CN110433836A - A kind of melten salt electriochemistry preparation method of silicon carbide/carbon optic catalytic composite material - Google Patents
A kind of melten salt electriochemistry preparation method of silicon carbide/carbon optic catalytic composite material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 39
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 38
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 150000003839 salts Chemical class 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 14
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000010703 silicon Substances 0.000 claims abstract description 24
- 239000002028 Biomass Substances 0.000 claims abstract description 22
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000012298 atmosphere Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 24
- 229910002804 graphite Inorganic materials 0.000 claims description 16
- 239000010439 graphite Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000638 solvent extraction Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 229910021389 graphene Inorganic materials 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 229910003481 amorphous carbon Inorganic materials 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002070 nanowire Substances 0.000 claims description 4
- 240000007594 Oryza sativa Species 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 240000008042 Zea mays Species 0.000 claims description 3
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims description 3
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 3
- 235000005822 corn Nutrition 0.000 claims description 3
- 239000010903 husk Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- 239000010907 stover Substances 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 2
- 244000105624 Arachis hypogaea Species 0.000 claims description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 2
- 235000018262 Arachis monticola Nutrition 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229910052914 metal silicate Inorganic materials 0.000 claims description 2
- 239000002071 nanotube Substances 0.000 claims description 2
- 235000020232 peanut Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000010902 straw Substances 0.000 claims description 2
- 229910003978 SiClx Inorganic materials 0.000 claims 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 claims 1
- 229940005991 chloric acid Drugs 0.000 claims 1
- 125000005842 heteroatom Chemical group 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 230000006872 improvement Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000001507 sample dispersion Methods 0.000 description 3
- 235000019795 sodium metasilicate Nutrition 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 2
- 235000012241 calcium silicate Nutrition 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003426 co-catalyst Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-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
- 241001659863 Panna Species 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Inorganic materials [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000000584 ultraviolet--visible--near infrared spectrum Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
- B01J27/224—Silicon carbide
-
- 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
- B01J35/39—Photocatalytic 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention discloses a kind of melten salt electriochemistry preparation method of silicon carbide/carbon optic catalytic composite material, which mainly uses high temperature fused salt electrolysis method to prepare, and raw material is mainly from the biomass for being rich in element silicon.It by additional silicon source or calcines biomass in advance and silicon, carbon mass ratio in raw material is adjusted; to reach the controllable adjustment of SiC and C mass in product; then it is electrolysed with adjusting in the fused salt that the raw material tabletting of silicon, carbon mass ratio is made under electrode inertness atmosphere protection; it washes, filter or is centrifugated after electrolysis, be dried to obtain silicon carbide/carbon optic catalytic composite material.Nano shape is mainly presented in silicon carbide in obtained product, and is in close contact with carbon, which is conducive to electron transmission and can effectively inhibit the compound of photo-generated carrier.The composite material has stronger application in photocatalysis field, and its preparation process is simple, energy consumption is lower, spatiotemporal efficiency is high, is easy to continuous production.
Description
Technical field
The invention belongs to field of photocatalytic material, are related to a kind of photocatalysis preparation method, and in particular to a kind of silicon carbide/carbon
The melten salt electriochemistry preparation method of optic catalytic composite material.
Background technique
SiC material hardness is extremely strong, with thermal coefficient is high, thermal stability is good, high temperature anti-pressure ability is strong, fusing point is high, heat is swollen
The advantageous properties such as swollen coefficient is low, breakdown electric field is high, good in oxidation resistance and acid-alkali-corrosive-resisting, are widely used in ceramic base material
Material, semiconductor (high-temperature electronic, UV sensor, light emitting diode and high speed device) and aerospace field.Wherein, as
Semiconductor material, SiC have wider band gap, high carrier saturation drift velocity, thus photocatalysis field occupy greatly it is excellent
Gesture.(wherein 3C-SiC is~2.4eV to the band gap of this material, and 6H-SiC is~3.0eV, 2H- generally between 2.3-3.3eV
SiC is~3.3eV), there is stronger absorbability to light.In addition, its conduction band bottom ratio H+/H2Reduction potential it is more negative (-
0.41eV vs.NHE, pH=7.0), valence band current potential ratio O2/O2-Oxidizing potential corrects (- 0.82eV vs.NHE, pH=7.0), this
There is the full photodissociation using water.Inoue et al. is for the first time using SiC as photochemical catalyst, for CO under the conditions of pure water2Reduction, and
Successfully prepare formaldehyde and methanol product.However, SiC is as a kind of photochemical catalyst, photo-generated carrier combined efficiency is higher, deposits
In short slab.In order to overcome this disadvantage, many experts and scholars have carried out numerous studies, and the main microstructure including material changes
Into, doping, carried noble metal and addition co-catalyst formed compound (typical document are as follows: Catal.Today, 2013,212:
220-224；Nanoscale,2015,7(19):8955-8961；J.Mater.Chem.A,2014,2(18):6296-6300；
Electrochim.Acta,2018,267:24-33).In addition, SiC material can also be improved to a certain extent by introducing appropriate carbon source
Photocatalysis performance, this is mainly due to carbon material and has such as biggish electron storage capacitance, good electron conduction, change
Stability, excellent mechanical strength and big specific surface area are learned, quick transmission channel can be provided for electron transmission, effectively
Carrier recombination efficiency is reduced, while absorption band is extended into visible light region, to improve photocatalysis performance (typical document
Are as follows: Nano Research, 2016,9 (3): 886-898.；J.Mater.Chem.A,2015,3(20):10999-11005；
Catal.Sci.Technol.,2015,5(5):2798-2806.)。
The preparation method of silicon carbide/carbon composite material mainly include with additional graphene, organic matter (sucrose, glucose or
Resorcinol etc.) be carbon source, sodium metasilicate, tetraethyl orthosilicate, silicon powder and chloroform etc. be silicon source, after evenly mixing in
Under the conditions of 1000-1500 DEG C carbon thermal reduction generate obtain SiC/C material (typical document are as follows: J.Am.Chem.Soc.2018,140,
14595-14598, Appl.Catal.B-Environ.206 (2017) 158-167, J.Mater.Chem.A, 2015,3,
10999–11005；Exemplary patents are as follows: 105506579 A of CN 106629734 A, CN 1083104050 A, CN).But the party
The problems such as method is used there are hot conditions, operating procedure complexity and additional chemical reagent.Fused salt has good thermal stability, low
Vapour pressure, low viscosity, high conductivity, high specific heat capacity and wider temperature range and by favor.Britain's chemist's Chinese is not
In 1807, electrolyzing fused NaOH was prepared for metallic sodium to Lai Daiwei (H.Davy) for the first time.Subsequent metal Ti, K, Li and Al etc. are golden
Category is produced out by fused salt electrolysis process, and extends to commercial scale.Fused salt has good heat-transfer character and high specific heat capacity can
It is wide in biomass preparation porous charcoal technical aspect for the quick heat supply of biomass thermal treatment process and to provide inert reaction environment
General research (typical document are as follows: Environ.Sci.Technol., 2014,48 (14): 8101-8108；Carbon,2014,69:
460-466；RSC Advances,2015,5(92):75728-75734).Utilize fused salt processing silicon containing biomass preparation carbonization
The great development prospect of silicon/carbon composite.
Summary of the invention
It is an object of the present invention to solve existing silicon substrate or it is carbon-based there is lack of raw materials and silicon carbide technology of preparing existing for it is multiple
Miscellaneous, inefficiency problem provides a kind of melten salt electriochemistry preparation method of silicon carbide/carbon composite material, develops catalysis material.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that:
A kind of melten salt electriochemistry preparation method of silicon carbide/carbon optic catalytic composite material, which is characterized in that including following step
It is rapid:
Step 1, using silicon containing biomass as raw material, adjust silicon containing biomass raw material C, Si element mass ratio；
Biomass material after adjusting C, Si element mass ratio is crushed tabletting by step 2, and electrode is made；
Step 3 is electrolysed certain time in the fused salt under inert atmosphere protection；
After the completion of step 4, electrolysis, product cools down under an inert atmosphere, then washes, filters or is centrifugated, dry
To silicon carbide/carbon optic catalytic composite material.
As an improvement, it is described adjust silicon containing biomass raw material C, Si element mass ratio method include in air calcining,
Solvent extraction and additional silicon source.
As an improvement, the silicon containing biomass includes rice husk, corn stover, peanut shell, shuck, straw and diatom, but
It is not limited to these types of biomass material.
As an improvement, the calcination time calcined in the air is 0-100h, temperature is 100-1000 DEG C；The solvent extraction
The solvent extraction agent followed the example of includes any one in formic acid, dilute sulfuric acid, acetic acid and hypochlorous acid or several combinations；The additional silicon
The silicon source in source is silica, metal silicate (calcium silicates, sodium metasilicate etc.) and metasilicate (calcium metasilicate, sodium metasilicate etc.)
In any one or a few combination.
As an improvement, in the step 1, C and Si elemental mole ratios 1:0.001-1:1 in silicon containing biomass raw material.
As an improvement, electrolytic method is two electrolysis (permanent slot pressure or constant current) or three electrolysis in the step 3
(constant potential or constant current)；In two-stage electrolysis method, manufactured electrode is cathode after biomass material crushes tabletting, and graphite is sun
Pole；In three electrolysis methods, manufactured electrode is working electrode after biomass material crushes tabletting, and graphite is to electrode, reference
Electrode is high-temperature full sealed reference electrode disclosed in patent CN 2004200174467.
As an improvement, electrolysis time 0.1-120h, electrolysis temperature is 400-1200 DEG C, skill of the present invention in the step 3
Art scheme makes electrolysis electricity reach theoretical by comprehensively control electrolytic cell pressure (or electrolytic potential, Faradaic current) and electrolysis time
Institute's electricity demand or more.
As an improvement, the fused salt is CaCl2Unitary salt contains CaCl2Polynary mixed salt.
As an improvement, the silicon carbide size in the step 4, in the product silicon carbide/carbon optic catalytic composite material of preparation
At 5nm-1 μm, pattern includes one of nano wire, nano particle and nanotube or a variety of.
As an improvement, the carbon in the product silicon carbide/carbon optic catalytic composite material of preparation is mainly nothing in the step 4
Shape one of carbon, graphite, graphene or the heteroatomic amorphous carbon of doping, graphite, graphene or a variety of.
The silicon carbide/carbon optic catalytic composite material of technical solution of the present invention preparation is mainly used for making photochemical catalyst, including
Photocatalysis carbon dioxide reduction, Photocatalyzed Hydrogen Production and contaminant degradation can be widely used for environmental pollution degradation treatment.
The medicine have the advantages that
(1) present invention process one-step synthesis silicon carbide/carbon material, it is easy to operate, low in cost, it can be achieved that large-scale production
With；
(2) by regulation raw material silicon carbon ratio, the silicon carbide/carbon compound of heterogeneity ratio is realized；
(3) silicon carbide/carbon of this method preparation has good photocatalysis performance.
Detailed description of the invention
The following drawings remarks additionally to a specific embodiment of the invention.
Fig. 1 is silicon carbide/graphite mixture XRD schematic diagram that embodiment 1 obtains；
Fig. 2 is silicon carbide/graphite mixture SEM schematic diagram that embodiment 1 obtains；
Fig. 3 is silicon carbide/graphite mixture photocatalysis CO that embodiment 1 obtains2Reducing property.
Specific embodiment
In order to further illustrate the present invention, silicon carbide/carbon material provided by the invention is carried out below with reference to embodiment detailed
It carefully describes, but they cannot be interpreted as to limiting the scope of the present invention, the tabletting in the embodiment of the present invention refers both to machine
The technique that electrode is made in tool crushing tabletting is repeated no more again using routine techniques in the prior art.
Embodiment 1
Using rice husk as raw material, directly crushes, a certain amount of SiO is added2, adjusting carbon silicon ratio is 1:0.05, and yin is used as after tabletting
Pole material, the CaCl using graphite rod as anode, under argon atmosphere protection2With 800 DEG C, 2.2V slot pressure in-NaCl Molten Binary Salts
Condition electrolysis 2h after obtain product.It washed, be centrifuged, carry out XRD test after dry, product X RD result is as shown in Figure 1, main
It to be the mixed phase of silicon carbide and graphite.Its pattern is mainly shown as that nano wire is attached on graphite (Fig. 2).
Material prepared is used as photocatalysis carbon dioxide reduction catalyst.50mg sample is taken to be placed in 200mL customization
In quartz reaction tank, 2mL deionized water injection reaction pot bottom is pipetted using pipette, ultrasonic 30min is uniform to sample dispersion,
60 DEG C of dry 12h in an oven, are prepared into catalyst film；Reactor both ends are sealed with rubber stopper, are passed through Ar gas 30min to go
Except air.With NaHCO3And H2SO4It is in situ to generate CO for raw material2And H2O gas is as reaction gas.Reactor tank is placed on visible
Under light (420-780nm, 300W Xe lamp, Perfectlight, Beijing), illumination 5h takes 1mL gas test every 1h,
Gaseous product content is mainly using the gas chromatograph (PGC- for being configured with flame ionization detector (FID) and methane reborner
80, PANNA instrument, Changzhou, China) detection.The photocatalytic activity of material is as shown in figure 3, can from figure
Know, product shows good photocatalytic activity, primary product CO, and yield is 10.1 μm of ol g-1h-1。
Embodiment 2
Using corn stover as raw material, after calcining 2h in 600 DEG C of air, tabletting is crushed, is used as cathode material, with graphite rod
CaCl for anode, under argon atmosphere protection2After being electrolysed 1h in fused salt with the condition of 900 DEG C, 2.6V slot pressure, through washing, from
The heart is dried to obtain silicon carbide/amorphous carbon composite material.Its pattern is mainly shown as that nano wire is wrapped in carbon block.
The material of preparation is used as photocatalysis and produces H2Catalyst.It takes 50mg sample to be placed in having for 200mL customization to cool down
In the quartz reaction tank of water interlayer, 100mL 0.1M Na is pipetted using pipette2S solution is passed through Ar gas into reactor tank
30min removes air in reactor tank, and subsequent ultrasound 30min is uniform to sample dispersion, magneton is put into, in entire light-catalyzed reaction
It is persistently stirred in journey.With ultraviolet-visible light (300-780nm, 300W Xe lamp, Perfectlight, Beijing) for light
Source, illumination 5h take 1mL gas test every 1h.Gaseous product content is mainly using the gas phase for being configured with thermal conductivity detector (TCD) (TCD)
Chromatograph (GC-2014, Shimadzu) detection.In the case where not adding any co-catalyst state, H2Yield is about 500 μm of ol g- 1h-1。
Embodiment 3
Using shuck as raw material, a certain amount of SiO is added2Into raw material, adjusts C and Si element ratio is about 1:1, later powder
Broken tabletting is used as working electrode.It is to electrode with graphite rod, reference electrode is disclosed in patent CN 200420017446.7
High-temperature full sealed reference electrode, the CaCl under argon atmosphere protection2In-NaCl-CaO ternary molten salt, with 800 DEG C, -1.3V
After the condition electrolysis 10h of current potential, is washed, is centrifuged, be dried to obtain carbofrax material.Its pattern is mainly shown as nano particle
Shape.
The material of preparation is used as photocatalyst for degrading rhodamine B.Take 10mg sample dispersion in 50mL 10mg L-1Sieve
In red bright B solution, magnetic agitation 2h reaches the adsorption equilibrium to rhodamine B under a dark condition.With ultraviolet-visible light (300-
780nm, 300W Xe lamp, Perfectlight, Beijing) it is light source, illumination 2h is extracted every 0.5h using syringe
1mL suspension, and by 0.45 μm of teflon syringe filter membrane filtering to remove photochemical catalyst.Filtrate deionized water
4 times of dilution.By measuring the peak strength at 554nm with ultraviolet-visible-near-infrared spectrum meter (UV-2600, Shimadzu),
To determine the rhodamine B concentration under different time intervals.By 1h illumination, the degradation rate of rhodamine B has reached 95%.
The above is only a preferred embodiment of the present invention, it is not intended to limit the present invention in any form.It should
It points out, for those skilled in the art, without departing from the principle of the present invention, if can also make
Dry improvements and modifications, these modifications and embellishments should also be considered as the scope of protection of the present invention.
Claims (10)
1. a kind of melten salt electriochemistry preparation method of silicon carbide/carbon optic catalytic composite material, which is characterized in that including following step
It is rapid:
Step 1, using silicon containing biomass as raw material, adjust silicon containing biomass raw material C, Si element mass ratio；
Biomass material after adjusting C, Si element mass ratio is crushed tabletting by step 2, and electrode is made；
Step 3 is electrolysed certain time in the fused salt under inert atmosphere protection；
After the completion of step 4, electrolysis, product cools down under an inert atmosphere, then washes, filters or is centrifugated, is dried to obtain carbon
SiClx/carbon optic catalytic composite material.
2. melten salt electriochemistry preparation method as described in claim 1, it is characterised in that: the adjusting silicon containing biomass raw material
C, the method for Si element mass ratio includes calcining, solvent extraction and additional silicon source in air.
3. melten salt electriochemistry preparation method as claimed in claim 2, it is characterised in that: the silicon containing biomass include rice husk,
Corn stover, peanut shell, shuck, straw and diatom.
4. melten salt electriochemistry preparation method as claimed in claim 2, it is characterised in that: the calcination time calcined in the air
For 0-100h, temperature is 100-1000 DEG C；The solvent extraction agent of the solvent extraction includes formic acid, dilute sulfuric acid, acetic acid and secondary
Any one in chloric acid or several combinations；The silicon source of the additional silicon source is silica, metal silicate and metasilicate
In any one or a few combination.
5. melten salt electriochemistry preparation method as claimed in claim 2, it is characterised in that: in the step 1, silicon containing biomass is former
C and Si elemental mole ratios 1:0.01-1:1 in material.
6. melten salt electriochemistry preparation method as claimed in claim 2, it is characterised in that: in the step 3, electrolytic method two
Electrolysis or three electrolysis；In two-stage electrolysis method, manufactured electrode is cathode after biomass material crushes tabletting, and graphite is
Anode；In three electrolysis methods, manufactured electrode is working electrode after biomass material crushes tabletting, and graphite is to electrode.
7. melten salt electriochemistry preparation method as claimed in claim 6, it is characterised in that: in the step 3, electrolysis time is
0.1-120h, electrolysis temperature are 400-1200 DEG C.
8. melten salt electriochemistry preparation method as claimed in claim 2, it is characterised in that: the fused salt is CaCl2Unitary salt contains
There is CaCl2Polynary mixed salt.
9. the melten salt electriochemistry preparation method as described in claim 1 to 8 any one, it is characterised in that: in the step 4,
For silicon carbide size in the product silicon carbide/carbon optic catalytic composite material of preparation at 5nm-1 μm, pattern includes nano wire, nanometer
One of particle and nanotube are a variety of.
10. the melten salt electriochemistry preparation method as described in claim 1 to 8 any one, it is characterised in that: in the step 4,
Carbon in the product silicon carbide/carbon optic catalytic composite material of preparation is mainly amorphous carbon, graphite, graphene or doping hetero atom
Amorphous carbon, graphite, one of graphene or a variety of.
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