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A kind of method for preparing alcohol compound by hydrogenation of carbonyl compound

A technology of carbonyl compounds and compounds, which is applied in the field of hydrogenation of carbonyl-containing compounds to prepare alcohol compounds, which can solve the problems of low carrier binding, loss, and low selectivity

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst has high requirements on the preparation of the carrier, requires various additives for modification, and is still synthesized by the impregnation method, including multiple steps such as drying and high-temperature roasting. The preparation process is cumbersome, and the catalyst active elements are only loaded on the On the carrier, the degree of binding to the carrier is low, so it is easy to lose during the reaction
[0004] In the existing nickel-based catalyst system, the active elements are easily dissolved and lost in the carbonyl-containing compound raw materials, resulting in poor reactivity, low selectivity, and short service life of the catalyst

Method used

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  • A kind of method for preparing alcohol compound by hydrogenation of carbonyl compound
  • A kind of method for preparing alcohol compound by hydrogenation of carbonyl compound
  • A kind of method for preparing alcohol compound by hydrogenation of carbonyl compound

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Example 1 Hydrogenation of 3-hydroxypropionaldehyde to prepare 1,3-propanediol

[0046] Two sets of 300mL fixed bed reactors connected in series were used, the first set of fixed beds was filled with 340g nickel oxide particles (filling volume 200mL), nitrogen atmosphere, the pressure was 0.02MPaG, the temperature was 80°C, and the second set of fixed beds was filled with 160g titanium dioxide Particles (filling volume of 200 mL), hydrogen atmosphere, pressure of 5.0 MPaG, temperature of 120 ° C, and each set of fixed-bed liquid outlet pipelines are equipped with 1000-mesh sintered filters.

[0047] The aqueous solution with 3-hydroxypropionaldehyde content of 80% flows through two sets of fixed bed reactors in sequence at a flow rate of 0.2kg / h, and after 500h of continuous reaction, the nickel content in the solution at the outlet of the first set of fixed beds is about 0.07-0.08% , In the second set of fixed bed outlet reaction solution, the residual 3-hydroxypropion...

Embodiment 2

[0050] Example 2 Hydrogenation of 3-hydroxybutyraldehyde to prepare 1,3-butanediol

[0051] Two sets of 500mL stirred tanks connected in series were used. The first set of stirred tanks was filled with 80g of deactivated Raney nickel catalysts. In a nitrogen atmosphere, the pressure was 0.02MPaG and the temperature was 100°C. The second set of stirred tanks was filled with 1g of nickel load. The amount of zirconium dioxide particles is 0.01%, the hydrogen atmosphere, the pressure is 4.0 MPaG, the temperature is 130 ° C, and each set of the liquid outlet pipeline of the stirring tank is equipped with a 1000-mesh sintered filter.

[0052] The aqueous solution with 3-hydroxybutyraldehyde content of 40% flows through two sets of stirring tanks at a flow rate of 0.3kg / h, and after 400h of continuous reaction, the nickel content in the solution at the outlet of the first set of stirring tanks is about 0.05-0.06%. In the reaction solution at the outlet of the two sets of stirred tank...

Embodiment 3

[0053] Example 3 Hydrogenation of 3-hydroxybutyraldehyde to prepare 1,3-butanediol

[0054] After the device of Example 2 was continuously operated for 400h, the nickel content in the first set of stirred tanks was less than 10 g, and continued long-term operation would cause nickel to dissolve completely in the first set of stirred tanks, so the catalysts in the first set of stirred tanks were all removed. , and change the feeding pipeline, and change the feeding route of the reaction kettle to first enter the second set of stirred tanks, and then enter the first set of stirred tanks, and recycle the catalyst in the second set of stirred tanks. At the same time, the operating conditions of the two kettles were changed as the nitrogen atmosphere in the second set of stirred kettles, the pressure was 0.02MPaG, and the temperature was 100°C, and the first set of stirred kettles was hydrogen atmosphere, with a pressure of 4.0MPaG and a temperature of 130°C.

[0055] The aqueous s...

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Abstract

The invention provides a method for preparing alcohol compounds by hydrogenation of carbonyl-containing compounds. First, the carbonyl-containing compound is contacted with a nickel catalyst precursor to obtain a nickel-containing solution, and then the nickel-containing solution is contacted and reacted with hydrogen, wherein the nickel-containing It is converted into a nickel catalyst and in-situ catalyzes the hydrogenation reaction of carbonyl-containing compounds to obtain alcohol compounds. The preparation method provided by the invention places the preparation of the nickel catalyst and the hydrogenation reaction of the carbonyl compound in the same process for the first time. It has high yield and good selectivity, so it can significantly reduce the production cost of alcohol compounds, improve production efficiency, and is especially suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for preparing alcohol compounds by hydrogenation of carbonyl-containing compounds. Background technique [0002] Alcohol compounds are a class of widely used chemical raw materials. They have good solubility and can be used as solvents. At the same time, they can also be used as raw materials or intermediates for various reactions. The synthesis of alcohol compounds can be obtained by the hydrogenation process of carbonyl-containing compounds such as aldehydes or ketones. The hydrogenation process of carbonyl compounds can be divided into two types: gas phase method and liquid phase method. At present, the liquid phase process mainly adopts nickel-based catalyst system. [0003] Chinese patent CN 102309968A discloses the preparation of an aldehyde hydrogenation catalyst, the steps are divided into: (1) preparation of alumina carrier: a) mixing alumina powder, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/141C07C31/20C07C31/125
CPCC07C29/141C07C31/205C07C31/207C07C31/125Y02P20/584
Inventor 董龙跃袁帅赵聪刘喆刘振峰吕艳红黄少峰任亚鹏许振成
Owner WANHUA CHEM GRP CO LTD