CN105597764A - Preparation method of carbon quantum dot/zinc ferrite composite photocatalytic materials - Google Patents
Preparation method of carbon quantum dot/zinc ferrite composite photocatalytic materials Download PDFInfo
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- CN105597764A CN105597764A CN201610132912.3A CN201610132912A CN105597764A CN 105597764 A CN105597764 A CN 105597764A CN 201610132912 A CN201610132912 A CN 201610132912A CN 105597764 A CN105597764 A CN 105597764A
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- quantum dot
- carbon quantum
- zinc ferrite
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- ferrite composite
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 229910001308 Zinc ferrite Inorganic materials 0.000 title claims abstract description 98
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 230000001699 photocatalysis Effects 0.000 title abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 40
- 239000007864 aqueous solution Substances 0.000 claims abstract description 36
- 239000008367 deionised water Substances 0.000 claims abstract description 29
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 29
- 239000000725 suspension Substances 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 22
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 20
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 20
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 150000003751 zinc Chemical class 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims abstract 3
- 239000011941 photocatalyst Substances 0.000 claims description 56
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 21
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 16
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 14
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical group [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- 239000011592 zinc chloride Substances 0.000 claims description 8
- 235000005074 zinc chloride Nutrition 0.000 claims description 8
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000004246 zinc acetate Substances 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 238000000034 method Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 6
- 229910000608 Fe(NO3)3.9H2O Inorganic materials 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 238000007146 photocatalysis Methods 0.000 description 9
- 229910052799 carbon Inorganic materials 0.000 description 7
- 239000007900 aqueous suspension Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000011701 zinc Substances 0.000 description 6
- 238000005215 recombination Methods 0.000 description 5
- 230000006798 recombination Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 241000143437 Aciculosporium take Species 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000005352 clarification Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910000161 silver phosphate Inorganic materials 0.000 description 4
- 239000011029 spinel Substances 0.000 description 4
- 229910052596 spinel Inorganic materials 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 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 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- -1 zinc ferrite compound Chemical class 0.000 description 2
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- CQPFMGBJSMSXLP-UHFFFAOYSA-M acid orange 7 Chemical compound [Na+].OC1=CC=C2C=CC=CC2=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 CQPFMGBJSMSXLP-UHFFFAOYSA-M 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229940106691 bisphenol a Drugs 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- RLBIQVVOMOPOHC-UHFFFAOYSA-N parathion-methyl Chemical group COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C=C1 RLBIQVVOMOPOHC-UHFFFAOYSA-N 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/06—Polluted air
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)
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Abstract
Provided is a preparation method of carbon quantum dot/zinc ferrite composite photocatalytic materials. Ascorbic acid is added into a mixed solution of ethylene glycol and deionized water and evenly stirred, reaction is performed for 1-5 h at the temperature of 100-200 DEG C, and a carbon quantum dot aqueous solution is obtained; zinc salt and Fe(NO3)3.9H2O are added into water, a pH value is adjusted to be 8-14 after dissolution, and suspension liquid is obtained; the carbon quantum dot aqueous solution is added into the suspension liquid, standing is performed after uniform stirring, hydrothermal reaction is performed for 4-10 h at the temperature of 80-180 DEG C, washing and drying are performed, and the carbon quantum dot/zinc ferrite composite photocatalytic materials are obtained. The raw materials are low in price, easy to obtain, the photocatalytic materials are low in synthesis cost, the method is easy to implement, and carbon quantum dot/zinc ferrite has higher degradation efficiency on NOx compared with pure zinc ferrite within the range of visible light.
Description
Technical field
Photocatalysis technology of the present invention field, is specifically related to a kind of carbon quantum dot/zinc ferrite composite photocatalyst materialPreparation method.
Background technology
Nitrogen oxide (NOx) as common air pollutants, comprise NO and NO2, be produce greenhouse effects,Acid rain, ozone cavity, photochemical fog and PM2.5One of major pollutants, very harmful to environment,Also can work the mischief to human health directly or indirectly. Industrial main use gas denitrifying technology at present, fromAnd reach NOxCan discharge standard. But NOxConcentration is relatively low in air, cannot have by traditional methodEffect is removed. The nitrogen oxide accumulating in long-term air in the past can have influence on the air quality of human habitat, because ofThis is in the urgent need to effectively processing this pollutant. Research is found: photocatalytic redox reaction is at degradation of contaminantIn application, there is feature rapidly and efficiently, and equipment needed thereby is simple, good product selectivity, reaction condition gentlenessDeng, therefore this technology has broad application prospects at environmental pollution controlling party mask.
The ZnFe of spinel structure2O4The narrower semiconductor of a kind of band gap (～2.0eV), in solar spectrumVisible ray have response, raw material storage is abundant, cheap, nontoxic, and environmentally friendly. But its photoproductionThe recombination rate in electronics and hole is too fast, thereby has reduced its photocatalytic activity, therefore needs to find effectively a kind ofMethod reduces the recombination rate in its light induced electron and hole. Patent CN103887081A use Hydrothermal Synthesis nitrogen mixAssorted Graphene/zinc ferrite nano composite material, zinc ferrite, on the surface of nitrogen-doped graphene, has stoped nitrogen dopingGraphene accumulation is between layers reunited, and has improved its electrochemical properties. Patent CN104437573A adoptsIon exchange technique has been prepared ZnFe2O4/Ag3PO4Composite photo-catalyst, realizes light by building hetero-junctions systemThe high efficiente callback of catalyst, and ZnFe2O4/Ag3PO4Composite photo-catalyst is to antibiotic degraded effect in waste waterFruit is better than pure zinc ferrite and silver orthophosphate; Patent CN104437574A, taking carbosphere (CMSs) as core, adopts moltenThe hot method of agent and in situ Precipitation are by zinc ferrite (ZnFe2O4), silver orthophosphate (Ag3PO4) load on successively carbosphere tableFace, makes and has anti-light corrosive two-layer core shell structure composite catalyst MSsZnFe2O4Ag3PO4；The zinc ferrite load carbon nano-tube catalyst that patent CN104383930A adopts microwave-hydrothermal method to prepare, this catalysisFive kinds of organic pollutions in agent and microwave combined degradation water (neopelex, Acid Orange II, methyl orange,Parathion-methyl and bisphenol-A) speed, degradation efficiency high, do not have intermediate product generate, can not causeSecondary pollution; Patent CN104941671A has synthesized zinc ferrite/bismuth oxyiodide composite visible light by the precipitation method and has urgedAgent, under natural daylight to the degradation rate of methyl orange dye waste water up to 90%.
Carbon quantum dot (CarbonQuantumDots, CQDs) is a kind of novel carbon nanomaterial, sizeBelow 10nm, there is good water-soluble, hypotoxicity, be easy to the superiority such as functionalization and anti-light stabilityEnergy. In addition, the wavelength of photoluminescence excitation has further improved its photocatalysis performance. Therefore, carbon quantumPoint (CQDs) has tempting prospect aspect photocatalysis technology. Patent CN103480353A is with vitamin CFor carbon source, water and ethanol make mixed solvent, by hydrothermal synthesis of carbon quantum dot, by titanium dioxide powder and carbonQuantum dot solution mixing makes composite photo-catalyst, and this composite is higher to the degradation rate of methylene blue; PatentThe synthetic multi-functional mesoporous silicon/carbon dioxide amount with order mesoporous structure and fluorescence property of CN104877677ASon point nano composite material; Methyl in the degradation waste water that contains carbon quantum dot by preparation in prior artOrange, methylene blue etc., but can not degrade nitrogen oxide.
Research shows: carbon quantum dot (CQDs) can be used as electron storage device, accepts semiconductor catalystLight induced electron, thus semiconductor (SiO reduced2、TiO2、ZnO、Fe2O3、Cu2O、Ag3PO4Deng)The recombination rate in light induced electron and hole. Carbon quantum dot has up conversion property simultaneously, can absorb sunshine medium wavelengthLonger part, launches shortwave (325-425nm), and then excites the semiconductor light that energy gap is larger to urgeAgent forms electron hole pair, and electron hole pair can react to produce with the Oxidizing and Reducing Agents of absorption again and liveProperty oxygen radical, thereby degradation of contaminant.
Summary of the invention
The object of this invention is to provide a kind of preparation method of carbon quantum dot/zinc ferrite composite photocatalyst material, shouldComposite photocatalyst material prepared by method can be to NO in visible-rangexPhotocatalytic degradation, and synthetic sideMethod is simple, raw material is cheap is easy to get.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for carbon quantum dot/zinc ferrite composite photocatalyst material, comprises the following steps:
A. ascorbic acid is joined in the mixed solution of ethylene glycol and deionized water, after stirringAt 100-200 DEG C, react 1-5h, obtain the carbon quantum dot aqueous solution; Wherein, ascorbic acid, ethylene glycol, go fromThe ratio of sub-water is (0.5-5.0) g:(5.0-30) mL:(10-50) mL;
B. by zinc salt and Fe (NO3)3·9H2O is added to the water, and after dissolving, regulating pH value is 8-14, is suspendedLiquid; Wherein, zinc salt and Fe (NO3)3·9H2The mol ratio of O is 1:(0.1-5.0), Fe (NO3)3·9H2O and waterRatio be (1.0-5.0) g:(10-50) mL;
C. the carbon quantum dot aqueous solution is joined in suspension, after stirring, leave standstill, then at 80-180 DEG CHydro-thermal reaction 4-10h, then washs, dries, and obtains carbon quantum dot/zinc ferrite composite photocatalyst material; Wherein,The volume ratio of the carbon quantum dot aqueous solution and suspension is (0.1-25) mL:(10-50) mL.
In described step b, zinc salt is zinc nitrate, zinc chloride or zinc acetate.
In described step b, adopt sodium hydroxide solution or ammonia spirit to regulate pH value.
The concentration of described sodium hydroxide solution, ammoniacal liquor is 2mol/L.
In described step c, the standing time is 1 day.
In described step c, washing is specially: adopt respectively deionized water and ethanol washing.
The temperature of drying in described step c is 50-100 DEG C.
Compared with prior art, the beneficial effect that the present invention has:
The present invention adopts the low cost raw materials such as ascorbic acid, zinc nitrate, ferric nitrate, NaOH by simple waterHot method is synthesized carbon quantum dot/zinc ferrite composite photo-catalyst, and the raw material of this composite photo-catalyst is cheap to be easy to get, to closeBecome cost lower, method is simple, carbon quantum dot/zinc ferrite compared to pure zinc ferrite at visible-rangeInterior to NOxThere is higher degradation efficiency. The knot of carbon quantum dot/zinc ferrite composite photo-catalyst prepared by the present inventionStructure is identical with pure zinc ferrite, is all spinel structure; Ferrous acid in carbon quantum dot/zinc ferrite composite photo-catalystZinc is that average particle size is the spherical nanoparticle of 10nm, and carbon quantum dot is distributed in the surface of zinc ferrite; WhenWhen the consumption of the carbon quantum dot aqueous solution is 3mL, carbon quantum dot/zinc ferrite composite photo-catalyst reaches NO clearanceTo the highest, visible ray illumination 30min, NO clearance can reach 38%, compares pure zinc ferrite (NO clearanceBe only 29%) improve 9%. NO in the whole process of visible ray illumination 30min2Growing amount there is negative value,Carbon quantum dot/zinc ferrite composite photo-catalyst part NO that can also degrade is described2. When catalyst circulation is used six timesTime, there is not the phenomenon reducing in the clearance of NO, illustrates that the stability of composite photo-catalyst is higher, energy is manyInferior recycling. Due to the energy gap of zinc ferrite narrower (～2.0eV), under visible ray, can produce photoproduction skyCave duplet, but its recombination rate is high, therefore photocatalysis performance is lower, when carbon quantum dot and zinc ferrite compound after,The light induced electron of zinc ferrite is transferred to carbon quantum dot, reduces the light induced electron of zinc ferrite and the recombination rate in hole, entersAnd improved the photocatalysis performance of zinc ferrite, and therefore, compare pure zinc ferrite, carbon quantum dot/zinc ferrite is compoundPhotochemical catalyst is to NOxDegradation rate increase.
The present invention is by compound its utilization rate to solar energy that not only improved of carbon quantum dot and zinc ferrite, andImproved the photocatalysis stability of zinc ferrite, this research has far reaching significance to photocatalysis technology practical.
Brief description of the drawings
Fig. 1 is pure zinc ferrite and the XRD spectra of carbon quantum dot/zinc ferrite composite photo-catalyst;
Fig. 2 is pure zinc ferrite and the clearance of carbon quantum dot/zinc ferrite composite photo-catalyst NO under visible rayTime diagram;
Fig. 3 is pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst NO under visible ray2Growing amountTime diagram;
Fig. 4 is CQDs/ZnFe2O4The TEM figure of-2 composite photo-catalysts;
Fig. 5 is CQDs/ZnFe2O4What-2 composite photo-catalysts were degraded NO under visible ray recycles performance figure.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is done to concrete introduction.
Embodiment 1
A. take 1.6g ascorbic acid, join the mixed solution of 15mL ethylene glycol and 25mL deionized waterIn, stirring at room temperature 30min then reacts 70min at 160 DEG C, obtains the carbon quantum dot aqueous solution;
B. weigh respectively the Zn (NO of 1.189g3)2·6H2Fe (the NO of O and 3.232g3)3·9H2O, then addsEnter 20mL deionized water, under room temperature, be stirred to solution clarification;
C. the pH value of using the NaOH solution regulating step b gained solution of 2mol/L, makes pH value reach 13.0,Obtain suspension;
D. in above-mentioned steps c gained suspension, add the 1mL step a gained carbon quantum dot aqueous solution;
E. after stirring, leave standstill 1 day, then transfer in the polytetrafluoroethylliner liner of 100mL 100 DEG CLower hydro-thermal reaction 6h, then wash repeatedly with deionized water and ethanol respectively, 70 DEG C of oven dry, obtain carbon quantum dot/Zinc ferrite composite photocatalyst material.
Embodiment 2
A. take 1.6g ascorbic acid, join the mixed solution of 15mL ethylene glycol and 25mL deionized waterIn, stirring at room temperature 30min then reacts 70min at 160 DEG C, obtains the carbon quantum dot aqueous solution;
B. weigh respectively the Zn (NO of 1.189g3)2·6H2Fe (the NO of O and 3.232g3)3·9H2O, then addsEnter 20mL deionized water, under room temperature, be stirred to solution clarification;
C. the pH value of using the NaOH solution regulating step b gained solution of 2mol/L, makes pH value reach 13.0,Obtain suspension;
D. in above-mentioned steps c gained suspension, add the 3mL step a gained carbon quantum dot aqueous solution;
E. stir a period of time mix rear leave standstill 1 day, then transfer in the polytetrafluoroethylene (PTFE) of 100mLIn courage, hydro-thermal reaction 6h at 100 DEG C, then wash repeatedly with deionized water and ethanol respectively, 70 DEG C of oven dry,Obtain carbon quantum dot/zinc ferrite composite photocatalyst material.
Embodiment 3
A. take 1.6g ascorbic acid, join the mixed solution of 15mL ethylene glycol and 25mL deionized waterIn, stirring at room temperature 30min then reacts 70min at 160 DEG C, obtains the carbon quantum dot aqueous solution;
B. weigh respectively the Zn (NO of 1.189g3)2·6H2Fe (the NO of O and 3.232g3)3·9H2O, then addsEnter 20mL deionized water, under room temperature, be stirred to solution clarification;
C. the pH value of using the NaOH solution regulating step b gained solution of 2mol/L, makes pH value reach 13.0,Obtain suspension;
D. in above-mentioned steps c gained suspension, add the 5mL step a gained carbon quantum dot aqueous solution;
E. stirring a period of time makes to mix and leaves standstill 1 day afterwards, then transfers to the polytetrafluoroethyl-ne of 100mLIn alkene inner bag, hydro-thermal reaction 6h at 100 DEG C, then wash repeatedly respectively 70 DEG C of bakings with deionized water and ethanolDry, obtain carbon quantum dot/zinc ferrite composite photocatalyst material.
Embodiment 4
A. take 1.6g ascorbic acid, join the mixed solution of 15mL ethylene glycol and 25mL deionized waterIn, stirring at room temperature 30min then reacts 70min at 160 DEG C, obtains the carbon quantum dot aqueous solution;
B. weigh respectively the Zn (NO of 1.189g3)2·6H2Fe (the NO of O and 3.232g3)3·9H2O, then addsEnter 20mL deionized water, under room temperature, be stirred to solution clarification;
C. the pH value of using the NaOH solution regulating step b gained solution of 2mol/L, makes pH value reach 13.0,Obtain suspension;
D. in above-mentioned steps c gained suspension, add the 10mL step a gained carbon quantum dot aqueous solution;
E. stirring a period of time makes to mix and leaves standstill 1 day afterwards, then transfers to the polytetrafluoroethyl-ne of 100mLIn alkene inner bag, react 6h at 100 DEG C, wash repeatedly respectively with deionized water and ethanol, 70 DEG C of oven dry, mustTo carbon quantum dot/zinc ferrite composite photocatalyst material.
Pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst are carried out respectively to XRD test, resolution chartSpectrum as shown in Figure 1.
As can be seen from Figure 1: carbon quantum dot that embodiment 1, embodiment 2, embodiment 3, embodiment 4 obtain/Zinc ferrite composite photo-catalyst (is CQDs/ZnFe2O4-1、CQDs/ZnFe2O4-2、CQDs/ZnFe2O4-3And CQDs/ZnFe2O4-4) all diffraction maximums are all coincide with database JCPDS card No.22-1012 diffraction maximum,Belong to spinel structure, showing does not affect ZnFe in the existence of carbon quantum dot2O4Structure, due to carbon quantumIn point/zinc ferrite composite photo-catalyst, the content of carbon quantum dot is lower, therefore in XRD spectra, there is no its featurePeak;
Pure zinc ferrite and carbon quantum dot/zinc ferrite composite photo-catalyst are carried out respectively to visible light photocatalysis activeTest:
In continuous flow reactor, carry out photocatalytic degradation test taking NO as target contaminant. With the xenon of 300WLamp is radiation source, filters the light of wavelength X < 400nm by optical filter. To comprise 0.1g catalyst finesThe culture dish of sample is placed in the continuous flow reactor with quartz glass window, passes into initial concentration to beThe NO of 400ppb. After steady air current, open xenon lamp test. By NO optical analyser (U.S.'s thermoelectricity,Model42c) the NO concentration in dynamic monitoring reactor. With the ratio of NO exit concentration and initial concentration andNO2Growing amount evaluate the catalytic performance of photochemical catalyst.
Fig. 2 is pure zinc ferrite and the clearance time diagram of carbon quantum dot/zinc ferrite composite photo-catalyst to NO.As seen from Figure 2, prepared carbon quantum dot/zinc ferrite composite photo-catalyst shows preferably and falls NOSeparate performance. In the time that the consumption of the carbon quantum dot aqueous solution is less than 3mL, along with the increasing of carbon quantum dot amount of aqueous solution usedAdd, NO clearance also increases gradually; While increasing gradually the consumption of the carbon quantum dot aqueous solution afterwards, NO removes againJust there is the trend reducing in rate; Therefore, in the time that the consumption of the carbon quantum dot aqueous solution is 3mL, carbon quantum dot/Zinc ferrite composite photo-catalyst reaches the highest to NO clearance, visible ray illumination 30min, and NO clearance can reach38%, compare pure zinc ferrite (NO clearance is only 29%) and improved 9%.
Fig. 3 is pure zinc ferrite and the process NO of carbon quantum dot/zinc ferrite composite photo-catalyst removal NO2LifeOne-tenth amount-time diagram. In the time that photochemical catalyst is carbon quantum dot/zinc ferrite composite photo-catalyst, NO2Growing amount phaseLower than pure zinc ferrite, NO in the whole process of visible ray illumination 30min2Growing amount there is negative value,Carbon quantum dot/zinc ferrite composite photo-catalyst part NO that can also degrade is described2。
To CQDs/ZnFe2O4-2 carry out TEM test, and test collection of illustrative plates as shown in Figure 3.
As can be seen from Figure 4, the CQDs/ZnFe that embodiment 2 obtains2O4The TEM spectrum of-2 composite photo-catalystsThe lattice fringe of 0.25nm and 0.29nm corresponding ZnFe respectively in figure2O4(311) and (200) crystal face, 0.32(002) crystal face of the corresponding carbon quantum dot of lattice fringe of nm, zinc ferrite is spheric granules, average ion sizeFor 10nm, and carbon quantum dot is distributed in the surface of zinc ferrite.
Fig. 5 is CQDs/ZnFe2O4What-2 composite photo-catalysts were degraded NO under visible ray recycles performance figure.CQDs/ZnFe2O4-2 have higher degradation efficiency to NO under visible ray, when catalyst circulation is used six timesTime, there is not the phenomenon reducing in the clearance of NO, CQDs/ZnFe is described2O4-2 composite photo-catalysts steadyQualitative higher, can repeatedly recycle.
As can be seen here, the present invention can make the carbon having compared with high visible light catalytic activity by simple hydro-thermal methodQuantum dot/zinc ferrite composite photo-catalyst, not only preparation process is simple to operation, and the cheap nothing that is easy to get of raw materialPoison.
Because the carbon quantum dot in carbon quantum dot/zinc ferrite composite photo-catalyst can storage compartment electronics, favourableLight induced electron and the effective of photohole in zinc ferrite separate, and can also absorb long wavelength's light and then inspireShort wavelength's light, makes carbon quantum dot/zinc ferrite composite photo-catalyst have better photocatalysis than pure zinc ferritePerformance.
Embodiment 5
A. ascorbic acid is joined in the mixed solution of ethylene glycol and deionized water, after stirring at 100 DEG CLower reaction 5h, obtains the carbon quantum dot aqueous solution; Wherein, the ratio of ascorbic acid, ethylene glycol, deionized water is0.5g：30mL：20mL；
B. by zinc chloride and Fe (NO3)3·9H2O is added to the water, and adopts the sodium hydroxide solution of 2mol/L after dissolvingRegulating pH value is 8, obtains suspension; Wherein, zinc chloride and Fe (NO3)3·9H2The mol ratio of O is 1:0.5,Fe(NO3)3·9H2O is 1.0g:30mL with the ratio of water;
C. the carbon quantum dot aqueous solution is joined in suspension, after stirring, leave standstill 1d, then at 80 DEG CHydro-thermal reaction 10h, then adopts respectively the washing of deionized water and ethanol, 50 DEG C of oven dry, obtain carbon quantum dot/Zinc ferrite composite photocatalyst material; Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 0.1mL:30mL。
Embodiment 6
A. ascorbic acid is joined in the mixed solution of ethylene glycol and deionized water, after stirring at 200 DEG CLower reaction 1h, obtains the carbon quantum dot aqueous solution; Wherein, the ratio of ascorbic acid, ethylene glycol, deionized water is2g：5mL：10mL；
B. by zinc acetate and Fe (NO3)3·9H2O is added to the water, and adopts the sodium hydroxide solution of 2mol/L after dissolvingRegulating pH value is 9, obtains suspension; Wherein, zinc acetate and Fe (NO3)3·9H2The mol ratio of O is 1:5, Fe(NO3)3·9H2O is 3.0g:50mL with the ratio of water;
C. the carbon quantum dot aqueous solution is joined in suspension, after stirring, leave standstill 1d, then at 180 DEG CHydro-thermal reaction 4h, then adopts respectively the washing of deionized water and ethanol, 60 DEG C of oven dry, obtain carbon quantum dot/Zinc ferrite composite photocatalyst material; Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 5mL:50mL。
Embodiment 7
A. ascorbic acid is joined in the mixed solution of ethylene glycol and deionized water, after stirring at 120 DEG CLower reaction 3h, obtains the carbon quantum dot aqueous solution; Wherein, the ratio of ascorbic acid, ethylene glycol, deionized water is5g：20mL：36mL；
B. by zinc nitrate and Fe (NO3)3·9H2O is added to the water, and adopts the sodium hydroxide solution of 2mol/L after dissolvingRegulating pH value is 11, obtains suspension; Wherein, zinc nitrate and Fe (NO3)3·9H2The mol ratio of O is 1:1.5,Fe(NO3)3·9H2O is 2.0g:10mL with the ratio of water;
C. the carbon quantum dot aqueous solution is joined in suspension, after stirring, leave standstill 1d, then at 120 DEG CHydro-thermal reaction 8h, then adopts respectively the washing of deionized water and ethanol, 70 DEG C of oven dry, obtain carbon quantum dot/Zinc ferrite composite photocatalyst material; Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 25mL:10mL。
Embodiment 8
A. ascorbic acid is joined in the mixed solution of ethylene glycol and deionized water, after stirring at 180 DEG CLower reaction 2h, obtains the carbon quantum dot aqueous solution; Wherein, the ratio of ascorbic acid, ethylene glycol, deionized water is3g：10mL：50mL；
B. by zinc chloride and Fe (NO3)3·9H2O is added to the water, and adopts the sodium hydroxide solution of 2mol/L after dissolvingRegulating pH value is 14, obtains suspension; Wherein, zinc chloride and Fe (NO3)3·9H2The mol ratio of O is 1:3.5, Fe(NO3)3·9H2O is 5.0g:20mL with the ratio of water;
C. the carbon quantum dot aqueous solution is joined in suspension, after stirring, leave standstill 2d, then at 150 DEG CHydro-thermal reaction 7h, then adopts respectively the washing of deionized water and ethanol, 100 DEG C of oven dry, obtain carbon quantum dot/Zinc ferrite composite photocatalyst material; Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 0.8mL:20mL。
Embodiment 9
A. ascorbic acid is joined in the mixed solution of ethylene glycol and deionized water, after stirring at 110 DEG CLower reaction 4h, obtains the carbon quantum dot aqueous solution; Wherein, the ratio of ascorbic acid, ethylene glycol, deionized water is4g：25mL：40mL；
B. by zinc chloride and Fe (NO3)3·9H2O is added to the water, and adopts the ammoniacal liquor of 2mol/L to regulate pH after dissolvingValue is 12, obtains suspension; Wherein, zinc chloride and Fe (NO3)3·9H2The mol ratio of O is 1:0.8,Fe(NO3)3·9H2O is 4.0g:45mL with the ratio of water;
C. the carbon quantum dot aqueous solution is joined in suspension, after stirring, leave standstill 2d, then at 160 DEG CHydro-thermal reaction 6h, then adopts respectively the washing of deionized water and ethanol, 90 DEG C of oven dry, obtain carbon quantum dot/Zinc ferrite composite photocatalyst material; Wherein, the volume ratio of the carbon quantum dot aqueous solution and suspension is 15mL:45mL。
The invention discloses a kind of simple hydrothermal synthesis of carbon quantum dot/zinc ferrite (CQDs/ZnFe2O4) multipleClose photochemical catalyst, carbon quantum dot/zinc ferrite composite photocatalyst material is applied to photocatalytic degradation nitrogen oxide(NOx). Study and find under the optimum amount of carbon quantum dot, carbon quantum dot/zinc ferrite composite photo-catalystStructure is identical with pure zinc ferrite, is all spinel structure; Iron in carbon quantum dot/zinc ferrite composite photo-catalystAcid zinc is that average particle size is the spherical nanoparticle of 10nm, and carbon quantum dot is distributed in the surface of zinc ferrite;And carbon quantum dot/zinc ferrite composite photo-catalyst in visible-range to NOxClearance up to 38%,Than pure zinc ferrite height 9%, and the larger intermediate product NO of toxicity2Growing amount lower, therefore carbon amountSub-point/zinc ferrite composite photo-catalyst is to NOxThere is higher clearance; When carbon quantum dot/zinc ferrite complex lightWhen catalyst circulation is used six times, to NOxPhotocatalytic activity do not change, carbon quantum dot is described/ zinc ferrite composite photo-catalyst is photochemical catalyst efficient, environmental protection, and preparation method is simple, and raw material is cheapBe easy to get, there is application prospect more widely.
It should be noted that, above-described embodiment does not limit the present invention in any form, all employings be equal to replace or etc.The technical scheme that the mode of effect conversion obtains, all drops in protection scope of the present invention.
Claims (7)
1. a preparation method for carbon quantum dot/zinc ferrite composite photocatalyst material, is characterized in that, comprises the following steps:
A. ascorbic acid is joined in the mixed solution of ethylene glycol and deionized water, after stirring, at 100-200 DEG C, react 1-5H, obtains the carbon quantum dot aqueous solution; Wherein, the ratio of ascorbic acid, ethylene glycol, deionized water is (0.5-5.0) g:(5.0-30)mL：(10-50)mL；
B. by zinc salt and Fe (NO3)3·9H2O is added to the water, and after dissolving, regulating pH value is 8-14, obtains suspension; Wherein, zincSalt and Fe (NO3)3·9H2The mol ratio of O is 1:(0.1-5.0), Fe (NO3)3·9H2O is (1.0-5.0) g:(10-50 with the ratio of water)mL；
C. the carbon quantum dot aqueous solution is joined in suspension, after stirring, leave standstill then hydro-thermal reaction 4-10 at 80-180 DEG CH, then washs, dries, and obtains carbon quantum dot/zinc ferrite composite photocatalyst material; Wherein, the carbon quantum dot aqueous solution and suspensionThe volume ratio of liquid is (0.1-25) mL:(10-50) mL.
2. the preparation method of a kind of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, is characterized in that,In described step b, zinc salt is zinc nitrate, zinc chloride or zinc acetate.
3. the preparation method of a kind of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, is characterized in that,In described step b, adopt sodium hydroxide solution or ammonia spirit to regulate pH value.
4. the preparation method of a kind of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 3, is characterized in that,The concentration of described sodium hydroxide solution, ammoniacal liquor is 2mol/L.
5. the preparation method of a kind of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, is characterized in that,In described step c, the standing time is 1 day.
6. the preparation method of a kind of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, is characterized in that,In described step c, washing is specially: adopt respectively deionized water and ethanol washing.
7. the preparation method of a kind of carbon quantum dot/zinc ferrite composite photocatalyst material according to claim 1, is characterized in that,The temperature of drying in described step c is 50-100 DEG C.
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