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Hydrogenation catalyst, preparation method and application thereof, and preparation method of cyclohexyl formic acid

A technology of hydrogenation catalyst and auxiliary agent, which is used in catalyst activation/preparation, ozone oxidation to prepare carboxylic acid, metal/metal oxide/metal hydroxide catalyst, etc., can solve the problem of high unit consumption of precious metal catalyst, high separation difficulty, Reaction selectivity decline and other problems, to achieve the effect of continuous and stable operation, continuous and convenient operation, and improve catalytic activity

Pending Publication Date: 2022-06-21
HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The weak point of this method is: at first, the benzoic acid reactivity of fusion is low, and processing condition is harsh, and precious metal palladium is expensive; Secondly, when adopting still reaction technique to carry out benzoic acid hydrogenation reaction, technique is comparatively complicated, and product and Contacting the catalyst for a long time will increase the secondary reaction, reduce the reaction selectivity, and easily lead to catalyst poisoning and shorten the service life of the catalyst; in addition, because the hydrogenation catalyst is usually powdery, it is difficult to separate from the reaction raw materials and products. Larger losses during filtration separation and catalyst regeneration, resulting in higher unit consumption of precious metal catalysts

Method used

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  • Hydrogenation catalyst, preparation method and application thereof, and preparation method of cyclohexyl formic acid
  • Hydrogenation catalyst, preparation method and application thereof, and preparation method of cyclohexyl formic acid
  • Hydrogenation catalyst, preparation method and application thereof, and preparation method of cyclohexyl formic acid

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preparation example Construction

[0031] The preparation method according to the present invention includes step (2): contacting the modified carrier with a solution containing the precursor of the active component and the precursor of the auxiliary component to obtain the precursor loaded with the active component and the auxiliary component The supported carrier of the precursor is calcined after removing at least part of the volatile components in the supported carrier to obtain a hydrogenation catalyst precursor.

[0032] In step (2), the active component is ruthenium. In the present invention, the term "active component precursor" refers to a substance that can form an active component in the catalyst during the catalyst preparation process. The active component precursor is preferably one or more of ruthenium chloride, ruthenium nitrate and ruthenium acetate. The auxiliary components are one or more of nickel, iron and cobalt. In the present invention, the term "auxiliary component precursor" refers to...

preparation Embodiment 1

[0065] (1) At a temperature of 20 °C, impregnated activated carbon (purchased from Shenhua Group, with a specific surface area of ​​950 m) with 25 mL of sodium hydroxide aqueous solution 2 / g) for 2 hours, then the impregnated activated carbon was washed with deionized water until the pH value of the washed water was 7.2, and then the washed solid matter was dried at 100° C. for 10 hours to obtain a modified carrier.

[0066] (2) At a temperature of 50 °C, use 25 mL of RuCl 3 and NiCl 2 The modified carrier prepared in step (1) was impregnated with the aqueous solution for 15 hours, and the impregnated modified carrier was dried at 80°C for 20h, and then calcined in an air atmosphere at 180°C for 10h to obtain a catalyst precursor. Wherein, in the aqueous solution that step (2) adopts, RuCl 3 The concentration is 3.68×10 -5 mol / mL, NiCl 2 The concentration is 3.45×10 -5 mol / mL, the molar ratio of the NaOH used in step (1) to the total amount of Ru and Ni in step (2) is 3:...

preparation Embodiment 2

[0075] The hydrogenation catalyst was prepared by the same method as in Preparation Example 1, except that in step (2), the calcination was carried out at a temperature of 300°C. The compositions of the prepared hydrogenation catalysts are listed in Table 1.

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Abstract

The invention discloses a hydrogenation catalyst as well as a preparation method and application thereof, and further relates to a preparation method of cyclohexyl formic acid by adopting the hydrogenation catalyst. According to the present invention, the hydrogenation catalyst contains a carrier, and an active component, an auxiliary agent component and an alkali metal element loaded on the carrier, the active component is ruthenium, and the auxiliary agent component is one or more than two selected from nickel, iron and cobalt. The hydrogenation catalyst provided by the invention has high catalytic activity at low temperature, can be used as a catalyst for hydrogenation reaction for preparing cyclohexyl formic acid through benzoic acid hydrogenation, can perform reaction under mild reaction conditions, and can obtain improved product selectivity. According to the preparation method of the cyclohexyl formic acid, the continuous and stable operation of the device can be realized.

Description

technical field [0001] The invention relates to a hydrogenation catalyst, a preparation method and application thereof, and a preparation method of cyclohexylcarboxylic acid using the hydrogenation catalyst. Background technique [0002] Cyclohexylcarboxylic acid (ie, ) and its derivatives are important organic chemical raw materials and intermediates of drugs, and have a wide range of application value in drug synthesis and new material research and development. Cyclohexylformic acid is mainly used in the synthesis of photoinitiator 184 (ie, 1-carboxycyclohexyl phenyl ketone), and can also be used as a solubilizer for vulcanized rubber, a clarifying agent for petroleum and a pharmaceutical intermediate, and is used for anti-progesterone drugs. 392 and the synthesis of the schistosomiasis drug praziquantel. [0003] Cyclohexylcarboxylic acid can be produced by hydrogenating benzoic acid. The catalyst for the hydrogenation of benzoic acid to cyclohexyl formic acid is main...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J37/02B01J37/08B01J37/16B01J37/18C07C51/36C07C61/08
CPCB01J23/892B01J23/8906B01J23/8913B01J37/0207B01J37/082B01J37/16B01J37/18C07C51/36C07C2601/14C07C61/08
Inventor 佘喜春向明林王慧匡洪生敖博
Owner HUNAN CHANGLING PETROCHEM SCI & TECH DEV CO LTD
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