Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Catalyst for synthesizing cyclohexylamine by aniline hydrogenation and preparation method thereof

A catalyst, cobalt catalyst technology, applied in catalyst activation/preparation, preparation of organic compounds, preparation of amino compounds, etc., can solve the problems of low conversion rate and low selectivity of non-precious metal catalysts, and achieve improved stability and service life, The effect of improving reaction efficiency and improving conversion rate

Pending Publication Date: 2019-11-22
WANHUA CHEM GRP CO LTD
View PDF16 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] Aiming at the problems of low conversion rate and low selectivity of non-precious metal catalysts in the prior art, one of the problems to be solved by the present invention is to provide a low-cost, highly active modified hydrotalcite-like derived cobalt catalyst, which can Effectively improve the reaction efficiency, inhibit the formation of by-product dicyclohexylamine, and increase the yield of cyclohexylamine

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Preparation of modified hydrotalcite-like precursor:

[0047] First, 72.8g of cobalt nitrate (Co(NO 3 ) 2 ·6H 2 O, 291), 128.2g magnesium nitrate (Mg(NO 3 ) 2 ·6H 2 O, 256), 92.9g aluminum nitrate (Al(NO 3 ) 3 9H 2 O, 375), 1.1g lanthanum nitrate (La(NO 3 ) 3 ·6H 2 (2,433) and 600.1g urea (60) were dissolved in 1000mL deionized water to obtain a transparent solution; then the solution was transferred to an autoclave and crystallized at 110°C for 12h; , Methanol each washed 3 times; Then, the solid sample after separation was dispersed in Methanol (the consumption of Methanol is 55ml / g 固体 ), ultrasonicated at 25°C for 1h; then the sample was filtered and dried at 60°C for 12h to obtain a modified hydrotalcite-like precursor.

[0048] Preparation of modified hydrotalcite-like cobalt catalysts:

[0049] The above-mentioned hydrotalcite-like precursor was placed in a muffle furnace, and the temperature was raised to 550° C. at a rate of 3° C. / min, and kept for ...

Embodiment 2

[0053] Preparation of modified hydrotalcite-like precursor:

[0054] First, 131.0g of cobalt nitrate (Co(NO 3 ) 2 ·6H 2 O, 291), 38.5g magnesium nitrate (Mg(NO 3 ) 2 ·6H 2 O, 256), 35.4g calcium nitrate (Ca(NO 3 ) 2 4H 2 O, 236), 91.1g aluminum nitrate (Al(NO3) 3 9H 2 O, 375), 3.2g lanthanum nitrate (La(NO 3 ) 3 ·6H 2 O, 433) and 600.1g (60) urea were dissolved in 1000mL deionized water to obtain a transparent solution; then the solution was transferred to an autoclave, and crystallized at 120°C for 10h; , Methanol each washed 3 times; Then, the solid sample after separation was dispersed in Methanol (the consumption of Methanol is 55ml / g 固体 ), ultrasonicated at 25°C for 1h; then the sample was filtered and dried at 62°C for 10h to obtain a modified hydrotalcite-like precursor.

[0055] Preparation of modified hydrotalcite-like cobalt catalysts:

[0056] The above-mentioned hydrotalcite-like precursor was placed in a muffle furnace, and the temperature was raise...

Embodiment 3

[0060] Preparation of modified hydrotalcite-like precursor:

[0061] First, 109.1g of cobalt nitrate (Co(NO 3 ) 2 ·6H 2 O, 291), 88.6g calcium nitrate (Ca(NO 3 ) 2 4H 2 O, 236), 89.3g aluminum nitrate (Al(NO3) 3 9H 2 O, 375), 5.2g cerium nitrate (Ce(NO 3 ) 3 ·6H 2 (2,434) and 600.1g urea were dissolved in 1000mL deionized water to obtain a transparent solution. Then the solution was transferred to an autoclave and crystallized at 100°C for 18h. After the solid-liquid mixture of gained is filtered, respectively wash with water, acetone 3 times; Then, the solid sample after separation is dispersed in acetone (the consumption of acetone is 55ml / g 固体 ), ultrasonicated at 25°C for 1h; then the sample was filtered and dried at 55°C for 8h to obtain a modified hydrotalcite-like precursor.

[0062] Preparation of modified hydrotalcite-like cobalt catalysts:

[0063] The above-mentioned modified hydrotalcite-like precursor was placed in a muffle furnace, the temperature wa...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a modified hydrotalcite-like derived cobalt catalyst, general formula being M / M1(O)-M2(O)-M3(O), wherein M represents Co, M1 represents an alkaline earth metal, M2 representsa rare earth metal, M3 represents Al, n(Co+M1) / n (Al+M2)=2-4, the molar ratio of Co to M1 is 0.5-1.5, and the molar ratio of M2 to Al is 0.005-0.05. The preparation method comprises the following steps: dissolving various metal salts and urea in water to form an aqueous solution, crystallizing the aqueous solution to obtain a solid-liquid mixture, filtering the solid-liquid mixture, respectively washing with water and a modifier, dispersing the mixture in the modifier, carrying out ultrasonic treatment, and filtering and drying the product to obtain a modified hydrotalcite-like precursor; androasting and reducing the precursor to obtain the catalyst. The catalyst is used for synthesizing cyclohexylamine through aniline hydrogenation, the aniline conversion rate can reach 98% or above, andthe dicyclohexylamine selectivity is 3% or below.

Description

technical field [0001] The invention relates to the technical field of organic catalysis, in particular to a catalyst used for the hydrogenation of aniline to synthesize cyclohexylamine and a preparation method thereof. Background technique [0002] Cyclohexylamine is an important organic chemical and fine chemical intermediate, used in the production of petroleum product additives, metal corrosion inhibitors, fungicides and insecticides, antistatic agents, rubber accelerators and anti-aging agents, food and feed additives, syngas desulfurization agent etc. Due to the rapid development of food additives and rubber accelerators, cyclohexylamine as a raw material has been in short supply for a long time. [0003] At present, the production of cyclohexylamine is mainly through four process routes: aniline hydrogenation reduction method, cyclohexanol catalytic amination method, cyclohexanone catalytic amination method, and nitrocyclohexane reduction method. The aniline hydroge...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83B01J35/10B01J37/08B01J37/18C07C209/72C07C211/35
CPCB01J23/007B01J23/83B01J37/08B01J37/18C07C209/72C07C2601/14B01J35/394B01J35/60C07C211/35
Inventor 张立娟张聪颖刘振国姜瑞航李鑫任树杰王丛
Owner WANHUA CHEM GRP CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products