Acetophenone hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst, acetophenone technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problem of poor α-phenethyl alcohol selectivity, low dispersion of active component copper, and catalyst diffusion performance. It can achieve the effect of favorable activity and selectivity, improving the utilization rate of active sites, and reducing the influence of internal diffusion resistance.

Active Publication Date: 2019-03-29
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] At present, when the copper-based catalysts prepared by the precipitation method are used for the hydrogenation of acetophenone to prepare α-phenylethanol, there are usually problems such as low di

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] (1) Add 450g 8.0wt% hydrochloric acid, 16.3g F127, 41.5g KCl, 20.0g TMB and 5g PMMA microspheres (2 μm in particle size) in the reactor and mix well, then dropwise add 83.2g TEOS therein and The sol was obtained after fully reacting at 25°C for 8 hours;

[0067] (2) 388.8g copper nitrate, 30.27g 50wt% manganese nitrate aqueous solution, 3.0g lead nitrate and 3.4g bismuth nitrate are dissolved in 1140g water and prepare mixed metal salt solution, and preparation concentration is the sodium carbonate aqueous solution of 15wt%, then The prepared two solutions were respectively heated to 40°C and added dropwise to the sol obtained in step (1), and the dropwise addition time was 40min to carry out the precipitation reaction (adjust the amount of aqueous sodium carbonate solution according to the pH value of the system so that the precipitation of metal ions is complete. , the amount of sodium carbonate aqueous solution is slightly higher than the theoretical amount required ...

Embodiment 2

[0073] (1) Add 460g of 7.5wt% hydrochloric acid, 16.3g of F127, 41.5g of KCl, 20.0g of TMB and 4g of PMMA microspheres (3 μm in particle size) in the reactor and mix well, then drop 58.3g of TEOS therein and The sol was obtained after fully reacting at 20°C for 12 hours;

[0074] (2) 425.2g copper nitrate, 25.2g 50wt% manganese nitrate aqueous solution, 4.5g lead nitrate and 3.4g bismuth nitrate are dissolved in 1230g water and prepare mixed metal salt solution, and preparation concentration is the sodium carbonate aqueous solution of 15wt%, then The prepared two solutions were respectively heated to 45° C. and added dropwise to the sol obtained in step (1), and the dropwise addition time was 30 minutes to carry out the precipitation reaction (according to the pH value of the system, adjust the amount of aqueous sodium carbonate solution so that the metal ion precipitation is complete. , the amount of sodium carbonate aqueous solution is slightly higher than the theoretical am...

Embodiment 3

[0079] (1) Add 440g 8.0wt% hydrochloric acid, 16.3g F127, 41.5g KCl, 20.0g TMB and 6g PMMA microspheres (5 μm in particle size) in the reactor and mix well, then drop 54.1g TEOS therein and The sol was obtained after fully reacting at 30°C for 4 hours;

[0080] (2) 413.1g copper nitrate, 15.1g 50wt% manganese nitrate aqueous solution, 3.0g lead nitrate and 5.1g bismuth nitrate are dissolved in 1180g water and prepare mixed metal salt solution, and preparation concentration is the sodium carbonate aqueous solution of 15wt%, then The prepared two solutions were heated to 50°C respectively and added dropwise to the sol obtained in step (1), and the dropwise addition time was 50min to carry out the precipitation reaction (according to the pH value of the system, adjust the amount of aqueous sodium carbonate solution so that the metal ion precipitation is complete. , the amount of sodium carbonate aqueous solution is slightly higher than the theoretical amount required for the comp...

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Abstract

The invention relates to an acetophenone hydrogenation catalyst and a preparation method thereof, which comprises the following steps: (1) hydrochloric acid, F127, KCl, 1,3,5-trimethylbenzene and polymethyl methacrylate microspheres are mixed evenly, then tetraethylorthosilicate is added to the mixture, and 4-12 hour later, a sol is obtained; (2) a mixed metal salt solution containing Cu, Mn, Bi and Pb is prepared, a solution of an alkaline precipitant is prepared, the two kinds of solutions are allowed to contact with the obtained sol for precipitation reaction, heating and aging to obtain aslurry; (3) the slurry is subjected to filtering, washing, drying and roasting to obtain composite compound powder; (4) the composite compound powder is mixed with a binder, an alkaline auxiliary agent and a forming auxiliary agent and extruded to obtain the catalyst. The catalyst active component copper prepared by the method has high dispersion, the acidity is weak and mass transfer performanceis good, side reactions such as hydrogenolysis and the like are effectively inhibited, and good activity and selectivity are obtained.

Description

technical field [0001] The invention belongs to the technical field of catalysts, in particular to an acetophenone hydrogenation catalyst and a preparation method thereof. Background technique [0002] α-Phenylethyl alcohol is an important chemical intermediate widely used in the fields of medicine, fragrance manufacturing, cosmetics, food and fine chemicals. The existing α-phenylethanol synthesis methods mainly include microbial fermentation and acetophenone reduction / catalytic hydrogenation. [0003] Microbial fermentation generally uses phenylalanine and fluorophenylalanine as raw materials to produce α-phenylethanol through microbial fermentation conversion; the raw materials used in this method are expensive and the production cost is high. At present, the industrial production of α-phenylethanol usually adopts the hydrogenation method of acetophenone. This method has the advantages of low production cost, less by-products, high product yield, and high product purity, ...

Claims

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Application Information

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IPC IPC(8): B01J23/889C07C29/145C07C33/22
CPCB01J23/002B01J23/8892B01J2523/00C07C29/145B01J2523/12B01J2523/17B01J2523/41B01J2523/44B01J2523/54B01J2523/72B01J2523/13C07C33/22
Inventor 李作金沙宇于海波詹吉山孙康初乃波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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