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Alpha, beta-unsaturated aldehyde ketone hydrogenation catalyst and preparation method thereof

An aldehyde and ketone hydrogenation and unsaturated technology, applied in the alpha field, can solve the problems of irregular dispersion, decreased catalytic activity, short catalyst life, etc., and achieve the effects of simple process, low energy consumption and low cost

Pending Publication Date: 2021-09-24
YINGKOU INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problem that the metal active center of the supported catalyst for α, β-unsaturated aldehyde / ketone / ketone catalysis is not positioned, the dispersion is irregular, and the catalytic activity decreases, the invention creatively adopts a three-phase emulsion polymerization process. Precisely prepare the active center of the catalyst at the three-phase interface. While solving the dispersion problem, the use of 5-50nm emulsion polymerization particles can realize the precise positioning of the metal active center; at the same time, the precise preparation of the emulsion polymerization at the three-phase interface can achieve nano-level exquisite control and save more than ordinary technology. In order to solve the problem that the loaded catalyst is easily poisoned by sulfur impurities and the catalyst life is short, the sulfur impurity shielding technology is used ingeniously, and the sulfur-friendly active metal is used to preferentially react with the sulfur impurities in the reaction system, and then shield the active center of the catalyst and protection

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  • Alpha, beta-unsaturated aldehyde ketone hydrogenation catalyst and preparation method thereof
  • Alpha, beta-unsaturated aldehyde ketone hydrogenation catalyst and preparation method thereof
  • Alpha, beta-unsaturated aldehyde ketone hydrogenation catalyst and preparation method thereof

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preparation example Construction

[0032] This paper discloses a preparation method of α, β-unsaturated aldehyde and ketone hydrogenation catalyst, comprising the following steps:

[0033] (1) Disperse the surfactant and the oil phase solvent in the co-surfactant to form an emulsified system;

[0034] (2) adding a certain concentration of chloroplatinic acid aqueous solution and the carrier to the emulsification system in sequence, adding an alkali solution to adjust the pH, continuing to drop the reducing agent until the emulsification system completely changes color, and continuing to stir for a period of time to obtain a mixing system 1;

[0035] (3) After adding solvent 1 to mixing system 1 and mixing uniformly, product 1 is obtained by filtration, and repeatedly washed several times with solvent 2 and solvent 3;

[0036] (4) After repeated washing, the product 1 was dried in a vacuum drying oven at a drying temperature of 50°C-100°C for 4-48 hours to obtain the product 2.

[0037] Preferably, the product ...

Embodiment 1

[0056] On the basis of disclosed embodiments, a method for preparing a catalyst for α, β-unsaturated aldehyde / ketone hydrogenation is disclosed, comprising the following steps:

[0057] (1) Triton X-100 and n-heptane are dispersed in n-hexanol to prepare a mixed solution;

[0058] (2) Add a certain concentration of chloroplatinic acid aqueous solution into the above mixed solution. Then add mordenite molecular sieves to the above system, adjust the pH with sodium hydroxide solution, add hydrazine hydrate solution dropwise until the emulsified system completely changes color, and stir vigorously for a period of time;

[0059] (3) Add tetrahydrofuran solution dropwise to the above system, stir vigorously for a period of time, and rinse repeatedly 4 times with distilled water and ethanol;

[0060] (4) drying in a vacuum drying oven at a drying temperature of 50° C. for 4 h to obtain a Pt-based catalyst for hydrogenation of α, β-unsaturated aldehydes / ketones.

[0061] Catalysts ...

Embodiment 2

[0071] On the basis of disclosed embodiments, a method for preparing a catalyst for α, β-unsaturated aldehyde / ketone hydrogenation is disclosed, comprising the following steps:

[0072] (1) Disperse AEO-15 and n-heptane in n-hexanol to prepare a mixed solution;

[0073] (2) Add a certain concentration of chloroplatinic acid aqueous solution to the above mixed solution, then add mordenite molecular sieve to the above system, adjust the pH with sodium hydroxide solution, add hydrazine hydrate solution dropwise until the emulsified system changes color completely, and stir vigorously a period of time;

[0074] (3) Add tetrahydrofuran solution dropwise to the above system, stir vigorously for a period of time, and rinse repeatedly 4 times with distilled water and ethanol;

[0075] (4) drying in a vacuum drying oven at a drying temperature of 100°C for 48 hours to obtain a Pt-based catalyst for hydrogenation of α,β-unsaturated aldehydes / ketones.

[0076] Preferably, the product t...

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Abstract

The invention relates to the technical field of organic chemical industry, in particular to an alpha, beta-unsaturated aldehyde ketone hydrogenation catalyst and a preparation method thereof. The invention provides the alpha, beta-unsaturated aldehyde ketone hydrogenation catalyst, and the catalyst utilizes three-phase emulsion polymerization and anti-sulfur poisoning modification, and has the following characteristics: a catalyst active center is accurately prepared on a three-phase interface of a load, a water phase and an oil phase, and accurate positioning of a metal active center can be realized while the dispersion problem is solved; nano-scale exquisite control can be achieved, and compared with a common technology, the using amount of loaded metal is saved; a sulfur impurity shielding technology is creatively adopted, sulfur-loving active metal is adopted and preferentially reacts with sulfur impurities in a reaction system, and then the active center of the catalyst is shielded and protected; the final product can be obtained through one-step reaction, calcination is not needed, and other non-volatile cations are not introduced into reaction liquid, so the method is simple in process, low in energy consumption and low in cost.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to an α, β-unsaturated aldehyde and ketone hydrogenation catalyst and a preparation method thereof. Background technique [0002] α, β-unsaturated aldehydes / ketones / ketones (cinnamaldehyde, citral, furfural and crotonaldehyde, etc.) are important chemical raw materials and intermediates. The target product α, β-unsaturated alcohol obtained by its selective hydrogenation is an important raw material and reaction intermediate in the production of perfume, medicine and other fine chemical products, and is widely used in organic synthesis. Since its own structure contains both C=C bonds and C=O bonds, the selective hydrogenation of C=O has more important significance in many studies. On the one hand, it is because the industrial value of the product obtained by the hydrogenation of the C=O bond is much higher than that of the product obtained by the hydrogenation of t...

Claims

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Application Information

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IPC IPC(8): B01J29/24C07C29/141C07C33/02C07C33/03C07C33/32C07D307/44
CPCB01J29/24C07C29/141C07D307/44B01J2229/186B01J35/23C07C33/32C07C33/02C07C33/03Y02P20/584
Inventor 高爽李振陈晓陆于悦张京京赵小龙吴晓陈红何萍葛登文
Owner YINGKOU INST OF TECH