MOF-based platinum monatomic catalyst, and preparation and application thereof

A catalyst and atom technology, which is applied in the field of electrochemical energy, achieves the effects of simple preparation method, reduced cost, and favorable promotion and use

Pending Publication Date: 2021-06-25

TONGJI UNIV

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AI-Extracted Technical Summary

Problems solved by technology

The preparation of stable single-atom catalysts du...

Method used

As shown in Figure 6, with ZrO standard spectrum (card: PDF#49-1642-ZrO ) comparison shows, the MOF catalyst (marked as UIO-66-NH ) prepared by embodiment 7, in embodiment 2 Both the solution (marked as chloroplatinic acid) after high temperature carbonization and the solution without pickling after high temperature carbonization (marked as platinum acetylacetonate) in Example 6 contained zirconium dioxide. Therefore, the step of adding acid washing can wash off the inert substances on the catalyst, so that the active sites can be fully exposed, thereby improving the catalytic performance.

This catalyzer is applied on fuel cell cathode, has made a kind of fuel cell cathode electrode with good electrochemical performance, through electrochemical test, the half-slope point position of this electrode in 0.1M KOH solution is 0.75V, The stability in ammonia solution is higher than that of ...

Abstract

The invention belongs to the technical field of electrochemical energy, and provides an MOF-based platinum monatomic catalyst, preparation and application. Zirconium chloride, 2-aminoterephthalic acid and a platinum source are used as raw materials, a regulating acid is used for regulating the nucleation speed of a metal framework, and the MOF-based platinum monatomic catalyst is synthesized in situ through a solvothermal method. The molar ratio of the zirconium chloride to the 2-aminoterephthalic acid to the platinum source is 0.9: 0.9: (0.5-3), and the high-temperature carbonization temperature is 800-1000 DEG C. The catalyst takes a metal framework as a monatomic carrier, and platinum is dispersed on the metal framework in a monatomic dispersion state. The catalyst is applied to a fuel cell cathode, a fuel cell cathode electrode with high electrochemical performance is prepared, the half slope point position of the electrode in a 0.1 M KOH solution is 0.75 V, and the stability of the electrode in an ammonia solution is higher than that of commercial platinum carbon. The preparation method is simple, the cost of the catalyst is reduced to a great extent, and popularization and application are facilitated.

Application Domain

Cell electrodes

Technology Topic

CarbonizationMetal framework +9

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Examples

Experimental program(8)
Effect test(7)

Example Embodiment

[0031] The method of preparing a MOF-based platinum monoimer catalyst provided by the present invention includes the following steps:

[0032] Step S1, the zirconium chloride, 2-amino group terephthalic acid and the platinum source were added to the mixed solution of DMF and the acidic mixed solution, and the reaction was carried out, then washed, then the washed substance was dried, and the film was dried to give a dry material ;

[0033] Step S2, in an inert gas atmosphere, a high temperature carbonization of 800 ° C to 1000 ° C is carbonized to obtain a carbonized substance;

[0034] Step S3, submerged the carbonized substance is soaked, and the MOF-based platinum monoimer catalyst is obtained.

[0035] In the above step S1, zirconium chloride, 2-amino phenylene terephthalic acid and a platinum source of 0.9: 0.9: 0.5 to 3. Platinum source is any one of chloroplatinic acid, acetylacettone or platinum. In the present invention, only chloroplatinic acid and acetylacetoplatin are described as an example, and platinum can achieve the same technical effect. The chloroplatinate used in the present invention is H 2 PTCL 6.6h 2 O, use DMF as a solvent, formulated a concentration of 1 mg / ml of chloroplatinic acid solution. Accordingly, zirconium chloride, 2-amino phenylene terephthalic acid to a platinum source is 210 mg of zirconium chloride, 2-amino paffle terephthalic acid is from 163 mg and platinum source 0.5 ml to 3 ml.

[0036] In the above step S1, the acid was adjusted as glacial acetic acid (concentration 17.5 mol / L) or concentrated hydrochloric acid (concentration: 12 mol / L). When the amount of zirconium chloride was added to 0.9 mmol (210 mg), DMF was 10 mL to 40 mL, and the acid was 2.4 ml to 9.6 mL.

[0037] Glacial acetic acid and hydrochloric acid can regulate the nucleation speed of the metal skeleton. The nucleation speed of the metal skeleton is adjusted with glacial acetic acid, and most of the transistor materials are generated. Most of the MOF-regulated MOF-adjusted hydrochloric acid forms an amorphous material. For the present invention, the adjustment effect of the glacial acetic acid is better than the modulation effect of hydrochloric acid, but the performance of the catalyst prepared using hydrochloric acid is still better than commercial platinum carbon catalysts.

[0038] In the above step S1, zirconium chloride, 2-amino group is dissolved in dimethylformamide and the platinum-containing solution, and the vial is placed in an oven to react in an oven, the oven temperature is 120 ° C. ~ 180 ° C. After the reaction, centrifugation was centrifuged after cooling to room temperature, and the wash solvent was one or several of methanol, dimethylformamide, ethanol. The centrifugation speed is 6000 rpm to 10,000 rpm, and the centrifugal time is 1 min ~ 5min. The centrifuged substance was dried in vacuo to 60 ° C to 80 ° C for 8 h to 12 hours to give a dry material.

[0039]In the above step S2, the dried material is taken from 1 h to 4 h under nitrogen or argon atmosphere, and the high temperature treatment temperature is 800 ° C to 1000 ° C to obtain a carbonized substance.

[0040] In the above-described step S3, the carbonized substance was soaked for 2H to 6 hours with 1% to 10% hydrofluoric acid (etch acid), and then washed with water, the centrifugal rotation was 6000 to 10,000 rpm, the centrifugal time was 1 min ~ 5 min. After washing, vacuum drying for 8 h ~ 12h, the vacuum drying temperature was 60 ° C to 80 ° C.

[0041] The prepared MOF-based platinum monoimer catalyst is used as a catalyst application in the fuel cell, the application steps are as follows:

[0042] With a ratio of mass ratio of perfluorosulfonic acid: dispersion solvent = 1: 30, a dispersant is formulated with a dispersant with a dispersion solvent, and then a dispersant 1 ml is mixed with a 2 mgmof-based platinum monoimer catalyst, ultrasonic mixed dispersion. The rear platinum carbon electrode was dried. In the present invention, the drying is retracted after drying. The dispersant is isopropyl alcohol or ethanol.

Example Embodiment

[0043]

[0044] In the present embodiment, the platinum source is chloroplatinate, and the obtained MOF-based platinum monoimer material is Pt (IV) -SACS material.

[0045] 210 mg of zirconium chloride, 163 mg 2-amino group terephthalic acid and 0.5 ml (solvent: DMF; concentration: 1 mg / mL) chloroplatinic acid were dissolved in 40 ml dimethylformamide and 4.8 ml of glacial acetic acid, loaded into a vial The reaction was reacted at 120 ° C for 12 h, and the reaction was cooled. 甲醇 : V DMF = 1: 4 washing 3 times at 8,000 rpm for 5 minutes; the centrifugation was washed under vacuum at 60 ° C for 12 h; the dried sample was treated with a high temperature of 900 ° C under a nitrogen atmosphere, and then naturally cooled to room temperature, obtained The catalyst material is soaked in a 5% HF solution for 2 h with a 5% HF solution, and then centrifuged at 8000 rpm for 5 minutes, and the washed material was dried under vacuum at 60 ° C for 12 h, resulting in a MOF-based platinum monoimer catalyst (PT (IV) -SAC).

Example Embodiment

[0046]

[0047] In the present embodiment, the platinum source is chloroplatinate, and the obtained MOF-based platinum monoimer material is Pt (IV) -SACS material.

[0048] 210 mg of zirconium chloride, 163 mg 2-amino group was dissolved in 40 ml of dimethylformamide and 4.8 ml of glacial acetic acid in a vial in a vial in a vial in a vial in a vial in a vial in a vial in a vial in a vial in a vial. 12h, reactive cooling 甲醇 : V DMF = 1: 4 washed 3 times at 8000 rpm to centrifuge at 8000 rpm for 5 minutes; the centrifugation was washed in vacuo 12h at 60 ° C; the dried sample was taken at 1000 ° C under a nitrogen atmosphere for 3 h, then naturally cooled to room temperature, obtained The catalyst material is soaked in a 5% HF solution for 2 h with a 5% HF solution, and then centrifuged at 8000 rpm for 5 minutes, and the washed material was dried under vacuum at 60 ° C for 12 h, resulting in a MOF-based platinum monoimer catalyst (PT (IV) -SAC).

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Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

Easy to prepare
low cost

MOF-based platinum monatomic catalyst, and preparation and application thereof

A catalyst and atom technology, which is applied in the field of electrochemical energy, achieves the effects of simple preparation method, reduced cost, and favorable promotion and use

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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