CN110449149A - A kind of preparation method of carbon network supported noble metals nano-particle material - Google Patents

A kind of preparation method of carbon network supported noble metals nano-particle material Download PDF

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Publication number
CN110449149A
CN110449149A CN201910570848.0A CN201910570848A CN110449149A CN 110449149 A CN110449149 A CN 110449149A CN 201910570848 A CN201910570848 A CN 201910570848A CN 110449149 A CN110449149 A CN 110449149A
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chloride
potassium
acid
sodium
platinum
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赵乃勤
朱杉
沙军威
马丽颖
何春年
师春生
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Tianjin University
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Tianjin University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/42—Platinum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44—Palladium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/48—Silver or gold
    • B01J23/50—Silver
    • B01J35/23—
    • B01J35/33—
    • B01J35/393—
    • B01J35/399—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B01J37/084—Decomposition of carbon-containing compounds into carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/082—Decomposition and pyrolysis
    • B01J37/088—Decomposition of a metal salt

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Catalysts (AREA)

Abstract

The present invention relates to a kind of preparation methods of carbon network supported noble metals nano-particle material, including the following steps: water-soluble salt, carbon source, noble metal precursor body are dissolved in water according to a certain ratio, obtain mixed solution；It is dried to obtain mixed-powder；Gained powder in (2) is heated to 350~1200 DEG C under the mixed atmosphere of protection gas and hydrogen, after keeping the temperature a period of time, the carbonization of carbon source and the decomposition of noble metal precursor body is carried out, cools to room temperature with the furnace, obtain powder mixture；Will be dry after mixture cleaning in (3), obtain the composite material of carbon network supported noble metals nano particle.

Description

A kind of preparation method of carbon network supported noble metals nano-particle material
Technical field
The present invention relates to a kind of preparation methods of carbon network supported noble metals nano-particle material, belong to advanced material neck Domain.
Background technique
Noble metal (such as platinum, rhodium, palladium, ruthenium, gold) is important catalyst, suffers from fields such as chemical industry, the energy, environmental protection Important application.In order to improve the reactivity of catalyst, main stream approach is to reduce the particle size of catalyst at present, to be promoted Active surface area improves catalyst use efficiency.In chemical industry synthesis, hydrolysis produces hydrogen, and organic matter decomposes, the fields such as fuel cell, The application of noble metal nano particles catalyst can be seen.For example, its nanometer of the platinum catalyst requirement of hydrogen fuel cell Grain diameter is at 3~5 nanometers.
However, there are many problems, including preparation link to be not easy to disperse for nano particle, use process can reunite, and And discrete nano particle it is poor there is also electronics conduction efficiency the deficiencies of.Therefore, it can be used and load catalyst nano-particles In the mode of specific support, improve problem as above.
Skeleton of the catalyst carrier as catalyst activity component is responsible for support active component, divides active component It dissipates, while the intensity of catalyst can also be increased.Common carrier has aluminium oxide, silica gel, activated carbon etc..However metal or nothing Machine object carrier is often limited to the acid or alkali environment of reaction system, is not easy to be made into universal carrier.In contrast, the chemistry of carbon material Stability is preferable.Currently, the common active carbon of precious metal catalyst agent carrier, carbon black etc..However, these traditional carbon material holes The problems such as structure distribution is mostly micropore, is unable to fully contact with liquid, gaseous reactant, and low there are ion transmission efficiency.And And the preparation cost of these materials is higher, structural controllability is poor.
Carbon network is a kind of carbon material with three-dimensional communication nanostructure, has both the spies such as bigger serface, high conductivity Point.Compared to traditional carbon material, connectivity structure the coming into full contact with particularly suitable for reactant of carbon network, and ion can be improved Mass transport process.These advantages make a kind of catalyst carrier of the carbon network material as great potential.
To sum up, a kind of composite material of carbon network supported noble metals nano particle is developed, wherein specific surface area height, aperture point The excellent carbon network carrier of cloth can give full play to the catalytic performance of noble metal nano particles.The material will have very high using valence Value.
Summary of the invention
Object of the present invention is to develop a kind of composite material and preparation method thereof of carbon network supported noble metals nano particle, specific skill Art method is to realize target material preparation in conjunction with high temperature cabonization technique using water-soluble salt as template.Technical solution is as follows:
A kind of preparation method of carbon network supported noble metals nano-particle material, including the following steps:
(1) water-soluble salt, carbon source, noble metal precursor body are dissolved in water according to a certain ratio, obtain mixed solution；
(2) it is dried gained mixed solution in (1) to obtain mixed-powder；
(3) by gained powder in (2), under the mixed atmosphere of protection gas and hydrogen, 350~1200 DEG C are heated to, heat preservation After a period of time, the carbonization of carbon source and the decomposition of noble metal precursor body are carried out, room temperature is cooled to the furnace, obtains powder-mixed Object；
(4) will be dry after mixture cleaning in (3), obtain the composite material of carbon network supported noble metals nano particle.
(1) by water-soluble salt, carbon source, noble metal precursor body according to (0.5~50) in: (0.01~10): (0.01~10) Ratio is dissolved in water.Water-soluble salt is sodium chloride, sodium carbonate, sodium metasilicate, sodium sulphate, potassium chloride, potassium sulfate, calcium sulfate, potassium carbonate, chlorine Change one or more combinations of calcium, calcium carbonate.The carbon source includes glucose, sucrose, fructose, citric acid, polyvinyl alcohol, winestone Acid, one of gelatin or multiple combinations.(1) noble metal precursor body described in include chloroplatinic acid, potassium chloroplatinate, platinic sodium chloride, Ammonium chloroplatinate, platinum mercaptides, four platinum potassium cyanide, dinitroso diammonia platinum, cyaniding platinum, platinum nitrate, platinum chloride, dintrile phenyl dichloro Change platinum, triphenylphosphine platinum chloride, radium chloride, rhodium chloride, chlorine rhodium acid, rhodium sulfate, rhodium nitrate, rhodium acetate, chlorine rhodium acid potassium, chlorine rhodium Sour sodium, chlorine rhodium acid ammonium, palladium nitrate, palladium chloride, palladium sulfate, potassium chloropalladate, chlorine palladium acid sodium, ammonium chloropalladate, ruthenic chloride, tri-chlorination Ruthenium, ruthenium hydrochloride potassium, ruthenium hydrochloride sodium, ruthenium hydrochloride ammonium, chloro-iridic acid, iridous chloride, acetic acid iridium, ammonium chloroiridate, potassium hexachloroiridate, chloro-iridic acid Sodium, chlorauride, gold chloride, gold hydroxide, potassium chloroaurate, ammonium chloraurate, sodium chloraurate, potassium auricyanide, silver nitrate, silver chlorate, One or more combinations of silver acetate, silver carbonate, silver sulfate, silver orthophosphate, silver potassium cyanide.(3) 500-700 DEG C is heated in.
Compared with prior art, the beneficial effects of the present invention are: raw materials used abundant, simple process, yield height.It is obtained Material in noble metal nano grain even particle distribution, the diameter of particle is controllable within the scope of 0.5~100nm, gives full play to expensive The catalytic performance of metal nanoparticle；Carbon network has bigger serface and ultra-thin nano-lamellar structure, and this carbon structure is made For the carrier of noble metal granule, its reunion can be prevented, and improves ion transmission and electronics conductive process simultaneously.
Detailed description of the invention
Fig. 1 is the pictorial diagram of the immobilized Pt nanoparticle material of carbon network prepared by the embodiment of the present invention one
Fig. 2 is the transmission electron microscope figure of the immobilized Pt nanoparticle material of carbon network obtained by the embodiment of the present invention one
Transmission electron microscope figure of the Fig. 3 for immobilized Pt nanoparticle on carbon network obtained by the embodiment of the present invention one
Fig. 4 is that the immobilized Pt nanoparticle material of carbon network prepared by the embodiment of the present invention one measures analysis in 1M KOH solution Hydrogen reacts chemical property figure
Specific embodiment
Technology path of the invention is illustrated first: salt is dispersed in water, carbon source and noble metal is then added Catalyst precursor, after mixing, by drying, high-temperature calcination, the techniques such as desalination are gone in washing, obtain the composite material, Technique is as follows:
(1) by water-soluble salt, carbon source, noble metal precursor body according to mass ratio (0.5~50): (0.01~10): (0.01~ 10) ratio is dissolved in water, obtains mixed solution.The water-soluble salt includes but is not limited to sodium chloride, sodium carbonate, sodium metasilicate, sulphur One or more combinations of sour sodium, potassium chloride, potassium sulfate, calcium sulfate, potassium carbonate, calcium chloride, calcium carbonate；The carbon source include but It is not limited to glucose, sucrose, fructose, citric acid, polyvinyl alcohol, tartaric acid, one of gelatin or multiple combinations；Your gold Belonging to presoma includes but is not limited to chloroplatinic acid, potassium chloroplatinate, platinic sodium chloride, ammonium chloroplatinate, platinum mercaptides, four platinum potassium cyanide, two Nitroso diamino platinum, cyaniding platinum, platinum nitrate, platinum chloride, dintrile phenyl dichloro platinum, triphenylphosphine platinum chloride, radium chloride, trichlorine Change rhodium, chlorine rhodium acid, rhodium sulfate, rhodium nitrate, rhodium acetate, chlorine rhodium acid potassium, chlorine rhodium acid sodium, chlorine rhodium acid ammonium, palladium nitrate, palladium chloride, sulphur Sour palladium, potassium chloropalladate, chlorine palladium acid sodium, ammonium chloropalladate, ruthenic chloride, ruthenium trichloride, ruthenium hydrochloride potassium, ruthenium hydrochloride sodium, ruthenium hydrochloride ammonium, chlorine Iridium acid, iridous chloride, acetic acid iridium, ammonium chloroiridate, potassium hexachloroiridate, iridium sodium chloride, chlorauride, gold chloride, gold hydroxide, gold chloride Potassium, ammonium chloraurate, sodium chloraurate, potassium auricyanide, silver nitrate, silver chlorate, silver acetate, silver carbonate, silver sulfate, silver orthophosphate, cyaniding One or more combinations of silver-colored potassium.
(2) it is dried gained mixed solution in (1) to obtain mixed-powder.The drying mode includes the following: 1. cold It is lyophilized dry: mixed solution being placed in -5~-200 DEG C and is freezed, then freezing obtained solid is placed in freeze drier, In It is carried out in vacuum environment freeze-drying 12~72 hours；2. heating, drying: mixed solution is placed in 12 in 50~100 DEG C of baking ovens~ 200 hours；3. spray drying: mixed solution is removed moisture content by 80~200 DEG C of spray dried form.
(3) gained powder in (2) is placed in tube furnace, argon gas, nitrogen, hydrogen one or more mixed atmospheres Under, 350~1200 DEG C are heated to the heating rate of 0.5~500 DEG C/min, 0.01~12 hour is kept the temperature, carries out the carbon of carbon source Change and the decomposition of noble metal precursor body, cool to room temperature with the furnace, obtain powder mixture.
(4) mixture in (3) is used into deionized water filtering and washing, and product will be filtered in 50~100 DEG C of drying boxes It is 5~72 hours dry, obtain the composite material of carbon network supported noble metals nano particle.
The present invention will be further described below with reference to examples, these embodiments are only intended to illustrate the present invention, not The limitation present invention.
Embodiment one
Sodium chloride, glucose, potassium chloroplatinate are dissolved in water according to the ratio of mass ratio 2:0.1:0.05, obtain mixing molten Liquid.Mixed solution is placed in liquid nitrogen and is freezed, and is transferred to freeze drier (vacuum degree < 50Pa, -50 DEG C of condenser temperature) In, freeze-drying 12 hours is carried out, hybrid solid powder is obtained.The solid powder is placed in tube furnace, 200ml/min's Under argon atmosphere, 650 DEG C are heated to the heating rate of 50 DEG C/min, 10 minutes is kept the temperature, carries out carbonization and the platinum forerunner of carbon source The decomposition of body, cools to room temperature with the furnace, obtains powder mixture.Mixture uses deionized water filtering and washing, and will filter Product is 48 hours dry in 60 DEG C of drying boxes, obtains the immobilized Pt nanoparticle material of carbon network.
Embodiment two
Calcium chloride, sucrose, chlorine palladium acid sodium, water are dissolved in water according to the ratio of mass ratio 1:0.5:0.01, obtain mixing molten Liquid.Mixed solution is placed in 80 DEG C of baking ovens 72 hours, hybrid solid powder is obtained.The solid powder is placed in tube furnace, Under the mixed atmosphere of 50ml/min argon gas and 50ml/min hydrogen, 700 DEG C are heated to the heating rate of 5 DEG C/min, heat preservation 1 Hour, the carbonization of carbon source and the decomposition of platinum presoma are carried out, room temperature is cooled to the furnace, obtains powder mixture.Mixture uses Deionized water filtering and washing, and product drying 24 hours in 80 DEG C of drying boxes will be filtered, obtain the immobilized palladium nanometer of carbon network Grain material.
Embodiment three
Sodium chloride, sucrose, silver nitrate, water are dissolved in water according to the ratio of mass ratio 1:0.5:0.1, obtain mixed solution. Mixed solution is removed into moisture content by 150 DEG C of spray dried form.The solid powder is placed in tube furnace, in 100ml/ Under the hydrogen atmosphere of min, 600 DEG C are heated to the heating rate of 10 DEG C/min, 2 hours is kept the temperature, carries out carbonization and the platinum of carbon source The decomposition of presoma, cools to room temperature with the furnace, obtains powder mixture.Mixture uses deionized water filtering and washing, and will It is 12 hours dry in 90 DEG C of drying boxes to filter product, obtains the immobilized silver nano-grain material of carbon network.

Claims (6)

1. a kind of preparation method of carbon network supported noble metals nano-particle material, including the following steps:
(1) water-soluble salt, carbon source, noble metal precursor body are dissolved in water according to a certain ratio, obtain mixed solution.
(2) it is dried gained mixed solution in (1) to obtain mixed-powder；
(3) gained powder in (2) is heated to 350~1200 DEG C under the mixed atmosphere of protection gas and hydrogen, keeps the temperature one section After time, the carbonization of carbon source and the decomposition of noble metal precursor body are carried out, room temperature is cooled to the furnace, obtains powder mixture；
(4) will be dry after mixture cleaning in (3), obtain the composite material of carbon network supported noble metals nano particle.
2. preparation method according to claim 1, which is characterized in that (1) by water-soluble salt, carbon source, noble metal precursor body in According to (0.5~50): (0.01~10): the ratio of (0.01~10) is dissolved in water.
3. preparation method according to claim 1, which is characterized in that (1) in, water-soluble salt is sodium chloride, sodium carbonate, silicic acid One or more combinations of sodium, sodium sulphate, potassium chloride, potassium sulfate, calcium sulfate, potassium carbonate, calcium chloride, calcium carbonate.
4. preparation method according to claim 1, which is characterized in that (1) carbon source described in includes glucose, sucrose, fruit Sugar, citric acid, polyvinyl alcohol, tartaric acid, one of gelatin or multiple combinations.
5. preparation method according to claim 1, which is characterized in that (1) noble metal precursor body described in include chloroplatinic acid, Potassium chloroplatinate, platinic sodium chloride, ammonium chloroplatinate, platinum mercaptides, four platinum potassium cyanide, dinitroso diammonia platinum, cyaniding platinum, platinum nitrate, Platinum chloride, dintrile phenyl dichloro platinum, triphenylphosphine platinum chloride, radium chloride, rhodium chloride, chlorine rhodium acid, rhodium sulfate, rhodium nitrate, Rhodium acetate, chlorine rhodium acid potassium, chlorine rhodium acid sodium, chlorine rhodium acid ammonium, palladium nitrate, palladium chloride, palladium sulfate, potassium chloropalladate, chlorine palladium acid sodium, chlorine palladium Sour ammonium, ruthenic chloride, ruthenium trichloride, ruthenium hydrochloride potassium, ruthenium hydrochloride sodium, ruthenium hydrochloride ammonium, chloro-iridic acid, iridous chloride, acetic acid iridium, chloro-iridic acid Ammonium, potassium hexachloroiridate, iridium sodium chloride, chlorauride, gold chloride, gold hydroxide, potassium chloroaurate, ammonium chloraurate, sodium chloraurate, gold cyanide Potassium, one or more combinations of silver nitrate, silver chlorate, silver acetate, silver carbonate, silver sulfate, silver orthophosphate, silver potassium cyanide.
6. preparation method according to claim 1, which is characterized in that (3) be heated to 500-700 DEG C in.
CN201910570848.0A 2019-06-27 2019-06-27 A kind of preparation method of carbon network supported noble metals nano-particle material Pending CN110449149A (en)

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CN110814362A (en) * 2019-11-19 2020-02-21 广西大学 Preparation method of nano material with carbon-coated metal particle anchoring structure
CN110833835A (en) * 2019-11-19 2020-02-25 广西大学 Preparation method of carbon-coated metal particle anchored nano catalytic material
CN112736261A (en) * 2021-01-07 2021-04-30 天津大学 Porous carbon network supported platinum nanoparticle composite catalyst and preparation method thereof
CN114749172A (en) * 2022-04-21 2022-07-15 清华大学 Continuous preparation method of carbon nano material loaded with small-particle-size noble metal
CN117733167A (en) * 2024-02-20 2024-03-22 天津大学 Superfine metal nano-particles and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN110814362A (en) * 2019-11-19 2020-02-21 广西大学 Preparation method of nano material with carbon-coated metal particle anchoring structure
CN110833835A (en) * 2019-11-19 2020-02-25 广西大学 Preparation method of carbon-coated metal particle anchored nano catalytic material
CN110833835B (en) * 2019-11-19 2023-06-09 广西大学 Preparation method of carbon-coated metal particle anchored nano catalytic material
CN112736261A (en) * 2021-01-07 2021-04-30 天津大学 Porous carbon network supported platinum nanoparticle composite catalyst and preparation method thereof
CN114749172A (en) * 2022-04-21 2022-07-15 清华大学 Continuous preparation method of carbon nano material loaded with small-particle-size noble metal
CN117733167A (en) * 2024-02-20 2024-03-22 天津大学 Superfine metal nano-particles and preparation method thereof

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