Preparation method and application for high-activity hydrogenation reaction catalyst

A hydrogenation reaction and catalyst technology, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, organic compounds/hydrides/coordination complex catalysts, etc. High reproducibility, easy storage, and high catalytic activity

Active Publication Date: 2018-11-23
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Its disadvantage is that the preparation process of the catalyst is complicated, and it is easy to cause pollution during the preparation process.

Method used

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  • Preparation method and application for high-activity hydrogenation reaction catalyst
  • Preparation method and application for high-activity hydrogenation reaction catalyst
  • Preparation method and application for high-activity hydrogenation reaction catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Preparation of polystyrene aldehyde-based microspheres:

[0025] (1) Add 18mL of absolute ethanol, 25mL of deionized water and 2.5g of polyvinylpyrrolidone (PVP) into a three-necked flask equipped with a condenser, and place it in a constant temperature water bath at 70°C, mechanically stir and keep the speed at 315r / min.

[0026] (2) Dissolve 0.1 g of initiator AIBN in 6 mL of styrene to obtain monomeric styrene in which the initiator AIBN is dissolved.

[0027] (3) Add monomer styrene dissolved in initiator AIBN to the system obtained in (1), and add 2.53g (3.0ml) acrolein (C 3 h 4 O), after constant temperature reaction for 7 hours, add hydrochloric acid and increase the temperature of constant temperature water bath to 80°C for 12 hours, after stopping the reaction, wash with ethanol / water and ultrasonic several times, centrifuge and dry to obtain polystyrene aldehyde Ball (PS-CHO).

[0028] 2. Preparation of surface-modified palladium nanoparticles (PS-CHO@P...

Embodiment 2、3、4、5

[0036] The same steps as in Example 1 will not be repeated here, only the reaction time for preparing aniline in step 3 is changed, which are 5h, 24h, 48h, and 49h, respectively.

[0037] Other steps are the same as in Example 1.

[0038] Two, embodiment 1-5 test result analysis:

[0039] UV spectrum characterization:

[0040] The ultraviolet spectrum characterization was carried out on a UV-721 ultraviolet spectrophotometer, the experimental temperature was 25°C, and the solution was diluted to 10 -5~10 -6 Order of magnitude, the measurement wavelength range is 200-800nm, find out the maximum absorption peak, the absorption peak of nitrobenzene is around 260nm, and the absorption peak of aniline is around 286nm. At 4h, 5h, 24h, 48h, and 49h, the conversion rates of nitrobenzene were 5%, 7.66%, 20.01%, 40.53%, and 42.24% respectively; the yields of aniline were 0, 0, 6.8%, 8.7%, respectively. 11.82%.

Embodiment 6

[0042] A preparation method for a highly active hydrogenation reaction catalyst, comprising the steps of:

[0043] 1) Using azobisisobutyronitrile as the initiator, polyvinylpyrrolidone as the dispersant, and ethanol and water as the solvent, copolymerize styrene and acrolein to prepare a polystyrene aldehyde-based microsphere emulsion, which is centrifuged Separation, washing, and drying to obtain polystyrene aldehyde-based microspheres; wherein the mass of dispersant, initiator, styrene and acrolein are 2.4g, 0.08g, 5g (5.5ml), 2.2g (2.6ml) respectively; The specific method is: Dissolve polyvinylpyrrolidone in a mixed solution of ethanol and deionized water to form a polyvinylpyrrolidone solution, wherein the dosages of polyvinylpyrrolidone, ethanol and deionized water are 2.4g and 14g (17.5ml) respectively , 24g (24ml); The initiator azobisisobutyronitrile is dissolved in styrene to obtain the monomeric styrene that is dissolved with the initiator AIBN; then the polyvinylpy...

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Abstract

The invention discloses a preparation method for a high-activity hydrogenation reaction catalyst, and relates to the field of preparation methods for chemical materials. According to the preparation method, polystyrene microspheres subjected to surface functionalization serve as a matrix, the surfaces of the polystyrene microspheres are modified with palladium nanoparticles so as to obtain the catalyst of a palladium nanoparticle@PS core-shell structure, the catalyst can be used for carrying out catalytic hydrogenation reaction on nitrobenzene to prepare aniline, can be stably stored in the air and can be easily separated from reactants, the catalytic efficiency is high, the preparation process is simple, and the repeatability is high.

Description

technical field [0001] The invention relates to a material used as a catalyst, in particular to a hydrogenation reaction catalyst used in the preparation of aniline by catalytic hydrogenation of nitrobenzene. Background technique [0002] In the prior art, aniline is an important intermediate for the synthesis of many fine chemicals and has a wide range of uses. It is the raw material for more than 300 chemical products and intermediates, and has broad prospects for development and utilization. In the polyurethane synthesis industry, it is used as a raw material for isocyanate to meet the growing demand. The industrial production methods of aniline include nitrobenzene iron powder reduction method, nitrobenzene catalytic addition and phenol amination method, among which noble metal catalytic nitrobenzene catalytic hydrogenation method is the most common, noble metal catalytic system has the advantages of high catalytic activity and long service life. , but high production c...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C209/36C07C211/46
CPCC07C209/32B01J31/06B01J2231/64B01J35/393B01J35/397C07C211/46
Inventor 严长浩刘康宇陈灏洋吴翰
Owner YANGZHOU UNIV
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