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A kind of catalyst and its preparation method and application

A catalyst and metal technology, applied in the field of catalyst and its preparation and application, can solve problems such as large difference in properties, unsatisfactory, catalytic reaction, adverse effects of product quality and production equipment, etc., to achieve good stability, many application times, Remarkable effect of dechlorination inhibition effect

Active Publication Date: 2019-12-24
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there will be dechlorination phenomenon in this method, and other organic substances and hydrochloric acid will be generated, which will have serious adverse effects on catalytic reactions, product quality and production equipment.
[0005] The existing industrialization technology usually adopts the addition of dehalogenation inhibitors [Journal of Inner Mongolia University for Nationalities: Natural Science Edition, 2001, 16 (1): 96-100], metal additives [Petrochemical Industry, 2012, 14 (5): 515-519 ] and so on to achieve the purpose of inhibiting dehalogenation, but they are not ideal
In addition, the commonly used catalysts are activated carbon carriers. Due to the large differences in the properties of different manufacturers and different carbon sources, it has a great impact on the performance of the catalyst and its catalytic reaction.

Method used

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  • A kind of catalyst and its preparation method and application
  • A kind of catalyst and its preparation method and application
  • A kind of catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Measure 0.8mL of ammonia water with a mass concentration of 25% to 28%, 64mL of ethanol, and 160mL of deionized water, stir the three thoroughly, then add 1.6g of resorcinol, stir until completely dissolved, and slowly add 2.24ml Formaldehyde aqueous solution with a mass concentration of 37-40% was stirred at 20°C for 12 hours, then transferred to a hydrothermal reaction kettle at 80°C for 12 hours, and then centrifuged and washed to obtain a reddish-brown polymer solid powder.

[0049] Dissolve 2g of citric acid in 30ml of deionized water, then add 0.2942g of sodium chloropalladate and 6.67ml of ethylenediamine, mix and stir evenly, then transfer the mixture to a reaction kettle at 100°C for 5 hours, then freeze Drying, the relative vacuum degree is -0.05MPa, the temperature is -10°C, and freeze-drying is carried out for 10 hours to obtain a solid powder of composite noble metal carbon quantum dots. The result of ICP analysis in the composite carbon-metal quantum dots ...

Embodiment 2

[0053] Measure 0.8mL of ammonia water with a mass concentration of 25% to 28%, 48mL of ethanol, and 180mL of deionized water, stir the three thoroughly, then add 1.6g of resorcinol, stir until completely dissolved, and slowly add 1.6ml dropwise Formaldehyde aqueous solution with a mass concentration of 37-40% was stirred at 25°C for 20 hours, then transferred to a hydrothermal reaction kettle at 100°C for 15 hours, and then centrifuged and washed to obtain a reddish-brown polymer solid powder.

[0054] Dissolve 1.19g of citric acid in 165ml of deionized water, then add 0.5618g of sodium chloroplatinate and 6.67ml of ethylenediamine, mix and stir evenly, then transfer the mixture to a reaction kettle at 100°C for 24 hours, then carry out Freeze-drying, the relative vacuum degree is -0.05MPa, the temperature is -10°C, and the freeze-drying is carried out for 10 hours to obtain the quantum dot solid powder. Wherein the mass percentage of metal in the composite carbon-metal quantu...

Embodiment 3

[0058] Measure 0.8mL of ammonia water with a mass concentration of 25% to 28%, 96mL of ethanol, and 240mL of deionized water, stir the three thoroughly, then add 1.65g of resorcinol, stir until completely dissolved, then slowly add 4.48ml dropwise Formaldehyde aqueous solution with a mass concentration of 37-40% was stirred at 10°C for 30 hours, then transferred to a hydrothermal reaction kettle at 120°C for 12 hours, and then centrifuged and washed to obtain a reddish-brown polymer solid powder.

[0059] Dissolve 3g of citric acid in 60ml of deionized water, then add 0.2842g of ammonium tetrachloropalladate and 10ml of ethylenediamine, mix well, then transfer the mixture to a reaction kettle at 100°C for 20 hours, then freeze Drying, the relative vacuum degree is -0.099MPa, the temperature is -10°C, and the freeze-drying is carried out for 10 hours to obtain the quantum dot solid powder. Wherein the mass percentage of metal in the composite carbon-metal quantum dot is 90%.

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Abstract

The invention discloses a catalyst as well as a preparation method and application of the catalyst. The catalyst is composed of a carrier and a composite carbon-metal quantum dot supported on the carrier; the particle size of the catalyst ranges from 100nm to 1000nm; the carrier is a mesoporous carbon microsphere; the composite carbon-metal quantum dot is not larger than 15nm and contains 10-90% of metal; the metal in the composite carbon-metal quantum dot is one or a combination of several of platinum, palladium, iridium, ruthenium and rhodium; the loads of platinum, palladium, iridium, ruthenium and rhodium are respectively 0-10.0%, 0-10.0%, 0-10.0%, 0-10.0% and 0-5.0% based on the mass of the carrier, and the loads of palladium, platinum and rhodium are not equal to zero; and the total load of the metal is 1.0-11.5%. The invention provides the application of the catalyst to reaction for synthesizing a chlorinated aromatic amine compound shown as a formula (II) by carrying out selective catalytic hydrogenation on a chlorinated aromatic nitrocompound shown as a formula (I), and the catalyst has the characteristics of high hydrogenation reaction rate, high conversion rate, high catalytic activity and high stability.

Description

[0001] (1) Technical field [0002] The invention relates to a mesoporous carbon microsphere supported catalyst and its preparation method and application. The catalyst can be used for catalytic hydrogenation reduction reaction of chlorinated aromatic nitro compounds. [0003] (2) Technical background [0004] The process of reducing chlorinated aromatic nitro compounds to chlorinated arylamine compounds is an important basic organic synthesis reaction, and the product chlorinated arylamine compounds are a kind of organic chemical intermediates with a wide range of uses, occupying a pivotal role in the field of fine chemicals status. The reduction process mainly includes iron powder reduction method, electrochemical reduction method, alkali sulfide reduction method, catalytic hydrogenation reduction method, etc. Due to the advanced technology of catalytic hydrogenation, low energy consumption and less waste discharge, it is more in line with the requirements of modern chemical...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/42B01J23/44B01J23/46B01J32/00B01J21/18B01J37/03B01J37/08B01J37/10B01J37/18B82Y20/00B82Y30/00B82Y40/00
CPCB01J21/18B01J23/42B01J23/44B01J23/462B01J23/464B01J23/466B01J23/468B01J37/031B01J37/084B01J37/10B01J37/18B82Y20/00B82Y30/00B82Y40/00
Inventor 卢春山冯振龙齐亚妮王梦君丰枫马磊张群峰李小年
Owner ZHEJIANG UNIV OF TECH
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