CN103100398A - Preparation method of natural zeolite loaded one-dimensional TiO2 nanowire with high catalytic activity - Google Patents
Preparation method of natural zeolite loaded one-dimensional TiO2 nanowire with high catalytic activity Download PDFInfo
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- CN103100398A CN103100398A CN2011103509575A CN201110350957A CN103100398A CN 103100398 A CN103100398 A CN 103100398A CN 2011103509575 A CN2011103509575 A CN 2011103509575A CN 201110350957 A CN201110350957 A CN 201110350957A CN 103100398 A CN103100398 A CN 103100398A
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Abstract
The invention belongs to the technical field of photocatalysis, and in particular to a preparation method of natural zeolite loaded one-dimensional TiO2 nanowire with high catalytic activity and related technological parameters. The preparation method is a sol-gel / hydrothermal synthesis method and comprises steps of: first preparing a TiO2 sol from a precursor butyl titanate (Ti (OC4H9) 4), a complexing agent diethanol amine and a solvent absolute ethyl ethanol; then, loading the TiO2 sol on acid treated natural zeolite by an immersion method, drying and calcining; and finally, placing the zeolite loaded with TiO2 in a NaOH aqueous solution, and conducting a hydrothermal reaction at a certain temperature; washing the obtained product with deionized water, and dipping the product in a dilute HCl solution for a while; and then washing, drying and calcining the obtained product to obtain a natural zeolite loaded one-dimensional nano TiO2 composite material. The invention also discusses influence of technological parameters including sol precursor concentration, TiO2 loading amount and calcination time on the structure and properties of the composite material, and acquires the optimum technological parameters for preparation of the natural zeolite loaded one-dimensional TiO2 nanowire with high catalytic activity.
Description
Technical field
The invention belongs to the photocatalysis technology field, be specially a kind of high catalytic activity natural zeolite load one dimension TiO for preparing
2The method of nano wire composite and related process parameter.
Technical background
Water is lifespring, is the necessary condition that life exists.Human lives, industrial production, agricultural irrigation etc. all be unable to do without water.Along with developing rapidly of modern economy, many mankind's activities make a large amount of industry, agricultural and domestic refuse enter in water, and water body is polluted.The pollution of water resource not only worsens whole earth ecology, returns human health and has consisted of huge harm.Therefore, water pollution control is subject to the attention of global range as the important topic of field of Environment Protection.And the existing main method that solves the water pollution, as: biological degradation method, active carbon adsorption, filtration, chemical oxidization method etc. can not fundamentally make pollutant innoxious.Just because of this, promoted the research of people to the method for novel improvement pollution.
Found TiO from Fujishima in 1972 and Houda
2Since can carrying out the discovery of light decomposition water on electrode, TiO
2Catalysis material is the focus of many scholar's research always.Nano-TiO
2Because surperficial photohole has very strong oxidability, energy is degradation of organic substances thoroughly, and the advantage such as have that chemical stability is good, specific area is large, nontoxic, photocatalytic activity is high, applicable pollutant is wide, cheap and easy to get and extremely people pay close attention to, the improvement that is widely used in polluting, particularly as the photocatalyst for degrading trade effluent, under the irradiation of ultraviolet light, can make the organic matter in sewage thoroughly be converted into CO in the short time
2, H
2O and other organic matter.
Nano-TiO
2The application of photochemical catalyst mainly contains two kinds of forms: floating type and support type.But common suspended phase photocatalytic method exists the easy inactivation of catalyst, reclaims the shortcomings such as difficult, that expense is high, and supported titanium
2Catalyst is easily separated, be convenient to reclaim, can repeat to be suitable for, and is one of focus of current conductor photocatalysis material area research.Loaded nano TiO
2The carrier that photochemical catalyst is commonly used has: clay, glass fibre, SiO
2, activated carbon, zeolite etc.
Although load TiO
2Carrier numerous, but experiment shows most of loaded nano TiO
2The simple nano-TiO of the specific activity of photochemical catalyst
2Particle has reduction in various degree.Zeolite is a kind of moisture frame shape structure, porous aluminum silicate mineral, have larger specific area, strong ion-exchange capacity and absorption property, can form semiconductor nano cluster stable, molecular dimension in its structure, thereby zeolite-loaded type photochemical catalyst demonstrates the work higher than other carrier.And the natural zeolite raw material sources are abundant, cheap, have the ion-exchange absorption performance not second to synthetic zeolite, are a kind of very promising carrier of photocatalyst.
Main Problems is at present: at traditional zeolite-loaded TiO
2In nano particle photocatalysis system, mainly come from suction-operated and the TiO of zeolite for organic degraded
2Photocatalysis, and zeolite surface load TiO
2After nano particle, the specific area of compound often reduces, and is unfavorable for organic absorption and degraded.And, studies show that, one-dimensional nano line (pipe) material specific area is high and be easy to the electron hole separation, demonstrates development prospect preferably in photocatalysis field.In order further to improve zeolite-loaded TiO
2The photocatalytic activity of nano composite material, the present invention is to adopt collosol and gel/hydrothermal synthesis method to prepare natural zeolite load one dimension TiO
2The nano wire composite takes full advantage of absorption property and the TiO of natural zeolite
2The specific area that nano wire is high and photocatalytic activity improve the catalytic performance of composite, and solve traditional nano-TiO
2Photochemical catalyst reclaims the problems such as difficult.
Summary of the invention
The object of the invention is to propose a kind of high catalytic activity natural zeolite load one dimension TiO
2Nano wire composite manufacture method and related process parameter.
A kind of suitable preparation natural zeolite load one dimension TiO
2The method of nano wire composite.This preparation method is collosol and gel/hydrothermal synthesis method.At first, with butyl titanate (Ti (OC
4H
9)
4) be presoma, diethanol amine is complexing agent, absolute ethyl alcohol is solvent, preparation TiO
2Colloidal sol; Then, adopt infusion process, at load TiO on acid-treated natural zeolite
2Colloidal sol, dry, calcining; At last, with load TiO
2Zeolite place in the NaOH aqueous solution, carry out at a certain temperature hydro-thermal reaction; Products therefrom washs and is placed in rare HCl solution and floods certain hour with deionized water; With products therefrom washing, oven dry, calcining, can obtain natural zeolite load 1-dimention nano TiO again
2Composite.
The mechanism of action of the present invention is: by sol gel process at zeolite surface load TiO
2Then utilize hydro-thermal reaction, make TiO
2With high concentration NaOH effect, generate sodium titanate; With zeolite/sodium titanate compound and rare HCl effect, replace sodium ion again; At last, products therefrom is fully washed, dries, calcines, can obtain natural zeolite load one dimension TiO
2The nano wire composite.Natural zeolite load one dimension TiO
2The nano wire composite can take full advantage of absorption property and the TiO of natural zeolite
2The specific area that nano wire is high and photocatalysis performance, and solve traditional nano-TiO
2Photochemical catalyst reclaims the problems such as difficult.
The present invention also proposes above-mentioned preparation method's related process parameter, and is specific as follows:
TiO
2In the colloidal sol configuration, the concentration of butyl titanate is 0.5～0.7 ± 0.02mol/L, and the mol ratio of diethanol amine and butyl titanate is 1: 1.In the acid treatment of natural zeolite, the concentration of HCl is 0.3mol/L, and bath temperature is 93 ℃ ± 2 ℃, and mixing time is 4h, and product is dry 12h under 110 ℃ ± 5 ℃, then 550 ± 5 ℃ of calcinings 4 hours.Natural zeolite loaded with nano TiO
2Preparation in, zeolite is put into TiO
2In colloidal sol, 70 ℃ ± 5 ℃ lower stirring in water bath, with load TiO
2Zeolite dry 12h under 90 ℃ ± 5 ℃, repeat aforesaid operations TiO of load again
2, with 2 TiO of load
2Zeolite 500 ℃ ± 5 ℃ heat treatments 2 hours.At natural zeolite load one dimension TiO
2In the nano wire composite manufacture, with zeolite-loaded nano-TiO
2Be scattered in the NaOH aqueous solution of 10mol/L ± 0.2mol/L, in 180 ℃ ± 5 ℃ lower hydro-thermal reaction 4h, with products therefrom deionized water centrifuge washing 5 times, the rare HCl solution that is placed in 0.1mol/L ± 0.02mol/L floods 8h, wash away excessive HCl with deionized water afterwards, use again absolute ethanol washing 5 times, products therefrom is dried under 60 ℃ ± 5 ℃, then 500 ℃ ± 5 ℃ heat treatments 3 hours.
Characteristics of the present invention:
1, take full advantage of absorption property and the TiO of natural zeolite
2The specific area that nano wire is high and photocatalysis performance improve the catalytic activity of composite, and solve traditional nano-TiO
2Photochemical catalyst reclaims the problems such as difficult.
2, collosol and gel/hydro-thermal synthesis process process is comparatively simple, is easy to realize, is convenient to control.
3, load TiO
2Colloidal sol is easy to control, and the composite photocatalytic activity is high.
4, can obtain natural zeolite load one dimension TiO
2Nano wire composite (nanowire diameter scope: 100nm ± 50nm's) improves its photocatalytic activity.
This preparation technology's using method is as follows:
1, typical TiO
2The technological parameter of colloidal sol preparation: the concentration of butyl titanate is 0.6mol/L, and the mol ratio of diethanol amine and butyl titanate is 1: 1, and the ratio of water and absolute ethyl alcohol is 1: 10, and anhydrous ethanol solvent is 50ml.
2, the technological parameter of the acid treatment technology of typical natural zeolite: concentration of hydrochloric acid is 0.3mol/L, 93 ℃ of bath temperatures, and mixing time 4h, baking temperature and time are 110 ℃/12h, final calcining heat is 550 ℃/4h.
3, typical natural zeolite loaded with nano TiO
2Technological parameter: 70 ℃ of bath temperatures, baking temperature and time are 90 ℃/12h, final calcining heat is 500 ℃/2h.
4, typical natural zeolite load one dimension TiO
2The technological parameter of nano wire composite: NaOH concentration is 10mol/L, 180 ℃ of hydrothermal temperatures, and time 4h, watery hydrochloric acid concentration is 0.1mol/L, and dip time is 8h, and baking temperature is 60 ℃, and final calcining heat is 500 ℃/3h.
5, TiO wherein
2The process parameters range of colloidal sol preparation: butyl titanate (Ti (OC
4H
9)
4) concentration be 0.5～0.7 ± 0.02mol/L, the mol ratio of diethanol amine and butyl titanate is 1: 1, the ratio of water and absolute ethyl alcohol is 1: 10.
6, the process parameters range of the acid treatment technology of natural zeolite wherein: 93 ℃ ± 2 ℃ of bath temperatures, mixing time 4h, baking temperature and time are 110 ℃ ± 5 ℃/12h, final calcining heat is 550 ℃ ± 5 ℃/4h.。
7, natural zeolite loaded with nano TiO wherein
2Process parameters range: 70 ℃ ± 5 ℃ of bath temperatures, baking temperature and time are 90 ℃ ± 5 ℃/12h, final calcining heat is 500 ℃ ± 5 ℃/2h.
8, natural zeolite load one dimension TiO wherein
2The process parameters range of nano wire composite: NaOH concentration is 10mol/L ± 0.2mol/L, 180 ℃ ± 5 ℃ of hydrothermal temperatures, time 4h, watery hydrochloric acid concentration is 0.1mol/L ± 0.02mol/L, dip time is 8h, baking temperature is 60 ℃ ± 5 ℃, and final calcining heat is 500 ℃ ± 5 ℃/3h.
The specific embodiment
The invention is further illustrated by the following examples.
Embodiment
TiO
2The preparation of colloidal sol, the concentration of butyl titanate are 0.6, and the mol ratio of diethanol amine and butyl titanate is 1: 1, and the ratio of water and absolute ethyl alcohol is 1: 10, and anhydrous ethanol solvent is 50ml.The acid treatment of natural zeolite, with deionized water with the natural zeolite cyclic washing, until upper strata liquid limpid till, the zeolite of cleaning is added in the hydrochloric acid of 0.3mol/L, stir 4h under 93 ℃ of water bath condition, with deionized water to washing to remove Cl through acid-treated zeolite
-, with gains dry 12h under 110 ℃, then 550 calcining 4 hours.Natural zeolite loaded with nano TiO
2Preparation is put into TiO with acid-treated zeolite
2In colloidal sol, 70 ℃ of lower stirring in water bath, to TiO
2Till colloidal sol becomes gel, with load TiO
2Zeolite dry 12h under 90 ℃, repeat aforesaid operations TiO of load again
2, with 2 TiO of load
2Zeolite 500 ℃ of heat treatments 2 hours.Natural zeolite load one dimension TiO
2The preparation of nano wire composite is with zeolite-loaded nano-TiO
2Be scattered in the NaOH aqueous solution of 10mol/L, in 180 ℃ of lower hydro-thermal reaction 4h, with products therefrom deionized water centrifuge washing 5 times, the rare HCl solution that is placed in 0.1mol/L floods 8h, wash away excessive HCl with deionized water afterwards, use again absolute ethanol washing 5 times, products therefrom is dried under 60 ℃, then 500 ℃ of heat treatments 3 hours.
Press the preceding method preparation.
Can get catalytic activity higher than zeolite, TiO
2Nano powder, zeolite/TiO
2The natural zeolite load one dimension TiO of nano particle
2Nano wire composite, wherein TiO
2The nanowire diameter scope is 100nm ± 50nm.
Claims (6)
1. one kind is fit to preparation high catalytic activity natural zeolite load one dimension TiO
2The method of nano wire composite.The method is collosol and gel/hydrothermal synthesis method.At first, with butyl titanate (Ti (OC
4H
9)
4) be presoma, diethanol amine is complexing agent, absolute ethyl alcohol is solvent, preparation TiO
2Colloidal sol; Then, adopt infusion process, at load TiO on acid-treated natural zeolite
2Colloidal sol, dry, calcining; At last, with load TiO
2Zeolite place in the NaOH aqueous solution, carry out at a certain temperature hydro-thermal reaction; Products therefrom washs and is placed in rare HCl solution and floods certain hour with deionized water; With products therefrom washing, oven dry, calcining, can obtain natural zeolite load one dimension TiO again
2The nano wire composite.
2. one kind to require 1 described TiO
2The preparation of colloidal sol.It is characterized in that detailed process and technological parameter are as follows: butyl titanate, diethanol amine are joined in ethanol solution, and the normal temperature lower magnetic force stirred 2 hours, then added a small amount of water and absolute ethyl alcohol mixture, continued to stir 2 hours, got TiO
2Colloidal sol.Under metatitanic acid, the concentration of ester is 0.5～0.7 ± 0.02mol/L, and the mol ratio of diethanol amine and butyl titanate is 1: 1.
3. one kind to require the acid treatment technology of 1 described natural zeolite.It is characterized in that detailed process and related process parameter are as follows: at first, with deionized water with the natural zeolite cyclic washing, until upper strata liquid limpid till; Then, the zeolite of cleaning is added in the hydrochloric acid of 0.3mol/L, stir 4h under 93 ℃ ± 2 ℃ water bath condition; At last, with deionized water to washing to remove Cl through acid-treated zeolite
-, with gains dry 12h under 110 ℃ ± 5 ℃, then 550 ± 5 ℃ of calcinings 4 hours.
4. one kind to require 1 described natural zeolite loaded with nano TiO
2Preparation.It is characterized in that detailed process and related process parameter are as follows: at first, acid-treated zeolite is put into TiO
2In colloidal sol, 70 ℃ ± 5 ℃ lower stirring in water bath, to TiO
2Till colloidal sol becomes gel, with load TiO
2Zeolite dry 12h under 90 ℃ ± 5 ℃; Then, repeat aforesaid operations TiO of load again
2At last, with 2 TiO of load
2Zeolite 500 ℃ ± 5 ℃ heat treatments 2 hours.
5. one kind to require 1 described natural zeolite load one dimension TiO
2The preparation of nano wire composite.It is characterized in that detailed process and related process parameter are as follows: at first, with zeolite-loaded nano-TiO
2Be scattered in the NaOH aqueous solution of 10mol/L ± 0.2mol/L, in 180 ℃ ± 5 ℃ lower hydro-thermal reaction 4h; Then, with deionized water centrifuge washing 5 times, the rare HCl solution that is placed in 0.1mol/L ± 0.02mol/L floods 8h with products therefrom, washes away excessive HCl with deionized water afterwards, then uses absolute ethanol washing 5 times; At last, products therefrom is dried under 60 ℃ ± 5 ℃, then 500 ℃ ± 5 ℃ heat treatments 3 hours.Get the natural zeolite load diameter of high catalytic activity at the one dimension TiO of 100nm ± 50nm
2The nano wire composite.
6. one kind to require 1 described preparation load one dimension TiO
2The nano wire composite is characterized in that TiO
2Be wrapped in carrier surface, form firmly TiO
2Layer, then change TiO by hydrothermal treatment consists
2Pattern forms carrier loaded one dimension TiO
2The nano wire composite.
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| CN103285861A (en) * | 2013-06-24 | 2013-09-11 | 大连民族学院 | An Ag3VO4/TiO2 compound nano-wire having visible light activity, a preparation method and applications thereof |
| CN103990795A (en) * | 2014-05-30 | 2014-08-20 | 南开大学 | Ni-Ni2O3 nano composite material and preparation |
| CN104399457A (en) * | 2014-12-26 | 2015-03-11 | 中国科学院广州地球化学研究所 | Au/TiO2/CFP (carbon fiber paper) ternary composite nano photocatalyst as well as preparation method and application thereof |
| CN104998678A (en) * | 2015-06-03 | 2015-10-28 | 河南师范大学 | Supported natural zeolite/NiFe2O4/Bi2O2CO3 photocatalyst and preparation method thereof |
| CN105032479A (en) * | 2015-08-06 | 2015-11-11 | 丁德凤 | Preparation method of TiO2 photocatalyst |
| CN106629988A (en) * | 2016-10-07 | 2017-05-10 | 玉灵华科技有限公司 | Preparation and activation methods of quantum carbon light medium and sewage treatment method |
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| CN109865509A (en) * | 2017-12-04 | 2019-06-11 | 天津发洋环保科技有限公司 | A kind of preparation method of nano titania photocatalyst |
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| CN1861252A (en) * | 2006-05-22 | 2006-11-15 | 苏州科技学院 | Zeolite based nano-titanium dioxide double function material and its prepn. method |
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Patent Citations (2)
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| CN1724145A (en) * | 2005-06-30 | 2006-01-25 | 复旦大学 | Nano Titanium dioxide/fluorite photocataly tic material and preparation process thereof |
| CN1861252A (en) * | 2006-05-22 | 2006-11-15 | 苏州科技学院 | Zeolite based nano-titanium dioxide double function material and its prepn. method |
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| CN103285861A (en) * | 2013-06-24 | 2013-09-11 | 大连民族学院 | An Ag3VO4/TiO2 compound nano-wire having visible light activity, a preparation method and applications thereof |
| CN103990795A (en) * | 2014-05-30 | 2014-08-20 | 南开大学 | Ni-Ni2O3 nano composite material and preparation |
| CN104399457A (en) * | 2014-12-26 | 2015-03-11 | 中国科学院广州地球化学研究所 | Au/TiO2/CFP (carbon fiber paper) ternary composite nano photocatalyst as well as preparation method and application thereof |
| CN104998678A (en) * | 2015-06-03 | 2015-10-28 | 河南师范大学 | Supported natural zeolite/NiFe2O4/Bi2O2CO3 photocatalyst and preparation method thereof |
| CN105032479A (en) * | 2015-08-06 | 2015-11-11 | 丁德凤 | Preparation method of TiO2 photocatalyst |
| CN106629988A (en) * | 2016-10-07 | 2017-05-10 | 玉灵华科技有限公司 | Preparation and activation methods of quantum carbon light medium and sewage treatment method |
| CN106629988B (en) * | 2016-10-07 | 2019-07-26 | 玉灵华科技有限公司 | A kind of preparation, activation and the sewage water treatment method of quantum carbon element optical medium |
| CN109865509A (en) * | 2017-12-04 | 2019-06-11 | 天津发洋环保科技有限公司 | A kind of preparation method of nano titania photocatalyst |
| CN108760857A (en) * | 2018-06-01 | 2018-11-06 | 徐州医科大学 | A kind of titanium dioxide nanofiber enzyme electrode of decorated by nano-gold and its preparation method and application |
| CN108786784A (en) * | 2018-06-15 | 2018-11-13 | 南京中科水治理股份有限公司 | A kind of preparation method of photocatalytic degradation composite material |
| CN108753236A (en) * | 2018-06-22 | 2018-11-06 | 安徽索亚装饰材料有限公司 | A method of improving polyurethane hot melt adhesion strength |
| CN110026170A (en) * | 2019-05-23 | 2019-07-19 | 乐山师范学院 | A kind of TiO of photocatalytic degradation rhodamine B2Photochemical catalyst and preparation method thereof |
| CN110026170B (en) * | 2019-05-23 | 2022-07-08 | 乐山师范学院 | TiO for degrading rhodamine B through photocatalysis2Photocatalyst and preparation method thereof |
| CN112717993A (en) * | 2020-11-23 | 2021-04-30 | 中国矿业大学(北京) | Manganese-titanium composite modified zeolite, and preparation method and application thereof |
| CN116655048A (en) * | 2023-07-17 | 2023-08-29 | 重庆工商大学 | Special wet porous material fixed bed photocatalysis water treatment reactor |
| CN116655048B (en) * | 2023-07-17 | 2024-01-16 | 重庆工商大学 | Special wet porous material fixed bed photocatalysis water treatment reactor |
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