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Heterogeneous catalyst for preparing 3, 5-dimethylphenol from isophorone as well as preparation method and application of heterogeneous catalyst

A heterogeneous catalyst, dimethyl phenol technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of non-recyclable, etc., to solve the problem of separation and recycling, High conversion rate and selectivity, and the effect of reducing input costs

Active Publication Date: 2021-03-26
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is also to provide a kind of by above-mentioned heterogeneous catalyst Co-Ni-NiO-Co 3 o 4 /CN catalyzed isophorone to prepare 3,5-xylenol, which not only overcomes the problems of separation difficulty and non-recyclability of homogeneous catalysts, but also ha

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  • Heterogeneous catalyst for preparing 3, 5-dimethylphenol from isophorone as well as preparation method and application of heterogeneous catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Preparation of catalyst:

[0050] According to the mass ratio of 4:3:4:10:3000, the cobalt salt Co(NO 3 ) 2 ·6H 2 O, nickel salt Ni(NO 3 ) 2 ·6H 2 O. Trimellitic acid and 2-methylimidazole were dissolved in DMF. After they were completely dissolved, they were placed in a 170°C hydrothermal kettle and placed in an oven for hydrothermal reaction. The reaction time was 22 hours. After the reaction, centrifuged to obtain a precipitate ; Wash the precipitate with ethanol for 5 times and dry it in a vacuum oven with a vacuum degree of 50KPa at 90°C for 8h to obtain CoNi-MOFs;

[0051] CoNi-MOFs were placed in a tube furnace, calcined at 800 °C for 2 h in a nitrogen atmosphere, the heating rate was 2 °C / min, and the nitrogen flow rate was 45 mL / min, and carbonized to obtain Co-Ni-NiO-Co 3 o 4 / CN, where Co content is 0.76%, Ni content is 0.66%, NiO content is 4.5%, Co 3 o 4 The content is 12.8%, and the remaining components are CN.

[0052] The catalyst is cubic, wit...

Embodiment 2

[0058] Preparation of catalyst:

[0059] According to the mass ratio of 3:4:4:10:3500, the cobalt salt Co(NO 3 ) 2 ·6H 2 O, nickel salt NiCl 2 ·6H 2 O. Trimellitic acid and 2-methylimidazole are dissolved in DMF. After they are completely dissolved, they are placed in a hydrothermal kettle at 190°C and placed in an oven for hydrothermal reaction. The reaction time is 20 hours. After the reaction, centrifuge to obtain a precipitate ; Wash the precipitate with ethanol for 5 times and dry it in a vacuum oven with a vacuum degree of 30KPa at 80°C for 10h to obtain CoNi-MOFs;

[0060] CoNi-MOFs were placed in a tube furnace, calcined at 750 °C for 1 h in a nitrogen atmosphere, the heating rate was 2.5 °C / min, and the nitrogen flow rate was 45 mL / min, and carbonized to obtain Co / Ni / NiO / Co 3 o 4 / CN, where Co content is 0.55%, Ni content is 0.77%, NiO content is 4.1%, Co 3 o 4 The content is 12%, and the remaining components are CN.

[0061] The morphology of the catalyst is...

Embodiment 3

[0067] Preparation of catalyst:

[0068] According to the mass ratio of 5:3:3:10:2500, the cobalt salt CoCl 2 ·6H 2 O, nickel salt Ni(NO 3 ) 2 ·6H 2 O. Trimellitic acid and 2-methylimidazole were dissolved in DMF. After they were completely dissolved, they were placed in a 160°C hydrothermal kettle and placed in an oven for hydrothermal reaction. The reaction time was 18 hours. After the reaction, centrifuged to obtain a precipitate ; Wash the precipitate with ethanol for 5 times and dry it in a vacuum oven with a vacuum degree of 40KPa at 90°C for 6h to obtain CoNi-MOFs;

[0069] CoNi-MOFs were placed in a tube furnace and calcined at 700 °C for 3 h in a nitrogen atmosphere with a heating rate of 3 °C / min and a nitrogen flow rate of 35 mL / min to obtain Co / Ni / NiO / Co 3 o 4 / CN, where Co content is 0.88%, Ni content is 0.57%, NiO content is 5.3%, Co 3 o 4 The content is 13.4%, and the remaining components are CN.

[0070] The morphology of the catalyst is cubic, with an...

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Abstract

The invention provides a heterogeneous catalyst for preparing 3, 5-dimethylphenol from isophorone as well as a preparation method and application of the heterogeneous catalyst. The heterogeneous catalyst is a Co-Ni-NiO-Co3O4/CN composite material, does not need reduction activation before use, has good thermal stability and mechanical stability, and is easy to separate and recover. According to the present invention, with the catalyst, the isophorone is adopted as the raw material, and catalytic aromatization is performed to prepare the 3, 5-dimethylphenol in one step, such that the problems of difficult separation, non-reutilization and the like of the homogeneous catalyst can be overcome, the high conversion rate and the high selectivity are provided, the generation of carbon depositioncan be inhibited, and the catalyst inactivation due to carbon deposition and coking can be avoided; and passive shutdown caused by the fact that carbon powder generated in the reaction process accumulates and blocks the reactor is avoided, and operation continuity is guaranteed.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and relates to a heterogeneous catalyst and a preparation method thereof, and a method for preparing 3,5-dimethylphenol from isophorone and the heterogeneous catalyst. Background technique [0002] 3,5-Dimethylphenol is an important fine chemical raw material and organic synthesis intermediate. In addition, it also has anti-mildew and anti-bacterial effects. It is widely used in various fields of industrial and agricultural production, showing more and more broad application prospects . [0003] The methods for synthesizing 3,5-dimethylphenol mainly include: m-xylene sulfonation alkali fusion method, phenol alkylation method, acetone gas phase synthesis method, 3,5-dimethyl-2-cyclohexenone dehydrogenation method, isophorone (IP) aromatization method, etc., wherein isophorone (IP) aromatization method is the most widely used method in industry at present. In the method disclosed in the patent US408...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/10B01J37/10B01J37/08C07C37/07C07C37/50C07C39/07C01B3/40
CPCB01J27/24B01J23/002B01J35/1023B01J35/1061B01J35/002B01J37/10B01J37/084B01J37/086C07C37/07C07C37/50C01B3/40C01B2203/0233C01B2203/1058C07C39/07Y02P20/52
Inventor 刘超胡凯华刘振峰余炎冰王加琦丛鑫牟通黎源
Owner WANHUA CHEM GRP CO LTD