CN108837828A - An a kind of step Radiation Synthesis Method of nano metal simple substance/TiO2- hydrogel base optic catalytic material - Google Patents
An a kind of step Radiation Synthesis Method of nano metal simple substance/TiO2- hydrogel base optic catalytic material Download PDFInfo
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- CN108837828A CN108837828A CN201810764581.4A CN201810764581A CN108837828A CN 108837828 A CN108837828 A CN 108837828A CN 201810764581 A CN201810764581 A CN 201810764581A CN 108837828 A CN108837828 A CN 108837828A
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 46
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 32
- 239000002184 metal Substances 0.000 title claims abstract description 32
- 239000000126 substance Substances 0.000 title claims abstract description 31
- 230000005855 radiation Effects 0.000 title claims abstract description 27
- 238000001308 synthesis method Methods 0.000 title claims abstract description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000006185 dispersion Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 7
- 150000001455 metallic ions Chemical class 0.000 claims abstract description 7
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 12
- 238000010521 absorption reaction Methods 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- 150000004676 glycans Chemical class 0.000 claims description 5
- 239000003002 pH adjusting agent Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229920001282 polysaccharide Polymers 0.000 claims description 5
- 239000005017 polysaccharide Substances 0.000 claims description 5
- 239000002516 radical scavenger Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 235000010413 sodium alginate Nutrition 0.000 claims description 4
- 229920001661 Chitosan Polymers 0.000 claims description 3
- 102000008186 Collagen Human genes 0.000 claims description 3
- 108010035532 Collagen Proteins 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 229920001436 collagen Polymers 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 claims description 3
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- -1 septichen Chemical compound 0.000 claims description 3
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 2
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims description 2
- 229940123457 Free radical scavenger Drugs 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
- 235000011037 adipic acid Nutrition 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 235000010980 cellulose Nutrition 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000002534 radiation-sensitizing agent Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000000661 sodium alginate Substances 0.000 claims description 2
- 229940005550 sodium alginate Drugs 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 229910000031 sodium sesquicarbonate Inorganic materials 0.000 claims description 2
- 235000018341 sodium sesquicarbonate Nutrition 0.000 claims description 2
- WCTAGTRAWPDFQO-UHFFFAOYSA-K trisodium;hydrogen carbonate;carbonate Chemical compound [Na+].[Na+].[Na+].OC([O-])=O.[O-]C([O-])=O WCTAGTRAWPDFQO-UHFFFAOYSA-K 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 17
- 238000006555 catalytic reaction Methods 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000007146 photocatalysis Methods 0.000 abstract description 8
- 238000006722 reduction reaction Methods 0.000 abstract description 7
- 239000003638 chemical reducing agent Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 5
- 238000012986 modification Methods 0.000 abstract description 5
- 229910021645 metal ion Inorganic materials 0.000 abstract description 4
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- 230000009102 absorption Effects 0.000 description 11
- 239000000047 product Substances 0.000 description 10
- 239000000499 gel Substances 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000004698 Polyethylene Substances 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000011065 in-situ storage Methods 0.000 description 8
- 238000004132 cross linking Methods 0.000 description 7
- 235000013339 cereals Nutrition 0.000 description 6
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- 238000010894 electron beam technology Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 229910052738 indium Inorganic materials 0.000 description 4
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- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000010257 thawing Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000001828 Gelatine Substances 0.000 description 3
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000013067 intermediate product Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
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- 239000003431 cross linking reagent Substances 0.000 description 2
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- 230000009467 reduction Effects 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 231100000167 toxic agent Toxicity 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910004042 HAuCl4 Inorganic materials 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 229940107698 malachite green Drugs 0.000 description 1
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 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 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 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 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
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- 150000003254 radicals Chemical class 0.000 description 1
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- 238000005215 recombination Methods 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
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- 238000012546 transfer Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/50—Silver
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- 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
- B01J23/72—Copper
-
- 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
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/14—Decomposition by irradiation, e.g. photolysis, particle radiation or by mixed irradiation sources
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The present invention relates to environmental treatment and photosensitive antimicrobial technology field more particularly to a kind of nano metal simple substance/TiO2One step Radiation Synthesis Method of hydrogel base optic catalytic material.It includes the following steps：（1）It will include hydrogel material, nano-TiO2The mixed dispersion liquid operation that is first freezed, thawed again, the operation is repeated at least once more, and obtains precrosslink nano-TiO2Composite hydrogel；（2）By the precrosslink nano-TiO2Composite hydrogel and aqueous metallic ions carry out ionising radiation, obtain nano metal simple substance/TiO2Hydrogel base optic catalytic material.The present invention is with Metal Ions Modification TiO2And use hydrogel as TiO2Dispersible carrier to improve its photocatalysis performance, while overcoming the problems, such as that traditional technology prepares the influence hydrogel catalytic stability occurred during hydrogel catalysis material using chemical crosslink technique and chemical reduction method.
Description
Technical field
The present invention relates to environmental treatment and photosensitive antimicrobial technology field more particularly to a kind of nano metal simple substance/TiO2Water
One step Radiation Synthesis Method of gel base optic catalytic material.
Background technique
Nano-TiO2Conductor oxidate has aroused great concern in light-catalyzed reaction field.Work as TiO2Partly lead
After body absorbs energy greater than the luminous energy of forbidden bandwidth, valence-band electrons are excited to conduction band, generate one hole pair of electronics, and photoproduction is empty
Cave has strong oxidizing property, it can promote many chemical reactions to occur, such as photo-reduction, photocatalysis, light organic synthesis.However, receiving
Rice TiO2In the photocatalysis performance of visible region and bad, in order to adapt to more wide in range use condition and application range, to receiving
Rice TiO2Structurally-modified and surface modification receive more concerns and research.Nano-TiO at present2Research on Surface Modification master
There are the means such as containing transition metal ion, nonmetalloid and have stronger absorption to visible light using photosensitive reagents, light swashs
It can be by electronics transfer to TiO after hair2And achieve the purpose that visible light photocatalysis.Nano metal simple substance is a kind of stable nanocrystalline
Grain.Electronics in nano metal simple substance excitation state can be effectively injected TiO2In conduction band, electronics and hole-recombination are reduced
Chance improves the separating effect of charge, expands the range of its spectral response, enhances TiO2Photocatalysis efficiency.
Nano-TiO2Another limitation is that：Partial size is small, specific surface is big, surface energy is high, and nanoparticle is easy to reunite.It receives
Rice TiO2The compatibility of relatively low matrix is poor with surface energy, and the two cannot mix when being mutually mixed, and causes interface to occur empty
Gap, there are phenomenon of phase separation.In order to ensure nano-TiO2Particle is in the material with the presence of nanoscale size, it is necessary to by means of good
Good dispersible carrier improves photocatalysis performance, to reach the purpose applied.Hydrogel is three between liquid and solid
Porous network or interpenetrating porous network are tieed up, is a kind of hydrophilic polymeric that can significantly swell in water, but can not dissolve in water
Although object gel, hydrogel contain large quantity of moisture, certain shape can be but shown as solid, has been widely used for medicine
The material support of object, catalysis, biology, medicine etc..The nano metal simple substance of synchrotron radiation synthesis can be evenly distributed on load
Nano-TiO in gel gelatine2Surface, to nano-TiO2It is effectively modified and is not easily runed off, thus to nano metal list
Matter/TiO2Catalysis material plays the role of effective immobilized.
Traditional hydrogel catalysis material generallys use chemical crosslink technique and chemical reduction method.But the water-setting of method preparation
Glue not only easily discharges remaining hypertoxic crosslinking agent and reducing agent in water body, but also will appear uneven crosslinking, locally occurs " to burn
Burnt phenomenon ", and be chemically crosslinked and be difficult to control the degree of cross linking；Secondly the quantum dot of chemical reduction method preparation cannot be not only uniformly distributed
In gel gelatine system, and its active force between gel molecular it is too weak even without, allow it to be easily lost from gel hole,
To affect the catalytic stability of hydrogel, application of the hydrogel as multifunctional material is constrained.To overcome chemical crosslinking
Method and chemical reduction method bring are insufficient, nano metal simple substance/TiO2One step Radiation Synthesis Method of hydrogel base optic catalytic material
It comes into being.
Radiation method realizes effective supplement and perfect relative to chemical method, is embodied in：1. reaction process does not need
Any pair of toxic substance of human body is added, the degree of cross linking is high, hydrogel purity is high；It, at room temperature can be into 2. reaction condition is mild
Row, easy to operate, reaction time is short；3. can accurately regulate and control the mechanics of hydrogel by control polymers compositions and radiation parameter
Performance；4. the reduction process of hydrogel preparation, moulding and nano silver can synchronously complete；5. the nano silver for radiating preparation can uniformly divide
Cloth is in the nano-TiO being supported in gel gelatine2Surface, to nano-TiO2It is effectively modified and is not easily runed off.From comprehensive and
From the point of view of long-range, nano metal simple substance/TiO is prepared using irradiation technique2The economic cost that catalysis material is spent is lower.Cause
This, radiation synthetic technology has become intelligent aqueous gel and the preparation of associated catalytic material is rich in the Research approach of prospect.
Summary of the invention
The invention solves the above problems, provide a kind of nano metal simple substance/TiO2The one of hydrogel base optic catalytic material
Radiation Synthesis Method is walked, with Metal Ions Modification TiO2And use hydrogel as TiO2Dispersible carrier to improve its photocatalytic
Can, while traditional technology being overcome to prepare the shadow occurred during hydrogel catalysis material using chemical crosslink technique and chemical reduction method
The problem of Xiangshui County's gel catalytic stability.
The technical solution that the present invention solves the problems, such as is to provide a kind of nano metal simple substance/TiO2Hydrogel base optic catalytic material
One step Radiation Synthesis Method of material, includes the following steps：（1）It will include hydrogel material, nano-TiO2Mixed dispersion liquid carry out
The operation first freeze, thawed again, the operation are repeated at least once more, and obtain precrosslink nano-TiO2Composite hydrogel；（2）By institute
State precrosslink nano-TiO2Composite hydrogel and aqueous metallic ions carry out ionising radiation, obtain nano metal simple substance/TiO2-
Hydrogel base optic catalytic material.
Preferably, the raw material of the mixed dispersion liquid includes 0.1 ~ 5.0 part of nano-TiO according to mass parts2, 0.1 ~ 2.0 part
PH adjusting agent, 2 ~ 10 parts of hydrogel materials.
Preferably, the raw material of the mixed dispersion liquid further includes 0.5 ~ 2.5 part of radiosensitizer according to mass parts.
Preferably, the aqueous metallic ions include 0.01 ~ 0.1 part of metal salt and 0.1 ~ 2.0 part of hydroxyl according to mass parts
Base free radical scavenger.
Preferably, the aqueous metallic ions also include polyethylene glycol, polyvinylpyrrolidone.Wherein, polyethylene glycol,
Polyvinylpyrrolidone is as dispersing agent, and dosage those skilled in the art can determine according to standard empirical.
Preferably, the step（1）,（2）Between further include that 4 ~ 10 h of dark absorption are carried out under vacuum environment.
Preferably, the beam energy of the ionising radiation is 1 ~ 5 MeV, and dose of radiation is 60 ~ 120 kGy, dosage rate
For 10 ~ 60 kGy/pass.
Preferably, the pH adjusting agent be disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium sesquicarbonate, adipic acid, acetic acid,
One or more of Tris-HCl, iminodiacetic acid, triethanolamine.The introducing of pH adjusting agent, adjustable macromolecule and
The isoelectric point and stable dispersibility for the mixed emulsion system that nano material is formed, it is ensured that macromolecule itself does not tangle, and is conducive to
The radiation reduction in situ of later period macromolecule crosslinking with radiation and nano metal ion react synchronize go on smoothly.
Preferably, the hydrogel material is natural polysaccharide, including chitosan and its derivative, cellulose and its derivative
One or more of one or more of object, sodium alginate.One or more of natural polysaccharides, can during irradiation
Self-crosslinking occurs or is crosslinked each other, improve hydrogel mechanical property and flexibility, and introduced on its strand it is special
Functional group also acts as concerted catalysis effect.
Preferably, the irradiation sensitizer is one of collagen, polyvinyl alcohol, n-isopropyl acrylamide or several
Kind.In irradiation process, irradiation sensitizer generates rapidly living radical first, so that causing natural polysaccharide generates activity certainly
By base, crosslinks rapidly each other and prepare composite hydrogel.The introducing for irradiating sensitizer, shortens cross-linking radiation institute
The time needed, improve production efficiency, it is ensured that composite hydrogel has the degree of cross linking appropriate.
Preferably, the scavenger is isopropanol, in the tert-butyl alcohol, septichen, terephthalic acid (TPA)
One or more.Scavenger can effectively remove the secondary hydroxyl radical free radical that generates in irradiation, and its
Its secondary activity particle is unaffected, improves the radiation reduction yield in situ of nano metal ion precursor solution.
Preferably, the metal is that Ag, Au, Cu, Co, Ni, Fe, Mo, Bi are one such or several.
Beneficial effects of the present invention：
1. carrying out ionising radiation in situ prepares nano metal simple substance/TiO2Hydrogel base optic catalytic material, it is advantageous to realize
The combination of performance so that the raising of mechanical property, photosensitive antibacterial, catalysis synergy.
2. by absorption, photocatalysis, antibiotic and sterilizing organic unity, obtain mechanical strength it is excellent, expansion and systole response
Fastly, it is easy to supported catalyst and the stable hydrogel " soft reactor " of performance.
3. synchronizing the nano metal simple substance that radioreaction in situ obtains can effectively modify positioned at the three-dimensional mutual of porous aquagel
Wear nano-TiO in network structure2, the separating effect of charge is improved, the range of spectral response has been expanded, has strengthened photocatalytic
Can, it also improves hydrogel mechanical property, has reached the application purpose of the two mutual supplement with each other's advantages.
4. hydrogel " soft reactor " can provide extremely beneficial synergistic reaction platform for antibacterial, catalysis, active
Absorption bacterium, organic pollutant simultaneously dissolve out degradation product, it is also possible to change catalytic route, so that the effect of catalyst is able to maximum
It plays.
5. use biodegradable natural polysaccharide for the substrate of hydrogel " soft reactor ", what itself slowly degraded
The catalyst recoverable retained simultaneously.
6. irradiation technique is nontoxic, reaction condition is mild, reaction process does not add crosslinking agent, initiator and any couple of people
The toxic substance of body, can effectively avoid secondary pollution.
7. the nano metal simple substance/TiO being prepared2Hydrogel base optic catalytic material, which can be widely popularized, to be applied to be directed to
The fields such as environmental wastewater processing, photocatalysis, antibiotic and sterilizing.
Specific embodiment
It is a specific embodiment of the invention below, technical scheme of the present invention will be further described, but the present invention
It is not limited to these examples.
Embodiment 1
According to mass parts, by 0.1 part of nano-TiO2, 0.1 part of triethanolamine be dissolved in deionized water, 0.5 h is stirred by ultrasonic, makes it
It is even to form stable dispersion.2 parts of carboxymethyl chitosans, 0.5 part of polyvinyl alcohol are dissolved in deionized water, stirring is made
Even Polymer Solution is slowly added among above-mentioned dispersion, after 0.5 h is stirred by ultrasonic in inflated with nitrogen, stands de-bubble under negative pressure,
After gained mixed dispersion liquid carries out 3 circulating frozen-defrostings, it is transferred in the PE hermetic bag of about 2 mm of thickness.By polyethylene glycol,
Polyvinylpyrrolidone, 0.1 part of isopropanol, 0.01 part of AgNO3It is dissolved in 100 mL deionized waters, ultrasonic disperse is uniform, by institute
It obtains Ag ion precursor solution to be slowly injected into above-mentioned PE hermetic bag, 4 h of dark absorption is carried out under vacuum environment.After taking out dark absorption
Intermediate products, be placed under electron beam and carry out radioreaction in situ, the beam energy selected is 1MeV, dose of radiation 60
KGy, dosage rate are 10 kGy/pass, and last resulting product is nanometer Ag/TiO2Hydrogel base optic catalytic material.By institute
Sample is obtained through washing, drying, crushing, sieving, classification to get nanometer Ag/TiO of variable grain degree2Hydrogel base optic catalytic material
Expect particle.
Basis weight products are taken to put into the methylene blue of 250 mL, 4 mg/L（Simulate organic pollutant）In, at room temperature, to mould
Quasi- object carries out photocatalytic degradation experiment, after reacting 2 h, measures degradation rate and reaches 98.6%.
Embodiment 2
According to mass parts, by 0.5 part of nano-TiO2, 0.5 part of disodium hydrogen phosphate be dissolved in deionized water, 0.5 h is stirred by ultrasonic, makes it
It is formed uniformly stable dispersion.5 parts of carboxymethyl celluloses, 1 part of collagen are dissolved in deionized water, stirring is made
Even Polymer Solution is slowly added among above-mentioned dispersion, and after 1 h is stirred by ultrasonic in inflated with nitrogen, de-bubble, institute are stood under negative pressure
After obtaining mixed dispersion 3 circulating frozen-defrostings of progress, sample is transferred in the PE hermetic bag of about 2 mm of thickness.It will gather
Ethylene glycol, polyvinylpyrrolidone, 0.5 part of septichen, 0.02 part of Cu (NO3)2It is dissolved in 100 mL deionized waters, surpasses
Sound is uniformly dispersed, and gained Cu ion precursor solution is slowly injected into above-mentioned PE hermetic bag, and dark absorption 5 is carried out under vacuum environment
h.Intermediate products after taking out dark absorption are placed under electron beam and carry out radioreaction in situ, and the beam energy selected is 1
MeV, dose of radiation are 80 kGy, and dosage rate is 20 kGy/pass, and last resulting product is nanometer Cu/TiO2Hydrogel
Base optic catalytic material.By gained sample through washing, drying, crushing, sieving, classification to get the nanometer Cu/ of variable grain degree
TiO2Hydrogel base optic catalytic material particle.
Basis weight products are taken to put into the methyl orange of 250 mL, 4 mg/L（Simulate organic pollutant）In, at room temperature, to simulation
Object carries out photocatalytic degradation experiment, after reacting 2 h, measures degradation rate and reaches 96.5%.
Embodiment 3
According to mass parts, by 2 parts of nano-TiOs2, 1 part of acetic acid be dissolved in deionized water, 2 h are stirred by ultrasonic, it is made to be formed uniformly stabilization
Dispersion.8 parts of sodium alginates, 2 parts of n-isopropyl acrylamide are dissolved in deionized water, uniform macromolecule is made in stirring
Solution is slowly added among above-mentioned dispersion, and after 2 h are stirred by ultrasonic in inflated with nitrogen, de-bubble, gained mixing point are stood under negative pressure
After granular media system carries out 3 circulating frozen-defrostings, sample is transferred in the PE hermetic bag of about 2 mm of thickness.By polyethylene glycol, gather
Vinylpyrrolidone, 1 part of tert-butyl alcohol, 0.06 part of HAuCl4It is dissolved in 100 mL deionized waters, ultrasonic disperse is uniform, by gained Au
Ion precursor solution is slowly injected into above-mentioned PE hermetic bag, and dark absorption 8h is carried out under vacuum environment.It takes out in after dark absorption
Between product, be placed under electron beam and carry out radioreaction in situ, the beam energy selected be 1MeV, and dose of radiation is 100 kGy,
Dosage rate is 50 kGy/pass, and last resulting product is nanometer Au/TiO2Hydrogel base optic catalytic material.By gained sample
Product are through washing, drying, crushing, sieving, classification to get the nanometer Au/TiO of variable grain degree2Hydrogel base optic catalytic material
Grain.
Basis weight products are taken to put into the rhodamine B of 250 mL, 4 mg/L（Simulate organic pollutant）In, at room temperature, to mould
Quasi- object carries out photocatalytic degradation experiment, after reacting 2 h, measures degradation rate and reaches 97.8%.
Embodiment 4
According to mass parts, by 5 parts of nano-TiOs2, 2 parts of iminodiacetic acids be dissolved in deionized water, 2 h are stirred by ultrasonic, make it uniformly
Form stable dispersion.10 parts of sodium alginates, 2.5 parts of polyvinyl alcohol are dissolved in deionized water, uniform height is made in stirring
Molecular solution is slowly added among above-mentioned dispersion, after 2 h are stirred by ultrasonic in inflated with nitrogen, de-bubble is stood under negative pressure, gained is mixed
After closing dispersion 3 circulating frozen-defrostings of progress, sample is transferred in the PE hermetic bag of about 2 mm of thickness.By poly- second two
Alcohol, polyvinylpyrrolidone, 2 parts of terephthalic acid (TPA)s, 0.1 part of CoCl2It being dissolved in 100 mL deionized waters, ultrasonic disperse is uniform,
Gained Co ion precursor solution is slowly injected into above-mentioned PE hermetic bag, dark absorption 10h is carried out under vacuum environment.Take out dark inhale
Attached intermediate products are placed under electron beam and carry out radioreaction in situ, and the beam energy selected is 1MeV, and dose of radiation is
120 kGy, dosage rate are 60 kGy/pass, and last resulting product is nano Co/TiO2Hydrogel base optic catalytic material.
By gained sample through washing, drying, crushing, sieving, classification to get nano Co/TiO of variable grain degree2Water-setting matrix light is urged
Change material granule.
Basis weight products are taken to put into the malachite green of 250 mL, 4 mg/L（Simulate organic pollutant）In, at room temperature, to mould
Quasi- object carries out photocatalytic degradation experiment, after reacting 2 h, measures degradation rate and reaches 98.7%.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (10)
1. a kind of nano metal simple substance/TiO2One step Radiation Synthesis Method of hydrogel base optic catalytic material, it is characterised in that：Including
Following steps：（1）It will include hydrogel material, nano-TiO2The mixed dispersion liquid operation that is first freezed, thawed again, it is described
Operation is repeated at least once more, and obtains precrosslink nano-TiO2Composite hydrogel；（2）By the precrosslink nano-TiO2Compound water congealing
Glue and aqueous metallic ions carry out ionising radiation, obtain nano metal simple substance/TiO2Hydrogel base optic catalytic material.
2. a kind of nano metal simple substance/TiO according to claim 12One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The raw material of the mixed dispersion liquid includes 0.1 ~ 5.0 part of nano-TiO according to mass parts2, 0.1 ~ 2.0 part
PH adjusting agent, 2 ~ 10 parts of hydrogel materials and 0.5 ~ 2.5 part of radiosensitizer.
3. a kind of nano metal simple substance/TiO according to claim 12One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The aqueous metallic ions include 0.01 ~ 0.1 part of metal salt and 0.1 ~ 2.0 part of hydroxyl according to mass parts
Base free radical scavenger；The aqueous metallic ions also include polyethylene glycol, polyvinylpyrrolidone.
4. a kind of nano metal simple substance/TiO according to claim 12One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The step（1）,（2）Between further include that 4 ~ 10 h of dark absorption are carried out under vacuum environment.
5. a kind of nano metal simple substance/TiO according to claim 12One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The beam energy of the ionising radiation is 1 ~ 5 MeV, and dose of radiation is 60 ~ 120 kGy, dosage rate
For 10 ~ 60 kGy/pass.
6. a kind of nano metal simple substance/TiO according to claim 22One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The pH adjusting agent be disodium hydrogen phosphate, sodium dihydrogen phosphate, sodium sesquicarbonate, adipic acid, acetic acid,
One or more of Tris-HCl, iminodiacetic acid, triethanolamine.
7. a kind of nano metal simple substance/TiO according to claim 12One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The hydrogel material is natural polysaccharide, including chitosan and its derivative, cellulose and its is spread out
One or more of one or more of biology, sodium alginate.
8. a kind of nano metal simple substance/TiO according to claim 22One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The irradiation sensitizer be one of collagen, polyvinyl alcohol, n-isopropyl acrylamide or
It is several.
9. a kind of nano metal simple substance/TiO according to claim 32One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The scavenger is isopropanol, in the tert-butyl alcohol, septichen, terephthalic acid (TPA)
One or more.
10. a kind of nano metal simple substance/TiO according to claim 12One step of hydrogel base optic catalytic material, which radiates, closes
Cheng Fa, it is characterised in that：The metal is that Ag, Au, Cu, Co, Ni, Fe, Mo, Bi are one such or several.
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