylcyclohexyl...

Embodiment 3

[0064] Embodiment 3: in the autoclave of 1L, add 140g 3,3,5-trimethylcyclohexylamine (the obtaining route of 3,3,5-trimethylcyclohexylamine is the same as embodiment 1), 243g content is 37% formaldehyde in water. 1.1 g of a common commercially available Ru / C catalyst with a Ru content of 5% was added. Seal the reaction kettle, replace the air with nitrogen 3 times, and replace the nitrogen with hydrogen 3 times. Turn on the stirring to 600 rpm, raise the temperature in the reactor to 70° C., and increase the pressure in the reactor to 3 MPa. React until the system no longer absorbs hydrogen, and the reaction time is about 3 hours. After the reaction is finished, the reactant and the catalyst are filtered, and the reaction product is divided into a water phase and an oil phase. Separate the oily and aqueous phases with a pear-shaped separatory funnel. The oil phase was taken for gas chromatography analysis, and the content of N,N-dimethyl-3,3,5-trimethylcyclohexylamine was ...

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Abstract

The invention provides a preparation method and application of N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine. The method comprises enabling 3, 3, 5-trimethyl cyclohexylamine, formaldehyde and hydrogen to undergo an amination hydrogenation reaction under a fixed temperature and pressure under the effect of a catalyst so as to prepare N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine. The obtained N, N-dimethyl-3, 3, 5-trimethyl cyclohexylamine can be used as a catalyst for polyurethane foaming after purification.

Description

technical field [0001] The invention relates to the utilization of by-product 3,3,5-trimethylcyclohexylamine in the production process of isophoronediamine (3-aminomethyl-3,5,5-trimethylcyclohexylamine). Specifically, it is a method for preparing N,N-dimethyl-3,3,5-trimethylcyclohexylamine from 3,3,5-trimethylcyclohexylamine, and involves N, Use of N-dimethyl-3,3,5-trimethylcyclohexylamine. Background technique [0002] Isophorone diamine (3-aminomethyl-3,5,5-trimethylcyclohexylamine, referred to as IPDA, hereinafter no longer specified) is the preparation of isophorone diisocyanate (IPDI) (a kind of fat It can also be used as a curing agent for epoxy resins. Usually, 3-cyano-3,5,5-trimethylcyclohexanone (isophorone nitrile, referred to as IPN, hereinafter not specified), ammonia, and hydrogen are subjected to amination and hydrogenation under the action of a hydrogenation catalyst. And made. [0003] During the manufacture of isophoronediamine, 3,3,5-trimethylcyclohexyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/35C07C209/60C08G18/18C08G101/00
Inventor 黎源齐旺顺陈长生周明星崔洪寅赵文娟汪波王学勇华卫琦丁建生
Owner WANHUA CHEM GRP CO LTD
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