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A heterogeneous catalyst and its preparation method, and a method for preparing 3,5-dimethylphenol using the catalyst

A technology of heterogeneous catalysts and additives, applied in chemical instruments and methods, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problem of difficulty in obtaining products with high purity, decreased catalytic effect, and low product selectivity and other problems, to achieve the effects of inhibiting the formation of carbon deposits, improving catalytic performance, and high catalytic activity

Active Publication Date: 2019-04-23
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main problems of the first three methods are: low product selectivity and low by-products; strong acid and / or strong alkali are used in the process, the equipment is severely corroded, the process is complicated, and it is difficult to obtain a product with higher purity
[0008] (1) The catalyst mostly uses a single type of catalyst, and the single-phase catalyst has a decline in catalytic effect due to its own limitations;
[0009] (2) Carbon deposition is serious during the reaction process, and the carbon powder generated during the reaction process will block the reactor after a long period of accumulation, causing the passive shutdown of the entire reaction system;

Method used

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  • A heterogeneous catalyst and its preparation method, and a method for preparing 3,5-dimethylphenol using the catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Prepare the catalyst by precipitation method, add 2kg of water, 2.6g of polyethylene glycol and 15.6g of Ni powder into the kettle, and heat to 70°C. 273.7g Cr(NO 3 ) 3 .9H 2 O, 23.57g Co(NO 3 ) 2 .6H 2 O, 40.47g Ni(NO 3 ) 2 .6H 2 O and 200.8g Al(NO 3 ) 3 .9H 2 O was dissolved in water to prepare a 1.5mol / L mixed salt solution. Drop the mixed salt solution and 15wt% sodium carbonate solution into the reaction kettle at the same time, the titration time is 1h, keep the reaction temperature at 70°C during the titration process, and add 18.2g of inert Al in 4 times during the precipitation process 2 o 3 , the system pH is controlled at 6.5. After adding the mixed salt solution, adjust the pH of the system to 7.5 with sodium carbonate solution, and age at 70°C for 3h, then filter, wash and dry the filter cake at 110°C for 12h, and roast at 600°C for 3h. Obtain 1# heterogeneous catalyst 40Cr 2 o 3 / 8NiO / 12Ni / 5Co 3 o 4 / 35Al 2 o 3 , the values ​​in the het...

Embodiment 2

[0059] Prepare the catalyst by precipitation method, add 2kg of water, 2.6g of polyethylene glycol and 11.7g of Ni powder into the kettle, and heat to 70°C. 239.5g Cr(NO 3 ) 3 .9H 2 O, 23.57g Co(NO 3 ) 2 .6H 2 O, 45.5g Ni(NO 3 ) 2 .6H 2 O, 41.36g Mg(NO 3 ) 2 .6H 2 O and 247.7g Al(NO 3 ) 3 .9H 2 O was dissolved in water to prepare a 1mol / L mixed salt solution. Drop the mixed salt solution and 15wt% sodium carbonate solution into the reaction kettle at the same time, the titration time is 2h, keep the reaction temperature at 70°C during the titration process, and add 14.4g of inert Al in 4 times during the precipitation process 2 o 3 , the system pH is controlled at 6.0. After adding the mixed salt solution, adjust the pH of the system to 7.0 with sodium carbonate solution, and age at 70°C for 3h, then filter, wash and dry the filter cake at 110°C for 12h, and roast at 700°C for 3h. Obtain 2# heterogeneous catalyst 35Cr 2 o3 / 9NiO / 9Ni / 5MgO / 5Co 3 o 4 / 37Al 2 ...

Embodiment 3

[0063] The catalyst was prepared by precipitation method, 2kg of water, 2.0g of polyethylene glycol and 7.8g of Ni powder were added to the kettle, heated to 75°C, and 205.28g of Cr(NO 3 ) 3 .9H 2 O, 70.71g Co(NO 3 ) 2 .6H 2 O, 45.5g Ni(NO 3 ) 2 .6H 2 O and 229.49g Al(NO 3 ) 3 .9H 2 O was dissolved in water to prepare a 1.5mol / L mixed salt solution. Drop the mixed salt solution and 15wt% sodium carbonate solution into the reaction kettle at the same time, the titration time is 1.5h, keep the reaction temperature at 75°C during the titration process, and add 20.8g of inert Al in 4 times during the precipitation process 2 o 3 , the system pH is controlled at 7.0. After adding the mixed salt solution, adjust the pH of the system to 8.0 with sodium carbonate solution, and age at 75°C for 3h, then filter, wash and dry the filter cake at 110°C for 12h, and roast at 650°C for 3h. Obtain 3# heterogeneous catalyst 30Cr 2 o 3 / 9NiO / 6Ni / 15Co 3 o 4 / 40Al 2 o 3 , the val...

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PUM

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Abstract

The present invention relates to a heterogeneous catalyst and a preparation method thereof, and also relates to a method for preparing 3,5-dimethylphenol by aromatization of isophorone (IP) using the heterogeneous catalyst. The heterogeneous catalyst comprises an active component, a carrier, and optional additives, the active component comprising Ni, NiO, Cr 2 o 3 and Co 3 o 4 . Activated heterogeneous catalyst for isophorone aromatization with simultaneous aromatization activity and methane CO 2 Reforming reaction activity, the heterogeneous catalyst has good activity, high selectivity, and good stability. When used in conjunction with a homogeneous catalyst, it can effectively reduce the amount of homogeneous catalyst used, and at the same time reduce the amount of carbon deposition and prolong the use of the catalyst time.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to a catalyst for preparing 3,5-dimethylphenol from isophorone and a preparation method thereof, and also to a method for preparing 3,5-dimethylphenol. Background technique [0002] 3,5-Dimethylphenol is an important organic synthesis intermediate and fine chemical raw material, widely used in the production of vitamins, disinfectants, rubber, dyes, paints, etc. The main domestic use is to chlorinate 3,5-dimethylphenol to produce 4-chloro-3,5-dimethylphenol (PCMX), which is a highly effective disinfectant and preservative used in soaps and Detergents such as hand sanitizer. Under the catalysis of noble metal catalyst, 3,5-dimethylphenol can synthesize high-grade dye intermediate 3,5-dimethylaniline by introducing hydrogen and ammonia gas; Kylation reaction can produce 2,3,5-trimethylphenol, which is used as a raw material for the preparation of medicines. The reaction of dimethyl disulfi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/86C07C39/07C07C37/50
Inventor 詹吉山初乃波尹育王同济李作金邵亮峰黎源
Owner WANHUA CHEM GRP CO LTD
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