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N-doped graphene loaded Pd catalyst, preparation method thereof and application of catalyst

A catalyst, graphene technology, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as reducing catalyst activity and stability, increasing operational complexity and cost, and secondary pollution. , to achieve good catalytic dechlorination performance, simplified separation or purification process, good stability

Active Publication Date: 2018-03-09
舞阳县奥凯医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of catalytic hydrodechlorination, a large amount of by-product HCl will be produced, which will cause catalyst Cl poisoning or dissolve the catalyst, reducing the activity and stability of the catalyst.
Adding a large amount of alkali additives such as NaOH and triethylamine to the reaction system can effectively inhibit catalyst poisoning, but the addition of alkali additives in the reaction system will cause secondary pollution, increasing the complexity and cost of the operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The preparation process of the present embodiment N-doped graphene supported Pd catalyst and its application process in chlorinated phenol catalytic dechlorination are as follows:

[0041] 10 mg of palladium chloride and 50 mg of dicyandiamide were dissolved in 40 ml of ethanol and stirred at 50 °C for two hours, then 0.10 g of graphene was added, and the suspension was stirred at 50 °C for another two hours. The mixture was cooled to room temperature, vacuum-dried at 60 °C for two hours, and then pyrolyzed at 800 °C for two hours under an argon atmosphere to reduce metal palladium at high temperature to obtain an N-doped graphene-supported Pd catalyst.

[0042] Add 5.0 mg of the catalyst into 6 mL of 4-chlorophenol solution with a concentration of 2.5 g / L, pass in hydrogen gas at a pressure of 1 atm, react at room temperature for 1.5 h, and take out the reaction solution after cooling. The reaction liquid was analyzed by gas chromatography, and the dechlorination conve...

Embodiment 2

[0044] The preparation process of the present embodiment N-doped graphene supported Pd catalyst and its application process in chlorinated phenol catalytic dechlorination are as follows:

[0045] 30 mg of palladium nitrate and 150 mg of urea were dissolved in 40 ml of n-propanol and stirred at 70 °C for two hours, then 0.20 g of graphene was added and the suspension was stirred at 70 °C for another two hours. The mixture was cooled to room temperature, vacuum-dried at 70 °C for two hours, and then pyrolyzed at 600 °C for two hours under an argon atmosphere to reduce metal palladium at high temperature to obtain N-doped graphene-supported Pd catalyst.

[0046] Add 5.0 mg of the catalyst into 3 mL of 4-chlorophenol solution with a concentration of 3.0 g / L, pass in hydrogen gas at a pressure of 1 atm, react at room temperature for 2 h, and take out the reaction solution after cooling. The reaction liquid was analyzed by gas chromatography, and the dechlorination conversion rate o...

Embodiment 3

[0048] The preparation process of the present embodiment N-doped graphene supported Pd catalyst and its application process in chlorinated phenol catalytic dechlorination are as follows:

[0049] 70 mg of palladium sulfate and 200 mg of urea were dissolved in 30 ml of isopropanol and stirred at 60 °C for two hours, then 0.4 g of graphene was added and the suspension was stirred at 60 °C for another two hours. The mixture was cooled to room temperature, vacuum-dried at 60 °C for two hours, and then pyrolyzed at 800 °C for two hours under an argon atmosphere to reduce metal palladium at high temperature to obtain an N-doped graphene-supported Pd catalyst.

[0050] Add 5.0 mg of the catalyst into 3 mL of 4-chlorophenol solution with a concentration of 3.0 g / L, pass in hydrogen gas at a pressure of 1 atm, react at room temperature for 2 h, and take out the reaction solution after cooling. The reaction liquid was analyzed by gas chromatography, and the dechlorination conversion rat...

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Abstract

The invention provides an N-doped graphene loaded Pd catalyst, and belongs to the technical field of chlorinated phenol catalyzed dechlorination environmental protection. The catalyst takes N-doped layered graphene as a carrier and a metal Pd as an active component, and the metal Pd accounts for 0.1-9% of the weight of the whole catalyst. The invention further provides a preparation method and anapplication of the catalyst. The preparation method includes the steps: dissolving metal Pd compounds and nitrogen compounds in alcohol; stirring mixture, adding the graphene, and continuing to stir mixture; cooling the mixture to reach the indoor temperature, and performing high-temperature reduction after vacuum drying until a loaded metal element palladium reach zero valence to obtain the N-doped graphene loaded Pd catalyst. The catalyst is mild in reaction condition when being used for chlorinated phenol dechlorination, the chlorinated phenol can be completely dechlorinated at normal temperature and normal pressure, the catalyst is good in stability, the chlorinated phenol with high concentration can be catalyzed and dechlorinated by the catalyst, and reactant concentration can reach 3.0g / L when the chlorinated phenol catalyzed and dechlorinated by the catalyst prepared by the method.

Description

technical field [0001] The invention belongs to the technical field of chlorinated phenol catalytic dechlorination and environmental protection, and specifically relates to an N-doped graphene-supported Pd catalyst, a preparation method and application thereof. Background technique [0002] Chlorinated phenolic organic compounds are a very important class of chemical raw materials and are widely used in the production of dyes, preservatives, herbicides and insecticides. Such compounds have good chemical stability and thermal stability, and are not easy to be decomposed or biodegraded. The extensive use in industrial and agricultural production has caused serious pollution to the environment. Therefore, the study on the removal of chlorinated phenol pollutants is of great significance to the ecological environment and human health. [0003] In recent years, catalytic hydrodechlorination technology has been widely used in the elimination of hydrodechlorination of chlorinated ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24A62D3/34A62D101/22A62D101/47
CPCA62D3/34A62D2101/22A62D2101/47B01J27/24B01J37/08B01J37/16
Inventor 蒋维东徐斌
Owner 舞阳县奥凯医药科技有限公司
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