CN106215915A - A kind of preparation method of the carrier loaded titanium dioxide optical catalyst of adsorbent class - Google Patents

A kind of preparation method of the carrier loaded titanium dioxide optical catalyst of adsorbent class Download PDF

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Publication number
CN106215915A
CN106215915A CN201610600665.5A CN201610600665A CN106215915A CN 106215915 A CN106215915 A CN 106215915A CN 201610600665 A CN201610600665 A CN 201610600665A CN 106215915 A CN106215915 A CN 106215915A
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titanium dioxide
preparation
sol
optical catalyst
carrier
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CN106215915B (en
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陈奎
张天云
魏伟
高国亮
晏丽琴
王宏强
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Lanzhou City University
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Lanzhou City University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063Titanium; Oxides or hydroxides thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • C02F2101/345Phenols
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/40Organic compounds containing sulfur
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Catalysts (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses the preparation method of a kind of carrier loaded titanium dioxide optical catalyst of adsorbent class.By aluminum isopropylate., alcohol, water are mixed with acid, 80~90 DEG C of return stirrings 6~18h, obtain boehmite sol;Under stirring condition, the mixed solution of tetrabutyl titanate and alcohol is dropped in boehmite sol, stirring at normal temperature 1~3h, obtain complex sol;After this complex sol is sealed ageing 12~48h at normal temperatures, dry 6~8h in 80~100 DEG C, be then heated to 450~550 DEG C, be incubated 3~5h, grind the titanium dioxide optical catalyst of the adsorbent class carrier gamma-alumina load obtaining the present invention.The load type titania photocatalyst of the present invention, after recycling for 8 times to catalytic degradation clearance organic in sewage more than 80%, can be used for organic catalytic degradation in sewage.The load type titania photocatalyst of the present invention, improves titanium dioxide load capacity on carrier, reduces cost, have a wide range of applications at industrial circle.

Description

A kind of preparation method of the carrier loaded titanium dioxide optical catalyst of adsorbent class
Technical field
The present invention relates to photocatalyst field, be specifically related to a kind of carrier loaded titanium dioxide optical catalyst of adsorbent class Preparation method.
Background technology
Nano titanium oxide has stronger photocatalytic activity, chemical stability, low cost and the advantage such as nontoxic, can pass through Photocatalyst is at normal temperatures and pressures nothings such as poisonous, harmful organic matter degradation Cheng Shui multiple in sewage and carbon dioxide Pest matter, enjoys favor in terms of sewage disposal.But photocatalytic speed is low and low to the utilization rate of solar energy, constrain titanium dioxide The heavy industrialization application of titanium photocatalyst.By on titanium dichloride load to adsorbent class carrier, it is possible not only to increase dioxy Change organic contact area in titanium self and sewage, it is also possible to by the adsorptivity of carrier by Adsorption of Organic to titanium dioxide Around granule, it is achieved organic rapid photocatalytic is degraded, and improves the photo-catalysis capability of titanium dioxide.
The preparation method of the carrier loaded titanium dioxide optical catalyst of adsorbent class mainly has hydro-thermal method, chemical precipitation method and molten Glue-gel method.Compared with first two method, sol-gel process is simple to operate, easy to control, and can be in the forming process of colloidal sol In be conveniently added with various material, to titanium dioxide implement element mix modification.Therefore, use sol-gel process in recent years more Carry out the exploitation of titanium dioxide optical catalyst.Urge using sol-gel process to prepare the carrier loaded titanium-dioxide photo of adsorbent class In the report of agent, it is in TiO 2 sol mostly by that prepare or existing support dispersion, by gel with follow-up forge Burn the preparation realizing photocatalyst, because easily forming the secondary core of titanium dioxide, titanium dioxide in the method gained photocatalyst The load capacity of titanium is relatively low.
Summary of the invention
In sum, it is an object of the invention to disclose the system of a kind of carrier loaded titanium dioxide optical catalyst of adsorbent class Preparation Method.
A kind of preparation method of the carrier loaded titanium dioxide optical catalyst of adsorbent class, its step is as follows:
A, the preparation of boehmite sol
Aluminum isopropylate., alcohol, deionized water are mixed for 1:50~100:100~200:0.1~0.3 in molar ratio with acid, 80~90 DEG C it are warmed up under stirring condition, return stirring 6~18h, natural cooling, obtain stable transparent boehmite sol;
B, the preparation of complex sol
Under stirring condition, the mixed solution that tetrabutyl titanate that mol ratio is 1:20~100 and alcohol are made into is slowly added dropwise to In a step gained boehmite sol, room temperature is stirred vigorously 1~3h, obtains homogeneous transparent complex sol;
Wherein, aluminum isopropylate. is 1:0.1~2 with the mol ratio of tetrabutyl titanate;
C, the preparation of loaded photocatalyst
After the complex sol of b step gained is sealed ageing 12~48h at normal temperatures, in the drying baker ventilated in 80~ Dry 6~8h, be then placed in Muffle furnace being heated to 450~550 DEG C for 100 DEG C, be incubated 3~5h, naturally cool to room temperature, finally Grind the titanium dioxide optical catalyst obtaining the load of adsorbent class carrier gama-alumina;
Above-mentioned alcohol is ethanol, or isopropanol, or n-butyl alcohol, or propylene glycol;
Above-mentioned acid is hydrochloric acid, or nitric acid, or acetic acid, or oxalic acid.
The present invention is according in certain acid range, and boehmite sol is stable, and TiO 2 sol this characteristic of easy gel, Use titania gel cutting boehmite sol, then prepare carrier and loaded article by high temperature sintering, it is achieved dioxy simultaneously Change titanium and be carried on gama-alumina with chemical bond.Not only increase titanium dioxide in photocatalytic process with catalysis the contacting of object Area, also gives the absorption property of catalyst gama-alumina, improves photocatalytic speed and the effect of titanium dioxide.
The present invention compared with prior art, has the advantage that:
1, the present invention is with aluminum isopropylate. and tetrabutyl titanate as primary raw material, prepares gama-alumina carried titanium dioxide light Catalyst, as one of primary raw material preparing gama-alumina, aluminum isopropylate. price is relatively cheap, it replace gama-alumina Directly prepare photocatalyst can reduce cost with tetrabutyl titanate.
2, in photocatalyst prepared by the present invention, titanium dioxide may be up to 2:1, greatly with the mol ratio of carrier gama-alumina Improve greatly titanium dioxide load capacity on gamma-alumina.
3, photocatalyst prepared by the present invention, can be used for bisphenol-A, or methyl orange, or methylene blue, or Congo red, or sieve The catalytic degradation of red bright gas chromatography, applied range.
4, the photocatalyst prepared by the present invention, after 8 times recycle, removes organic catalytic degradation in sewage Rate, still more than 80%, can be used for organic catalytic degradation in sewage.
Detailed description of the invention
Embodiment 1
Aluminum isopropylate., ethanol, deionized water are mixed for 1:100:100:0.15 in molar ratio with acetic acid, under stirring condition It is warmed up to 90 DEG C, return stirring 6h, natural cooling, obtain stable transparent boehmite sol.
Under stirring condition, the mixed solution that 0.5mol tetrabutyl titanate and 50mol ethanol are made into is slowly added dropwise to above-mentioned suddenly In nurse stone colloidal sol, room temperature is stirred vigorously 1.5h, obtains homogeneous transparent complex sol.
By complex sol after room temperature seals ageing 18h, in the drying baker ventilated, dry 8h in 80 DEG C, be then placed in horse Stove is not heated to 450 DEG C, is incubated 5h, naturally cools to room temperature, finally grind and obtain the load of adsorbent class carrier gama-alumina Titanium dioxide optical catalyst.
Embodiment 2
It is that 1:75:150:0.2 mixes by aluminum isopropylate., isopropanol, deionized water with hydrochloric acid mol ratio, rises under stirring condition Warm to 85 DEG C, return stirring 12h, natural cooling, obtain stable transparent boehmite sol.
Under stirring condition, the mixed solution that 1mol tetrabutyl titanate and 75mol isopropanol are made into is slowly added dropwise to above-mentioned suddenly In nurse stone colloidal sol, room temperature is stirred vigorously 2h, obtains homogeneous transparent complex sol;
By complex sol after room temperature seals ageing 24h, in the drying baker ventilated, dry 7h in 85 DEG C, be then placed in horse Stove is not heated to 500 DEG C, is incubated 4h, naturally cools to room temperature, finally grind and obtain the load of adsorbent class carrier gama-alumina Titanium dioxide optical catalyst.
Embodiment 3
It is that 1:70:100:0.1 mixes by aluminum isopropylate., n-butyl alcohol, deionized water with oxalic acid mol ratio, rises under stirring condition Warm to 80 DEG C, return stirring 18h, natural cooling, obtain stable transparent boehmite sol.
Under stirring condition, the mixed solution that 0.1mol tetrabutyl titanate and 5mol n-butyl alcohol are made into is slowly added dropwise to above-mentioned In boehmite sol, room temperature is stirred vigorously 1h, obtains homogeneous transparent complex sol.
By complex sol after room temperature seals ageing 12h, in the drying baker ventilated, dry 6h in 90 DEG C, be then placed in horse Stove is not heated to 550 DEG C, is incubated 3h, naturally cools to room temperature, finally grind and obtain the load of adsorbent class carrier gama-alumina Titanium dioxide optical catalyst.
Embodiment 4
It is that 1:50:200:0.3 mixes by aluminum isopropylate., propylene glycol, deionized water with nitric acid mol ratio, rises under stirring condition Warm to 85 DEG C, return stirring 12h, natural cooling, obtain stable transparent boehmite sol.
Under stirring condition, the mixed solution that 2mol tetrabutyl titanate and 40mol propylene glycol are made into is slowly added dropwise to above-mentioned suddenly In nurse stone colloidal sol, room temperature is stirred vigorously 3h, obtains homogeneous transparent complex sol.
By complex sol after room temperature seals ageing 48h, in the drying baker ventilated, dry 6h in 95 DEG C, be then placed in horse Stove is not heated to 550 DEG C, is incubated 3h, naturally cools to room temperature, finally grind and obtain the load of adsorbent class carrier gama-alumina Titanium dioxide optical catalyst.
Although the present invention is open the most as above with preferred embodiment, but it is not limited to the present invention, any is familiar with this The people of technology, without departing from the spirit and scope of the present invention, can do various change and modification, the therefore protection of the present invention Scope should be with being as the criterion that claims are defined.

Claims (2)

1. a preparation method for the carrier loaded titanium dioxide optical catalyst of adsorbent class, its step is as follows:
A, the preparation of boehmite sol
Aluminum isopropylate., alcohol, deionized water are mixed for 1:50~100:100~200:0.1~0.3 in molar ratio with acid, stirring Under the conditions of be warmed up to 80~90 DEG C, return stirring 6~18h, natural cooling, obtain stable transparent boehmite sol;
B, the preparation of complex sol
Under stirring condition, the mixed solution that tetrabutyl titanate that mol ratio is 1:20~100 and alcohol are made into is slowly added dropwise to a and walks In rapid gained boehmite sol, room temperature is stirred vigorously 1~3h, obtains homogeneous transparent complex sol;
Wherein, aluminum isopropylate. is 1:0.1~2 with the mol ratio of tetrabutyl titanate;
C, the preparation of loaded photocatalyst
After the complex sol of b step gained is sealed ageing 12~48h at normal temperatures, in 80~100 in the drying baker ventilated DEG C dry 6~8h, be then placed in Muffle furnace being heated to 450~550 DEG C, be incubated 3~5h, naturally cool to room temperature, finally grind Mill obtains the titanium dioxide optical catalyst of adsorbent class carrier gama-alumina load.
The preparation method of a kind of carrier loaded titanium dioxide optical catalyst of adsorbent class the most as claimed in claim 1, its feature It is: described alcohol is ethanol, or isopropanol, or n-butyl alcohol, or propylene glycol;Described acid is hydrochloric acid, or nitric acid, or acetic acid, or grass Acid.
CN201610600665.5A 2016-07-28 2016-07-28 Preparation method of adsorbent carrier-loaded titanium dioxide photocatalyst Expired - Fee Related CN106215915B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108358613A (en) * 2018-01-31 2018-08-03 武汉理工大学 A kind of compound hot spray powder of alundum (Al2O3)/TiO 2 precursor and preparation method thereof
CN109364882A (en) * 2018-10-04 2019-02-22 南京航空航天大学溧水仿生产业研究院有限公司 Poriferous titanium dioxide material and preparation method thereof
CN112624165A (en) * 2020-12-15 2021-04-09 安徽壹石通材料科技股份有限公司 Preparation method of boehmite solution and electrolyte containing solution
CN113198430A (en) * 2021-05-15 2021-08-03 兰州城市学院 Preparation method of composite nano material
CN114523103A (en) * 2022-03-03 2022-05-24 浙江同擎科技有限公司 Ceramic particle reinforced titanium-based composite material for 3D printing and preparation method thereof

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EP0937764A1 (en) * 1998-02-24 1999-08-25 Washington Mills Electro Minerals Corporation Sol gel abrasive containing reduced titania and process for its preparation
CN102921474A (en) * 2012-10-30 2013-02-13 陕西高新能源发展有限公司 Preparation method of TiO2/Al2O3 composite carrier
CN103962118A (en) * 2014-05-17 2014-08-06 天津微能新材料有限公司 Preparation method of TiO2 photocatalyst mesh and TiO2 photocatalyst mesh

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EP0937764A1 (en) * 1998-02-24 1999-08-25 Washington Mills Electro Minerals Corporation Sol gel abrasive containing reduced titania and process for its preparation
CN102921474A (en) * 2012-10-30 2013-02-13 陕西高新能源发展有限公司 Preparation method of TiO2/Al2O3 composite carrier
CN103962118A (en) * 2014-05-17 2014-08-06 天津微能新材料有限公司 Preparation method of TiO2 photocatalyst mesh and TiO2 photocatalyst mesh

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108358613A (en) * 2018-01-31 2018-08-03 武汉理工大学 A kind of compound hot spray powder of alundum (Al2O3)/TiO 2 precursor and preparation method thereof
CN109364882A (en) * 2018-10-04 2019-02-22 南京航空航天大学溧水仿生产业研究院有限公司 Poriferous titanium dioxide material and preparation method thereof
CN112624165A (en) * 2020-12-15 2021-04-09 安徽壹石通材料科技股份有限公司 Preparation method of boehmite solution and electrolyte containing solution
CN112624165B (en) * 2020-12-15 2023-04-18 安徽壹石通材料科技股份有限公司 Preparation method of boehmite solution and electrolyte containing boehmite solution
CN113198430A (en) * 2021-05-15 2021-08-03 兰州城市学院 Preparation method of composite nano material
CN114523103A (en) * 2022-03-03 2022-05-24 浙江同擎科技有限公司 Ceramic particle reinforced titanium-based composite material for 3D printing and preparation method thereof
CN114523103B (en) * 2022-03-03 2023-11-07 浙江同擎科技有限公司 Ceramic particle reinforced titanium-based composite material for 3D printing and preparation method thereof

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