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
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  • 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

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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...

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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

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83B01J35/10B01J37/08B01J37/18C07C209/72C07C211/35
CPCB01J23/007B01J23/83B01J35/0066B01J35/10B01J37/08B01J37/18C07C209/72C07C2601/14C07C211/35
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
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