CN110508311A - A kind of porous boron doped carbon supported platinum nano beaded catalyst and its preparation method and application based on electrostatic spinning technique - Google Patents
A kind of porous boron doped carbon supported platinum nano beaded catalyst and its preparation method and application based on electrostatic spinning technique Download PDFInfo
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- CN110508311A CN110508311A CN201910816300.XA CN201910816300A CN110508311A CN 110508311 A CN110508311 A CN 110508311A CN 201910816300 A CN201910816300 A CN 201910816300A CN 110508311 A CN110508311 A CN 110508311A
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 239000003054 catalyst Substances 0.000 title claims abstract description 92
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 52
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 45
- 238000010041 electrostatic spinning Methods 0.000 title claims abstract description 32
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 37
- 239000002105 nanoparticle Substances 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000009987 spinning Methods 0.000 claims abstract description 23
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 230000003647 oxidation Effects 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 9
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 9
- 238000005253 cladding Methods 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- 239000004327 boric acid Substances 0.000 claims description 7
- 235000013339 cereals Nutrition 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- -1 Boratex Substances 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 241000209094 Oryza Species 0.000 claims 2
- 230000003197 catalytic effect Effects 0.000 abstract description 14
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 description 17
- 239000012528 membrane Substances 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 16
- 229920000557 Nafion® Polymers 0.000 description 14
- 238000006555 catalytic reaction Methods 0.000 description 10
- 230000035484 reaction time Effects 0.000 description 8
- 238000002474 experimental method Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002070 nanowire Substances 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 238000011017 operating method Methods 0.000 description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 230000036647 reaction Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000006197 hydroboration reaction Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 230000000754 repressing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011877 solvent mixture Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/391—Physical properties of the active metal ingredient
- B01J35/393—Metal or metal oxide crystallite size
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/396—Distribution of the active metal ingredient
- B01J35/399—Distribution of the active metal ingredient homogeneously throughout the support particle
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/13—Ozone
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Textile Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of porous boron doped carbon supported platinum nano beaded catalyst and its preparation method and application based on electrostatic spinning technique, catalyst of the present invention the preparation method comprises the following steps: the surfactant that Pt nanoparticle will be coated, boron-containing compound and high molecular polymer are added in organic solvent, it is stirred at 60-80 DEG C 2-4 hours and forms sticky mixed liquor, it is 14-18 kV that the sticky mixed liquor of gained, which is transferred in syringe in voltage, spinning obtains blocky spinning material under conditions of fltting speed 1-2.5mL/h, gained bulk spinning material is in air atmosphere, it is aoxidized at a temperature of 180-250 DEG C, oxidization time 1-3 h, material after gained oxidation carries out high-temperature calcination under the atmosphere of high-purity gas, high-temperature calcination temperature is 700-1000 DEG C, when high-temperature calcination Between 2-4h to get catalyst of the invention.Not only preparation cost is low for catalyst of the invention, but also prepares in ozone being applied to electrolysis water, electro catalytic activity with higher, superpower stability, hence it is evident that improve electrolysis water and prepare ozone current efficiency.
Description
Technical field
The porous boron doped carbon supported platinum nano beaded catalyst that the present invention relates to a kind of based on electrostatic spinning technique and its
Preparation method and application.
Background technique
With the rapid development and production-scale continuous expansion of industrial technology, problem of environmental pollution is on the rise, organic
Industrial geomantic omen pollution, which becomes, influences one of extensive, serious pollutant of harm in current water quality and water process.Ozone is a kind of strong
Oxidant has highest oxidation potential in common oxidants.Therefore, ozone can effectively destroy most of organic matter in water, go
The stink and color of water removal, while drinking water, the bacterium in dirty water and air and virus are effectively killed, and itself is reduced to oxygen
Gas does not generate secondary pollution.Therefore, many countries have used it to replace chlorine as the disinfectant of tap water.
Currently, the production method of ozone is mainly corona discharge method, UV radiation and electrochemical process.Wherein electrolysis water
Ozone technology processed is easy to operate, product purity is high and preparation process is comparatively safe, is most suitable ozone process processed.Electricity at present
Xie Shui prepares ozone mainly under neutral or acid condition, using catalyst such as platinum, brown lead oxide and stannic oxides, above-mentioned catalysis
Agent has that stability is poor.
Therefore, the primary restraining factors that electrolysis water prepares ozone development are exactly the problems such as catalyst toxicity is big, the service life is short.Such as
What is developed one kind electrolysis water ozone working electrode catalyst that cost is relatively low, performance is stable and improves ozone production efficiency, is
Electrolysis water prepares the research emphasis of ozone.
Summary of the invention
For above-mentioned technical problem of the existing technology, the purpose of the present invention is to provide one kind to be based on electrostatic spinning skill
Porous boron doped carbon supported platinum nano beaded catalyst of art and its preparation method and application, catalyst of the invention is not only prepared
It is at low cost, and prepared in ozone being applied to electrolysis water, current efficiency is high, stability is good.
A kind of preparation side of the porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique
Method, it is characterised in that the following steps are included:
1) surfactant, boron-containing compound and high molecular polymer that coat Pt nanoparticle are added in organic solvent,
It is stirred 2-4 hours under 60-80 DEG C of oil bath, forms uniform sticky mixed liquor；Wherein, the surface of the cladding Pt nanoparticle
The mass ratio of activating agent, boron-containing compound and high molecular polymer is 0.2: 0.1-0.4: 0.8-1.2；
2) sticky mixed liquor obtained by step 1) is transferred in syringe, is 14-18 kV, fltting speed 1-2.5mL/h in voltage
Under conditions of carry out spinning, obtain blocky spinning material；
3) blocky spinning material obtained by step 2 is aoxidized in air atmosphere, oxidizing temperature is 180-250 DEG C, when oxidation
Between 1-3 h, the flexible material after being aoxidized；
4) flexible material after oxidation obtained by step 3) carries out high-temperature calcination under the atmosphere of high-purity gas, and high-temperature calcination temperature is
700-1000 DEG C, high-temperature calcination time 2-4h receives to get the porous boron doped carbon Supported Pt Nanoparticles based on electrostatic spinning technique
Rice grain catalyst.
A kind of preparation side of the porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique
Method, it is characterised in that in step 1), boron-containing compound is boric acid, Boratex, sodium borohydride or potassium borohydride, preferably boric acid.
A kind of preparation side of the porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique
Method, it is characterised in that in step 1), the high molecular polymer is polyacrylonitrile or polyvinylpyrrolidone, the polyacrylonitrile
Molecular weight be 130000-160000, the molecular weight of the polyvinylpyrrolidone is 24000-1500000.
A kind of preparation side of the porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique
Method, it is characterised in that in step 1), the organic solvent be n,N-Dimethylformamide or n,N-dimethylacetamide, preferably
N,N-dimethylformamide；The ratio between the high molecular polymerization amount of substance and organic solvent volume be 1:10-50, mass unit g,
Volume unit is mL；In step 4), high-purity gas is nitrogen or argon gas, preferably nitrogen.
A kind of preparation side of the porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique
Method, it is characterised in that in step 1), the preparation method of the surfactant of the cladding Pt nanoparticle will be the following steps are included: will
0.05-0.1g chloroplatinic acid or chloroplatinate, 10-15ml water and 0.4-0.6 g surfactant are dissolved in 150-200ml alcohols solvent
In, gained mixed liquor is bubbled under protective condition through high-purity gas, and the oil bath reflux 2-5h at 80-150 DEG C, then revolving removes molten
Agent rotates addition acetone in residue and obtains muddy mixed liquor, is centrifugally separating to obtain sticky precipitating to get the cladding platinum nanometer
The organic matter of grain.
A kind of preparation side of the porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique
Method, it is characterised in that the alcohols solvent is methanol, ethyl alcohol, ethylene glycol or butanol, preferably methanol；The surfactant is
Polyvinylpyrrolidone or lauryl sodium sulfate, preferably polyvinylpyrrolidone.
The porous boron doped carbon supported platinum nano particulate catalytic based on electrostatic spinning technique prepared according to above-mentioned method
Agent.
The porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique is in catalytic electrolysis water
Prepare the application in ozone.
Compared with the existing technology, the beneficial effect that the present invention obtains is:
1) problem short for traditional business platinum carbon catalyst life and that platinum load capacity is high, it is of the invention for electrolysis ozone
Catalyst, electro catalytic activity with higher, superpower stability, hence it is evident that improve electrolysis water and prepare ozone current efficiency, lead to
It crosses and verifies the performance of catalyst electrolysis water catalytic production ozone of the invention and be far superior to traditional business platinum carbon catalyst.
2) catalyst of the invention during the preparation process, the alcohols solvent as reducing agent by chloroplatinic acid or chloroplatinate also
Original passes through control optimization oil bath reflux temperature, the additive amount of surfactant, chloroplatinic acid or chloroplatinic acid salinity at Pt nanoparticle
Dissipate the conditions such as the concentration in alcohols solvent, be made cladding Pt nanoparticle surfactant (partial size of Pt nanoparticle compared with
It is small, about 1-5nm size.Be conducive to compared with the Pt nanoparticle of small particle evenly dispersed in porous boron doped carbon).
3) in catalyst preparation process of the invention, during the spinning process, liquid is pushed to syringe needle, syringe needle institute by sample injector
The small liquid pearl of injection surface tension, gravity, electric field force collective effect under, can be become from spherical shape conical (i.e. taylor cone),
Conical tip further extends under the collective effect of three kinds of power obtains nano-fiber filaments.It will be sticky by electrostatic spinning technique
Precipitating, high molecular polymer, solvent mixture carry out electrostatic spinning.By changing the ginseng such as voltage, spinning distance, spinning flow velocity
Number, obtains the spinning finished product of the fiber filament of different nanometer diameters.The fiber of different-diameter not only directly affect the later period oxidation and
Stability and structure-preserved integrality in calcination process also directly influence exposure and the mass transfer energy of active site
Power, therefore parameter setting plays vital influence to catalytic effect during the spinning process.
4) in the preparation process of catalyst of the present invention, the use of electrostatic spinning technique and subsequent oxidation, high-temperature calcination
Journey makes material form block-like flexible electrode, is conducive to the transmission of reactive material and the simplification of material later period use process.
The preparation condition of flexible electrode catalyst is relatively simple, at low cost, and resistance to mechanical intensity is strong in use process, stability is good and active
Height, later period are easily recycled, and can directly recycle monolith electrode, and relative to business platinum carbon, with it is at low cost, using simple, surely
The advantages that qualitative good, makes it possible that it is commercialized.
Both 5) dosage of the platinum of catalyst of the present invention is low, incorporation and the very big boron of platinum electronegativity difference in catalyst, make
Electron orbit be overlapped, have adjusted the electronic structure of Pt nanoparticle, electrolysis water production ozone reaction process in platinum
More easily receiving and losing electrons improve catalytic activity, and effectively prevent the reunion of platinum grain.The high molecular polymer that the present invention uses is equal
Containing N element, so that N adulterates the band structure that can change carbon, doped with N in final catalyst obtained so as to improve it
Electronic conductivity.
6) in the preparation process of the surfactant of present invention cladding Pt nanoparticle, surfactant is not only advantageously used for
The dispersion of Pt nanoparticle, and being uniformly mixed for spinning material is also beneficial to during subsequent electrostatic spinning, later
High-temperature calcination is changed into carbon material.
Detailed description of the invention
Fig. 1 is the shooting photo of porous boron doped carbon supported platinum nano beaded catalyst prepared by embodiment 1；
Fig. 2 is the SEM figure of porous boron doped carbon supported platinum nano beaded catalyst prepared by embodiment 1；
Fig. 3 is the TEM figure of porous boron doped carbon supported platinum nano beaded catalyst prepared by embodiment 1；
Fig. 4 is that porous boron doped carbon supported platinum nano beaded catalyst prepared by embodiment 1 ~ 5 and 20% business platinum carbon catalyst are made
When preparing ozone reaction for electrolysis water for membrane electrode anode, the ozone concentration of generation is reacted with the variation relation in reaction time
Curve comparison figure.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but the scope of protection of the present invention is not limited thereto.
Embodiment 1:
A kind of flexible electrode catalyst of boron doping carbon supported platinum nano particle based on electrostatic spinning technique is prepared, including following
Step:
1) 0.533 g PVP is dissolved in 180 ml methanol, add 6.25ml concentration be 10 g/L chloroplatinic acid aqueous solution and
13.75ml deionized water is first cooled to room temperature after oil bath flows back 3 h at a temperature of nitrogen is bubbled atmospheric condition and 100 DEG C, then
It is 10ml that revolving, which removes solvent to volume, rotates addition acetone in residue and obtains muddy mixed liquor, it is sticky heavy to be centrifugally separating to obtain
It forms sediment；
2) sticky precipitating obtained by step 1) is taken to be added to 10ml N with 1 g polyacrylonitrile (molecular weight 150000), 0.5 g boric acid,
In dinethylformamide, is stirred 2-4 hours under 80 DEG C of oil baths, form uniform mixed liquor；
3) mixed liquor obtained by step 2 is transferred in the syringe of 10 mL, Static Spinning is carried out under the fltting speed of 1 mL/h
Silk, it is 10cm that adjustment syringe needle, which is 10 cm(i.e. spinning distance at a distance from tinfoil), voltage is 16 kV, and spinning 5h obtains flexibility
Spinning material.
4) flexible spinning material obtained by step 3) is aoxidized first, process are as follows: in air atmosphere, from room temperature with 5
DEG C/rate of min is warming up to 210 DEG C, 2h then is aoxidized at 210 DEG C, the flexible material after obtaining oxidation；
5) flexible material after oxidation obtained by step 4) is subjected to high-temperature calcination, process in a nitrogen atmosphere are as follows: in nitrogen atmosphere
Under, 900 DEG C are warming up to from room temperature with the rate of 2 DEG C/min, calcines 2h at 900 DEG C then to get negative to porous boron doped carbon
Carry Pt nanoparticle catalyst.
The shooting photo of porous boron doped carbon supported platinum nano beaded catalyst prepared by embodiment 1 is as described in Figure 1, from figure
1 it can be seen that prepared catalyst is blocky flexible material.Porous boron doped carbon supported platinum nano particle prepared by embodiment 1
The SEM of catalyst schemes as shown in Fig. 2, the porous boron doped carbon supported platinum nano particle that as can be seen from Figure 2 prepared by embodiment 1 is urged
Agent has good nano wire microstructure, and the catalyst of this structure is conducive to the transmission of reactive material, is conducive to keep
Higher catalytic activity.Embodiment 1 prepare porous boron doped carbon supported platinum nano beaded catalyst TEM figure as shown in figure 3,
Pt nanoparticle is evenly dispersed on a catalyst as can be seen from Figure 3, the partial size of Pt nanoparticle substantially within the scope of 1-5 nm,
And the average grain diameter of Pt nanoparticle is about within the scope of 2-3nm.
Electrolysis water prepares ozone experiment:
Membrane electrode material is prepared first, and preparation process is as follows:
Membrane electrode cathode preparation: taking the 20% business platinum carbon catalyst of 150mg, (i.e. in platinum carbon catalyst, the load capacity of platinum is
20wt%), it the 5wt% Nafion solution of 100mg and is distributed in 20ml isopropanol, is evaporated to paste shape, obtains platinum carbon catalyst
Slurry.Obtained platinum carbon catalyst pulp is coated on the one side of 117 film of Nafion, hot repressing makes platinum carbon catalyst
The bonding of the one side of slurry and 117 film of Nafion is close, and hot pressing temperature is 140 DEG C, and the film electricity of the 117 film side Nafion is made
Pole cathode.
The preparation of membrane electrode anode: the 5wt% Nafion solution of 100mg is distributed in 20ml isopropanol, obtains mixing molten
Liquid A.The mixed solution A for taking 0.1ml to be configured uniformly is applied on the one side of the catalyst of the preparation of embodiment 1, and embodiment 1 is made
The one side that standby catalyst is coated with mixed solution A passes through hot pressing again and above-mentioned 117 film of Nafion does not smear platinum carbon catalysis
The one side of agent slurry is bonded together, and hot pressing temperature is 140 DEG C, and the membrane electrode anode of the 117 film other side Nafion is made.
That is the one side of 117 film of proton exchange membrane Nafion is coated with platinum carbon catalyst, and 117 film of Nafion is corresponding another
Side is adhesive with the catalyst of the preparation of embodiment 1.
It carries out when electrolysis water prepares ozone experiment using ozone generator as electrochemistry generating device, cathode chamber and anode
117 film of proton exchange membrane Nafion of the above-mentioned preparation in room separates, and 117 film of Nafion is adhesive with the catalysis of the preparation of embodiment 1
The side of agent is located in anode chamber.Using ultrapure water as electrolyte, the reaction of electrolysis water production ozone, test voltage range are carried out
For 4-10V, electric current is maintained at 10A.Since cathode chamber and anode chamber are separated by proton exchange membrane, the ozone that cell reaction generates is only
Can occur in anode chamber, the ozone generated in anode chamber is collected, is analyzed, the ozone that electrolysis water catalysis reaction generates is dense
It spends as shown in Figure 4 with the variation relation in reaction time.
Embodiment 2:
Prepare a kind of flexible electrode catalyst of boron doping carbon supported platinum nano particle based on electrostatic spinning technique, preparation side
Method step repeats embodiment 1, the difference is that: the boric acid in 1 step 2 of embodiment is replaced with to the Boratex of equal quality,
Porous boron doped carbon supported platinum nano beaded catalyst is finally made with embodiment 1 in other operating procedures.
Electrolysis water prepares ozone experiment:
In 1 membrane electrode anode preparation process of embodiment, 1 catalyst of embodiment of addition is replaced with to the embodiment of equal quality
The catalyst of 2 preparations, remaining operating condition prepare ozone experimentation with the electrolysis water of embodiment 1, and electrolysis water catalysis reaction produces
Raw ozone concentration is as shown in Figure 4 with the variation relation in reaction time.
Embodiment 3:
Prepare a kind of flexible electrode catalyst of boron doping carbon supported platinum nano particle based on electrostatic spinning technique, preparation side
Method step repeats embodiment 1, the difference is that: the boric acid in 1 step 2 of embodiment is replaced with to the hydroboration of equal quality
Porous boron doped carbon supported platinum nano beaded catalyst is finally made with embodiment 1 in sodium, other operating procedures.
Electrolysis water prepares ozone experiment:
In 1 membrane electrode anode preparation process of embodiment, 1 catalyst of embodiment of addition is replaced with to the embodiment of equal quality
The catalyst of 3 preparations, remaining operating condition prepare ozone experimentation with the electrolysis water of embodiment 1, and electrolysis water catalysis reaction produces
Raw ozone concentration is as shown in Figure 4 with the variation relation in reaction time.
Embodiment 4:
Prepare a kind of flexible electrode catalyst of boron doping carbon supported platinum nano particle based on electrostatic spinning technique, preparation side
Method step repeats embodiment 1, the difference is that: the polyacrylonitrile in 1 step 2 of embodiment is replaced with into the poly- of equal quality
Vinylpyrrolidone (molecular weight of polyvinylpyrrolidone is 80000), other operating procedures are finally made more with embodiment 1
Hole boron doping carbon supported platinum nano beaded catalyst.
Electrolysis water prepares ozone experiment:
In 1 membrane electrode anode preparation process of embodiment, 1 catalyst of embodiment of addition is replaced with to the embodiment of equal quality
The catalyst of 4 preparations, remaining operating condition prepare ozone experimentation with the electrolysis water of embodiment 1, and electrolysis water catalysis reaction produces
Raw ozone concentration is as shown in Figure 4 with the variation relation in reaction time.
Embodiment 5:
Prepare a kind of flexible electrode catalyst of boron doping carbon supported platinum nano particle based on electrostatic spinning technique, preparation side
Method step repeats embodiment 1, the difference is that: the n,N-Dimethylformamide in 1 step 2 of embodiment is replaced on an equal basis
Porous boron doped carbon supported platinum nano is finally made with embodiment 1 in the n,N-dimethylacetamide of volume, other operating procedures
Grain catalyst.
Electrolysis water prepares ozone experiment:
In 1 membrane electrode anode preparation process of embodiment, 1 catalyst of embodiment of addition is replaced with to the embodiment of equal quality
The catalyst of 5 preparations, remaining operating condition prepare ozone experimentation with the electrolysis water of embodiment 1, and electrolysis water catalysis reaction produces
Raw ozone concentration is as shown in Figure 4 with the variation relation in reaction time.
Comparative example 1:
20% business platinum carbon catalyst (i.e. in platinum carbon catalyst, the load capacity of platinum is 20wt%) is prepared into ozone reality for electrolysis water
It tests:
20% business platinum carbon catalyst is applied in the two sides of 117 film of Nafion, the method for coating is the same as membrane electrode in embodiment 1
The two sides of cathode preparation process, final 117 film of proton exchange membrane Nafion are coated with platinum carbon catalyst.
It carries out when electrolysis water prepares ozone experiment using ozone generator as electrochemistry generating device, cathode chamber and anode
117 film of proton exchange membrane Nafion of the above-mentioned preparation in room separates.Using ultrapure water as electrolyte, it is smelly to carry out electrolysis water production
The reaction of oxygen, test voltage range are 4-10V, and electric current is maintained at 10A.Due to cathode chamber and anode chamber by proton exchange membrane every
It opens, the ozone that cell reaction generates can only occur in anode chamber, and the ozone generated in anode chamber is collected, is analyzed, electricity
The ozone concentration that Xie Shui catalysis reaction generates is as shown in Figure 4 with the variation relation in reaction time.
Fig. 4 is porous boron doped carbon supported platinum nano beaded catalyst prepared by embodiment 1 ~ 5 and the catalysis of 20% business platinum carbon
When agent prepares ozone reaction for electrolysis water as membrane electrode anode, the ozone concentration for reacting generation is closed with the variation in reaction time
The curve comparison figure of system.From fig. 4, it can be seen that porous boron doped carbon supported platinum nano particle prepared by the embodiment of the present invention 1 ~ 5
Catalyst is best in embodiment 1, and the catalyst of embodiment 1 and embodiment 2 is better than 20% business platinum carbon catalyst, i.e.,
Catalytic performance with superior electrochemical length of schooling ozone, and it is able to maintain good stability.
For catalyst prepared by embodiment 3 when preparing ozone reaction applied to electrolysis water, catalytic activity is not obviously strictly according to the facts
The catalyst of example 1 ~ 2 is applied, this may be that can just be dissolved in n,N-Dimethylformamide solvent because are as follows: polyacrylonitrile needs to heat
In, it is just able to maintain preferable mixed style and carries out spinning, final catalyst obtained has good nano wire microstructure.But
That will contain after boride replaces with sodium borohydride, since sodium borohydride has a very strong reproducibility, sodium borohydride may by N,
Dinethylformamide reduction is to destroy the structure of n,N-Dimethylformamide, so that polyacrylonitrile under heating can not
It dissolves well, spinning material is not able to maintain good mixed style, and spinning process is difficult to form uniform nanowire structure.
For catalyst prepared by embodiment 4 when preparing ozone reaction applied to electrolysis water, catalytic activity is not obviously strictly according to the facts
Apply the catalyst of example 1 ~ 2, this may be because are as follows: polyacrylonitrile can be very good to bear subsequent as the base material of nano wire
High-temperature calcination and be not easy that deformation occurs, the porous boron doping carbon material that high-temperature calcination is formed keeps the nanowire structure of rule.And
Polyvinylpyrrolidone can be shunk after the heating, be may result in a nanometer thread breakage, curled, be not able to maintain good array
Structure.
For catalyst prepared by embodiment 5 when preparing ozone reaction applied to electrolysis water, catalytic activity is not obviously strictly according to the facts
Apply the catalyst of example 1 ~ 2, this may be because are as follows: n,N-Dimethylformamide, can be in 14-18 kV electrostatic as spin solvent
The nano wire of uniformly continuous rule is formed under power effect, and n,N-dimethylacetamide causes viscosity to wait it due to its structure difference
His property, cannot cause catalytic effect to be deteriorated under electrostatic force well at line.
Content described in this specification is only to enumerate to inventive concept way of realization, and protection scope of the present invention is not answered
When the concrete form for being seen as limited by embodiment and being stated.
Claims (8)
1. a kind of preparation method of the porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique, feature
Be the following steps are included:
1) surfactant, boron-containing compound and high molecular polymer that coat Pt nanoparticle are added in organic solvent,
It is stirred 2-4 hours under 60-80 DEG C of oil bath, forms uniform sticky mixed liquor；Wherein, the surface of the cladding Pt nanoparticle
The mass ratio of activating agent, boron-containing compound and high molecular polymer is 0.2: 0.1-0.4: 0.8-1.2；
2) sticky mixed liquor obtained by step 1) is transferred in syringe, is 14-18 kV, fltting speed 1-2.5mL/h in voltage
Under conditions of carry out spinning, obtain blocky spinning material；
3) blocky spinning material obtained by step 2 is aoxidized in air atmosphere, oxidizing temperature is 180-250 DEG C, when oxidation
Between 1-3 h, the flexible material after being aoxidized；
4) flexible material after oxidation obtained by step 3) carries out high-temperature calcination under the atmosphere of high-purity gas, and high-temperature calcination temperature is
700-1000 DEG C, high-temperature calcination time 2-4h receives to get the porous boron doped carbon Supported Pt Nanoparticles based on electrostatic spinning technique
Rice grain catalyst.
2. a kind of porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique as described in claim 1
Preparation method, it is characterised in that in step 1), boron-containing compound be boric acid, Boratex, sodium borohydride or potassium borohydride, preferably
For boric acid.
3. a kind of porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique as described in claim 1
Preparation method, it is characterised in that in step 1), the high molecular polymer be polyacrylonitrile or polyvinylpyrrolidone, it is described
The molecular weight of polyacrylonitrile is 130000-160000, and the molecular weight of the polyvinylpyrrolidone is 24000-1500000.
4. a kind of porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique as described in claim 1
Preparation method, it is characterised in that in step 1), the organic solvent be n,N-Dimethylformamide or N, N- dimethylacetamide
Amine, preferably n,N-Dimethylformamide；The ratio between the high molecular polymerization amount of substance and organic solvent volume are 1:10-50, matter
Amount unit is g, volume unit mL；In step 4), high-purity gas is nitrogen or argon gas, preferably nitrogen.
5. a kind of porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique as described in claim 1
Preparation method, it is characterised in that in step 1), it is described cladding Pt nanoparticle surfactant preparation method include with
Lower step:
0.05-0.1g chloroplatinic acid or chloroplatinate, 10-15ml water and 0.4-0.6 g surfactant are dissolved in 150-200ml alcohol
In class solvent, gained mixed liquor is bubbled under protective condition through high-purity gas, and oil bath reflux 2-5h, then rotates at 80-150 DEG C
Solvent is removed, addition acetone in residue is rotated and obtains muddy mixed liquor, be centrifugally separating to obtain sticky precipitating to get the cladding platinum
The organic matter of nano particle.
6. a kind of porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique as claimed in claim 5
Preparation method, it is characterised in that the alcohols solvent is methanol, ethyl alcohol, ethylene glycol or butanol, preferably methanol；The surface
Activating agent is polyvinylpyrrolidone or lauryl sodium sulfate, preferably polyvinylpyrrolidone.
7. the porous boron doped carbon Supported Pt Nanoparticles based on electrostatic spinning technique prepared by the method as described in claim 1 ~ 6 is any are received
Rice grain catalyst.
8. the porous boron doped carbon supported platinum nano beaded catalyst based on electrostatic spinning technique is being urged as claimed in claim 7
Change electrolysis water and prepares the application in ozone.
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