CN104689852A - Preparation of benzotriazole modified and carbon carrier loaded palladium-based catalyst - Google Patents
Preparation of benzotriazole modified and carbon carrier loaded palladium-based catalyst Download PDFInfo
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Abstract
The invention provides a preparation method of a benzotriazole modified and carbon carrier loaded palladium-based catalyst. The preparation method comprises the following steps: dissolving a carbon material and benzotriazole into an organic solvent, stirring for 2-24 hours, removing the solvent, and drying to obtain a benzotriazole modified carbon carrier; dissolving palladium chloride or palladium chloride and a metal salt mixture in a protonic solvent, adding a complexing agent and the benzotriazole modified carbon carrier, reacting at high temperature for a period of time, cooling, washing and drying to obtain the benzotriazole modified and carbon carrier loaded palladium-based catalyst. Compared with the traditional C carrier loaded palladium-based nanoparticles, the carrier prepared by the preparation method provided by the invention has the advantages that catalytic performance and stability are better, moreover the preparation process is simple and the cost is low, and thus the benzotriazole modified and carbon carrier loaded palladium-based catalyst can be used as an excellent palladium-based catalyst of a fuel cell.
Description
Technical field
the present invention relates to the preparation that a kind of modified carbon carrier supported palladium is catalyst based, particularly relate to the preparation that the carbon carrier supported palladium of a kind of benzotriazole modification is catalyst based, belong to field of fuel cell technology.
Background technology
It is clean energy conversion system that the fuel cell of efficient low-discharging is recognized, but catalyst is its business-like one large restraining factors of restriction.The noble metal being representative with platinum base is optimal catalyst.It all has catalytic activity for the negative electrode of fuel cell and anode reaction, and can long-term work.But the noble metal reserves such as platinum are limited, expensive, platinum based catalyst electro catalytic activity is lower in addition, is easily poisoned by intermediate product.Therefore, reduce the cost of catalyst, the catalyst preparing low noble metal load capacity and high catalytic activity is the key realizing commercializing fuel cells.In catalyst field, people find the catalyst of low noble metal amount high catalytic activity on the one hand, the nano particle of the component differences such as research special appearance, alloy, nucleocapsid structure or special construction; Find various high performance carrier on the other hand.
In fuel cell, most widely used catalyst carrier is carbon dust (VulcanXC-72).Carbon dust is not only cheap, and preparation is simple, and it also has following characteristic: surface area is large, and electric conductivity is strong, and special pore structure.But at fuel cell start-up with when stopping, carbon carrier is easy to be corroded, and this can cause the nano particle of its area load to reunite, and has had a strong impact on the performance of catalyst, thus has reduced the life-span of catalyst.Because the carbon carrier modified can change the interaction between carrier and metallic, the dispersion of nano particle on carrier can be improved, reduce the take-off potential of catalyst, and then improve activity and the persistence of catalyst.Therefore modifying material with carbon element is the effective ways improving catalyst performance.
At present, the method preparing modified carbon carrier conventional mainly comprises following several: chemical vapour deposition (CVD), high temperature pyrolysis, nitrogen-atoms sputtering etc.Although said method effectively can improve the performance of carbon carrier, improve the activity of catalyst, also there is certain defect, as temperature required too high, preparation process is loaded down with trivial details, and cost is higher, is difficult to its commercialization.In addition compared with platinum, because palladium low price, rich reserves, catalytic activity and anti-poisoning capability are higher, thus cause the extensive concern of people.Therefore, replace platinum with palladium, development low cost, the catalyst of high activity and stability is the key realizing commercializing fuel cells.
Summary of the invention
The object of this invention is to provide the preparation method that the carbon carrier supported palladium of a kind of benzotriazole modification is catalyst based.
One, the preparation that the carbon carrier supported palladium of benzotriazole modification is catalyst based
(1) preparation of the carbon carrier of benzotriazole modification: material with carbon element and benzotriazole (TBA) are dissolved in organic solvent with the mass ratio of 0.5:1 ~ 20:1, stirring reaction 2 ~ 24 h at 20 ~ 60 DEG C, except desolventizing, dry, obtain the carbon carrier that benzotriazole is modified; Organic solvent is at least one of methyl alcohol, ethanol, ethylene glycol, glycerine, benzene, toluene, chloroform;
(2) preparation that supported palladium is catalyst based: be dissolved in protonic solvent by palladium bichloride or palladium bichloride and metal salt mixture, adds after complexing agent is uniformly dispersed and stirs 20 ~ 60 min, regulate pH=7 ~ 12; Add the carbon carrier of the benzotriazole modification of above-mentioned preparation, stirring, each 30 ~ 80 min of ultrasonic disperse, then react 4 ~ 8 h at 150 ~ 180 DEG C, and cooling, washing, drying, obtain modified carbon carrier supported palladium catalyst based.
Described slaine is the chlorate of cobalt, nickel, silver, iron, tin, copper; Palladium bichloride mixes with the mass ratio of 0.2:1 ~ 5:1 with slaine; Described protonic solvent is hydrazine, ethylene glycol, glycerine, the aqueous solution of sodium borohydride or the aqueous solution of ethanol; Described complexing agent is triethanolamine, natrium citricum, sodium tartrate, EGTA, calgon, EDTA; The mass ratio of palladium bichloride or palladium bichloride and metal salt mixture and complexing agent is 0.2:1 ~ 5:1; Mass ratio 1:3 ~ the 1:6 of the carbon carrier that above-mentioned palladium bichloride or palladium bichloride and metal salt mixture and benzotriazole are modified.
Two, the stuctures and properties that modified carbon carrier supported palladium is catalyst based
Below for modified carbon carrier supported palladium nano particle, the structure of catalyst (Pd/BTA-C) and ethanol electrocatalysis characteristic are described.The Pd/C catalyst simultaneously prepared with same procedure compares.
Fig. 1 is X-ray diffraction (XRD) figure of Pd/BTA-C and Pd/C catalyst.As can be seen from Figure 1, in Pd/BTA-C catalyst prepared by the present invention, there is the characteristic diffraction peak of the face-centred cubic structure of Pd, illustrate that the palladium nano-particles of load on it is face-centred cubic structure.
Fig. 2 is the transmission electron microscope picture of Pd/BTA-C catalyst.Can be seen by Fig. 2, Pd nano particle is evenly distributed on modified carbon carrier, does not have agglomeration.
Fig. 3 is the grain size distribution of Pd/BTA-C catalyst.Can be seen by Fig. 3, its average grain diameter is 4.2
+0.3 nm.
Fig. 4 is the cyclic voltammetry of Pd/BTA-C and Pd/C catalyst in 0.1 M KOH solution.The electrochemical surface area of two kinds of catalyst can be calculated by the reduction peak of Fig. 3, be respectively 312.78 cm
2/ mg and 582.98 cm
2/ mg, illustrates that the electrochemical surface area of Pd/BTA-C is obviously greater than Pd/C.
Fig. 5 is that Pd/BTA-C and Pd/C catalyst is at 0.1 M KOH+0.5 M C
2h
5cyclic voltammetry in OH solution.As can be seen from Figure 4, the take-off potential of Pd/BTA-C is not only negative compared with Pd/C moves 70 mV, and its oxidation peak current density is 175.25 mA/mg
pd, be 1.72 times of Pd/C catalyst.
Fig. 6 is that Pd/BTA-C and Pd/C catalyst is at 0.1 M KOH+0.5 M C
2h
5chronoamperogram in OH solution.After result shows 3000 s, the current density of Pd/BTA-C is 25.72 mA/mg
pd, Pd/C is 19.53 mA/mg
pd(being only 75.9 % of Pd/BTA-C current density), simultaneously compared with initial current density, the attenuation of Pd/BTA-C is the attenuation of 57.4 %, Pd/C is 69.7 %.Illustrate that Pd/BTA-C has better stability.
In sum, the carbon carrier supported palladium that benzotriazole of the present invention is modified is catalyst based, effectively improves the catalytic performance of metal nanoparticle.In addition, synthesis technique of the present invention is simple, with low cost, and has good catalytic activity and stability, is the palladium-based catalyst of the excellence that can be applicable in fuel cell.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of Pd/BTA-C and Pd/C catalyst.
Fig. 2 is the transmission electron microscope picture of Pd/BTA-C catalyst.
Fig. 3 is the grain size distribution of Pd/BTA-C catalyst.
Fig. 4 is the cyclic voltammetry of Pd/BTA-C and Pd/C catalyst in 0.1 M KOH solution.
Fig. 5 is that Pd/BTA-C and Pd/C catalyst is at 0.1 M KOH+0.5 M C
2h
5catalysis ethanol performance test in OH solution.
Current density block diagram corresponding after the chronoamperogram that Fig. 6 is Pd/BTA-C and Pd/C catalyst in oxidation of ethanol reaction during-0.2 V and 3000 s.
Fig. 7 is current density block diagram corresponding after 3000 s are reacted in the oxidation of ethanol of Pd/BTA-C and Pd/C catalyst.
Detailed description of the invention
Below by instantiation, the preparation of palladium-based catalyst of the present invention and electrocatalysis characteristic are described further.
embodiment 1,the preparation of Pd/BTA-C catalyst
In the round-bottomed flask of 100 mL, add 500 mg carbon dusts and 100 mg benzotriazoles (BTA), dissolve with the ethanol of 40 mL, stir 18 h; Except after desolventizing at 50 DEG C dry 7 h, obtain carrier B TA-C;
41.68 mg palladium bichlorides are joined in 100 mL round-bottomed flasks, add the ethylene glycol of 30 mL after dissolving with 5 ~ 10 concentrated hydrochloric acids, the natrium citricum of 150 mg, until completely dissolved stirring reaction 1 h; Add the carrier B TA-C of the above-mentioned preparation of 100 mg after regulating pH=9 again, stir 30 min, ultrasonic 1 h; Then back flow reaction 6 h at 160 DEG C of temperature, cooling, suction filtration, dry at 50 DEG C, obtain Pd/BTA-C catalyst.
In the performance test of catalysis ethanol oxidation, Pd/BTA-C catalyst oxidation peak current density is 175.25 mA/mg
pd, be 1.72 times of Pd/C catalyst, take-off potential is negative moves 70 mV; In the chrono-amperometric test of-0.2 V, after 3000 s, the current density of Pd/BTA-C is 25.72 mA/mg
pd, be 1.3 times of Pd/C.
embodiment 2, PdNi/BTA-C catalyst preparation
In the round-bottomed flask of 100 mL, add carbon dust and the 150 mg benzotriazoles (BTA) of 500 mg, dissolve with the ethanol of about 40 mL, stirring reaction 18 h, except desolventizing, at 50 DEG C, dry 7 h, obtain carrier B TA-C;
26.61 mg palladium bichlorides and 35.65 mg nickel chlorides are joined in 100 mL round-bottomed flasks, dissolve with 4 ~ 8 concentrated hydrochloric acids, after add the ethylene glycol of 30 mL, the natrium citricum of 100 mg; Stirring reaction 1h until completely dissolved, regulates pH=8 ~ 9, then adds the prepared carrier B TA-C of the above-mentioned preparation of 100 mg, stir 30 min, ultrasonic 1 h; Then back flow reaction 6 h at 160 DEG C of temperature, cooling, suction filtration, dry at 50 DEG C, obtain PdNi/BTA-C catalyst.
In the performance test of catalysis methanol oxidation, PdNi/BTA-C catalyst oxidation peak current density is 173.60 mA/mg
pd, be its 1.7 times of Pd/C catalyst, take-off potential is negative moves 60 mV; In the chrono-amperometric test of-0.1 V, after 3000 s, the current density of PdNi/BTA-C is 24.38 mA/mg
pd, be Pd/C catalyst be 1.25 times of Pd/C.
embodiment 3, PdCo/BTA-C catalyst preparation
In the round-bottomed flask of 100 mL, add carbon dust and the 150 mg benzotriazoles (BTA) of 600 mg, dissolve with the ethanol of about 40 mL, stirring reaction 20 h, except desolventizing, at 50 DEG C, dry 7 h, obtain carrier B TA-C;
26.83 mg palladium bichlorides and 35.98 mg cobalt chlorides are joined in 100 mL round-bottomed flasks, adds the ethylene glycol of 30 mL after dissolving with 4 ~ 7 concentrated hydrochloric acids, the natrium citricum of 80 mg; Stirring reaction 1 h until completely dissolved, adds the carrier of the above-mentioned preparation of 100 mg, stirs 30 min, ultrasonic 1 h after regulating pH to 8 ~ 9; Then back flow reaction 6 h at 160 DEG C of temperature, cooling, suction filtration, dry at 50 DEG C, obtain PdCo/BTA-C catalyst.
In the performance test of catalysis ethanol oxidation, PdCo/BTA-C catalyst oxidation peak current density is 178.71 mA/mg
pd, be 1.75 times of Pd/C catalyst, take-off potential is negative moves 58 mV; In the chrono-amperometric test of-0.2 V, after 3000 s, the current density of PdCo/BTA-C is 25.39 mA/mg
pd, be 1.3 times of Pd/C.
embodiment 4, PdAg/BTA-C catalyst preparation
In the round-bottomed flask of 100 mL, add carbon dust and the 200 mg benzotriazoles (BTA) of 500 mg, dissolve with the ethanol of about 40 mL, stirring reaction 20 h, except desolventizing, at 50 DEG C, dry 7 h, obtain carrier B TA-C;
20.69 mg palladium bichlorides and 19.82 mg silver nitrates are joined in 100 mL round-bottomed flasks, the ethylene glycol of 30 mL is added after dissolving with 2 ~ 6 concentrated hydrochloric acids, the natrium citricum of 100 mg, until completely dissolved, stirring reaction 1, regulates pH to 9 ~ 10, then adds the carrier of the above-mentioned preparation of 100 mg, stir 30 min, ultrasonic 1 h; Then back flow reaction 6 h at 160 DEG C of temperature, cooling, suction filtration, dry at 50 DEG C, obtain PdAg/BTA-C catalyst.
In the performance test of catalysis oxidation of glycol, PdAg/BTA-C catalyst oxidation peak current density is 174.63 mA/mg
pd, be 1.71 times of Pd/C catalyst, take-off potential is negative moves 64 mV; In the chrono-amperometric test of-0.2 V, after 3000 s, the current density of PdAg/BTA-C is 21.68 mA/mg
pd, be 1.11 times of Pd/C catalyst.
embodiment 5, PdFe/BTA-C catalyst preparation
In the round-bottomed flask of 100 mL, add carbon dust and the 200 mg benzotriazoles (BTA) of 600 mg, dissolve with the ethanol of about 40 mL, stirring reaction 21 h, except desolventizing, at 50 DEG C, dry 7 h, obtain carrier B TA-C;
27.30 mg palladium bichlorides and 41.60 mg iron chloride are joined in the round-bottomed flask of 100 mL, then adds the ethylene glycol of 30 mL, the natrium citricum of 100 mg, until completely dissolved stirring reaction 1 h; Regulate pH=8 ~ 9 of solution, then add the carrier of the above-mentioned preparation of 100 mg, stir 30 min, ultrasonic 1 h; Then back flow reaction 4 h at 180 DEG C of temperature, cooling, suction filtration, dry at 50 DEG C, obtain PdFe/BTA-C catalyst.
In the performance test of catalysis methanol oxidation, PdFe/BTA-C catalyst oxidation peak current density is 125.61 mA/mg
pd, be 1.23 times of Pd/C catalyst, take-off potential is negative moves 50 mV; In the chrono-amperometric test of-0.1 V, after 3000 s, the current density of PdFe/BTA-C is 22.50 mA/mg
pd, be 1.15 times of Pd/C catalyst.
embodiment 6, PdSn/BTA-C catalyst preparation
In the round-bottomed flask of 100 mL, add carbon dust and the 150 mg benzotriazoles (BTA) of 550 mg, dissolve with the ethanol of about 40 mL, stirring reaction 18 h, except desolventizing, at 50 DEG C, dry 7 h, obtain carrier B TA-C;
19.70 mg palladium bichlorides and 38.94 mg stannic chlorides are joined in 100 mL round-bottomed flasks, then the ethylene glycol of 30 mL is added, the natrium citricum of 75 mg, until completely dissolved, stirring reaction 1 h, the carrier of the above-mentioned preparation of 100 mg is added again after regulating pH to 8 ~ 9, stir 0.5 h, ultrasonic 1 h, then back flow reaction 5 h at 170 DEG C of temperature, cooling, suction filtration, dry at 50 DEG C, obtain PdSn/BTA-C catalyst.
In the performance test of catalysis glycerine oxidation, PdSn/BTA-C catalyst oxidation peak current density is 163.39 mA/mg
pd, be 1.6 times of Pd/C catalyst, take-off potential is negative moves 65 mV; In-0.2 V chrono-amperometric test, after 3000 s, the current density of PdSn/BTA-C is 20.51 mA/mg
pd, be 1.05 times of Pd/C catalyst.
Claims (8)
1. the preparation method that the carbon carrier supported palladium of benzotriazole modification is catalyst based, comprises following processing step:
(1) preparation of the carbon carrier of benzotriazole modification: material with carbon element and benzotriazole are dissolved in organic solvent with the mass ratio of 0.5:1 ~ 20:1, stir process 2 ~ 24 h at 20 ~ 60 DEG C, except desolventizing, dry, obtain the carbon carrier that benzotriazole is modified;
(2) preparation that supported palladium is catalyst based: be dissolved in protonic solvent by palladium bichloride or palladium bichloride and metal salt mixture, add complexing agent ultrasonic disperse and evenly stir 20 ~ 60 min afterwards, regulates pH=7 ~ 12; Add the carbon carrier of benzotriazole modification, stirring, each 30 ~ 80 min of ultrasonic disperse, then at 150 ~ 180 DEG C, react 4 ~ 8 h, cooling, washing, drying, obtain modified carbon carrier supported palladium catalyst based.
2. the preparation method that the carbon carrier supported palladium of benzotriazole modification is catalyst based as claimed in claim 1, is characterized in that: the organic solvent in step (1) is at least one of methyl alcohol, ethanol, ethylene glycol, glycerine, benzene, toluene, chloroform.
3. the preparation method that the carbon carrier supported palladium of benzotriazole modification is catalyst based as claimed in claim 1, is characterized in that: slaine described in step (2) is the chlorate of cobalt, nickel, silver, iron, tin, copper.
4. the preparation method that the carbon carrier supported palladium of benzotriazole modification is catalyst based as claimed in claim 1, is characterized in that: in step (2), palladium bichloride mixes with the mass ratio of 0.2:1 ~ 5:1 with slaine.
5. the preparation method that the carbon carrier supported palladium of benzotriazole modification is catalyst based as claimed in claim 1, is characterized in that: the protonic solvent in step (2) is hydrazine, ethylene glycol, glycerine, the aqueous solution of sodium borohydride or the aqueous solution of ethanol.
6. the preparation method that the carbon carrier supported palladium of benzotriazole modification is catalyst based as claimed in claim 1, is characterized in that: described in step (2), complexing agent is triethanolamine, natrium citricum, sodium tartrate, EGTA, calgon or EDTA.
7. the preparation method that the carbon carrier supported palladium of benzotriazole modification is catalyst based as claimed in claim 6, is characterized in that: the mass ratio of palladium bichloride or palladium bichloride and metal salt mixture and complexing agent is 0.2:1 ~ 5:1.
8. the catalyst based preparation method of carbon carrier supported palladium that modifies of benzotriazole as claimed in claim 1, is characterized in that: in step (2), the mass ratio 1:3 ~ 1:6 of the carbon carrier that palladium bichloride or palladium bichloride and metal salt mixture and benzotriazole are modified.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112349918A (en) * | 2020-11-06 | 2021-02-09 | 昆明理工大学 | Method for preparing nitrogen-doped platinum-carbon catalyst by pyrolyzing chitosan and application thereof |
| CN113745552A (en) * | 2021-08-17 | 2021-12-03 | 西安交通大学 | Carbon-supported palladium tin tantalum nitride nano electro-catalyst for direct ethanol and methanol fuel cell and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112349918A (en) * | 2020-11-06 | 2021-02-09 | 昆明理工大学 | Method for preparing nitrogen-doped platinum-carbon catalyst by pyrolyzing chitosan and application thereof |
| CN112349918B (en) * | 2020-11-06 | 2023-03-10 | 昆明理工大学 | Method for preparing nitrogen-doped platinum-carbon catalyst by pyrolyzing chitosan and application thereof |
| CN113745552A (en) * | 2021-08-17 | 2021-12-03 | 西安交通大学 | Carbon-supported palladium tin tantalum nitride nano electro-catalyst for direct ethanol and methanol fuel cell and preparation method thereof |
| CN113745552B (en) * | 2021-08-17 | 2024-04-09 | 西安交通大学 | Carbon-supported palladium-tin tantalum nitride nano electrocatalyst for direct ethanol and methanol fuel cells and preparation method thereof |
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