Method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine

Patent metadata

Field	Value
Publication number	US-11180440-B2
Application number	US-201816954774-A
Country	US
Kind code	B2
Filing date	Nov 30, 2018
Priority date	Dec 22, 2017
Publication date	Nov 23, 2021
Grant date	Nov 23, 2021

Abstract

The present disclosure relates to a method for preparing isophorone diamine by means of a hydrogenation reduction of isophorone nitrile imine. The hydrogenation reduction is continuously carried out in a multi-stage bubble column reactor loaded with a supported alkaline cobalt-based catalyst, wherein isophorone nitrile imine is successively in countercurrent contact with hydrogen in each stage of the reactor to carry out a hydrogenation reduction reaction, so as to obtain the isophorone diamine. The preparation method solves the problem of back-mixing, and further improves the conversion rate and the cis/trans ratio of the product.

First claim

What is claimed is:

1. A method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine, wherein the hydrogenation reduction is carried out continuously in a multistage bubble column reactor loaded with a supported alkaline cobalt-based catalyst, and isophorone nitrile imine comes sequentially in countercurrent contact with hydrogen in each stage reactor to carry out a hydrogenation reduction reaction, thereby obtaining isophorone diamine, wherein the multistage bubble column reactor includes 6 to 12 stage reactors.

2. The method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine according to claim 1 , wherein a sieve plate is used for separation between each stage reactor of the multistage bubble column reactor.

3. The method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine according to claim 2 , wherein pores on the sieve plate only enable hydrogen to pass while not allowing a reaction liquid to pass, and the reaction liquid enters the next stage reactor through a downcomer pipe and a downcomer ring.

4. The method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine according to claim 2 , wherein the supported alkaline cobalt-based catalyst is separately provided in each stage reactor, and is fixed by using the sieve plate, a pressing plate, and a dead plate; and pores of the pressing plate and the dead plate enable hydrogen and a reaction liquid to pass.

5. The method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine according to claim 1 , wherein the supported alkaline cobalt-based catalyst comprises a carrier, an active component, and an alkaline component; the carrier includes one or more of alumina, titania, zirconium dioxide, and magnesia; the active component is Co; and the alkaline component includes an oxide of Mg, Ca, Na or K.

6. The method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine according to claim 5 , wherein the active component has a mass fraction of 30% to 50%; and the alkaline component has a mass fraction of 0.1% to 5%.

7. The method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine according to claim 1 , wherein isophorone nitrile imine, when added as a reaction material, has a mass fraction of 97% or more.

8. The method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine according to claim 1 , wherein a molar ratio of hydrogen to isophorone nitrile imine during the hydrogenation reduction reaction is 5 to 100:1; and a space-time processing capacity of catalyst of the multistage bubble column reactor is 0.05 to 0.3 mol/(L*h).

9. The method for preparing isophorone diamine by means of hydrogenation reduction of isophorone nitrile imine according to claim 1 , wherein a reaction temperature in the multistage bubble column reactor is 60° C. to 160° C., and the temperatures in adjacent stage reactors are the same or increase successively; and a reaction pressure in the multistage bubble column reactor is 3 to 10 MPa.

Assignees

• Zhejiang Nhu Co Ltd
• Univ Zhejiang
• Shandong Nhu Amino Acid Co Ltd
• Shandong Nhu Fine Chemical Science And Tech Company Ltd

Inventors

• Chen Zhirong
• Mao Jianyong
• Hu Baishan
• Li Guanbing
• Li Haoran
• Wang Yu
• Yang Yingkuo
• Liu Qing
• Tang Jiyu
• Chen Weiyong

Classifications

• C07C209/48 Primary

  by reduction of nitriles · CPC title

• C07C209/52 Primary

  by reduction of imines or imino-ethers (C07C209/24 takes precedence) · CPC title

• B01J8/0292

  with stationary packing material in the bed, e.g. bricks, wire rings, baffles · CPC title

• B01J23/78

  with alkali- or alkaline earth metals · CPC title

• B01J35/04

  Operations & Transport · mapped topic