CN1846852A - Prepn process of carbon supported platinum catalyst - Google Patents
Prepn process of carbon supported platinum catalyst Download PDFInfo
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- CN1846852A CN1846852A CNA2005100645801A CN200510064580A CN1846852A CN 1846852 A CN1846852 A CN 1846852A CN A2005100645801 A CNA2005100645801 A CN A2005100645801A CN 200510064580 A CN200510064580 A CN 200510064580A CN 1846852 A CN1846852 A CN 1846852A
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Abstract
The preparation process of carbon supported platinum catalyst includes the following steps: 1. dispersing carrier carbon in solvent to prepare suspension; 2. adding solution compounded with M2Pt(OH)6, with M being H,NH4, Na or K, and containing platinum in 0.01-20 g/l into the suspension through stirring, and regulating pH to 1-10; 3. adding excessive reductant into the mixed solution to perform reduction reaction; and 4. filtering, washing and drying the reduction product to obtain the carbon supported platinum catalyst. The present invention has the advantages of fine and homogeneous catalyst grain, less impurity and high catalytic performance.
Description
Technical field
The present invention relates to a kind of preparation method of fuel cell carbon platinum catalyst, belong to the field that catalyst is made.
Background technology
Fuel cell is a kind of energy conversion device, it is different from the battery on the ordinary meaning, as long as constantly supply with fuel and oxidant to it, the just continual generating of energy, and battery is limited energy storage and output device, it also is different from internal combustion engine and thermal power generation, it presses electrochemical principle, directly chemical energy is converted to electric energy and need not pass through fuel combustion, make this intermediate steps of mechanical power, owing to be not subjected to card if loop limit, has very high energy conversion efficiency, its product is a water, and is environmentally friendly, in addition also has reliable, advantage such as flexibly, make fuel cell be with a wide range of applications, be the low-temperature fuel cell of representative wherein, can start fast at low temperatures, be expected to be applied at aspects such as electric automobile and small-sized mobile power stations with PEMFC and DMFC, be the energy power system of new generation of domestic and international emphasis research and development, industrialization and commercialization prospect are obvious day by day.
Low-temperature fuel cell uses noble metal platinum as eelctro-catalyst, owing to the platinum scarcity of resources, cost an arm and a leg, for the use amount that reduces platinum, increase operation rate, reduce the catalyst cost, main at present employing load type platinum sill is as catalyst, its principal mode is, carbon carries platinum, and carbon carries platinum+transition metal or transition metal oxide etc., and the catalytic performance of carbon-carried platinum-based catalyst is relevant with the intrinsic physical and chemical performance and the preparation method of catalyst.
The intrinsic physical and chemical performance that influences the electrocatalysis characteristic of carbon supported platinum catalyst comprises, nano platinum belongs to particle size, nano platinum and belongs to the degree of scatter of particle on carbon, thing mutually and the influence of chemical composition, impurity etc., general requirement is that the nano platinum of certain particle size range (being generally 2-5nm) belongs to particle evenly distribution on carbon, objectionable impurities content the least possible (Cl, S etc.).
The preparation method of carbon current platinum catalyst mainly contains two kinds, and a kind of is colloid method, a kind of for liquid phase reduction.As U.S. Pat 3'992'331, US 3'992'512, US 4'044'193, disclose and adopted colloid method to prepare the method for carbon supported platinum catalyst, this method is the sulphite complex compound that contains platinum that can oxidized part of system earlier, adds oxide oxidation part, obtains the oxide colloid of platinum, load on the carbon, obtain carbon supported platinum catalyst through reduction.This technology preparation process complexity, and contain a certain amount of sulphur in the product.Liquid phase reduction also is the method for using always for preparing carbon supported platinum catalyst, and it is (as H with the platinum precursor solution
2Pt (Cl)
6Deng) mix with carrier, adding reducing agent, reduction obtains loaded catalyst, most typical have Brown method and a Kaffer method, and this method is simple, and shortcoming is that condition is wayward, it is tiny to be difficult to obtain size, uniform catalyst granules, the skewness on carbon carrier.
In open source literature data, the selection of the preparation precursor of platinum mainly is the halogen complex of platinum, sulphite complex compound etc., halogen complex with platinum, the sulphite complex compound is the precursor preparation carbon supported platinum catalyst, because the existence of the carbon of the strong adsorption capacity of high-ratio surface, make the halogens such as Cl in the catalyst, the content of impurity such as S is higher, be very difficult to remove clean, and these elements have the suitable ability that poisons to the performance of catalyst, (T.J.Schmidt such as T.J.Schmidt, U.A.Paulus, J.Electroanal.Chem, 2001,508, studies show that 41), the existence of the chlorion of 4ppm will cause the fuel cell voltage loss up to 50mv, this be because these impurity strong adsorption on the active sites of Pt, thereby reduced activity of such catalysts.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of fuel cell carbon carried platinum-based catalyst, adopt the tiny homogeneous of the made catalyst granules of this method, on carbon, be evenly distributed, composition is clean relatively, contain impurity such as halogens, S such as Cl hardly, catalyst is compared than similar catalyst has catalytic performance preferably.
For achieving the above object, the present invention takes following technical scheme:
A kind of preparation method of carbon supported platinum catalyst, this method comprise following each step:
(1), carrier carbon is dispersed in makes suspension in the solvent;
(2), add M in the suspension that in step (1), obtains
2Pt (OH)
6Be mixed with the solution of platinum content 0.01-20g/l, mix, regulate PH to 1-10, wherein, M is H, NH
4 +, alkali metal such as Na, K;
(3), add excessive reducing agent in the mixed liquor that in step (2), obtains, carry out reduction reaction;
(4), the product after the reduction reaction is filtered, washing, carry out drying again after, promptly obtain the carbon-carried platinum-based eelctro-catalyst of making.
In described step (1), described solvent comprises acetone, ethanol, isopropyl alcohol, butanols, N, the organic solvent that U.S. Cabot Co.,Ltd such as dinethylformamide (CABOT corporation) recommend to use, and with the mixed solvent of water.Activated carbon is in g, and solvent is in l, and its cooperation ratio is 0.01-10g/l.
Under the mixed solvent situation of above-mentioned organic solvent and water, solvent burden ratio is that the volume ratio of organic solvent and water is 100: 5 to 5: 100.
In described step (3), the temperature of described reduction reaction is 40-100 ℃, and the time of reaction is 5min-24h.
In described step (3), described reducing agent is the aqueous solution of formic acid, formaldehyde, hydrazine hydrate, sodium borohydride or potassium borohydride or the like.By the amount of the required reducing agent of chemical reaction requirement, the excessive 2-20 of reducing agent doubly, the amount of described reducing agent is the amount of pure formic acid, formaldehyde, hydrazine hydrate, sodium borohydride or potassium borohydride.
In the described step (4), described drying is carried out under 40-100 ℃ of vacuum condition.
Advantage of the present invention is:
The preparation method of this fuel cell carbon carried platinum-based catalyst of the present invention is by adopting a kind of compound-M that does not contain the platinum of impurity such as halogens, S such as Cl
2Pt (OH)
6(M is H, NH
4 +, alkali metal such as Na, K) as the preparation precursor, obtaining relatively clean carbon-carried platinum-based catalyst, thereby prepare high performance low-temperature fuel cell eelctro-catalyst.
Another feature of the present invention is, is lower than under 10 conditions at PH, and the platinum in these compounds is with H
2Pt (OH)
6The nano-precipitation form exist.Then by the conditioned reaction condition, can make controlled the discharging of platinum, reduction obtains tiny and uniform nano metal platinum under the effect of reducing agent.Avoided in direct liquid-phase reduction process, change in reaction conditions is big, and course of reaction is difficult to shortcomings such as control.
In a word, the invention has the advantages that the tiny homogeneous of prepared catalyst granules, be evenly distributed on carbon that composition is clean relatively, contains impurity such as halogens, S such as Cl hardly, catalyst is compared than similar catalyst has catalytic performance preferably.
Description of drawings
Fig. 1 is prepared catalyst EDX spectrogram, and wherein Pt/C (A) is the prepared catalyst of embodiment 1, and Pt/C (B) is the prepared catalyst of comparative example 1.
Fig. 2 is prepared catalyst TEM photo, and Fig. 2 (a) is the prepared catalyst of embodiment 1, and 2 (b) are the prepared catalyst of comparative example 1.
The specific embodiment
Embodiment 1
800mgVulcan XC-72 carbon black is joined in the 1000ml solvent, stirred 1 hour, employed solvent is the mixed solvent of isopropyl alcohol and water, and the volume ratio of isopropyl alcohol and water is 30: 70.Slowly drip Na
2Pt (OH)
6, be mixed with the solution that platinum content is 0.2g/L, regulating PH is 6, stirs 1 hour, stirs the formalin that slowly drips 2ml 37wt% down, and 80 degree reduction 40min reduce to room temperature, filter, and deionized water washs repeatedly, and temperature is that 70 degree, vacuum are 10
-3Vacuum drying under the condition of Pa obtains the carbon supported platinum catalyst of nano-scale.Solvent can be written as the mixed solvent of isopropyl alcohol and water among the embodiment, and volume ratio is 30: 70.
Comparative example 1
The 800mg activated carbon is joined in the 1000ml solvent, stirred 1 hour, employed solvent is the mixed solvent of isopropyl alcohol and water, and the volume ratio of isopropyl alcohol and water is 30: 70.Slowly drip H
2Pt (Cl)
6Solution, platinum content are 0.2g/L, stir 1 hour, and regulating PH is 6, stir the formalin that slowly drips 2ml 37wt% down, and 80 degree reduction 40min reduce to room temperature, filter, and deionized water washs repeatedly, and temperature is that 70 degree, vacuum are 10
-3Vacuum drying under the condition of Pa obtains the carbon supported platinum catalyst of nano-scale.
As shown in Figure 1, in this EDX spectrogram, Pt/C (A) is the prepared catalyst of embodiment 1; Pt/C (B) is that the prepared catalyst of comparative example 1 is (promptly with H
2Pt (Cl)
6For precursor directly reduce the preparation catalyst), Fig. 1 shows, the carbon supported platinum catalyst of embodiment 1 resultant nano-scale is found to contain impurity such as Cl, S hardly in the product by EDX, and the carbon supported platinum catalyst of comparative example 1 preparation contains a large amount of Cl, and its chlorinity is apparently higher than embodiment 1.
As shown in Figure 2, Fig. 2 (a) is the prepared catalyst of embodiment 1, and the tiny homogeneous of catalyst granules, most particle diameter are distributed between 2-4nm (average-size is 3.6nm), are evenly distributed on carbon.Fig. 2 (b) is the prepared catalyst of comparative example 1, the catalyst particle size heterogeneity, and it is serious to reunite, and it is very inhomogeneous to distribute on carbon.
Embodiment 2
Other conditions are with embodiment 1, and only changing PH is 2.
Embodiment 3
Other conditions are with embodiment 1, and only changing PH is 9.
Embodiment 4
Other conditions are with embodiment 2, and only changing reduction reaction temperature is 70 ℃.
Embodiment 5
Other conditions only change formaldehyde adding mode for after being warming up to 90 ℃ with embodiment 2, slowly drip the formalin of 10ml37%.
Embodiment 2-3 compares with embodiment 1, only change pH value, the carbon supported platinum catalyst of the resultant nano-scale of embodiment 2-3 is found to contain impurity such as Cl, S hardly in the product by EDX, and the TEM photo shows the tiny homogeneous of catalyst granules, most particle diameter is distributed between 2-4nm, is evenly distributed on carbon.
Embodiment 4 compares with embodiment 1, only changes reduction reaction temperature, but is between 50-90 ℃ in the temperature of reduction reaction all; Embodiment 5 compares with embodiment 1, only change formaldehyde adding mode for after being warming up to 90 ℃, slowly drip the formalin of 10ml37%, reduction reaction temperature is 90 ℃, but all the temperature in reduction reaction is between 40-100 ℃, and the carbon supported platinum catalyst of the resultant nano-scale of embodiment 4-5 is found to contain impurity such as Cl, S hardly in the product by EDX, and the TEM photo shows the tiny homogeneous of catalyst granules, most particle diameter is distributed between 2-4nm, is evenly distributed on carbon.
Embodiment 6
2gVulcan XC-72 carbon black is joined in the 1000ml solvent, stirred 0.5 hour, employed solvent is the mixed solvent of isopropyl alcohol and water, and the volume ratio of isopropyl alcohol and water is 30: 70.Slowly drip Na
2Pt (OH)
6, be mixed with the solution that platinum content is 1g/L, regulating PH is 9, stirs 0.5 hour, stirs the formalin that slowly drips 8ml 37wt% down, and 60 degree reduction 30min reduce to room temperature, filter, and deionized water washs repeatedly, and temperature is that 50 degree, vacuum are 10
-3Vacuum drying under the condition of Pa obtains the carbon supported platinum catalyst of nano-scale.
Embodiment 7
6gVulcan XC-72 carbon black is joined in the 1000ml solvent, stirred 1 hour, employed solvent is the mixed solvent of isopropyl alcohol and water, and the volume ratio of isopropyl alcohol and water is 40: 60.Slowly drip Na
2Pt (OH)
6, be mixed with the solution that platinum content is 10g/L, regulating PH is 8, stirs 1 hour, stirs the formalin that slowly drips 40ml 37wt% down, and 80 degree reduction 60min reduce to room temperature, filter, and deionized water washs repeatedly, and temperature is that 80 degree, vacuum are 10
-3Vacuum drying under the condition of Pa obtains the carbon supported platinum catalyst of nano-scale.
Embodiment 8
8gVulcan XC-72 carbon black is joined in the 1000ml solvent, stirred 1 hour, employed solvent is the mixed solvent of isopropyl alcohol and water, and the volume ratio of isopropyl alcohol and water is 50: 50.Slowly drip Na
2Pt (OH)
6, be mixed with the solution that platinum content is 15g/L, regulating PH is 8, stirs 1 hour, stirs the formalin that slowly drips 60ml 37wt% down, and 70 degree reduction 60min reduce to room temperature, filter, and deionized water washs repeatedly, and temperature is that 80 degree, vacuum are 10
-3Vacuum drying under the condition of Pa obtains the carbon supported platinum catalyst of nano-scale.
Embodiment 9
0.5gVulcan XC-72 carbon black is joined in the 1000ml solvent, stirred 1 hour, employed solvent is the mixed solvent of isopropyl alcohol and water, and the volume ratio of isopropyl alcohol and water is 20: 80.Slowly drip Na
2Pt (OH)
6, be mixed with the solution that platinum content is 0.05g/L, regulating PH is 8, stirs 1 hour, stirs the formalin that slowly drips 1ml 37wt% down, and 80 degree reduction 60min reduce to room temperature, filter, and deionized water washs repeatedly, and temperature is that 80 degree, vacuum are 10
-3Vacuum drying under the condition of Pa obtains the carbon supported platinum catalyst of nano-scale.
The carbon supported platinum catalyst of embodiment 6,7,8,9 resultant nano-scales is all found to contain impurity such as Cl, S hardly in the product by EDX respectively, and show from the TEM photo respectively, the tiny homogeneous of embodiment 6,7,8,9 resulting catalyst granules, most particle diameter is distributed between 2-4nm, is evenly distributed on carbon.
Claims (5)
- The preparation method of l, a kind of carbon supported platinum catalyst is characterized in that: this method comprises following each step:(1), carrier carbon is dispersed in makes suspension in the solvent;(2), add M in the suspension that in step (1), obtains 2Pt (OH) 6Be mixed with the solution of platinum content 0.01-20g/l, mix, regulate PH to 1-10, wherein, M is H, NH 4 +, Na, K alkali metal;(3), add excessive reducing agent in the mixed liquor that in step (2), obtains, carry out reduction reaction;(4), the product after the reduction reaction is filtered, washing, carry out drying again after, promptly obtain the carbon-carried platinum-based eelctro-catalyst of making.
- 2, the preparation method of carbon supported platinum catalyst according to claim 1, it is characterized in that: in described step (1), described solvent comprises acetone, ethanol, isopropyl alcohol, butanols, N, the dinethylformamide organic solvent, and with the mixed solvent of water, activated carbon is in g, and solvent is in 1, and its cooperation ratio is 0.01-10g/l.
- 3, the preparation method of carbon supported platinum catalyst according to claim 1 and 2 is characterized in that: in described step (3), the temperature of described reduction reaction is 40-100 ℃, and the time of reaction is 5min-24h.
- 4, the preparation method of carbon supported platinum catalyst according to claim 1 and 2, it is characterized in that: in described step (3), described reducing agent is the aqueous solution of formic acid, formaldehyde, hydrazine hydrate, sodium borohydride or potassium borohydride or the like, amount by the required reducing agent of chemical reaction requirement, the excessive 2-20 of reducing agent doubly, the amount of described reducing agent is the amount of pure formic acid, formaldehyde, hydrazine hydrate, sodium borohydride or potassium borohydride.
- 5, the preparation method of carbon supported platinum catalyst according to claim 1 and 2 is characterized in that: in the described step (4), described drying is carried out under 40-100 ℃ of vacuum condition.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549235A (en) * | 2014-12-19 | 2015-04-29 | 上海交通大学 | Preparation method of carbon supported nano platinum catalyst |
| CN104624185A (en) * | 2015-01-12 | 2015-05-20 | 鲁奎 | Method for preparing carbon-supported platinum catalyst by precipitation transformation |
| CN107029751A (en) * | 2017-06-01 | 2017-08-11 | 南通百应能源有限公司 | The preparation method of high activity platinum copper catalyst |
| CN108236951A (en) * | 2016-12-26 | 2018-07-03 | 天津仁智科技发展有限责任公司 | A kind of preparation method of the palladium on carbon powder as formaldehyde remover |
| CN113745542A (en) * | 2021-09-15 | 2021-12-03 | 北京化工大学 | High platinum loading platinum/carbon catalyst for fuel cell and preparation method thereof |
| CN115043757A (en) * | 2022-07-27 | 2022-09-13 | 南京桦冠生物技术有限公司 | Method for continuously preparing benzamidine hydrochloride |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1058283A (en) * | 1974-12-20 | 1979-07-10 | Henry G. Petrow | Fuel cell electrodes with finely divided platinum catalyst |
| US20050112432A1 (en) * | 2002-08-27 | 2005-05-26 | Jonah Erlebacher | Method of plating metal leafs and metal membranes |
| CN100356619C (en) * | 2002-10-10 | 2007-12-19 | 江苏隆源双登电源有限公司 | Method for preparing carbon-carried platinum/rare earth oxide composite electro catalyst for fuel cell |
| CN1240878C (en) * | 2003-11-21 | 2006-02-08 | 厦门大学 | Process for preparing carbon supported platinum-based surface alloy electrocatalytic electrode |
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2005
- 2005-04-15 CN CNB2005100645801A patent/CN100371070C/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549235A (en) * | 2014-12-19 | 2015-04-29 | 上海交通大学 | Preparation method of carbon supported nano platinum catalyst |
| CN104549235B (en) * | 2014-12-19 | 2018-02-27 | 上海唐锋能源科技有限公司 | A kind of preparation method of the immobilized nm Pt catalyst of carbon |
| CN104624185A (en) * | 2015-01-12 | 2015-05-20 | 鲁奎 | Method for preparing carbon-supported platinum catalyst by precipitation transformation |
| CN108236951A (en) * | 2016-12-26 | 2018-07-03 | 天津仁智科技发展有限责任公司 | A kind of preparation method of the palladium on carbon powder as formaldehyde remover |
| CN107029751A (en) * | 2017-06-01 | 2017-08-11 | 南通百应能源有限公司 | The preparation method of high activity platinum copper catalyst |
| CN113745542A (en) * | 2021-09-15 | 2021-12-03 | 北京化工大学 | High platinum loading platinum/carbon catalyst for fuel cell and preparation method thereof |
| CN115043757A (en) * | 2022-07-27 | 2022-09-13 | 南京桦冠生物技术有限公司 | Method for continuously preparing benzamidine hydrochloride |
| CN115043757B (en) * | 2022-07-27 | 2023-08-08 | 南京桦冠生物技术有限公司 | Method for continuously preparing benzamidine hydrochloride |
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Address after: 100088, 2, Xinjie street, Beijing Patentee after: Youyan Technology Group Co.,Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: GENERAL Research Institute FOR NONFERROUS METALS Address after: 100088, 2, Xinjie street, Beijing Patentee after: China Youyan Technology Group Co.,Ltd. Address before: 100088, 2, Xinjie street, Beijing Patentee before: Youyan Technology Group Co.,Ltd. |
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