CN108212223A - The preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic - Google Patents
The preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic Download PDFInfo
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- CN108212223A CN108212223A CN201810112014.0A CN201810112014A CN108212223A CN 108212223 A CN108212223 A CN 108212223A CN 201810112014 A CN201810112014 A CN 201810112014A CN 108212223 A CN108212223 A CN 108212223A
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- Prior art keywords
- titanium dioxide
- graphene oxide
- graphene
- toxic
- catalysis material
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 91
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 59
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 34
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 22
- 231100000252 nontoxic Toxicity 0.000 title claims abstract description 19
- 230000003000 nontoxic effect Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000005083 Zinc sulfide Substances 0.000 claims abstract description 23
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920001661 Chitosan Polymers 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 239000006185 dispersion Substances 0.000 claims description 14
- 238000002604 ultrasonography Methods 0.000 claims description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 8
- 238000004073 vulcanization Methods 0.000 claims description 8
- 229910052725 zinc Inorganic materials 0.000 claims description 8
- 239000011701 zinc Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 235000009508 confectionery Nutrition 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 229920005615 natural polymer Polymers 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- -1 therefore Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of preparation methods of the harmless titanium dioxide graphene catalysis material of novel non-toxic, are mainly made by graphene oxide, chitosan, titanium dioxide, zinc sulphide by hydro-thermal method.The present invention is compound with titanium dioxide by graphene, add in zinc sulphide, utilize the high conductivity of graphene, the service life of light induced electron and photohole can be extended, so as to improve the photocatalytic activity of titanium dioxide, zinc sulphide, while the introducing of natural polymer chitosan, the intensity and photocatalysis performance of material can be effectively improved, product is nontoxic, and whole preparation process processing step is simple, of low cost.
Description
Technical field
The invention belongs to field of photocatalytic material, and in particular to a kind of harmless titanium dioxide graphene photocatalysis of novel non-toxic
The preparation method of material.
Background technology
Titanium dioxide is commonly called as titanium dioxide, is a kind of widely used metal oxide materials, due to its good whiteness
And glossiness and characteristics, the titanium dioxide such as nontoxic are widely used in the fields such as coating, cosmetics and food and medicine.
More since it is easy to excite under the irradiation of ultraviolet light, lose electronics and form the free radical of strong oxidizing property, so as to fine
Ground oxygenolysis organic matter, therefore, titanium dioxide is also used in light-catalyzed reaction.
Graphene has very excellent electric conductivity, translucency and larger specific surface area, by by grapheme material
It is compound with titanium dioxide, when obtained composite photocatalyst material not only extends the separation of electron-hole in light-catalyzed reaction
Between, it can also improve the utilizing status to visible ray.
Invention content
The purpose of the present invention is to provide a kind of preparation sides of the harmless titanium dioxide graphene catalysis material of novel non-toxic
Method.
The technical solution adopted by the present invention to solve the technical problems is：The harmless titanium dioxide graphene light of novel non-toxic is urged
Change the preparation method of material, include the following steps：
1）It adds graphene oxide into deionized water, is ultrasonically treated 30-60 minutes, obtains graphene oxide dispersion；
2）Chitosan is added in the acetum of 2wt%, the 15-30 minutes chitosan acetic acid for obtaining a concentration of 2-4wt% of stirring is molten
Liquid；
3）Titanium dioxide is added in into ultrasound 30-60 minutes in absolute ethyl alcohol, obtains the titania solution of a concentration of 2-10wt%；
4）Zinc sulphide is added in sodium hydroxide solution and dissolves to obtain vulcanization zinc solution, a concentration of 1-4wt% of zinc sulphide；
5）Titania solution is added in vulcanization zinc solution and is uniformly mixed, then gathers graphene oxide dispersion and shell
Sweet and sour acid solution adds in, and ultrasound 1-2 hours, mixed liquor is transferred in polytetrafluoroethylliner liner hydrothermal reaction kettle, 210 after mixing
DEG C hydro-thermal reaction 12 hours, after being cooled to room temperature, washing is freeze-dried to obtain catalysis material three times.
Specifically, the step 1）A concentration of 3-6wt% of middle graphene oxide dispersion.
Specifically, the dosage of the chitosan is the 3-7% of graphene oxide quality.
Specifically, the dosage of the zinc sulphide is the 2-4% of graphene oxide quality.
Specifically, the dosage of the titanium dioxide is the 8-15% of graphene oxide quality.
Specifically, the step 4）A concentration of 2-5wt% of middle sodium hydroxide solution.
The invention has the advantages that：The present invention is compound with titanium dioxide by graphene, adds in zinc sulphide, utilizes stone
The high conductivity of black alkene can extend the service life of light induced electron and photohole, so as to improve the photocatalysis of titanium dioxide, zinc sulphide
Activity, while the introducing of natural polymer chitosan can effectively improve the intensity and photocatalysis performance of material, the nontoxic nothing of product
Evil, whole preparation process processing step is simple, of low cost.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention is described further, but the present invention
Protection domain is not limited to these embodiments.It is every to be included in the present invention without departing substantially from the change of present inventive concept or equivalent substitute
Protection domain within.
Embodiment 1
The preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic, includes the following steps：
1）It adds graphene oxide into deionized water, is ultrasonically treated 40 minutes, obtain the graphene oxide dispersion of a concentration of 5wt%
Liquid；
2）The chitosan for accounting for graphene oxide quality 5% is added in the acetum of 2wt%, stirring obtains a concentration of 3wt% in 30 minutes
Chitosan-acetic acid solution；
3）The titanium dioxide for accounting for graphene oxide quality 10% is added in into ultrasound 50 minutes in absolute ethyl alcohol, obtains a concentration of 5wt%'s
Titania solution；
4）The zinc sulphide for accounting for graphene oxide quality 2% is added in the sodium hydroxide solution of a concentration of 5wt% and dissolves to obtain zinc sulphide
Solution, a concentration of 3wt% of zinc sulphide；
5）Titania solution is added in vulcanization zinc solution and is uniformly mixed, then gathers graphene oxide dispersion and shell
Sweet and sour acid solution adds in, and ultrasound 2 hours, mixed liquor are transferred in polytetrafluoroethylliner liner hydrothermal reaction kettle, 210 DEG C after mixing
Hydro-thermal reaction 12 hours, after being cooled to room temperature, washing is freeze-dried to obtain catalysis material three times.
Embodiment 2
The preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic, includes the following steps：
1）It adds graphene oxide into deionized water, is ultrasonically treated 30 minutes, obtain the graphene oxide dispersion of a concentration of 4wt%
Liquid；
2）The chitosan for accounting for graphene oxide quality 7% is added in the acetum of 2wt%, stirring obtains a concentration of 4wt% in 25 minutes
Chitosan-acetic acid solution；
3）The titanium dioxide for accounting for graphene oxide quality 12% is added in into ultrasound 30 minutes in absolute ethyl alcohol, obtains a concentration of 2wt%'s
Titania solution；
4）The zinc sulphide for accounting for graphene oxide quality 4% is added in the sodium hydroxide solution of a concentration of 4wt% and dissolves to obtain zinc sulphide
Solution, a concentration of 2wt% of zinc sulphide；
5）Titania solution is added in vulcanization zinc solution and is uniformly mixed, then gathers graphene oxide dispersion and shell
Sweet and sour acid solution adds in, and ultrasound 2 hours, mixed liquor are transferred in polytetrafluoroethylliner liner hydrothermal reaction kettle, 210 DEG C after mixing
Hydro-thermal reaction 12 hours, after being cooled to room temperature, washing is freeze-dried to obtain catalysis material three times.
Embodiment 3
The preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic, includes the following steps：
1）It adds graphene oxide into deionized water, is ultrasonically treated 50 minutes, obtain the graphene oxide dispersion of a concentration of 3wt%
Liquid；
2）The chitosan for accounting for graphene oxide quality 3% is added in the acetum of 2wt%, stirring obtains a concentration of 2wt% in 15 minutes
Chitosan-acetic acid solution；
3）The titanium dioxide for accounting for graphene oxide quality 15% is added in into ultrasound 40 minutes in absolute ethyl alcohol, obtains a concentration of 10wt%'s
Titania solution；
4）The zinc sulphide for accounting for graphene oxide quality 4% is added in the sodium hydroxide solution of a concentration of 3wt% and dissolves to obtain zinc sulphide
Solution, a concentration of 4wt% of zinc sulphide；
5）Titania solution is added in vulcanization zinc solution and is uniformly mixed, then gathers graphene oxide dispersion and shell
Sweet and sour acid solution adds in, and ultrasound 1 hour, mixed liquor is transferred in polytetrafluoroethylliner liner hydrothermal reaction kettle, 210 DEG C after mixing
Hydro-thermal reaction 12 hours, after being cooled to room temperature, washing is freeze-dried to obtain catalysis material three times.
Embodiment 4
The preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic, includes the following steps：
1）It adds graphene oxide into deionized water, is ultrasonically treated 60 minutes, obtain the graphene oxide dispersion of a concentration of 6wt%
Liquid；
2）The chitosan for accounting for graphene oxide quality 4% is added in the acetum of 2wt%, stirring obtains a concentration of 3wt% in 20 minutes
Chitosan-acetic acid solution；
3）The titanium dioxide for accounting for graphene oxide quality 8% is added in into ultrasound 60 minutes in absolute ethyl alcohol, obtains the two of a concentration of 8wt%
Titanium oxide solution；
4）The zinc sulphide for accounting for graphene oxide quality 3% is added in the sodium hydroxide solution of a concentration of 2wt% and dissolves to obtain zinc sulphide
Solution, a concentration of 1wt% of zinc sulphide；
5）Titania solution is added in vulcanization zinc solution and is uniformly mixed, then gathers graphene oxide dispersion and shell
Sweet and sour acid solution adds in, and ultrasound 1 hour, mixed liquor is transferred in polytetrafluoroethylliner liner hydrothermal reaction kettle, 210 DEG C after mixing
Hydro-thermal reaction 12 hours, after being cooled to room temperature, washing is freeze-dried to obtain catalysis material three times.
Claims (6)
1. the preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic, which is characterized in that include the following steps：
1) it adds graphene oxide into deionized water, is ultrasonically treated 30-60 minutes, obtains graphene oxide dispersion；
2) chitosan is added in the acetum of 2wt%, the 15-30 minutes chitosan acetic acid for obtaining a concentration of 2-4wt% of stirring
Solution；
3) titanium dioxide is added in into ultrasound 30-60 minutes in absolute ethyl alcohol, obtains the titania solution of a concentration of 2-10wt%；
4) zinc sulphide is added in sodium hydroxide solution and dissolves to obtain vulcanization zinc solution, a concentration of 1-4wt% of zinc sulphide；
5) titania solution is added in vulcanization zinc solution and be uniformly mixed, then gather graphene oxide dispersion and shell
Sweet and sour acid solution adds in, and ultrasound 1-2 hours, mixed liquor is transferred in polytetrafluoroethylliner liner hydrothermal reaction kettle, 210 after mixing
DEG C hydro-thermal reaction 12 hours, after being cooled to room temperature, washing is freeze-dried to obtain catalysis material three times.
2. the preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic as described in claim 1, feature
It is, a concentration of 3-6wt% of graphene oxide dispersion in the step 1).
3. the preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic as described in claim 1, feature
It is, the dosage of the chitosan is the 3-7% of graphene oxide quality.
4. the preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic as described in claim 1, feature
It is, the dosage of the zinc sulphide is the 2-4% of graphene oxide quality.
5. the preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic as described in claim 1, feature
It is, the dosage of the titanium dioxide is the 8-15% of graphene oxide quality.
6. the preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic as described in claim 1, feature
It is, a concentration of 2-5wt% of sodium hydroxide solution in the step 4).
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| CN201810112014.0A CN108212223A (en) | 2018-02-05 | 2018-02-05 | The preparation method of the harmless titanium dioxide graphene catalysis material of novel non-toxic |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109363055A (en) * | 2018-09-18 | 2019-02-22 | 广州先护特农业科技有限公司 | A kind of composition, preparation method and its application in fresh protection |
| CN109794263A (en) * | 2019-03-25 | 2019-05-24 | 东华大学 | The preparation method and application of ZnS/GO porous microsphere nano material |
| CN112499854A (en) * | 2020-10-26 | 2021-03-16 | 武汉理工大学 | Integrated drinking water treatment system |
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| CN101003020A (en) * | 2007-01-11 | 2007-07-25 | 南京大学 | Sensitized titanium oxide and zinc sulfide visible light responsing photocalalyst, and its preparing method |
| CN103521191A (en) * | 2013-10-15 | 2014-01-22 | 湖南大学 | Preparation method and application of titanium dioxide/chitosan/oxidized graphene composite material |
| CN106799219A (en) * | 2016-12-22 | 2017-06-06 | 南昌航空大学 | A kind of preparation method of titania nanoparticles/Graphene composite photocatalyst material |
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2018
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Patent Citations (3)
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| CN101003020A (en) * | 2007-01-11 | 2007-07-25 | 南京大学 | Sensitized titanium oxide and zinc sulfide visible light responsing photocalalyst, and its preparing method |
| CN103521191A (en) * | 2013-10-15 | 2014-01-22 | 湖南大学 | Preparation method and application of titanium dioxide/chitosan/oxidized graphene composite material |
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|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109363055A (en) * | 2018-09-18 | 2019-02-22 | 广州先护特农业科技有限公司 | A kind of composition, preparation method and its application in fresh protection |
| CN109794263A (en) * | 2019-03-25 | 2019-05-24 | 东华大学 | The preparation method and application of ZnS/GO porous microsphere nano material |
| CN112499854A (en) * | 2020-10-26 | 2021-03-16 | 武汉理工大学 | Integrated drinking water treatment system |
| CN112499854B (en) * | 2020-10-26 | 2023-04-18 | 武汉理工大学 | Integrated drinking water treatment system |
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Application publication date: 20180629 |