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Method for preparing alpha-phenylethanol catalyst through hydrogenation of acetophenone and application

A technology for the preparation of catalysts and hydrogen, which is applied in the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc. Problems such as low conversion rate and reduced catalyst use strength, to achieve good mass transfer/heat transfer performance, uniform distribution of active components, and improved mass transfer and heat transfer performance

Active Publication Date: 2019-03-19
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1557545A has prepared Ni-Sn-B / SiO2 catalyst by impregnation method, adopts KBH after low-temperature roasting 4 As a reducing agent for reduction, when it catalyzes the reaction, the highest selectivity of phenylethyl alcohol reaches 97.5%, but its active component Ni and carrier SiO 2 Weak interaction, easy to lose
[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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  • Method for preparing alpha-phenylethanol catalyst through hydrogenation of acetophenone and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Weigh 11.67g of zinc nitrate to prepare a 1mol / L aqueous solution, carry out co-precipitation reaction with 10wt% sodium carbonate aqueous solution, control the reaction temperature at 60°C, and pH=6.8; after the reaction is completed, age at 75°C for 20min to obtain slurry 1.

[0043] Weigh 82.55g of copper nitrate and 8.48g of bismuth nitrate to prepare a mixed aqueous solution of 1mol / L, and add dropwise to slurry 1 together with 10wt% sodium carbonate aqueous solution to carry out coprecipitation reaction, control the reaction temperature to 45°C, and pH=7.2; After completion, it was aged at 65° C. for 2 hours to obtain slurry 2 .

[0044] After the aging was completed, 183.3 g of 30% silica sol was added to the slurry 2, mixed evenly, filtered, washed, dried at 100°C for 6 hours, and then calcined at 280°C for 4 hours.

[0045] After the calcination is completed, add 2g of PMMA to the catalyst powder, mix evenly, and press into tablets. The molded catalyst was sub...

Embodiment 2

[0048] Weigh 25.19g of zinc chloride to prepare a 1.5mol / L aqueous solution, carry out co-precipitation reaction with 15wt% sodium bicarbonate aqueous solution, control the reaction temperature at 65°C, and pH=7.0; after the reaction is completed, age at 70°C for 25min to obtain a slurry 1.

[0049] Take by weighing 69.36g cupric chloride and 4.06g bismuth chloride and be mixed with the mixed aqueous solution of 1.5mol / L, and add dropwise in slurry 1 together with 15wt% sodium carbonate aqueous solution and carry out co-precipitation reaction, control reaction temperature 40 ℃, PH= 7.0; aging at 70° C. for 2.5 hours after completion of the reaction to obtain slurry 2.

[0050] After aging, add 41g of fumed silica with a particle size of 5-10nm to the slurry 2, mix evenly, filter, wash, dry at 105°C for 7h, and bake at 300°C for 5h.

[0051] After the calcination is completed, 4 g of microcrystalline cellulose is added to the catalyst powder, mixed evenly, and then pressed int...

Embodiment 3

[0054] Weigh 25.84g of zinc sulfate to prepare a 2mol / L aqueous solution, carry out co-precipitation reaction with 20wt% potassium carbonate aqueous solution, control the reaction temperature to 70°C, pH=7.2; after the reaction is completed, age at 65°C for 30min to obtain slurry 1.

[0055] Weigh 100.31g of copper sulfate and 6.06g of bismuth sulfate to prepare a mixed aqueous solution of 2mol / L, and dropwise add it to slurry 1 together with 20wt% potassium carbonate aqueous solution to carry out coprecipitation reaction, control the reaction temperature to 35°C, and pH=6.8; After completion, it was aged at 75°C for 3 hours to obtain slurry 2.

[0056] After the aging was completed, 38.9 g of diatomite with a silicon dioxide content of 90% was added to the slurry 2, mixed evenly, filtered, washed, dried at 110°C for 8 hours, and calcined at 320°C for 6 hours.

[0057] After the calcination is completed, add 6 g of scallop powder to the catalyst powder, mix evenly, and press i...

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Abstract

The invention relates to a method for preparing an alpha-phenylethanol catalyst through hydrogenation of acetophenone and application. The catalyst contains copper oxide, zinc oxide, silicon dioxide and bismuth oxide. The method of the catalyst is realized by virtue of a sub-step precipitation method and comprises the following steps: precipitating zinc salt and a precipitator at a certain temperature, and aging, so as to obtain slurry (1); adding a mixed solution of copper salt and bismuth salt as well as the precipitator into the slurry (1), carrying out coprecipitation, and aging, so as toobtain slurry (2); adding carrier silicon into the slurry (2), and uniformly stirring and mixing, so as to obtain slurry (3); filtering, washing, drying and roasting the slurry (3), so as to obtain catalyst powder; adding a certain amount of pore forming agents into the catalyst powder, and carrying out piece formation; and carrying out secondary roasting on the formed catalyst, so as to obtain the final catalyst. The catalyst prepared by virtue of the method is large in pore volume and aperture, good in mass transfer property and heat transfer property and high in activity and selectivity.

Description

technical field [0001] The invention belongs to the technical field of catalytic hydrogenation, and in particular relates to a preparation method of a catalyst for preparing α-phenethyl alcohol by liquid-phase hydrogenation of acetophenone. 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 catalytic hydrogenation of acetophenone. [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 of low production cost, few by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/843C07C33/22C07C29/145
CPCB01J23/002B01J23/8437B01J2523/00C07C29/145B01J2523/17B01J2523/27B01J2523/54C07C33/22
Inventor 于海波李作金詹吉山沙宇孙康初乃波黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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