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Diadema setosum-type PdCuIr nitrogen reduction electrocatalyst and preparation method thereof

An electrocatalyst, sea urchin-like technology, applied in the field of long-needle sea urchin-like PdCuIr nitrogen reduction electrocatalysts and its preparation, can solve the problems of unfavorable and sustainable development, complicated synthesis process, etc., achieve rapid reaction, simple synthesis, and high application prospects Effect

Active Publication Date: 2019-01-11
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the synthesis process of these methods is complex and requires the use of toxic solvents, which is not conducive to sustainable development

Method used

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  • Diadema setosum-type PdCuIr nitrogen reduction electrocatalyst and preparation method thereof
  • Diadema setosum-type PdCuIr nitrogen reduction electrocatalyst and preparation method thereof
  • Diadema setosum-type PdCuIr nitrogen reduction electrocatalyst and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] A kind of preparation method of long needle sea urchin shape PdCuIr nitrogen reduction electrocatalyst, described method comprises the steps:

[0040] 1) Prepare a 20mM aqueous solution of sodium chloropalladate, copper chloride and iridium chloride, then mix 2.5mL, 1.0mL and 1.0mL of sodium chloropalladate, copper chloride and iridium chloride respectively;

[0041] 2) 2.0 mL of hydrochloric acid with a concentration of 6M, 2.0 mL of ascorbic acid solution with a concentration of 0.1 M, 200 mg of KBr and 50 mg of F127 were ultrasonically mixed, and ultrasonicated for 10 minutes to form a clear solution;

[0042] 3) Mix the two solutions under stirring, put them in an oil bath and react at 95°C for 30 minutes, after the reaction is completed, wash, centrifuge, and dry to obtain the long-needle sea urchin-like PdCuIr nitrogen-reducing electrocatalyst .

[0043] The SEM picture of the long needle sea urchin shape PdCuIr catalyst obtained sees figure 1 , the TEM image of...

Embodiment 2

[0046] A kind of preparation method of long needle sea urchin shape PdCuIr nitrogen reduction electrocatalyst, described method comprises the steps:

[0047] 1) Prepare a 20mM aqueous solution of sodium chloropalladate, copper chloride and iridium chloride, then mix 1.5mL, 1.5mL and 1.5mL of sodium chloropalladate, copper chloride and iridium chloride solutions;

[0048] 2) 2.0 mL of hydrochloric acid with a concentration of 6M, 2.0 mL of ascorbic acid solution with a concentration of 0.1 M, 200 mg of KBr and 50 mg of F127 were ultrasonically mixed, and ultrasonicated for 10 minutes to form a clear solution;

[0049] 3) Mix the two solutions under stirring, put them in an oil bath and react at 95°C for 60 minutes, after the reaction is completed, wash, centrifuge, and dry to obtain the long-needle sea urchin-like PdCuIr nitrogen-reducing electrocatalyst .

[0050] The SEM picture of the sea urchin shape PdCuIr catalyst that obtains sees Figure 10 , the electric double layer...

Embodiment 3

[0053] A kind of preparation method of long needle sea urchin shape PdCuIr nitrogen reduction electrocatalyst, described method comprises the steps:

[0054] 1) Sodium chloropalladate, cupric chloride and iridium chloride are dissolved in deionized water, and their concentration is 1mM;

[0055] 2) 0.1 mL of hydrochloric acid with a concentration of 1M, 0.5 mL of ascorbic acid solution with a concentration of 0.01 M, 10 mg of KBr and 10 mg of F127 were ultrasonically mixed, and ultrasonicated for 5 minutes to form a clear solution;

[0056] 3) Mix the two solutions under stirring, put them into an oil bath and react at 80° C. for 5 minutes, after the reaction is completed, wash, centrifuge, and dry to obtain the catalyst.

[0057] Due to the low concentration of sodium chloropalladate, copper chloride and iridium chloride solution, few products are obtained, and the amount of ascorbic acid and KBr is very small, it is difficult to completely reduce the Pd and Ru metal sources,...

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Abstract

The invention discloses a diadema setosum-type PdCuIr nitrogen reduction electrocatalyst and a preparation method thereof. The preparation method comprises: dissolving sodium chloropalladite, copper chloride and iridium chloride in deionized water, controlling concentrations in a range of 1 and 40 mM, mixing the solution, adding 10 to 500 mg of KBr, 10 to 100 mg of a surfactant F127, 0.5 to 5 mL of ascorbic acid having a concentration of 0.01 to 0.1 mol / L and 0.1 to 1 mL of a HCl solution with a concentration of 1 to 10 mol / L into the mixture, carrying out ultrasound treatment for 5 to 15 minto obtain a clear solution, putting the clear solution in an oil bath pot, carrying out a reaction process at 80 to 120 DEG C for 5 to 90 min, and carrying out washing, centrifugation and drying to obtain the diadema setosum-type PdCuIr nitrogen reduction electrocatalyst. The preparation method has simple processes and very short reaction time. The diadema setosum-type PdCuIr nitrogen reduction electrocatalyst has excellent electrochemical synthetic ammonia performances.

Description

(1) Technical field [0001] The invention relates to a long-needle sea urchin-like PdCuIr nitrogen reduction electrocatalyst and a preparation method thereof, and the catalyst can be used in the research of electrochemical synthesis of ammonia. (2) Background technology [0002] Ammonia can be used to synthesize fertilizers, dyes, fibers, explosives and other important materials, so it is extremely important to human survival and development. In addition, ammonia contains high hydrogen content and does not contain carbon elements, so it is an ideal clean energy carrier. In 2017, the global ammonia production was about 150 million tons, and it will continue to grow at an annual rate of 8%. At present, ammonia is mainly synthesized by the Haber-Bosch method in industry, and its main mechanism is to dissociate nitrogen and hydrogen under the action of a catalyst and high temperature and pressure, and then combine into ammonia (Ertl, G. Reactions at Surfaces: From Atoms to Compl...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J35/02B01J35/10B01J37/16C25B1/00C25B11/06
CPCC25B1/00B01J23/8926B01J37/16C25B11/091B01J35/50B01J35/33B01J35/61
Inventor 王亮杨良明王自强薛海荣许友王鸿静
Owner ZHEJIANG UNIV OF TECH
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