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Modified graphene platinized catalyst, preparation method of modified graphene platinized catalyst and application of modified graphene platinized catalyst

A technology of platinum catalyst and graphene, which is applied in the field of modified graphene-supported platinum catalyst and its preparation, and achieves the effects of good stability, simple preparation method and mild reaction conditions

Inactive Publication Date: 2015-12-09
GUANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, 1,3-propanediamine is covalently bonded to graphene and used as a Pt catalyst carrier for the electrocatalytic oxidation of methanol, and there are no related reports.

Method used

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  • Modified graphene platinized catalyst, preparation method of modified graphene platinized catalyst and application of modified graphene platinized catalyst
  • Modified graphene platinized catalyst, preparation method of modified graphene platinized catalyst and application of modified graphene platinized catalyst
  • Modified graphene platinized catalyst, preparation method of modified graphene platinized catalyst and application of modified graphene platinized catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Example 1: Preparation of Pt / 1,3-PDA-rGO catalyst according to the method of the present invention

[0043] 1) At room temperature, mix 3.0g of natural flake graphite, 3.0g of potassium persulfate and 3.0g of phosphorus pentoxide in a 100mL round-bottomed flask, then add 24mL of concentrated sulfuric acid and mix, at 80℃, oil bath constant temperature magnetic stirring The reaction is pre-oxidized for 120 minutes, cooled to room temperature, washed with deionized water to neutrality, and dried in vacuum at 60°C to obtain pre-oxidized graphite;

[0044] 2) Add 1.0g of pre-oxidized graphite to a 250mL round-bottomed flask under an ice water bath at 0℃, then add 35mL concentrated sulfuric acid and 5mL concentrated phosphoric acid, magnetically stir evenly, and then slowly add 0.5g NaNO 3 And 3.0gKMnO 4 ,Stir the reaction for another 30min; Heat up to 35℃ and stir for 120min at constant temperature, slowly add 98mL of deionized water, then heat up to 98℃, and slowly add 30mLH 2 O...

Embodiment 2

[0069] Example 2 (The co-solvent in this example is absolute ethanol)

[0070] 1) Same as Example 1;

[0071] 2) Same as Example 1;

[0072] 3) Take 250mg of graphene oxide into a 100mL round bottom flask, add 25mL of thionyl chloride, reflux and stir for 40h at 70℃, and then distill out the excess oxalyl chloride at 110℃ to obtain graphite acyl chloride Ene

[0073] 4) In the device of step 3), add 10mL 1,3-propanediamine and 50mL freshly distilled N,N-dimethylformamide (the analytically pure N,N-dimethylformamide will be collected after vacuum distillation N,N-dimethylformamide), under the protection of nitrogen, the reaction was reacted for 12h at 85°C with constant magnetic stirring, then N,N-dimethylformamide was removed by distillation under reduced pressure, and washed with acetone and absolute ethanol each , And then washed with deionized water to neutrality, and vacuum-dried the product at 60°C for 24h to obtain 1,3-propanediamine modified graphene, denoted as 1,3-PDA-rGO; ...

Embodiment 3

[0078] Example 3 (No co-solvent is added in this example)

[0079] 1) At room temperature, mix 3.0g of natural flake graphite, 3.0g of potassium persulfate and 3.0g of phosphorus pentoxide in a 100mL round-bottom flask, then add 24mL of concentrated sulfuric acid to mix, and stir at 50°C in an oil bath at constant temperature. The reaction is pre-oxidized for 180 minutes, cooled to room temperature, washed with deionized water to neutrality, and dried in vacuum at 70°C to obtain pre-oxidized graphite;

[0080] 2) Under 2℃ ice water bath, add 1.0g of pre-oxidized graphite to 250mL round bottom flask, then add 35mL concentrated sulfuric acid and 5mL concentrated phosphoric acid, magnetically stir evenly, and then slowly add 0.5g NaNO 3 And 3.0gKMnO 4 ,Stir the reaction for another 30min; Heat to 40℃ and stir for 240min at constant temperature, slowly add 98mL of deionized water, then heat to 95℃, slowly add 30mLH 2 O 2 The concentration is 30% hydrogen peroxide and 48mL deionized wate...

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Abstract

The invention discloses a modified graphene platinized catalyst, a preparation method of the modified graphene platinized catalyst and application of the modified graphene platinized catalyst. The preparation method of the modified graphene platinized catalyst comprises the following steps that 1, graphene oxide is obtained; 2, the graphene oxide and acyl chloride agents take reaction under the heated condition to obtain acyl chloride graphene; 3, chlorization graphene and 1, 3-propane diamine are taken, methylbenzene or DMF is used as solvents, and heating reaction is carried out under the nitrogen gas protection condition to obtain 1, 3-propane diamine modified graphene; 4, the 1, 3-propane diamine modified graphene is uniformly dispersed into water to obtain mixed liquid A; predecessors of Pt catalysts are added into the mixed liquid A; ultrasonic dispersion is performed to obtain mixed liquid B; 5, NaBH4 is added into the mixed liquid B; ultrasonic dispersion is performed; modified graphene platinized catalyst is obtained. The catalyst provided by the invention has the advantages that the specific surface is large; the Pt particle dispersion is uniform; the particle size is smaller; when the modified graphene platinized catalyst is applied to DMFC (Direct Methanol Fuel Cells), higher electric catalysis capability and good long-time circulation stability are realized.

Description

Technical field [0001] The invention relates to a catalyst, in particular to a modified graphene-supported platinum catalyst and a preparation method and application thereof. Background technique [0002] Direct methanol fuel cell (DirectMethanolFuelCell, DMFC) is a new type of environmentally friendly energy conversion device. It has the advantages of small size, high specific energy density, low price, environmental friendliness, and easy storage and transportation of raw materials. It is used in aerospace, defense and military, There are broad application prospects in transportation, household portable power supplies and other fields. However, the high cost of DMFC anode catalyst, low electrocatalytic activity, and poor stability are still the main factors restricting its commercialization. [0003] Pt catalyst is currently recognized as an ideal DMFC anode catalyst. Its electrocatalytic performance for methanol is not only related to the composition, relative crystallinity and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42H01M4/92
CPCY02E60/50
Inventor 钟新仙冯崎鹏李庆余林有铖曾建强王红强
Owner GUANGXI NORMAL UNIV