CN106268743A - A kind of preparation method of ultraviolet wideband Nano semiconductor heterojunction material - Google Patents
A kind of preparation method of ultraviolet wideband Nano semiconductor heterojunction material Download PDFInfo
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- CN106268743A CN106268743A CN201610672656.7A CN201610672656A CN106268743A CN 106268743 A CN106268743 A CN 106268743A CN 201610672656 A CN201610672656 A CN 201610672656A CN 106268743 A CN106268743 A CN 106268743A
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- 239000000463 material Substances 0.000 title claims abstract description 38
- 239000004065 semiconductor Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000008187 granular material Substances 0.000 claims description 23
- YDIYEOMDOWUDTJ-UHFFFAOYSA-N 4-(dimethylamino)benzoic acid Chemical compound CN(C)C1=CC=C(C(O)=O)C=C1 YDIYEOMDOWUDTJ-UHFFFAOYSA-N 0.000 claims description 18
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 18
- 239000004408 titanium dioxide Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910000611 Zinc aluminium Inorganic materials 0.000 claims description 12
- 230000032683 aging Effects 0.000 claims description 12
- 239000012670 alkaline solution Substances 0.000 claims description 12
- HXFVOUUOTHJFPX-UHFFFAOYSA-N alumane;zinc Chemical compound [AlH3].[Zn] HXFVOUUOTHJFPX-UHFFFAOYSA-N 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 12
- 230000004048 modification Effects 0.000 claims description 12
- 238000012986 modification Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 4
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Inorganic materials [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 abstract description 9
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 229910010413 TiO 2 Inorganic materials 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 2
- 238000006731 degradation reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 description 8
- 239000003504 photosensitizing agent Substances 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 238000004042 decolorization Methods 0.000 description 4
- 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 4
- 229940012189 methyl orange Drugs 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of zinc, cadmium or mercury
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B01J35/39—
-
- B01J35/40—
-
- 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
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- 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
- C02F2101/40—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 invention discloses the preparation method of a kind of ultraviolet wideband Nano semiconductor heterojunction material, belong to Nano semiconductor heterojunction material preparing technical field.For existing TiO2Semiconductor catalyst photocatalysis narrower width, it is impossible to utilize visible ray as light source, the problem that when using as light-sensitive material, the scope of application is less, it is provided that a kind of by by Zn(NO3)2With Al(NO3)3Preparation ultraviolet intercalated houghite, prepare ultraviolet wideband Nano semiconductor heterojunction material by modified intercalated houghite simultaneously, optically catalytic TiO 2 width is effectively made to improve,) Organic substance can be degraded by the present invention ultraviolet wideband Nano semiconductor heterojunction material prepared under visible light, and degradation time shortens 25～30%, and processing technology is simple, and raw material is easy to get, and is effectively saved preparation cost.
Description
Technical field
The invention discloses the preparation method of a kind of ultraviolet wideband Nano semiconductor heterojunction material, belong to Nano semiconductor
Heterojunction material preparing technical field.
Background technology
Hetero-junctions is made up of two kinds of different semi-conducting materials and has the structure being different from single semiconductor property.Receive
Rice heterojunction material is especially with the characteristic of heterojunction structure Yu nano material so that it is have more advantage, such as nanometer different
Matter structure is less demanding to the lattice match of two kinds of quasiconductors relative to heterojunction structure, therefore applies the most extensive.Nanometer is different
Matter structure is widely used in the fields such as solaode, sensor, photocatalysis hydrogen production, environmental conservation.Semiconductor heterostructure
Photocatalysis be based on different quasiconductors between the transfer between different quasiconductors of photoinduced electron and hole realize, at purple
Under conditions of outer visible ray, photosensitizer is excited with broadband semiconductor simultaneously, and the electronics in photosensitizer flows in broadband semiconductor,
The electron concentration on broadband semiconductor surface increases and reduction reaction can occur, and hole produced by broadband semiconductor is transferred to photosensitive
Agent surface, owing to the hole concentration on photosensitizer surface increases, can occur oxidation reaction on its surface.Under visible light conditions, by
Conduction band current potential in broadband semiconductor is corrected, and therefore, photoinduced electron is the conduction band being transferred to broadband semiconductor by photosensitizer, due to
Broadband semiconductor sheet electron concentration increase and reduction reaction can occur, and due to photosensitizer valence band than broadband semiconductor more
Negative, hole can not be transferred to broadband semiconductor by photosensitizer, and therefore oxidation reaction can only occur on photosensitizer, thus by photic
The reduction of electronics separates with the oxidation reaction in hole and carries out.
TiO2It is the most commonly used semiconductor light-catalyst, but owing to its quantum yield is than relatively low and can not utilize visible
The shortcomings such as light and make it apply and be greatly limited.Optically catalytic TiO 2 narrower width, it is impossible to utilize visible ray as light
Source, when using as light-sensitive material, the scope of application is narrower, so by TiO2Heterojunction structure is formed with other quasiconductors, hetero-junctions
Built in field can stop the compound of quantity of photogenerated charge, improves quantum efficiency, necessary.
Summary of the invention
The technical problem that present invention mainly solves: for existing TiO2Semiconductor catalyst photocatalysis narrower width, nothing
Method utilizes visible ray as light source, the problem that when using as light-sensitive material, the scope of application is less, it is provided that a kind of by by Zn
(NO3)2With Al(NO3)3Preparation ultraviolet intercalated houghite, prepares ultraviolet wideband nanometer by modified intercalated houghite simultaneously and partly leads
Bulk heterojunction material, effectively makes optically catalytic TiO 2 width improve, solves existing TiO2Semiconductor catalyst light is urged
Change narrower width, it is impossible to utilize visible ray as light source, the problem that when using as light-sensitive material, the scope of application is less.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) 1:5 in mass ratio, mixes p-(dimethylamino)-benzoic acid with the stirring of 1mol/L sodium hydroxide solution, the most quiet
Put 3～5h, be prepared into p-(dimethylamino)-benzoic acid alkaline solution, press Zn subsequently2+: Al3+Mol ratio 2:1, by Zn(NO3)2With Al
(NO3)3Stirring mixing, is prepared into mixed-powder, the most in mass ratio 1:10, is stirred with 1mol/L sodium hydroxide by mixed-powder
Mixing, the most still aging 3～5h, it is prepared into nano zinc aluminum mixed liquor；
(2) under nitrogen protection, 1:1 by volume, by nano zinc aluminum mixed liquor and the p-(dimethylamino)-benzoic acid of above-mentioned preparation
Alkaline solution stirring mixing is placed in there-necked flask, and water-bath 20～24h at 65～70 DEG C are filtered and collected filtering residue subsequently, use
After 85～90 DEG C of deionized water wash are to leacheate pH to 7.0, at 65～70 DEG C, it are dried 10～12h, are prepared into ultraviolet modified
Intercalated houghite material, standby；
(3) 1:10 in mass ratio, mixes perfluorooctanoic acid with dichloromethane stirring, and under 200～300W, sonic oscillation processes
15～20min, the most still aging 20～24h, it is prepared into organically-modified liquid, the most in mass ratio 1:5, by organic
Modification liquid mixes with titanium dioxide granule stirring, heating in water bath 2～3h at 45～50 DEG C, after heating in water bath completes, then
Rotary evaporated to dryness at 65～70 DEG C, collect be dried granule, be washed with deionized 3～5 times, at 65～70 DEG C be dried 6～
8h, is prepared into modifying titanium dioxide granule；
(4) 1:5 in mass ratio, ultraviolet modification intercalated houghite material step (2) prepared stirs with modifying titanium dioxide granule
Mix mixing to be placed in ball grinder, ball milling 3～5h at 450～500 DEG C, after ball milling completes, a kind of ultraviolet can be prepared into
Wideband Nano semiconductor heterojunction material.
The application process of the present invention is: choose the Methyl Orange in Wastewater solution of 0.008～0.010g/mL, with the sulfur of 1mol/L
Acid solution regulation pH to 3～4, at 50～70 DEG C, adds above-mentioned preparation ultraviolet wideband Nano semiconductor heterojunction material extremely
In waste water, dosage is 450～500g/T, and after adding after 150min, percent of decolourization is up to 85～90%.
The invention has the beneficial effects as follows:
(1) Organic substance can be degraded by the ultraviolet wideband Nano semiconductor heterojunction material that prepared by the present invention under visible light,
And degradation time shortens 25～30%；
(2) processing technology of the present invention is simple, and raw material is easy to get, and is effectively saved preparation cost.
Detailed description of the invention
1:5 the most in mass ratio, mixes p-(dimethylamino)-benzoic acid, in room temperature with the stirring of 1mol/L sodium hydroxide solution
Lower standing 3～5h, is prepared into p-(dimethylamino)-benzoic acid alkaline solution, presses Zn subsequently2+: Al3+Mol ratio 2:1, by Zn(NO3)2With
Al(NO3)3Stirring mixing, is prepared into mixed-powder, the most in mass ratio 1:10, is stirred with 1mol/L sodium hydroxide by mixed-powder
Mix mixing, the most still aging 3～5h, it is prepared into nano zinc aluminum mixed liquor；Under nitrogen protection, 1:1 by volume, will
The nano zinc aluminum mixed liquor of above-mentioned preparation stirs to mix with p-(dimethylamino)-benzoic acid alkaline solution and is placed in there-necked flask, 65
～water-bath 20～24h at 70 DEG C, filter subsequently and collect filtering residue, with 85～90 DEG C of deionized water wash to leacheate pH to 7.0
After, at 65～70 DEG C, it is dried 10～12h, is prepared into ultraviolet modification intercalated houghite material, standby；1:10 in mass ratio, will
Perfluorooctanoic acid mixes with dichloromethane stirring, sonic oscillation process 15～20min under 200～300W, the most at room temperature
Still aging 20～24h, it is prepared into organically-modified liquid, the most in mass ratio 1:5, organically-modified liquid is stirred with titanium dioxide granule
Mix mixing, heating in water bath 2～3h at 45～50 DEG C, after heating in water bath completes, then rotary evaporated to dryness at 65～70 DEG C,
Collect and be dried granule, be washed with deionized 3～5 times, at 65～70 DEG C, be dried 6～8h, be prepared into modifying titanium dioxide
Grain；1:5 in mass ratio, mixes ultraviolet modification intercalated houghite material with the stirring of modifying titanium dioxide granule and is placed in ball grinder
In, ball milling 3～5h at 450～500 DEG C, after ball milling completes, a kind of ultraviolet wideband Nano semiconductor can be prepared into heterogeneous
Knot material.
Example 1
1:5 the most in mass ratio, mixes p-(dimethylamino)-benzoic acid with the stirring of 1mol/L sodium hydroxide solution, the most quiet
Put 3h, be prepared into p-(dimethylamino)-benzoic acid alkaline solution, press Zn subsequently2+: Al3+Mol ratio 2:1, by Zn(NO3)2With Al(NO3)3
Stirring mixing, is prepared into mixed-powder, the most in mass ratio 1:10, is mixed with the stirring of 1mol/L sodium hydroxide by mixed-powder,
The most still aging 3h, is prepared into nano zinc aluminum mixed liquor；Under nitrogen protection, 1:1 by volume, by above-mentioned preparation
Nano zinc aluminum mixed liquor stirs to mix with p-(dimethylamino)-benzoic acid alkaline solution and is placed in there-necked flask, water-bath at 65 DEG C
20h, filters subsequently and collects filtering residue, with 85 DEG C of deionized water wash to leacheate pH to 7.0 after, at 65 DEG C be dried 10h, system
The standby ultraviolet modification intercalated houghite material that obtains, standby；1:10 in mass ratio, mixes perfluorooctanoic acid with dichloromethane stirring,
Under 200W, sonic oscillation processes 15min, the most still aging 20h, is prepared into organically-modified liquid, subsequently by quality
Ratio 1:5, mixes organically-modified liquid with titanium dioxide granule stirring, heating in water bath 2h at 45 DEG C, after heating in water bath completes,
Rotary evaporated to dryness at 65 DEG C again, collects and is dried granule, be washed with deionized 3 times, is dried 6h, is prepared into and changes at 65 DEG C
Property titanium dioxide granule；1:5 in mass ratio, mixes ultraviolet modification intercalated houghite material with the stirring of modifying titanium dioxide granule
It is placed in ball grinder, ball milling 3h at 450 DEG C, after ball milling completes, a kind of ultraviolet wideband Nano semiconductor can be prepared into
Heterojunction material.
Choose the Methyl Orange in Wastewater solution of 0.008g/mL, regulate pH to 3 with the sulfuric acid solution of 1mol/L, at 50 DEG C, will
Above-mentioned preparation ultraviolet wideband Nano semiconductor heterojunction material adds to waste water, and dosage is 450g/T, after adding
After 150min, percent of decolourization is up to 85%.
Example 2
1:5 the most in mass ratio, mixes p-(dimethylamino)-benzoic acid with the stirring of 1mol/L sodium hydroxide solution, the most quiet
Put 4h, be prepared into p-(dimethylamino)-benzoic acid alkaline solution, press Zn subsequently2+: Al3+Mol ratio 2:1, by Zn(NO3)2With Al(NO3)3
Stirring mixing, is prepared into mixed-powder, the most in mass ratio 1:10, is mixed with the stirring of 1mol/L sodium hydroxide by mixed-powder,
The most still aging 4h, is prepared into nano zinc aluminum mixed liquor；Under nitrogen protection, 1:1 by volume, by above-mentioned preparation
Nano zinc aluminum mixed liquor stirs to mix with p-(dimethylamino)-benzoic acid alkaline solution and is placed in there-necked flask, water-bath at 67 DEG C
22h, filters subsequently and collects filtering residue, with 87 DEG C of deionized water wash to leacheate pH to 7.0 after, at 67 DEG C be dried 11h, system
The standby ultraviolet modification intercalated houghite material that obtains, standby；1:10 in mass ratio, mixes perfluorooctanoic acid with dichloromethane stirring,
Under 250W, sonic oscillation processes 17min, the most still aging 22h, is prepared into organically-modified liquid, subsequently by quality
Ratio 1:5, mixes organically-modified liquid with titanium dioxide granule stirring, heating in water bath 3h at 47 DEG C, after heating in water bath completes,
Rotary evaporated to dryness at 67 DEG C again, collects and is dried granule, be washed with deionized 4 times, is dried 7h, is prepared into and changes at 67 DEG C
Property titanium dioxide granule；1:5 in mass ratio, mixes ultraviolet modification intercalated houghite material with the stirring of modifying titanium dioxide granule
It is placed in ball grinder, ball milling 4h at 475 DEG C, after ball milling completes, a kind of ultraviolet wideband Nano semiconductor can be prepared into
Heterojunction material.
Choose the Methyl Orange in Wastewater solution of 0.009g/mL, regulate pH to 4 with the sulfuric acid solution of 1mol/L, at 55 DEG C, will
Above-mentioned preparation ultraviolet wideband Nano semiconductor heterojunction material adds to waste water, and dosage is 475g/T, after adding
After 150min, percent of decolourization is up to 87%.
Example 3
1:5 the most in mass ratio, mixes p-(dimethylamino)-benzoic acid with the stirring of 1mol/L sodium hydroxide solution, the most quiet
Put 5h, be prepared into p-(dimethylamino)-benzoic acid alkaline solution, press Zn subsequently2+: Al3+Mol ratio 2:1, by Zn(NO3)2With Al(NO3)3
Stirring mixing, is prepared into mixed-powder, the most in mass ratio 1:10, is mixed with the stirring of 1mol/L sodium hydroxide by mixed-powder,
The most still aging 5h, is prepared into nano zinc aluminum mixed liquor；Under nitrogen protection, 1:1 by volume, by above-mentioned preparation
Nano zinc aluminum mixed liquor stirs to mix with p-(dimethylamino)-benzoic acid alkaline solution and is placed in there-necked flask, water-bath at 70 DEG C
24h, filters subsequently and collects filtering residue, with 85 DEG C of deionized water wash to leacheate pH to 7.0 after, at 70 DEG C be dried 12h, system
The standby ultraviolet modification intercalated houghite material that obtains, standby；1:10 in mass ratio, mixes perfluorooctanoic acid with dichloromethane stirring,
Under 300W, sonic oscillation processes 20min, the most still aging 24h, is prepared into organically-modified liquid, subsequently by quality
Ratio 1:5, mixes organically-modified liquid with titanium dioxide granule stirring, heating in water bath 3h at 50 DEG C, after heating in water bath completes,
Rotary evaporated to dryness at 70 DEG C again, collects and is dried granule, be washed with deionized 5 times, is dried 8h, is prepared into and changes at 70 DEG C
Property titanium dioxide granule；1:5 in mass ratio, mixes ultraviolet modification intercalated houghite material with the stirring of modifying titanium dioxide granule
It is placed in ball grinder, ball milling 5h at 500 DEG C, after ball milling completes, a kind of ultraviolet wideband Nano semiconductor can be prepared into
Heterojunction material.
Choose the Methyl Orange in Wastewater solution of 0.010g/mL, regulate pH to 4 with the sulfuric acid solution of 1mol/L, at 70 DEG C, will
Above-mentioned preparation ultraviolet wideband Nano semiconductor heterojunction material adds to waste water, and dosage is 500g/T, after adding
After 150min, percent of decolourization is up to more than 90%.
Claims (1)
1. the preparation method of a ultraviolet wideband Nano semiconductor heterojunction material, it is characterised in that concrete preparation process is:
(1) 1:5 in mass ratio, mixes p-(dimethylamino)-benzoic acid with the stirring of 1mol/L sodium hydroxide solution, the most quiet
Put 3～5h, be prepared into p-(dimethylamino)-benzoic acid alkaline solution, press Zn subsequently2+: Al3+Mol ratio 2:1, by Zn(NO3)2With Al
(NO3)3Stirring mixing, is prepared into mixed-powder, the most in mass ratio 1:10, is stirred with 1mol/L sodium hydroxide by mixed-powder
Mixing, the most still aging 3～5h, it is prepared into nano zinc aluminum mixed liquor；
(2) under nitrogen protection, 1:1 by volume, by nano zinc aluminum mixed liquor and the p-(dimethylamino)-benzoic acid of above-mentioned preparation
Alkaline solution stirring mixing is placed in there-necked flask, and water-bath 20～24h at 65～70 DEG C are filtered and collected filtering residue subsequently, use
After 85～90 DEG C of deionized water wash are to leacheate pH to 7.0, at 65～70 DEG C, it are dried 10～12h, are prepared into ultraviolet modified
Intercalated houghite material, standby；
(3) 1:10 in mass ratio, mixes perfluorooctanoic acid with dichloromethane stirring, and under 200～300W, sonic oscillation processes
15～20min, the most still aging 20～24h, it is prepared into organically-modified liquid, the most in mass ratio 1:5, by organic
Modification liquid mixes with titanium dioxide granule stirring, heating in water bath 2～3h at 45～50 DEG C, after heating in water bath completes, then
Rotary evaporated to dryness at 65～70 DEG C, collect be dried granule, be washed with deionized 3～5 times, at 65～70 DEG C be dried 6～
8h, is prepared into modifying titanium dioxide granule；
(4) 1:5 in mass ratio, ultraviolet modification intercalated houghite material step (2) prepared stirs with modifying titanium dioxide granule
Mix mixing to be placed in ball grinder, ball milling 3～5h at 450～500 DEG C, after ball milling completes, a kind of ultraviolet can be prepared into
Wideband Nano semiconductor heterojunction material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111437820A (en) * | 2020-03-25 | 2020-07-24 | 东华大学 | Composite nano material for producing hydrogen by photocatalytic water decomposition and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318595A (en) * | 2000-04-17 | 2001-10-24 | 北京化工大学 | Composite oganic-inorganic selective ultraviolet blocking material and its preparation |
| CN103191783A (en) * | 2013-04-18 | 2013-07-10 | 北京化工大学 | Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof |
| CN103212393A (en) * | 2013-04-26 | 2013-07-24 | 长江水利委员会长江科学院 | Nano titanium dioxide (TiO2)/ montmorillonite composite photocatalysis water treatment material and preparation method thereof |
-
2016
- 2016-08-16 CN CN201610672656.7A patent/CN106268743A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318595A (en) * | 2000-04-17 | 2001-10-24 | 北京化工大学 | Composite oganic-inorganic selective ultraviolet blocking material and its preparation |
| CN103191783A (en) * | 2013-04-18 | 2013-07-10 | 北京化工大学 | Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof |
| CN103212393A (en) * | 2013-04-26 | 2013-07-24 | 长江水利委员会长江科学院 | Nano titanium dioxide (TiO2)/ montmorillonite composite photocatalysis water treatment material and preparation method thereof |
Non-Patent Citations (9)
| Title |
|---|
| JIN YANG等: ""Superoleophobicity of a Material Made from Fluorinated Titania Nanoparticles"", 《JOURNAL OF DISPERSION SCIENCE AND TECHNOLOGY》 * |
| VULIC TATJANA等: ""PHOTOCATALYTIC ACTIVITY OF TiO2/ZnAl LDH BASED COATING IN RELATION TO MECHANICAL TREATMENT OF THE POWDER"", 《REVUE ROUMAINE DE CHIMIE》 * |
| XIANGHUI XUA等: ""Fabrication of superhydrophobic surfaces with perfluorooctanoic acid modified TiO2/polystyrene nanocomposites coating"", 《COLLOIDS AND SURFACES A: PHYSICOCHEM. ENG. ASPECTS》 * |
| 卡恩 CAHN.: "《金属与合金工艺》", 31 December 1999, 科学出版社 * |
| 卢晟等: ""超疏油表面研究进展"", 《材料导报A：综述篇》 * |
| 张彩山等: "《中国人该怎么活》", 30 November 2013, 天津科学技术出版社 * |
| 路璐: ""水滑石层柱紫外吸收材料的制备及性能研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 郑德等: "《热稳定剂的生产应用及进展》", 30 June 2011, 国防工业出版社 * |
| 魏文德等: "《有机化工原料大全 下》", 31 August 1999, 化学工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111437820A (en) * | 2020-03-25 | 2020-07-24 | 东华大学 | Composite nano material for producing hydrogen by photocatalytic water decomposition and preparation method thereof |
| CN111437820B (en) * | 2020-03-25 | 2022-03-18 | 东华大学 | Composite nano material for producing hydrogen by photocatalytic water decomposition and preparation method thereof |
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