CN109913892A - A method of utilizing indium sulfide/ferronickel houghite composite membrane photoelectrocatalysioxidization oxidization xylose - Google Patents
A method of utilizing indium sulfide/ferronickel houghite composite membrane photoelectrocatalysioxidization oxidization xylose Download PDFInfo
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- CN109913892A CN109913892A CN201910211462.0A CN201910211462A CN109913892A CN 109913892 A CN109913892 A CN 109913892A CN 201910211462 A CN201910211462 A CN 201910211462A CN 109913892 A CN109913892 A CN 109913892A
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- China
- Prior art keywords
- ferronickel
- indium sulfide
- xylose
- houghite
- composite membrane
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- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 title claims abstract description 96
- GKCNVZWZCYIBPR-UHFFFAOYSA-N sulfanylideneindium Chemical compound [In]=S GKCNVZWZCYIBPR-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910000863 Ferronickel Inorganic materials 0.000 title claims abstract description 53
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 title claims abstract description 48
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 239000012528 membrane Substances 0.000 title claims abstract description 31
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 31
- 239000011521 glass Substances 0.000 claims abstract description 53
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 22
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 11
- 238000005286 illumination Methods 0.000 claims abstract description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 25
- 239000013078 crystal Substances 0.000 claims description 23
- 239000010408 film Substances 0.000 claims description 22
- 239000010409 thin film Substances 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 13
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- 239000004202 carbamide Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- ODHZEGQLIOGNFQ-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;indium Chemical compound [In].OC(=O)CC(O)(C(O)=O)CC(O)=O ODHZEGQLIOGNFQ-UHFFFAOYSA-N 0.000 claims description 10
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 8
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 7
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 7
- 229960001545 hydrotalcite Drugs 0.000 claims description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- 150000002815 nickel Chemical class 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 239000003792 electrolyte Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical group [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims 1
- 229940075397 calomel Drugs 0.000 claims 1
- LITYQKYYGUGQLY-UHFFFAOYSA-N iron nitric acid Chemical group [Fe].O[N+]([O-])=O LITYQKYYGUGQLY-UHFFFAOYSA-N 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract description 2
- 239000003115 supporting electrolyte Substances 0.000 abstract 1
- 230000003287 optical effect Effects 0.000 description 24
- 230000003647 oxidation Effects 0.000 description 21
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 16
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 238000004090 dissolution Methods 0.000 description 12
- 239000003643 water by type Substances 0.000 description 12
- 229910052738 indium Inorganic materials 0.000 description 11
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 11
- 150000003742 xyloses Chemical class 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 229910002651 NO3 Inorganic materials 0.000 description 6
- 239000007832 Na2SO4 Substances 0.000 description 6
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 6
- 150000001408 amides Chemical class 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
- 201000006747 infectious mononucleosis Diseases 0.000 description 6
- SPIFDSWFDKNERT-UHFFFAOYSA-N nickel;hydrate Chemical compound O.[Ni] SPIFDSWFDKNERT-UHFFFAOYSA-N 0.000 description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 6
- 229910052724 xenon Inorganic materials 0.000 description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 235000005979 Citrus limon Nutrition 0.000 description 4
- 244000131522 Citrus pyriformis Species 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000004073 vulcanization Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000010815 organic waste Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 101710088194 Dehydrogenase Proteins 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 241000589236 Gluconobacter Species 0.000 description 1
- 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
- 206010054949 Metaplasia Diseases 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- SIXIBASSFIFHDK-UHFFFAOYSA-N indium(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[In+3].[In+3] SIXIBASSFIFHDK-UHFFFAOYSA-N 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- -1 weaving Substances 0.000 description 1
- 125000000969 xylosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)CO1)* 0.000 description 1
Abstract
The invention belongs to photoelectrocatalysis fields, indium sulfide/ferronickel houghite composite membrane photoelectrocatalysioxidization oxidization xylose method is utilized more particularly to a kind of: using indium sulfide/ferronickel houghite composite membrane for being carried on electro-conductive glass as light anode, using platinum plate electrode as to electrode, using saturated calomel electrode as reference electrode, in illumination and under conditions of be biased, photoelectrocatalysioxidization oxidization is carried out to the xylose solution in electrolytic cell containing supporting electrolyte, xylonic is prepared.Xylose can be oxidized to xylonic rapidly under sunlight, ultraviolet light and radiation of visible light, there is simple process, advantage low in cost, suitable for large-scale production, have broad application prospects.
Description
Technical field
The invention belongs to photoelectrocatalysis fields, and in particular to a kind of to utilize indium sulfide/ferronickel houghite composite membrane photoelectricity
The method of catalysis oxidation xylose.
Background technique
The renewable biomass resources such as agriculture and forestry organic waste material are made full use of to produce green chemical products, to realize chemical industry
Sustainable development obtains more and more concerns.Hemicellulose is the second largest component in agriculture and forestry organic waste material in addition to cellulose,
Content of its xylosyl in agriculture and forestry organic waste material may be up to 18 ~ 30%, using in the cob of agricultural wastes such as corn, stalk
Hydrolysis of hemicellulose can produce xylose, xylose, which further aoxidizes, can produce xylonic.Xylonic is that one kind most develops
The xylose product of future.It can be used as a kind of multi-functional platform chemicals, in leather, weaving, medicine, building, change
It learns the every field such as chemical industry, metallurgy to be applied, great development and application prospect.
It include biological oxidation process, chemical oxidization method, electrochemistry currently with the main method that xylose oxidation prepares xylonic
Oxidizing process and photocatalytic oxidation.Biological oxidation process is to utilize the oxidation of the microbial fermentations such as Gluconobacter oxvdans or glucose
Oxidizing ferment and xylose dehydrogenase catalysis oxidation xylose prepare xylonic, and manufacturing condition is more mild, will not cause to environment
Harm, but it is stringenter to working condition requirement, and the production cycle is long, by-product is difficult to separate.Chemical oxidization method can be divided into again
Homogeneous catalytic oxidation method and heterogeneous catalytic oxidation method, homogeneous catalytic oxidation method are to prepare xylonic using catalysis of iodine oxidation xylose,
It is needed in reaction process by the hydroxyl protection in xylose molecule, to which hydroxyl protection base is taken off again after the reaction was completed, production
The problems such as complex process, by-product is more, and product is difficult to separate, and there are catalyst recycling；The common catalysis of heterogeneous catalytic oxidation method
Agent is precious metal palladium or activated carbon, although solving the separation problem of catalyst, need heating and under conditions of logical oxygen into
Row, reaction condition are also considerably complicated.Electrolytic oxidation simple process is generated without by-product, but energy consumption is high, and condition is not easily-controllable
System.Photocatalytic oxidation is the method that catalysis oxidation xylose prepares xylonic under such as modified carbonitride of photochemical catalyst and illumination,
Solving the disadvantage that electrocatalytic oxidation, energy consumption is high, but the recombination rate in light induced electron and hole is high, cause light-catalyzed reaction efficiency compared with
It is low.Therefore, current xylonic preparation method is still further improved.
Summary of the invention
For the deficiency of current xylose oxidation technology, xylose system is aoxidized using photo-electrocatalytic technology the invention proposes a kind of
The method of standby xylonic, this method both have the advantages that electrolytic oxidation, urge further through light is overcome using photo-electrocatalytic technology
The deficiency that the recombination rate in light induced electron and hole is high in change, reaction efficiency is low, have simple process, it is low in cost, be suitable for scale
The advantage that metaplasia produces.
A method of using indium sulfide/ferronickel houghite composite membrane photoelectrocatalysioxidization oxidization xylose, to be carried on conduction
Indium sulfide/ferronickel houghite composite membrane on glass is as light anode, using platinum plate electrode as to electrode, to be saturated calomel electricity
Pole in illumination and under conditions of be biased, carries out light to the xylose solution in electrolytic cell containing electrolyte as reference electrode
Xylonic is prepared in electrocatalytic oxidation.
Preferably, the electro-conductive glass is tin oxide (FTO) electro-conductive glass for adulterating fluorine.
Preferably, the electro-conductive glass is cleaned using preceding through acetone and deionized water.
Preferably, the molar ratio of nickel and iron is 3:1 in the ferronickel houghite.
Preferably, the illumination is one of sunlight, ultraviolet light, visible light and near infrared light；
Preferably, the bias is 0.1 ~ 0.3 V；Preferably 0.2V.
Preferably, the electrolyte is the Na of 0.25mol/L2SO4Aqueous solution.
Preferably, the concentration of the xylose solution is 0.1-2wt%.
The indium sulfide of the present invention being carried on electro-conductive glass/ferronickel houghite composite film photo-anode refers in conduction
First depositing indium sulfide thin film on glass, then ferronickel hydrotalcite film institute is deposited on the electro-conductive glass for be deposited with indium sulfide thin film
The compound film optoelectronic pole of composition.
A kind of indium sulfide/ferronickel houghite composite membrane, is prepared by following steps:
(1) thioacetyl amine aqueous solution is added in the citric acid indium complex solution that citric acid and inidum chloride are formed, formation
Mixed liquor is transferred in reaction kettle, while being vertically put into FTO electro-conductive glass and being sealed, and it is small that 6 ~ 10 are reacted under the conditions of 80 ± 5 DEG C
When, obtain the electro-conductive glass for being deposited with indium sulfide thin film；
(2) nickel salt, molysite, urea and ammonium fluoride are blended and dissolved in water, form mixed solution, is transferred in reaction kettle,
It is vertically put into the electro-conductive glass obtained in step (1) for being deposited with indium sulfide thin film and sealing simultaneously, is reacted at 120 ± 5 DEG C
10 ~ 15 hours, obtain the indium sulfide/ferronickel houghite composite membrane being attached on electro-conductive glass.
In the presence of citric acid, low-temperature hydrothermal is passed through as indium source using thioacetamide as sulphur source using inidum chloride
The indium sulfide thin film material that the indium sulfide crystal and in-situ deposition of method synthesis highly crystalline are formed on FTO electro-conductive glass.?
In the presence of ammonium fluoride, passed through using nickel nitrate and ferric nitrate as divalent and trivalent metal salt using urea as precipitating reagent
Hydro-thermal method synthesizes nickel-ferric spinel and in-situ deposition on the indium sulfide thin film of conductive glass surface, forms indium sulfide/ferronickel class
The laminated film light positive electrode of hydrotalcite.
Preferably, the molar ratio of citric acid and inidum chloride as described in step (1) is 4 ~ 8:1；
Preferably, the molar ratio of thioacetamide and inidum chloride as described in step (1) is 1:3 ~ 5.
Preferably, nickel salt described in step (2), molysite, urea and ammonium fluoride molar ratio are 3:1:6 ~ 8:1 ~ 4.
Preferably, nickel salt described in step (2) is nickel nitrate.
Preferably, molysite described in step (2) is ferric nitrate.
Preferably, 0.5 ~ 1.0 micron of indium sulfide thin film thickness as described in step (1), by 50 ~ 500 nanometers of granularity and
The cubic phase indium sulfide crystal composition of 1 ~ 2 micron of degree.
Preferably, 1.0 ~ 20 microns of thickness of ferronickel houghite film described in step (2), by 20 ~ 50 nanometers of thickness,
300 ~ 800 nanometers of diameter of sheet ferronickel houghite crystal composition.
Indium sulfide prepared by the present invention/ferronickel houghite composite membrane is due to Full spectrum photocatalyst indium sulfide and in purple
Outside, there is the presence of the ferronickel houghite of good absorption performance in visible and near infrared light region, to sunlight, ultraviolet light, can
Light-exposed and near infrared light all has responding ability, can be under sunlight, ultraviolet, visible and near infrared light irradiation, in aqueous medium
In xylose is directly oxidized to xylonic, but oxidation rate is more slow.Prepared indium sulfide and ferronickel houghite are answered
Film is closed as light anode, platinum plate electrode as cathode, using saturated calomel electrode as reference electrode, together with light source and power supply
Photoelectro catalytic system is formed, the bias of 0.2V is applied, due to the export of light induced electron, promotes point in light induced electron and hole
From, the photohole on indium sulfide and ferronickel houghite laminated film is greatly improved to the oxidation of xylose, even if
Under near infrared light, also xylose can be oxidized to xylonic.
The utility model has the advantages that
Indium sulfide of the invention/ferronickel houghite laminated film has excellent photoelectrocatalysioxidization oxidization performance.Applying 0.2V
Under conditions of bias, ultraviolet light 2 hours, xylose was that the ratio of xylonic is up to 97.8%；Irradiation 2 is small under visible light
When, xylose is that the ratio of xylonic reaches 86.4%；Near infrared light 2 hours, xylose was that the ratio of xylonic is
31.4%；Simulated solar irradiation irradiates 1 hour, and xylose is that the ratio of xylonic is 92.7%.Therefore, load of the invention is utilized
In the indium sulfide on electro-conductive glass/ferronickel houghite composite membrane as light anode, platinum plate electrode is saturated calomel electricity as cathode
Xylose can be oxidized to xylonic rapidly under sunlight, ultraviolet light and radiation of visible light as reference electrode by pole.With technique
Simply, advantage low in cost, suitable for large-scale production, has broad application prospects.
Detailed description of the invention
Fig. 1 indium sulfide (In2S3) and indium sulfide/ferronickel houghite composite membrane (In2S3/ NiFe-LDH) X- of material penetrates
Ray diffraction diagram spectrum, wherein abscissa is angle of diffraction, and ordinate is diffracted intensity；
Fig. 2 indium sulfide/ferronickel houghite composite membrane scanning electron microscope image.
Specific embodiment
The present invention is further explained in the light of specific embodiments, and the present embodiment before being with technical solution of the present invention
It puts and is implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to down
The embodiment stated；Except as otherwise indicating, the described ground number in embodiment is mass parts.
Embodiment 1
(1) 5.7 parts of Citric Acid Monos are added in 20 parts of deionized waters, after completely dissolution, 1 part of inidum chloride, stirring are added
After dissolution, citric acid indium complex solution is formed.1.36 parts of thioacetamides are dissolved in 20 parts of deionized waters, thio second is formed
Amide solution.Thioacetyl amine aqueous solution is slowly dropped under stiring in citric acid indium complex solution and forms mixed solution,
And it is transferred in reaction kettle, while being vertically put into 10 × 30 mm FTO electro-conductive glass through acetone and deionized water cleaning, sealing
It is reacted 8 hours at 80 DEG C afterwards, obtains the electro-conductive glass for being deposited with indium sulfide thin film.0.8 ~ 1 micron of indium sulfide thin film thickness, by
100 ~ 500 nanometers of granularity of cubic phase indium sulfide crystal and 1 ~ 2 micron of granularity of cubic phase indium sulfide crystal group being sporadicly distributed
At；
(2) 2.16 part of six water nickel nitrate, 1 part of nine water ferric nitrate, 1 part of urea and 0.2 point of ammonium fluoride are successively dissolved in 40 parts
In ionized water, mixed solution is formed, and is transferred in reaction kettle, while is vertically put into and obtained in step (1) being deposited with vulcanization
The electro-conductive glass of indium film reacts 12 hours at 120 DEG C after sealing, the indium sulfide/ferronickel class that must be attached on electro-conductive glass
The composite membrane of hydrotalcite.Wherein 15 ~ 20 microns of the thickness of ferronickel houghite film, by 20 ~ 50 nanometers of thickness, diameter 300 ~ 800
The sheet ferronickel houghite crystal composition of nanometer；
(3) 1 part of xylose is dissolved in 250 parts of 0.25mol/L Na2SO4Aqueous solution is simultaneously added in electrolytic cell, with system in step (2)
The standby electro-conductive glass for being attached with indium sulfide/ferronickel houghite composite membrane is as light anode, using platinum plate electrode as to electricity
Pole under the irradiation of 40 W xenon lamps, adds 0.2V bias using saturated calomel electrode as reference electrode, under conditions of optical filter is not added,
2 hours, xylose was that the ratio of xylonic is 98.5%；After adding optical filter to remove the visible above light of 380 nm and near infrared light,
It is 97.8% that 2 hours xyloses, which are the ratio of xylonic,；After adding optical filter to filter 380 nm or less ultraviolet lights, xylose turns within 2 hours
The ratio for turning to xylonic is 86.4%；After adding optical filter to filter 720 nm or less ultraviolet lights and visible light, 2 hours xyloses
Ratio for xylonic is 31.4%.
Embodiment 2
(1) 5.7 parts of Citric Acid Monos are added in 20 parts of deionized waters, after completely dissolution, 1 part of inidum chloride, stirring are added
After dissolution, citric acid indium complex solution is formed.1.36 parts of thioacetamides are dissolved in 20 parts of deionized waters, thio second is formed
Amide solution.Thioacetyl amine aqueous solution is slowly dropped under stiring in citric acid indium complex solution and forms mixed solution,
And it is transferred in reaction kettle, while being vertically put into 10 × 30 mm FTO electro-conductive glass through acetone and deionized water cleaning, sealing
It is reacted 8 hours at 80 DEG C afterwards, obtains the electro-conductive glass for being deposited with indium sulfide thin film.0.8 ~ 1 micron of indium sulfide thin film thickness, by
100 ~ 500 nanometers of granularity of cubic phase indium sulfide crystal and 1 ~ 2 micron of granularity of cubic phase indium sulfide crystal group being sporadicly distributed
At；
(2) 2.16 part of six water nickel nitrate, 1 part of nine water ferric nitrate, 1 part of urea and 0.2 point of ammonium fluoride are successively dissolved in 40 parts
In ionized water, mixed solution is formed, and is transferred in reaction kettle, while is vertically put into and obtained in step (1) being deposited with vulcanization
The electro-conductive glass of indium film reacts 12 hours at 120 DEG C after sealing, the indium sulfide/ferronickel class that must be attached on electro-conductive glass
The composite membrane of hydrotalcite.Wherein 15 ~ 20 microns of the thickness of ferronickel houghite film, by 20 ~ 50 nanometers of thickness, diameter 300 ~ 800
The sheet ferronickel houghite crystal composition of nanometer；
(3) 0.25 part of xylose is dissolved in 250 parts of 0.25mol/L Na2SO4Aqueous solution is simultaneously added in electrolytic cell, with step (2)
The electro-conductive glass for being attached with indium sulfide/ferronickel houghite composite membrane of middle preparation is made as light positive electrode with platinum plate electrode
Using saturated calomel electrode as reference electrode, under the irradiation of 40 W xenon lamps, to add 0.2V bias, optical filter being not added to electrode
Under the conditions of, 2 hours, xylose was that the ratio of xylonic is 99.2%；Optical filter is added to remove the visible above light of 380 nm and close red
After outer light, it is 98.8% that 2 hours xyloses, which are the ratio of xylonic,；After adding optical filter to filter 380 nm or less ultraviolet lights, 2 is small
When xylose be the ratio of xylonic be 89.4%；After adding optical filter to filter 720 nm or less ultraviolet lights and visible light, 2 hours
Xylose is that the ratio of xylonic is 44.5%.
Embodiment 3
(1) 5.7 parts of Citric Acid Monos are added in 20 parts of deionized waters, after completely dissolution, 1 part of inidum chloride, stirring are added
After dissolution, citric acid indium complex solution is formed.1.36 parts of thioacetamides are dissolved in 20 parts of deionized waters, thio second is formed
Amide solution.Thioacetyl amine aqueous solution is slowly dropped under stiring in lemon acid indium complex solution and forms mixed solution, and
It is transferred in reaction kettle, while being vertically put into 10 × 30 mm FTO electro-conductive glass pieces through acetone and deionized water cleaning, sealing
It is reacted 8 hours at 80 DEG C afterwards, obtains the electro-conductive glass for being deposited with indium sulfide thin film.0.8 ~ 1 micron of indium sulfide thin film thickness, by
100 ~ 500 nanometers of granularity of cubic phase indium sulfide crystal and 1 ~ 2 micron of granularity of cubic phase indium sulfide crystal group being sporadicly distributed
At；
(2) 2.16 part of six water nickel nitrate, 1 part of nine water ferric nitrate, 1 part of urea and 0.2 point of ammonium fluoride are successively dissolved in 40 parts
In ionized water, mixed solution is formed, and is transferred in reaction kettle, while is vertically put into and obtained in step (1) being deposited with vulcanization
The electro-conductive glass of indium film reacts 12 hours at 120 DEG C after sealing, the indium sulfide/ferronickel class that must be attached on electro-conductive glass
The composite membrane of hydrotalcite.Wherein 15 ~ 20 microns of the thickness of ferronickel houghite film, by 20 ~ 50 nanometers of thickness, diameter 300 ~ 800
The sheet ferronickel houghite crystal composition of nanometer；
(3) 5 parts of xyloses are dissolved in 250 parts of 0.25mol/L Na2SO4Aqueous solution is simultaneously added in electrolytic cell, with system in step (2)
The standby electro-conductive glass for being attached with indium sulfide/ferronickel houghite composite membrane as light positive electrode, using platinum plate electrode as pair
Electrode under the irradiation of 40 W xenon lamps, adds 0.2V bias, in the condition that optical filter is not added using saturated calomel electrode as reference electrode
Under, 2 hours, xylose was that the ratio of xylonic is 78.9%；Optical filter is added to remove the visible above light of 380 nm and near infrared light
Afterwards, it is 78.2% that 2 hours xyloses, which are the ratio of xylonic,；After adding optical filter to filter 380 nm or less ultraviolet lights, 2 hours wood
The ratio that sugar is converted into xylonic is 56.4%；After adding optical filter to filter 720 nm or less ultraviolet lights and visible light, 2 hours xyloses
The ratio for being converted into xylonic is 21.1%.
Embodiment 4
(1) 3.8 parts of Citric Acid Monos are added in 20 parts of deionized waters, after completely dissolution, 1 part of inidum chloride, stirring are added
After dissolution, citric acid indium complex solution is formed.1.70 parts of thioacetamides are dissolved in 20 parts of deionized waters, thio second is formed
Amide solution.Thioacetyl amine aqueous solution is slowly dropped to lemon acid indium complex solution under stiring and forms mixed solution, and is turned
It moves on in reaction kettle, while being vertically put into 10 × 30 mm FTO electro-conductive glass pieces through acetone and deionized water cleaning, after sealing
It is reacted 6 hours at 80 DEG C, obtains the electro-conductive glass for being deposited with indium sulfide thin film.0.5 ~ 0.8 micron of indium sulfide thin film thickness, by
100 ~ 500 nanometers of granularity of cubic phase indium sulfide crystal and 1 ~ 2 micron of granularity of cubic phase indium sulfide crystal group being sporadicly distributed
At；
(2) 2.16 part of six water nickel nitrate, 1 part of nine water ferric nitrate, 0.9 part of urea and 0.4 point of ammonium fluoride are successively dissolved in 40 parts
In deionized water, mixed solution is formed, and is transferred in reaction kettle, while is vertically put into and obtained in step (1) being deposited with sulphur
The electro-conductive glass for changing indium film, reacts 15 hours at 120 DEG C, the indium sulfide/ferronickel that must be attached on electro-conductive glass after sealing
The composite membrane of houghite.Wherein 12 ~ 18 microns of the thickness of ferronickel houghite film, by 20 ~ 50 nanometers of thickness, diameter 300 ~
800 nanometers of sheet ferronickel houghite crystal composition；
(3) 1 part of xylose is dissolved in 250 parts of 0.25mol/L Na2SO4Aqueous solution is simultaneously added in electrolytic cell, with system in step (2)
The standby electro-conductive glass for being attached with indium sulfide/ferronickel houghite composite membrane as light positive electrode, using platinum plate electrode as pair
Electrode under the irradiation of 40 W xenon lamps, adds 0.2V bias, in the condition that optical filter is not added using saturated calomel electrode as reference electrode
Under, 2 hours, xylose was that the ratio of xylonic is 97.3%；Optical filter is added to remove the visible above light of 380 nm and near infrared light
Afterwards, it is 96.8% that 2 hours xyloses, which are the ratio of xylonic,；After adding optical filter to filter 380 nm or less ultraviolet lights, 2 hours wood
The ratio that sugar is converted into xylonic is 81.7%；After adding optical filter to filter 720 nm or less ultraviolet lights and visible light, 2 hours xyloses
The ratio for being converted into xylonic is 29.6%.
Embodiment 5
(1) 7.6 parts of Citric Acid Monos are added in 20 parts of deionized waters, after completely dissolution, 1 part of inidum chloride, stirring are added
After dissolution, citric acid indium complex solution is formed.1.02 parts of thioacetamides are dissolved in 20 parts of deionized waters, thio second is formed
Amide solution.Thioacetyl amine aqueous solution is slowly dropped under stiring in lemon acid indium complex solution and forms mixed solution, and
It is transferred in reaction kettle, while being vertically put into 10 × 30 mm FTO electro-conductive glass pieces through acetone and deionized water cleaning, sealing
It is reacted 10 hours at 80 DEG C afterwards, obtains the electro-conductive glass for being deposited with indium sulfide thin film.0.8 ~ 1 micron of indium sulfide thin film thickness,
1 ~ 2 micron of granularity of cubic phase indium sulfide crystal by 100 ~ 500 nanometers of granularity of cubic phase indium sulfide crystal and being sporadicly distributed
Composition；
(2) 2.16 part of six water nickel nitrate, 1 part of nine water ferric nitrate, 1.2 parts of urea and 0.09 point of ammonium fluoride are successively dissolved in 40 parts
In deionized water, mixed solution is formed, and is transferred in reaction kettle, while is vertically put into and obtained in step (1) being deposited with sulphur
The electro-conductive glass for changing indium film, reacts 10 hours at 120 DEG C, the indium sulfide/ferronickel that must be attached on electro-conductive glass after sealing
The composite membrane of houghite.Wherein 10 ~ 15 microns of the thickness of ferronickel houghite film, by 20 ~ 50 nanometers of thickness, diameter 300 ~
800 nanometers of sheet ferronickel houghite crystal composition；
(3) 1 part of xylose is dissolved in 250 parts of 0.25mol/L Na2SO4Aqueous solution is simultaneously added in electrolytic cell, with system in step (2)
The standby electro-conductive glass for being attached with indium sulfide/ferronickel houghite laminated film as light positive electrode, using platinum plate electrode as
To electrode, using saturated calomel electrode as reference electrode, under the irradiation of 40 W xenon lamps, add 0.2V bias, in the item that optical filter is not added
Under part, 2 hours, xylose was that the ratio of xylonic is 96.1%；Optical filter is added to remove the visible above light of 380 nm and near-infrared
After light, it is 94.5% that 2 hours xyloses, which are the ratio of xylonic,；After adding optical filter to filter 380 nm or less ultraviolet lights, 2 hours
Xylose is that the ratio of xylonic is 79.4%；After adding optical filter to filter 720 nm or less ultraviolet lights and visible light, 2 hours wood
The ratio that sugar is converted into xylonic is 27.9%.
Comparative example 1
(1) 5.7 parts of Citric Acid Monos are added in 20 parts of deionized waters, after completely dissolution, 1 part of inidum chloride, stirring are added
After dissolution, citric acid indium complex solution is formed.1.36 parts of thioacetamides are dissolved in 20 parts of deionized waters, thio second is formed
Amide solution.Thioacetyl amine aqueous solution is slowly dropped under stiring in lemon acid indium complex solution and forms mixed solution, and
It is transferred in reaction kettle, while being vertically put into 10 × 30 mm FTO electro-conductive glass pieces through acetone and deionized water cleaning, sealing
It is reacted 8 hours at 80 DEG C afterwards, obtains the electro-conductive glass for being deposited with indium sulfide thin film.0.8 ~ 1 micron of indium sulfide thin film thickness, by
100 ~ 500 nanometers of granularity of cubic phase indium sulfide crystal and 1 ~ 2 micron of granularity of cubic phase indium sulfide crystal group being sporadicly distributed
At；
(2) 2.16 part of six water nickel nitrate, 1 part of nine water ferric nitrate, 1 part of urea and 0.2 part of ammonium fluoride are successively dissolved in 40 parts
In ionized water, mixed solution is formed, and is transferred in reaction kettle, while is vertically put into and obtained in step (1) being deposited with vulcanization
The electro-conductive glass of indium film reacts 12 hours at 120 DEG C after sealing, the indium sulfide/ferronickel class that must be attached on electro-conductive glass
The composite membrane of hydrotalcite.Wherein 15 ~ 20 microns of the thickness of ferronickel houghite film, by 20 ~ 50 nanometers of thickness, diameter 300 ~ 800
The sheet ferronickel houghite crystal composition of nanometer；
(3) 1 part of xylose is dissolved in 250 parts of 0.25mol/L Na2SO4Aqueous solution is simultaneously added in electrolytic cell, with system in step (2)
The standby electro-conductive glass for being attached with indium sulfide/ferronickel houghite composite membrane as light positive electrode, using platinum plate electrode as pair
Electrode, using saturated calomel electrode as reference electrode, under the irradiation of 40 W xenon lamps, not under conditions of biasing and optical filter, 2 is small
When, xylose is that the ratio of xylonic is 52.3%；After adding optical filter to remove the visible above light of 380 nm and near infrared light, 2 is small
When xylose be the ratio of xylonic be 47.7%；After adding optical filter to filter 380 nm or less ultraviolet lights, 2 hours xyloses
Ratio for xylonic is 24.0%；After adding optical filter to filter 720 nm or less ultraviolet lights and visible light, xylose is within 2 hours
The ratio of xylonic is 4.8%.
Claims (10)
1. a kind of utilize indium sulfide/ferronickel houghite composite membrane photoelectrocatalysioxidization oxidization xylose method, which is characterized in that with negative
Indium sulfide/ferronickel houghite composite membrane on electro-conductive glass is loaded in as light anode, using platinum plate electrode as to electrode, with full
It is molten to the xylose in electrolytic cell containing electrolyte in illumination and under conditions of be biased with calomel electrode as reference electrode
Liquid carries out photoelectrocatalysioxidization oxidization, and xylonic is prepared.
2. the method according to claim 1, wherein the electro-conductive glass is the fin oxide condutire glass for adulterating fluorine
Glass.
3. the method according to claim 1, wherein the molar ratio of ferronickel is 3 in the ferronickel houghite:
1。
4. the method according to claim 1, wherein the illumination is sunlight, ultraviolet light, visible light and close
One of infrared light；The bias is 0.1 ~ 0.3 V.
5. the method according to claim 1, wherein the bias is 0.2V.
6. the method according to claim 1, wherein the electrolyte is the Na of 0.25mol/L2SO4It is water-soluble
Liquid；The concentration of the xylose solution is 0.1-2wt%.
7. a kind of indium sulfide as claimed in any one of claims 1 to 6/ferronickel houghite composite membrane, which is characterized in that pass through
Following steps are prepared:
Thioacetyl amine aqueous solution is added in the citric acid indium complex solution that citric acid and inidum chloride are formed, the mixing of formation
Solution is transferred in reaction kettle, while being vertically put into electro-conductive glass and being sealed, and is reacted 6 ~ 10 hours, is obtained under the conditions of 80 ± 5 DEG C
To the electro-conductive glass for being deposited with indium sulfide thin film；
Nickel salt, molysite, urea and ammonium fluoride are blended and dissolved in water, mixed solution is formed, is transferred in reaction kettle, simultaneously
It is vertically put into the electro-conductive glass obtained in step (1) for being deposited with indium sulfide thin film and sealing, 10 ~ 15 are reacted at 120 ± 5 DEG C
Hour, obtain the indium sulfide/ferronickel houghite composite membrane being attached on electro-conductive glass.
8. indium sulfide according to claim 7/ferronickel houghite composite membrane, which is characterized in that as described in step (1)
The molar ratio of citric acid and inidum chloride is 4 ~ 8:1；The molar ratio of the thioacetamide and inidum chloride is 1:3 ~ 5.
9. indium sulfide according to claim 7/ferronickel houghite composite membrane, which is characterized in that nickel described in step (2)
Salt, molysite, urea and ammonium fluoride molar ratio are 3:1:6 ~ 8:1 ~ 4；The nickel salt is nickel nitrate；The molysite is nitric acid
Iron.
10. indium sulfide according to claim 7/ferronickel houghite composite membrane, which is characterized in that described in step (1)
0.5 ~ 1.0 micron of indium sulfide thin film thickness, by 50 ~ 500 nanometers of granularity and 1 ~ 2 micron of granularity of cubic phase indium sulfide crystal group
At；1.0 ~ 20 microns of the thickness of ferronickel hydrotalcite film described in step (2), by 20 ~ 50 nanometers of thickness, diameter 300 ~
800 nanometers of sheet ferronickel houghite crystal composition.
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