Catalyst, preparation method and application of acetophenone hydrogenation to prepare α-phenylethanol

A hydrogenation catalyst and catalyst technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, metal/metal oxide/metal hydroxide catalyst, etc. Low conversion rate of ketones and other problems, to achieve the effect of improving catalyst activity and selectivity, improving catalyst activity, and smoothing catalyst pores

Active Publication Date: 2019-07-30
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1557545A prepared Ni-Sn-B / SiO by dipping method 2 Catalyst, after low-temperature roasting, KBH4 is used as a reducing agent for reduction. During the catalytic reaction, the highest selectivity of phenylethyl alcohol is 97.5%, but the interaction between the active component Ni and the carrier SiO2 is weak and easy to be lost
[0006] US4996374 discloses a kind of Pd-C catalyst, but its catalyst stability is relatively poor, needs to constantly improve reaction temperature when applying mechanically
CN1315226A discloses a reduction-treated copper-based catalyst and a method for preparing α-phenylethanol, but it needs to adopt a liquid-phase reduction method to improve the stability of the catalyst, and the process is complicated and the cost is high
CN1911883A discloses a method for preparing α-phenylethanol with Raney nickel as a catalyst, but there are more aromatic ring hydrogenation products α-cyclohexyl alcohol in its acetophenone hydrogenation product, and α-phenylethanol selectivity lower
[0010] In the prior art, copper-based catalysts used in liquid-phase hydrogenation reactions are not only affected by various internal or external forces in the process of storage / filling / reduction / reaction, but also due to liquid immersion, swelling, etc. The strength is greatly reduced, causing the catalyst to be easily broken and pulverized in the liquid phase hydrogenation system, threatening the stable operation of industrial equipment and affecting the life of the catalyst
[0011] At present, the hydrogenation of acetophenone prepared by the precipitation method to prepare α-phenylethyl alcohol copper catalysts usually has problems such as low dispersion of active component copper, strong catalyst acidity, weak interaction between the carrier and the active component, etc., resulting in acetophenone Low conversion rate, large amount of by-products such as ethylbenzene, poor selectivity of phenylethanol, poor catalyst strength

Method used

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  • Catalyst, preparation method and application of acetophenone hydrogenation to prepare α-phenylethanol

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Add 200g of water, 10g of methanol, 4.0g of PMMA with a particle size of 10-30μm, and 2.0g of C 16-6-16 The Gemini surfactant (purchased from Henan Dao Pure Chemical Co., Ltd.) was mixed evenly, and then 120.0 g of 30% concentration of silica sol was added and stirred evenly. Dissolve 332.2g of copper nitrate, 73.1g of zinc nitrate, 21.3g of lanthanum nitrate, and 12.7g of magnesium nitrate in 1.5kg of water to make a mixed salt solution, and dissolve 113.5g of sodium silicate and 142.5g of sodium carbonate in water to make a precipitant solution , respectively, the two solutions were heated to 70 ℃. The method of co-precipitation was adopted, and the two solutions were dropped into the reactor at the same time, and the temperature in the reactor was controlled to be 70° C., the pH of the system to be 7.0, and the reaction time to be 1 h during the precipitation process. After the two solutions are added dropwise, use 10wt% sodium carbonate solution to adjust the pH va...

Embodiment 2

[0049] Add 200g of water, 15g of ethanol, 6.0g of microcrystalline cellulose with a particle size of 5-30μm, and 0.5g of C 12-10-12 Gemini surfactant (purchased from Henan Dao Pure Chemical Co., Ltd.), then add 61.3g of 30% concentration of silica sol, and stir evenly. Dissolve 362.4g of copper nitrate, 87.7g of zinc nitrate, 22.7g of cerium nitrate, and 4.21g of calcium nitrate in 1.45kg of water to make a mixed salt solution, and dissolve 130.5g of sodium silicate and 149.0g of sodium carbonate in water to make a precipitant solution , respectively, the two solutions were heated to 75 ℃. The method of co-precipitation was adopted, and the two solutions were dropped into the reactor at the same time, and the temperature in the reactor was controlled to be 75° C., the pH of the system was 7.2, and the reaction time was 1 h during the precipitation process. After the two solutions are added dropwise, use 10wt% sodium carbonate solution to adjust the pH value of the system to >...

Embodiment 3

[0052] Add 200g of water, 10g of propanol, 10.0g of methylcellulose with a particle size of 5-20μm, and 1.0g of C 14-8-14 Gemini surfactant (purchased from Henan Dao Pure Chemical Co., Ltd.) was mixed evenly, then 116.7g of 30% concentration of silica sol was added and stirred evenly. 302g of copper nitrate, 87.7g of zinc nitrate, 5.0g of cerium nitrate, and 6.8g of barium nitrate were dissolved in 1.37kg of water to form a mixed salt solution, and 198.7g of sodium silicate and 93.6g of sodium carbonate were dissolved in water to form a precipitant solution. The two solutions were heated to 80°C separately. The method of co-precipitation was adopted, and the two solutions were dropped into the reactor at the same time, and the temperature in the reactor was controlled to be 80° C., the pH of the system was 8.0, and the reaction time was 1 h during the precipitation process. After the two solutions are added dropwise, use 10wt% sodium carbonate solution to adjust the pH value ...

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Abstract

The invention discloses a preparation method of a catalyst for preparing α-phenethyl alcohol by liquid-phase hydrogenation of acetophenone. sol, and stir evenly to prepare a silica sol water dispersion; configure a mixed salt solution containing copper, zinc, rare earth metal, alkaline earth metal compound salts and an alkaline precipitant, and add the two together to the silica sol water dispersion. In the process, the catalyst is obtained through precipitation reaction, aging, filtration, washing, drying, roasting and molding; the invention also discloses the prepared catalyst and its application. The invention adopts silica sol and silicate as composite silicon source, adds organic pore-forming agent before the precipitation process, and uses Zn, rare earth and alkaline earth metal to modify the catalyst, and is used for the liquid phase hydrogenation of acetophenone to prepare α-benzene When ethanol is used, it not only has high activity and good selectivity, but also effectively improves the liquid resistance of the catalyst, with high strength and good stability.

Description

technical field [0001] The invention belongs to the technical field of catalytic hydrogenation, and in particular relates to a catalyst for preparing α-phenethyl alcohol by liquid-phase hydrogenation of acetophenone, a preparation method and application thereof. Background technique [0002] α-Phenylethyl alcohol is an important chemical intermediate widely used in medicine, fragrance manufacturing, cosmetics, food and fine chemical industries. 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. The raw materials used in the microbial 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 o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/83B01J37/03B01J37/08B01J37/18C07C29/145C07C33/22
CPCC07C29/145B01J23/002B01J23/83B01J35/0093B01J37/0018B01J37/031B01J37/082B01J37/18B01J2523/00B01J2523/17B01J2523/22B01J2523/27B01J2523/3706B01J2523/41B01J2523/23B01J2523/3712B01J2523/25C07C33/22B01J37/03B01J37/0063
Inventor 李作金于海波詹吉山沙宇初乃波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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