CN106076302A - A kind of preparation method of nanometer black titanium dioxide optical catalyst - Google Patents
A kind of preparation method of nanometer black titanium dioxide optical catalyst Download PDFInfo
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- CN106076302A CN106076302A CN201610390623.3A CN201610390623A CN106076302A CN 106076302 A CN106076302 A CN 106076302A CN 201610390623 A CN201610390623 A CN 201610390623A CN 106076302 A CN106076302 A CN 106076302A
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- titanium dioxide
- optical catalyst
- black titanium
- solution
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 55
- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 230000003287 optical effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 9
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 9
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 9
- 150000003608 titanium Chemical class 0.000 claims abstract description 8
- 239000011941 photocatalyst Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 8
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 239000010936 titanium Substances 0.000 abstract description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 abstract description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 abstract description 4
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000002745 absorbent Effects 0.000 abstract description 3
- 239000002250 absorbent Substances 0.000 abstract description 3
- 230000002708 enhancing effect Effects 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 229910010062 TiCl3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003504 photosensitizing agent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
-
- 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
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to the preparation method of a kind of nanometer black titanium dioxide optical catalyst, the method with trivalent titanium salt as titanous chloride., TiOCl raw material, sodium borohydride, ascorbic acid or hydrazine hydrate are reducing agent, use hydrothermal synthesis method to prepare nanometer black titanium dioxide optical catalyst.By introducing Ti in titanium dioxide optical catalyst3+And oxygen defect, enhancing titanic oxide material, in ultraviolet, the visible and absorbent properties in infrared light district, can be added the consumption of reducing agent simultaneously, regulate the color of nano titanium dioxide photocatalyst by regulation.
Description
Technical field
The invention belongs to field of photocatalytic material, relate to the preparation method of a kind of nanometer black titanium dioxide optical catalyst.
Background technology
Photocatalysis technology is a kind of emerging technology grown up in the last thirty years, has wide at the energy and environmental area
Application prospect.Titanium dioxide is a class catalysis material most widely used in photocatalysis technology, due to its stable chemical nature,
The features such as photocatalysis efficiency height, environmental friendliness are it is considered to be the material of most application prospect in photocatalysis technology.But, tradition
Photocatalysis material of titanium dioxide be white powder, can only absorb ultraviolet light, and be excited thus produce photogenerated charge, Jin Erqi
To photochemical catalytic oxidation or the effect of opto-electronic conversion, it is impossible to the most energy in enough fully utilized sunlights.
In recent years, the biggest researcher is all inhaled at the full spectrum making great efforts to be improved titanic oxide material by various means
Receive performance, as metal and nonmetal doping, visible light-responded semi-conducting material meet, the multiple means such as photosensitizer sensitization,
And researcher finds by titanium dioxide self Ti recently3+, the design of oxygen defect can also improve titanic oxide material
Absorbing properties [4], spectral absorption scope is wide, photocatalytic activity is high due to it for this kind of photocatalyst, therefore has good answering
Use prospect.
Summary of the invention
Present invention aim at, it is provided that the preparation method of a kind of nanometer black titanium dioxide optical catalyst, the method is with three
Valency titanium salt is titanous chloride., TiOCl raw material, and sodium borohydride, ascorbic acid or hydrazine hydrate are reducing agent, uses Hydrothermal Synthesis legal system
Standby nanometer black titanium dioxide optical catalyst.By introducing Ti in titanium dioxide optical catalyst3+And oxygen defect, strengthen titanium dioxide
Titanium material, in ultraviolet, the visible and absorbent properties in infrared light district, can add the consumption of reducing agent simultaneously by regulation, and regulation is received
The color of rice titanium dioxide optical catalyst.
The preparation method of a kind of nanometer black titanium dioxide optical catalyst of the present invention, the method with trivalent titanium salt is
Raw material, uses hydro-thermal method method to prepare high dispersive, high-specific area nano black titanium dioxide photocatalyst, and concrete operations are by following
Step is carried out:
A, by 2-10g trivalent titanium salt it is titanous chloride. or TiOCl and 0-1g reducing agent is sodium borohydride, ascorbic acid or water
Close hydrazine to add in 20-100mL deionized water, continuously stirred 1-3 hour, obtain purple clear solution；
B, step a solution will add the sodium hydroxide solution of 0.2-1.5mol/L, until pH value is 2-10, continuously stirred
2-3 hour, obtain black titanium dioxide solution；
C, solution in step b is transferred in 100mL water heating kettle, reacts 4-20 hour at temperature 80-260 DEG C, obtain
Nanometer black titanium dioxide；
D, by nanometer black titanium dioxide in step c through 50mL deionized water, 50mL ethanol be respectively washed to pH be 7,
It is dried, i.e. obtains nanometer black titanium dioxide optical catalyst.
In step a, the addition of reducing agent is different, the color of obtained titanium dioxide optical catalyst be white, brown and
Black.
The preparation method of a kind of nanometer black titanium dioxide optical catalyst of the present invention, the feature of the method is main
Have: (1) is with trivalent titanium salt as raw material；(2) in titanium dioxide optical catalyst, Ti is introduced3+And oxygen defect；(3) in ultraviolet, visible
Stronger absorption is had with infrared light district；(4) photocatalyst color can be regulated by regulation reducing agent consumption.
The preparation method of a kind of nanometer black titanium dioxide optical catalyst of the present invention, the beneficial effect of the method:
With trivalent titanium salt as raw material, by introducing Ti in titanium dioxide optical catalyst3+And oxygen defect, strengthen titanic oxide material at purple
Outward, the visible and absorbent properties in infrared light district.
The titanous source used in the embodiment of the present invention is commercially available titanous chloride. (TiCl3), TiOCl, reducing agent is permissible
For sodium borohydride, ascorbic acid, hydrazine hydrate, and pass through hydrothermal synthesis method, it is thus achieved that nanometer black titanium dioxide optical catalyst, by
This infers: when using other titanous sources and reducing agent, also can realize the technique effect of the present invention.
Accompanying drawing explanation
Fig. 1 is the photo figure of present invention white, brown, black nano titanium dioxide optical catalyst, and wherein a is white, and b is
Brown, c is black；
Fig. 2 is transmission electron microscope of the present invention, X-ray diffractogram.
Detailed description of the invention
Following non-limiting example can make those of ordinary skill in the art that the present invention be more fully understood, but not with
Any mode limits the present invention；
Embodiment 1
A, 2g titanous chloride. and 0.1g sodium borohydride are added in 20mL deionized water, continuously stirred 1 hour, obtain purple
Clear solution；
B, solution step a obtained add the sodium hydroxide solution of 0.2mol/L, until pH value is 2, continuously stirred 2
Hour, obtain black titanium dioxide solution；
C, solution in step b is transferred in 100mL water heating kettle, reacts 4 hours at temperature 80 DEG C, obtain nanometer black
Titanium dioxide；
D, by the nanometer black titanium dioxide that obtains in step c through 50mL deionized water, 50mL ethanol be respectively washed to
PH is 7, is dried, obtains final nanometer black titanium dioxide optical catalyst.
Embodiment 2
A, 5g titanous chloride. and 0.7g ascorbic acid are added in 50mL deionized water, continuously stirred 2 hours, obtain purple
Clear solution；
B, solution step a obtained add the sodium hydroxide solution of 1.0mol/L, until pH value is 5, continuously stirred 2
Hour, obtain black titanium dioxide solution；
C, solution in step b is transferred in 100mL water heating kettle, reacts 12 hours at temperature 180 DEG C, obtain nano black
Color titanium dioxide；
D, by the nanometer black titanium dioxide that obtains in step c through 50mL deionized water, 50mL ethanol be respectively washed to
PH is 7, is dried, i.e. obtains final nanometer black titanium dioxide optical catalyst.
Embodiment 3
A, 8gTiOCl and 0.8g hydrazine hydrate is added in 70mL deionized water, continuously stirred 3 hours, obtain purple transparent
Solution；
B, solution step a obtained add the sodium hydroxide solution of 1.2mol/L, until pH value is 8, continuously stirred 3
Hour, obtain black titanium dioxide solution；
C, solution in step b is transferred in 100mL water heating kettle, reacts 18 hours at temperature 200 DEG C, obtain nano black
Color titanium dioxide；
D, by the nanometer black titanium dioxide that obtains in step c through 50mL deionized water, 50mL ethanol be respectively washed to
PH is 7, is dried, i.e. obtains final nanometer black titanium dioxide optical catalyst.
Embodiment 4
A, 10gTiOCl and 1.0g ascorbic acid is added in 100mL deionized water, continuously stirred 3 hours, obtain purple
Clear solution；
B, solution step a obtained add the sodium hydroxide solution of 1.5mol/L, until pH value is 10, continuously stirred
3 hours, obtain black titanium dioxide solution；
C, solution in step b is transferred in 100mL water heating kettle, reacts 20 hours at temperature 260 DEG C, obtain nano black
Color titanium dioxide；
D, by the nanometer black titanium dioxide that obtains in step c through 50mL deionized water, 50mL ethanol be respectively washed to
PH is 7, and after drying, obtains final nanometer black titanium dioxide optical catalyst.
Embodiment 5
A, 5g titanous chloride. and 0.5g ascorbic acid are added in 50mL deionized water, continuously stirred 2 hours, obtain purple
Clear solution；
B, solution step a obtained add the sodium hydroxide solution of 1.0mol/L, until pH value is 5, continuously stirred 2
Hour, obtain brown titania solution；
C, solution in step b is transferred in 100mL water heating kettle, reacts 12 hours at temperature 180 DEG C, obtain nanometer brown
Color titanium dioxide；
D, by the nanometer brown titanium dioxide that obtains in step c through 50mL deionized water, 50mL ethanol be respectively washed to
PH is 7, is dried, i.e. obtains final nanometer brown titanium dioxide optical catalyst.
Embodiment 6
A, 5g titanous chloride. and 0g ascorbic acid are added in 50mL deionized water, continuously stirred 2 hours, obtain purple saturating
Bright solution；
B, solution step a obtained add the sodium hydroxide solution of 1.0mol/L, until pH value is 5, continuously stirred 2
Hour, obtain black titanium dioxide solution；
C, solution in step b is transferred in 100mL water heating kettle, reacts 12 hours at temperature 180 DEG C, obtain nanometer white
Color titanium dioxide；
D, by the nanometer white titania that obtains in step c through 50mL deionized water, 50mL ethanol be respectively washed to
PH is 7, is dried, i.e. obtains final nanometer white titania photocatalyst.
Embodiment 7
Any one white, brown, black nano titanium dioxide optical catalyst in embodiment 1-6 are carried out X-ray diffraction
Analysis, tem study, color analysis, acquired results is shown in accompanying drawing 1, it was demonstrated that the titanium dioxide of preparation in the present embodiment
Photocatalyst is white, brown, black nano titanium dioxide optical catalyst.
Claims (2)
1. the preparation method of a nanometer black titanium dioxide optical catalyst, it is characterised in that with trivalent titanium salt as raw material, uses
Hydro-thermal method method prepares high dispersive, high-specific area nano black titanium dioxide photocatalyst, and concrete operations follow these steps to carry out:
A, by 2-10g trivalent titanium salt it is titanous chloride. or TiOCl and 0-1 g reducing agent is sodium borohydride, ascorbic acid or hydration
Hydrazine adds in 20-100 mL deionized water, continuously stirred 1-3 hour, obtains purple clear solution；
B, will in step a solution add 0.2-1.5 mol/L sodium hydroxide solution, until pH value is 2-10, continuously stirred 2-3
Hour, obtain black titanium dioxide solution；
C, solution in step b is transferred in 100 mL water heating kettles, reacts 4-20 hour at temperature 80-260 DEG C, obtain nanometer
Black titanium dioxide；
D, by nanometer black titanium dioxide in step c through 50mL deionized water, 50mL ethanol be respectively washed to pH be 7, be dried,
I.e. obtain nanometer black titanium dioxide optical catalyst.
The preparation method of nanometer black titanium dioxide optical catalyst the most according to claim 1, it is characterised in that in step a also
The addition of former dose is different, and the color of obtained titanium dioxide optical catalyst is white, brown and black.
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106582595A (en) * | 2016-12-28 | 2017-04-26 | 上海应用技术大学 | Preparation method for blue TiO2 catalyst |
| CN107010604A (en) * | 2017-04-17 | 2017-08-04 | 清华大学 | A kind of method for regulating and controlling oxide material defect density at normal temperatures |
| CN108455666A (en) * | 2018-05-08 | 2018-08-28 | 浙江大学台州研究院 | The hydrophilic TiO of black with photo-thermal effect2Preparation method |
| CN108745347A (en) * | 2018-05-08 | 2018-11-06 | 陕西科技大学 | Pt atom carried titanium dioxide catalysis material and preparation method thereof |
| CN108940245A (en) * | 2018-08-10 | 2018-12-07 | 大连工业大学 | A kind of black TiO2/ white TiO2Composite material and preparation method |
| CN110711574A (en) * | 2019-10-25 | 2020-01-21 | 攀枝花学院 | Method for preparing black titanium dioxide by low-temperature liquid-phase hydrothermal reduction method |
| CN110790305A (en) * | 2019-11-27 | 2020-02-14 | 湖南科莱新材料有限公司 | Preparation method of black titanium dioxide powder |
| CN110790307A (en) * | 2019-11-27 | 2020-02-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of colored titanium dioxide, product and application thereof |
| CN111151233A (en) * | 2019-12-31 | 2020-05-15 | 陕西科技大学 | Oxygen-deficient TiO2Normal temperature and pressure water phase preparation method |
| CN111298788A (en) * | 2019-12-02 | 2020-06-19 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of silver-loaded colored one-dimensional mesoporous titanium dioxide, product and application thereof |
| CN111533163A (en) * | 2020-05-20 | 2020-08-14 | 中国科学技术大学 | Black lithium titanate material for lithium ion battery cathode and preparation method and application thereof |
| CN111821966A (en) * | 2019-04-22 | 2020-10-27 | 新疆大学 | Black TiO2Preparation method of nanosheet photocatalyst |
| CN112371117A (en) * | 2020-11-13 | 2021-02-19 | 吉林大学 | High-dispersion ruthenium-loaded surface-modified layered titanate nanosheet photocatalyst, and preparation method and application thereof |
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| CN113582218A (en) * | 2021-07-30 | 2021-11-02 | 陕西科技大学 | Oxygen-deficient gray zinc oxide and preparation method and application thereof |
| CN113797910A (en) * | 2020-06-16 | 2021-12-17 | 中国科学院化学研究所 | Defect-containing nano microspheric perovskite catalyst and preparation method and application thereof |
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| CN106582595B (en) * | 2016-12-28 | 2019-07-23 | 上海应用技术大学 | A kind of blue TiO2The preparation method of catalyst |
| CN106582595A (en) * | 2016-12-28 | 2017-04-26 | 上海应用技术大学 | Preparation method for blue TiO2 catalyst |
| CN107010604A (en) * | 2017-04-17 | 2017-08-04 | 清华大学 | A kind of method for regulating and controlling oxide material defect density at normal temperatures |
| CN108455666A (en) * | 2018-05-08 | 2018-08-28 | 浙江大学台州研究院 | The hydrophilic TiO of black with photo-thermal effect2Preparation method |
| CN108745347A (en) * | 2018-05-08 | 2018-11-06 | 陕西科技大学 | Pt atom carried titanium dioxide catalysis material and preparation method thereof |
| CN108940245B (en) * | 2018-08-10 | 2020-10-23 | 大连工业大学 | Black TiO2White TiO2Composite material and preparation method thereof |
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| CN110711574A (en) * | 2019-10-25 | 2020-01-21 | 攀枝花学院 | Method for preparing black titanium dioxide by low-temperature liquid-phase hydrothermal reduction method |
| CN110790307A (en) * | 2019-11-27 | 2020-02-14 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of colored titanium dioxide, product and application thereof |
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