CN102626614A - Preparation method of photocatalytic photoconductive material - Google Patents
Preparation method of photocatalytic photoconductive material Download PDFInfo
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- CN102626614A CN102626614A CN2012100762542A CN201210076254A CN102626614A CN 102626614 A CN102626614 A CN 102626614A CN 2012100762542 A CN2012100762542 A CN 2012100762542A CN 201210076254 A CN201210076254 A CN 201210076254A CN 102626614 A CN102626614 A CN 102626614A
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Abstract
A preparation method of a photocatalytic photoconductive material is disclosed. A sol-gel method is adopted to prepare neodymium-doped nanometer TiO2 to enlarge the light response range of the neodymium-doped nanometer TiO2. The photoconductive material with photocatalytic performances is prepared by using high silica optical fibers as a carrier, and adopting a method combining vacuum dipping with sol-gel to coat modified nanometer TiO2 on surfaces of the high silica optical fibers. The immobilization of the nanometer TiO2 is realized, so problems of difficult separation and recovery, generation of secondary pollution and the like existing in the use process of a powdery photocatalyst are solved; the high silica fibers have high specific surface areas, so the amount for loading the nanometer TiO2 is substantially improved; and the photoconductive performances of the carrier material high silica fibers can furthest utilize the initiation capability of light to the catalyst, so the photocatalytic performances of the nanometer TiO2 are improved.
Description
Technical field
The present invention relates to belong to field of materials, be specifically related to a kind of preparation method of photocatalyst-type light-guide material of load neodymium-doped nano titanium oxide.
Background technology
The photocatalysis material of titanium dioxide prospect that has a very wide range of applications at the aspects such as processing of air cleaning, drinking water disinfection and industrial waste, thereby caused the generally attention of countries in the world government and scientists.But its Powdered photochemical catalyst in use exists and separates and recovery difficulty and generation secondary pollution problems, thereby film photocatalyst becomes a new research focus gradually.Usually technique for fixing exists influence catalytic activity, it is few and be prone to come off and shortcoming such as light utilization efficiency is low to be fixed on the supported catalyst amount, so prepares the nano-TiO with high catalytic activity
2And technique for fixing has become nano-TiO
2An importance of catalysis material research is the key of its practicability.
" Chinese patent 200610048742.7 " announced a kind of preparation method of glass fiber loaded optic catalyst, belongs to photocatalysis technology.Have that method is easy, the catalyst difficult drop-off of load, photocatalytic activity advantages of higher, be applicable to that the light catalytic purifying of organic pollution, foul smell etc. in the air is handled.
" Chinese patent 200710173058.6 " announced a kind of titanium dioxide optical catalyst with visible light photocatalysis active.Have the quantum yield of higher optically catalytic TiO 2 reaction and more wide in range photophase scope (i.e. " red shift "), lay a good foundation for the optically catalytic TiO 2 technology gets into the practicality stage.
" Chinese patent 200510064453 " announced a kind of nanometer titanium dioxide coating liquid and preparation method thereof, and this coating liquid is a kind of water-soluble coating liquid, includes the TiO of particle diameter less than 20nm
2Particle and the inorganic aqueous dispersant that sticks, the strong film that can form at various substrate surfaces, multiple use such as can be used for antibiosis and self-cleaning and eliminate the unusual smell.
" Chinese patent 201010115236 " announced a kind of preparation method of tungsten-doped anatase type nano titanium dioxide composite powder, adopts sol-gel and hydro-thermal method to combine to obtain tungsten-doped anatase type nano titanium dioxide composite powder.Have that cost is low, purity is high, technology is simple and powder has the characteristics of high visible photocatalytic activity.
" Chinese patent 200510095107 " announced a kind of preparation method of diffuse fiber supported nanometer photocatalytic titania film; It is characterized in that getting the dispersion fiber that surrounding layer is a silicon rubber; At its surface-coated silicon dioxide film; The dispersion fiber that will be coated with silicon dioxide film again places TiO 2 sol to flood 10～60 minutes; Carry film with the speed of 1～50 mm/min then, at last 100～200 ℃ keep 0.5～2 hour can be on diffuse fiber supported nanometer photocatalytic titania film.This method is simple, cost is low, quality of forming film is high.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with photocatalyst-type light-guide material of high efficiency photocatalysis property and high capacity amount.
For achieving the above object, the technical scheme that the present invention adopts is:
1) the former liquid that drives of preparation
By volume with the diethanol amine of 16%～23% butyl titanate and 4%～7% join fully mix in 70%～80% the absolute ethyl alcohol mixed solution; The neodymium nitrate that in mixed solution, adds mixed solution quality 1%～3% again, fully stir then the former liquid that drives;
2) preparation dropping liquid
By volume 8%～15% water is joined in 85%～92% the absolute ethyl alcohol, be stirred to abundant mixing and obtain dropping liquid;
3) preparation nano-TiO
2Colloidal sol
Under strong agitation, splash into dropping liquid in the liquid to former driving, continue powerful the stirring and make transparent nano TiO
2Colloidal sol, wherein the percent by volume of dropping liquid is 8～10%;
4) surface treatment
High silica optical fiber is carried out ultrasonic cleaning, and oven dry is immersed it in strong base solution again, carries out ultrasonic cleaning afterwards again, oven dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed nano-TiO
2In the colloidal sol, vacuum impregnation and oven dry place muffle furnace with 450～600 ℃ of temperature calcinings 6～8 hours the high silica optical fiber after the oven dry, obtain the high silica optical fiber of load neodymium-doped nano titanium oxide.
Described water is deionized water or distilled water.
The present invention is carrier with the high silica fiber, and the nano titanium oxide of doping neodymium is carried on the high silica fiber surface, processes a kind of light-guide material with high efficiency photocatalysis property and high capacity amount.This material has the efficient energy-saving double effects.It is in order to improve the photocatalysis performance of nano TiO 2, to widen the photoresponse scope of nano TiO 2 that rare earth metal neodymium is doped in the nano TiO 2 system; Select for use high silica optical fiber as carrier material; Realized the fixing of nano TiO 2 on the one hand, main is to want to utilize the fibre-optic photoconductive property of high silica, with the light source of excitation nano TiO2 photocatalysis performance; Can import by high silica optical fiber; And, the nano TiO 2 that is coated on fiber surface is fully contacted with light, thereby farthest bring into play the photocatalysis performance of nano TiO 2 along its conduction.
High silica optical fiber is a kind ofly to close at luminous energy in the fiber, produces the optical composite material of leaded light effect.It utilizes the electromagnetic wave energy that the form with light occurs the principle of total reflection to constrain in its interface, and guides light wave to advance along the direction of shaft axis of optic fibre, and the transmission characteristic of optical fiber is by its structure and material decision.Its photoconductive property can farthest be utilized the initiating power of light to catalyst, thereby improves the photocatalysis performance of its catalyst supported on surface.High silica optical fiber has good printing opacity gas permeability, big specific area, high temperature resistant processing, anticorrosive, structure and stable performance, to advantages such as human body are safe from harm, be desirable catalyst carrier material.And, improved carry the apply amount of catalyst greatly on its surface as carrier because he has bigger specific area, solved catalyst and uploaded the little difficult problem of the amount of applying at carrier.
The photocatalysis characteristic of nano titanium oxide makes it have using value potential or reality in environmental protection fields such as wastewater treatment, air cleaning, water oil stain processing, kill bacteria.The neodymium ion doped inhibition titanium dioxide of rare earth element crystalline phase is changed to rutile by anatase mutually; Because rear earth element nd has the 4f track and empty 5d track that not exclusively occupies; Having the ion that is full of entirely or partly is full of electron configuration can make the electronics of catching discharge easily; Thereby prolong the life-span in light induced electron-hole, thereby improved TiO
2Photocatalytic activity.
The present invention has adopted high silica optical fiber to come the nano titanium oxide of carried with doped neodymium.The doping neodymium ion can change TiO
2The charge density distribution of crystal forms lattice defect or changes lattice types, thus influence light induced electron-hole moving situation, adjust its distribution or change its band structure, finally improve nano-TiO
2Photocatalysis performance.Utilize the fibre-optic photoconductive property of high silica, ultraviolet ray can penetrate nano-titanium dioxide film fully, makes it carry out zero-decrement absorption to ultraviolet ray, and high silica fiber has higher specific surface area, can improve the load capacity of neodymium-doped nano titanium oxide.Therefore adopting high silica fiber is carrier, has not only made the photocatalysis performance of titanium dioxide farthest be initiated but also improve the photocatalysis utilization rate of its surface titanium dioxide.
Description of drawings
Fig. 1, the 2nd, the fibre-optic SEM photo of the photocatalyst-type that the present invention prepares.
The specific embodiment
Below in conjunction with specific embodiment the present invention is further specified
Embodiment 1:
1) the former liquid that drives of preparation
By volume with the diethanol amine of 16% butyl titanate and 5% join fully mix in 79% the absolute ethyl alcohol mixed solution, in mixed solution, add the neodymium nitrate of mixed solution quality 1% again, fully stir then the former liquid that drives;
2) preparation dropping liquid
By volume 8% distilled water is joined in 92% the absolute ethyl alcohol, be stirred to fully mix dropping liquid;
3) preparation nano-TiO
2Colloidal sol
Under vigorous stirring, splash into dropping liquid in the liquid to former driving, continue powerful the stirring and make transparent nano TiO
2Colloidal sol, wherein the percent by volume of dropping liquid is 9%;
4) surface treatment
High silica optical fiber is carried out ultrasonic cleaning, and oven dry is immersed it in strong base solution again, carries out ultrasonic cleaning afterwards again, oven dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed nano-TiO
2In the colloidal sol, vacuum impregnation and oven dry place muffle furnace with 450 ℃ of temperature calcinings 8 hours the high silica optical fiber after the oven dry, obtain the high silica optical fiber (referring to Fig. 1,2) of load neodymium-doped nano titanium oxide.
Embodiment 2:
1) the former liquid that drives of preparation
By volume with the diethanol amine of 20% butyl titanate and 4% join fully mix in 76% the absolute ethyl alcohol mixed solution, in mixed solution, add the neodymium nitrate of mixed solution quality 2% again, fully stir then the former liquid that drives;
2) preparation dropping liquid
By volume 15% distilled water is joined in 85% the absolute ethyl alcohol, be stirred to fully mix dropping liquid;
3) preparation nano-TiO
2Colloidal sol
Under vigorous stirring, splash into dropping liquid in the liquid to former driving, continue powerful the stirring and make transparent nano TiO
2Colloidal sol, wherein the percent by volume of dropping liquid is 10%;
4) surface treatment
High silica optical fiber is carried out ultrasonic cleaning, and oven dry is immersed it in strong base solution again, carries out ultrasonic cleaning afterwards again, oven dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed nano-TiO
2In the colloidal sol, vacuum impregnation and oven dry place muffle furnace with 500 ℃ of temperature calcinings 7.5 hours the high silica optical fiber after the oven dry, obtain the high silica optical fiber of load neodymium-doped nano titanium oxide.
Embodiment 3:
1) the former liquid that drives of preparation
By volume with the diethanol amine of 22% butyl titanate and 6% join fully mix in 72% the absolute ethyl alcohol mixed solution, in mixed solution, add the neodymium nitrate of mixed solution quality 3% again, fully stir then the former liquid that drives;
2) preparation dropping liquid
By volume 10% distilled water is joined in 90% the absolute ethyl alcohol, be stirred to fully mix dropping liquid;
3) preparation nano-TiO
2Colloidal sol
Under vigorous stirring, splash into dropping liquid in the liquid to former driving, continue powerful the stirring and make transparent nano TiO
2Colloidal sol, wherein the percent by volume of dropping liquid is 8%;
4) surface treatment
High silica optical fiber is carried out ultrasonic cleaning, and oven dry is immersed it in strong base solution again, carries out ultrasonic cleaning afterwards again, oven dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed nano-TiO
2In the colloidal sol, vacuum impregnation and oven dry place muffle furnace with 550 ℃ of temperature calcinings 7 hours the high silica optical fiber after the oven dry, obtain the high silica optical fiber of load neodymium-doped nano titanium oxide.
Embodiment 4:
1) the former liquid that drives of preparation
By volume with the diethanol amine of 23% butyl titanate and 7% join fully mix in 70% the absolute ethyl alcohol mixed solution, in mixed solution, add the neodymium nitrate of mixed solution quality 1.5% again, fully stir then the former liquid that drives;
2) preparation dropping liquid
By volume 12% distilled water is joined in 88% the absolute ethyl alcohol, be stirred to fully mix dropping liquid;
3) preparation nano-TiO
2Colloidal sol
Under vigorous stirring, splash into dropping liquid in the liquid to former driving, continue powerful the stirring and make transparent nano TiO
2Colloidal sol, wherein the percent by volume of dropping liquid is 9.5%;
4) surface treatment
High silica optical fiber is carried out ultrasonic cleaning, and oven dry is immersed it in strong base solution again, carries out ultrasonic cleaning afterwards again, oven dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed nano-TiO
2In the colloidal sol, vacuum impregnation and oven dry place muffle furnace with 600 ℃ of temperature calcinings 6 hours the high silica optical fiber after the oven dry, obtain the high silica optical fiber of load neodymium-doped nano titanium oxide.
Embodiment 5:
1) the former liquid that drives of preparation
By volume with the diethanol amine of 16% butyl titanate and 4% join fully mix in 80% the absolute ethyl alcohol mixed solution, in mixed solution, add the neodymium nitrate of mixed solution quality 2.5% again, fully stir then the former liquid that drives;
2) preparation dropping liquid
By volume 13% distilled water is joined in 86% the absolute ethyl alcohol, be stirred to fully mix dropping liquid;
3) preparation nano-TiO
2Colloidal sol
Under vigorous stirring, splash into dropping liquid in the liquid to former driving, continue powerful the stirring and make transparent nano TiO
2Colloidal sol, wherein the percent by volume of dropping liquid is 8.5%;
4) surface treatment
High silica optical fiber is carried out ultrasonic cleaning, and oven dry is immersed it in strong base solution again, carries out ultrasonic cleaning afterwards again, oven dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed nano-TiO
2In the colloidal sol, vacuum impregnation and oven dry place muffle furnace with 570 ℃ of temperature calcinings 6.5 hours the high silica optical fiber after the oven dry, obtain the high silica optical fiber of load neodymium-doped nano titanium oxide.
The high silica optical fiber of prepared load neodymium-doped nano titanium oxide has not only been realized nano-TiO
2Immobilization, solved Powdered photochemical catalyst and in use existed and separate and reclaim difficulty and produce secondary pollution problems; Also, therefore improved nano-TiO greatly because the high silica fiber of being selected for use has higher specific surface area
2The amount of carry applying; Because the photoconduction performance of carrier material high silica fiber is farthest utilized the initiating power of light to catalyst, thereby improve nano-TiO
2Photocatalysis performance.The photocatalysis performance methyl orange of taking to degrade is tested, with the high silica optical fiber and the loaded with nano TiO of load neodymium-doped nano titanium oxide
2Glass slide, put into the methyl orange solution of 50ml concentration 20mg/L, separate behind the ultra violet lamp 2h and survey its absorbance, calculate both degradation rates to methyl orange, the result finds that the former has higher degradation capability to methyl orange, has improved 30% than the latter.
Claims (2)
1. the preparation method of a photocatalyst-type light-guide material is characterized in that may further comprise the steps:
1) the former liquid that drives of preparation
By volume with the diethanol amine of 16%～23% butyl titanate and 4%～7% join fully mix in 70%～80% the absolute ethyl alcohol mixed solution; The neodymium nitrate that in mixed solution, adds mixed solution quality 1%～3% again, fully stir then the former liquid that drives;
2) preparation dropping liquid
By volume 8%～15% water is joined in 85%～92% the absolute ethyl alcohol, be stirred to fully mix dropping liquid;
3) preparation nano-TiO
2Colloidal sol
Under vigorous stirring, splash into dropping liquid in the liquid to former driving, continue powerful the stirring and make transparent nano TiO
2Colloidal sol, wherein the percent by volume of dropping liquid is 8～10%;
4) surface treatment
High silica optical fiber is carried out ultrasonic cleaning, and oven dry is immersed it in strong base solution again, carries out ultrasonic cleaning afterwards again, oven dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed nano-TiO
2In the colloidal sol, vacuum impregnation and oven dry place muffle furnace with 450～600 ℃ of temperature calcinings 6～8 hours the high silica optical fiber after the oven dry, obtain the high silica optical fiber of load neodymium-doped nano titanium oxide.
2. the preparation method of photocatalyst-type light-guide material according to claim 1 is characterized in that: described water is deionized water or distilled water.
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Cited By (7)
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| CN102895972A (en) * | 2012-10-17 | 2013-01-30 | 陕西科技大学 | Method for preparing negative ion material used for organic pollutant and sewage treatment and having photo-catalysis performance |
| CN107597164A (en) * | 2017-09-14 | 2018-01-19 | 重庆理工大学 | Photovoltaic/thermal changes the visible light catalytic optical fiber and preparation method with transmitting |
| CN108441098A (en) * | 2018-03-30 | 2018-08-24 | 天长市巨龙车船涂料有限公司 | A kind of antibacterial and mouldproof aqueous polyurethane coating |
| CN109496962A (en) * | 2018-12-18 | 2019-03-22 | 江苏省淡水水产研究所 | A kind of ornamental fish water circulating filter cultivating system |
| CN110280231A (en) * | 2019-08-01 | 2019-09-27 | 山东大学 | A kind of secondary structure TiO2Optical fiber catalysis material of load and the preparation method and application thereof |
| CN112592508A (en) * | 2019-10-01 | 2021-04-02 | 香港科技大学 | Method for producing optical fiber |
| CN112774729A (en) * | 2021-01-29 | 2021-05-11 | 西北工业大学 | Method for 3D printing of high-strength continuous flow photocatalytic system |
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| CN101181678A (en) * | 2007-10-26 | 2008-05-21 | 广东省生态环境与土壤研究所 | Rare earth modified photocatalyst as well as degradable plastic film prepared thereby and preparation method thereof |
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| WO2004002907A1 (en) * | 2002-06-28 | 2004-01-08 | Liekki Oy | A method for the preparation of doped oxide material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102895972A (en) * | 2012-10-17 | 2013-01-30 | 陕西科技大学 | Method for preparing negative ion material used for organic pollutant and sewage treatment and having photo-catalysis performance |
| CN107597164A (en) * | 2017-09-14 | 2018-01-19 | 重庆理工大学 | Photovoltaic/thermal changes the visible light catalytic optical fiber and preparation method with transmitting |
| CN107597164B (en) * | 2017-09-14 | 2020-05-15 | 重庆理工大学 | Visible light catalytic optical fiber for photoelectric and photothermal conversion and transfer and manufacturing method thereof |
| CN108441098A (en) * | 2018-03-30 | 2018-08-24 | 天长市巨龙车船涂料有限公司 | A kind of antibacterial and mouldproof aqueous polyurethane coating |
| CN109496962A (en) * | 2018-12-18 | 2019-03-22 | 江苏省淡水水产研究所 | A kind of ornamental fish water circulating filter cultivating system |
| CN110280231A (en) * | 2019-08-01 | 2019-09-27 | 山东大学 | A kind of secondary structure TiO2Optical fiber catalysis material of load and the preparation method and application thereof |
| CN110280231B (en) * | 2019-08-01 | 2022-01-21 | 山东大学 | TiO with secondary structure2Loaded optical fiber photocatalytic material and preparation method and application thereof |
| CN112592508A (en) * | 2019-10-01 | 2021-04-02 | 香港科技大学 | Method for producing optical fiber |
| CN112592508B (en) * | 2019-10-01 | 2022-09-20 | 香港科技大学 | Method for producing optical fiber |
| CN112774729A (en) * | 2021-01-29 | 2021-05-11 | 西北工业大学 | Method for 3D printing of high-strength continuous flow photocatalytic system |
| CN112774729B (en) * | 2021-01-29 | 2023-12-22 | 西北工业大学 | Method for 3D printing of high-strength continuous flow photocatalytic system |
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