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Mild and rapid synthesis of NMPA and Pd@RGO catalyst

A catalyst, palladium carbon catalyst technology, applied in the field of Pd@RGO catalyst, can solve the problems of cumbersome steps and achieve the effect of simple process conditions, strong adhesion and high purity

Inactive Publication Date: 2017-12-05
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the supported palladium carbon catalyst can be prepared using the above method, the steps are relatively cumbersome

Method used

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  • Mild and rapid synthesis of NMPA and Pd@RGO catalyst
  • Mild and rapid synthesis of NMPA and Pd@RGO catalyst
  • Mild and rapid synthesis of NMPA and Pd@RGO catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Accurately weigh 1 g of palladium chloride, dissolve it completely with a certain amount of concentrated hydrochloric acid, and dilute to 100 mL with distilled water to prepare a 10 mg / mL palladium chloride solution. Weigh 400 mg of reduced graphene oxide and add it to a beaker filled with 10 mL of distilled water, seal it with a plastic film and sonicate it for 20 minutes at 298±1K. Then 10 mL of 10 mg / mL palladium chloride solution was weighed and added to the suspension, and then ultrasonicated at the same temperature for 20 minutes. Immediately adjust the pH value to 9-10 with sodium hydroxide. Then let it stand for 24 hours, filter, dry for 8 hours, cool to room temperature, treat at 300°C for 2 hours, and finally 300°C under H 2 After reduction for 3h, the Pd@RGO catalyst was obtained.

[0044] X-ray powder diffraction (XRD), field emission scanning electron microscopy (FESEM), low temperature nitrogen adsorption (BET), inductively coupled plasma optical emissio...

Embodiment 2

[0048] Accurately weigh 5 g of N-methylene-4-aminoanisole, dissolve it in 50 mL of tetrahydrofuran and pour it into the autoclave, then add 50 mg of the catalyst of Example 1, and feed into H 2 After replacing the air in the reactor, close the outlet valve. At room temperature, H 2 To 6MPa, turn on the stirring to start the reaction, react for 2h, after the end of the reaction, centrifuge, and remove the reaction liquid for gas chromatographic analysis. The conversion rate of N-methylene-4-aminoanisole is 80.95%, and the selectivity of N-methyl-4-aminoanisole is 85%, which is better than the Pd / C catalyst purchased on the market under the same conditions .

Embodiment 3

[0050] Weigh 400mg of activated carbon and add it to a beaker filled with 10mL of distilled water, seal it with a plastic film and ultrasonicate for 20 minutes at 298±1K. Then 10 mL of 10 mg / mL palladium chloride solution was weighed and added to the suspension, and then ultrasonicated at the same temperature for 20 minutes. Immediately adjust the pH value to 9-10 with sodium hydroxide. Then let it stand for 24 hours, filter, dry for 8 hours, cool to room temperature, treat at 300°C for 2 hours, and finally 300°C under H 2 After reduction for 3h, the Pd / C catalyst supported by activated carbon was obtained.

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Abstract

The invention discloses mild and rapid synthesis of NMPA (N-methyl-p-anisidine) and a Pd@RGO catalyst. The Pd@RGO catalyst is a uniformly-distributed Pd@RGO catalyst which is obtained by employing palladium chloride and reduced graphene oxide for impregnation adsorption and adopting a hydrogen reduction method for processing. The Pd@RGO catalyst prepared by a method disclosed by the invention is uniform in component distribution, strong in adhesive force, high in purity and free of impurities, and is excellent in catalytic performance. The method disclosed by the invention is simple in process conditions, reaction materials are cheap, palladium loading capacity is high, and the Pd@RGO catalyst is suitable for industrial production, and can be widely applied to a plurality of fields such as petrochemical engineering, medical industry, electronic industry, perfume industry and dye industry.

Description

technical field [0001] The invention relates to the synthesis of N-methyl-4-aminoanisole (NMPA) and the Pd@RGO catalyst used therein. Background technique [0002] N-methyl-4-aminoanisole is an ether-containing non-metal gasoline antiknock agent, which can be synthesized by N-alkylation of p-anisidine. Compared with non-metallic gasoline antiknock agents, metal antiknock agents are easy to accumulate in the combustion chamber, valves and spark plugs during use, which affects the working performance of the engine. Since the non-metallic gasoline antiknock agent can effectively overcome the above problems, it is of great significance to develop nonmetallic gasoline antiknock agents such as N-methyl-4-aminoanisole. [0003] At present, researchers at home and abroad have proposed different synthesis processes for N-methyl-4-aminoanisole, each with advantages and disadvantages. Elangovan S et al. (Elangovan S, Neumann J, Sortais J B, et al. Efficient and selective N-alkylation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/08B01J37/18B01J37/34C07C213/02C07C217/84
CPCB01J23/44B01J37/08B01J37/18B01J37/343C07C213/02C07C249/02C07C251/08C07C217/84
Inventor 黎学明舒湛杨海峰祝凡尹艳君杨文静
Owner CHONGQING UNIV