CN102626614B - Preparation method of photocatalytic photoconductive material - Google Patents
Preparation method of photocatalytic photoconductive material Download PDFInfo
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- CN102626614B CN102626614B CN 201210076254 CN201210076254A CN102626614B CN 102626614 B CN102626614 B CN 102626614B CN 201210076254 CN201210076254 CN 201210076254 CN 201210076254 A CN201210076254 A CN 201210076254A CN 102626614 B CN102626614 B CN 102626614B
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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 Material Field, 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 reclaim difficulty and produce secondary pollution problems, thereby film photocatalyst becomes a new study hotspot gradually.Usually technique for fixing exists affect catalytic activity, it is few and easily come off and the 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 its practical key.
" 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, the light catalytic purifying that is applicable to organic pollution, foul smell etc. in air is processed.
" Chinese patent 200710173058.6 " announced a kind of titanium dioxide optical catalyst with visible light photocatalysis active.There is 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 enters the practicality stage.
" Chinese patent 200510064453 " announced a kind of nanometer titanium dioxide coating liquid and preparation method thereof, and this coating solution is a kind of water-soluble coating liquid, includes the TiO that particle diameter is less than 20nm
2particle and the inorganic aqueous dispersant that sticks, the strong film that can form at various substrate surfaces, the 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 in conjunction with obtaining tungsten-doped anatase type nano titanium dioxide composite powder.Have that cost is low, purity is high, technique 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 silicon rubber, at its surperficial coating silicon dioxide film, the dispersion fiber that will be coated with again silicon dioxide film is placed in TiO 2 sol and floods 10～60 minutes, then carry film with the speed of 1～50 mm/min, finally 100～200 ℃ keep 0.5～2 hour can be on diffuse fiber supported nanometer photocatalytic titania film.The 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 and high capacity amount.
For achieving the above object, the technical solution used in the present invention is:
1) prepare the former liquid that drives
By volume the diethanol amine of 16%～23% butyl titanate and 4%～7% is joined in 70%～80% absolute ethyl alcohol and fully be mixed to get mixed solution, to the neodymium nitrate that adds mixed solution quality 1%～3% in mixed solution, then fully stir to obtain the former liquid that drives again;
2) preparation dropping liquid
By volume 8%～15% water is joined in 85%～92% absolute ethyl alcohol, be stirred to and fully be mixed to get dropping liquid;
3) prepare nano-TiO
2colloidal sol
Under strong agitation, splash into dropping liquid to former driving in liquid, continue strong 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 to ultrasonic cleaning, dry, then it is immersed in strong base solution, carry out again afterwards ultrasonic cleaning, dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed to nano-TiO
2in colloidal sol, vacuum impregnation is also dried, and the high silica optical fiber after drying is placed in to muffle furnace with 450～600 ℃ of temperature calcinings 6～8 hours, obtains the high silica optical fiber of load neodymium-doped nano titanium oxide.
Described water is deionized water or distilled water.
The present invention be take high silica fiber as carrier, and the nano titanium oxide of doping neodymium is carried on to the high silica fiber surface, makes a kind of light-guide material with high efficiency photocatalysis 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 that rare earth metal neodymium is doped in the nano TiO 2 system, widens the photoresponse scope of nano TiO 2; Select high silica optical fiber as carrier material, realized on the one hand the fixing of nano TiO 2, main is to want to utilize the fibre-optic photoconductive property of high silica, light source by excitation nano TiO2 photocatalysis performance, can be imported by high silica optical fiber, and, along its conduction, can make like this nano TiO 2 that is coated on fiber surface fully contact with light, thereby farthest bring into play the photocatalysis performance of nano TiO 2.
High silica optical fiber is a kind of luminous energy to be closed in fiber, produces the optical composite material of leaded light effect.The electromagnetic wave energy that it form with light occurs utilizes 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 determined by its structure and material.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 light transmission ventilation, large 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, because he has larger specific area, as carrier, greatly improved carry the apply amount of catalyst on its surface, solved catalyst and uploaded at carrier the difficult problem that the amount of applying is little.
The photocatalysis characteristic of nano titanium oxide makes it at field of Environment Protections such as wastewater treatment, air cleaning, water oil stain processing, kill bacteria, have using value potential or reality.The neodymium ion doped inhibition titanium dioxide of rare earth element crystalline phase is changed to Rutile Type by anatase, because rear earth element nd has the 4f track that not exclusively occupies and empty 5d track, having the ion that entirely is full of or partly is full of electron configuration can make the electronics of catching easily discharge, thereby extend the life-span in light induced electron-hole, thereby improved TiO
2photocatalytic activity.
The present invention has adopted high silica optical fiber to carry out the nano titanium oxide of carried with doped neodymium.The doping neodymium ion can change TiO
2the charge density distribution of crystal, form lattice defect or change lattice types, thus affect 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 to ultraviolet ray, carry out zero-decrement absorption, and high silica fiber has higher specific 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.
The accompanying drawing explanation
Fig. 1, the 2nd, the fibre-optic SEM photo of photocatalyst-type prepared by the present invention.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is further described
Embodiment 1:
1) prepare the former liquid that drives
By volume the diethanol amine of 16% butyl titanate and 5% is joined in 79% absolute ethyl alcohol and fully be mixed to get mixed solution, then, to the neodymium nitrate that adds mixed solution quality 1% in mixed solution, then fully stir to obtain the former liquid that drives;
2) preparation dropping liquid
By volume 8% distilled water is joined in 92% absolute ethyl alcohol, be stirred to and fully be mixed to get dropping liquid;
3) prepare nano-TiO
2colloidal sol
Under vigorous stirring, splash into dropping liquid to former driving in liquid, continue strong 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 to ultrasonic cleaning, dry, then it is immersed in strong base solution, carry out again afterwards ultrasonic cleaning, dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed to nano-TiO
2in colloidal sol, vacuum impregnation is also dried, and the high silica optical fiber after drying is placed in to muffle furnace with 450 ℃ of temperature calcinings 8 hours, obtains the high silica optical fiber (referring to Fig. 1,2) of load neodymium-doped nano titanium oxide.
Embodiment 2:
1) prepare the former liquid that drives
By volume the diethanol amine of 20% butyl titanate and 4% is joined in 76% absolute ethyl alcohol and fully be mixed to get mixed solution, then, to the neodymium nitrate that adds mixed solution quality 2% in mixed solution, then fully stir to obtain the former liquid that drives;
2) preparation dropping liquid
By volume 15% distilled water is joined in 85% absolute ethyl alcohol, be stirred to and fully be mixed to get dropping liquid;
3) prepare nano-TiO
2colloidal sol
Under vigorous stirring, splash into dropping liquid to former driving in liquid, continue strong 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 to ultrasonic cleaning, dry, then it is immersed in strong base solution, carry out again afterwards ultrasonic cleaning, dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed to nano-TiO
2in colloidal sol, vacuum impregnation is also dried, and the high silica optical fiber after drying is placed in to muffle furnace with 500 ℃ of temperature calcinings 7.5 hours, obtains the high silica optical fiber of load neodymium-doped nano titanium oxide.
Embodiment 3:
1) prepare the former liquid that drives
By volume the diethanol amine of 22% butyl titanate and 6% is joined in 72% absolute ethyl alcohol and fully be mixed to get mixed solution, then, to the neodymium nitrate that adds mixed solution quality 3% in mixed solution, then fully stir to obtain the former liquid that drives;
2) preparation dropping liquid
By volume 10% distilled water is joined in 90% absolute ethyl alcohol, be stirred to and fully be mixed to get dropping liquid;
3) prepare nano-TiO
2colloidal sol
Under vigorous stirring, splash into dropping liquid to former driving in liquid, continue strong 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 to ultrasonic cleaning, dry, then it is immersed in strong base solution, carry out again afterwards ultrasonic cleaning, dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed to nano-TiO
2in colloidal sol, vacuum impregnation is also dried, and the high silica optical fiber after drying is placed in to muffle furnace with 550 ℃ of temperature calcinings 7 hours, obtains the high silica optical fiber of load neodymium-doped nano titanium oxide.
Embodiment 4:
1) prepare the former liquid that drives
By volume the diethanol amine of 23% butyl titanate and 7% is joined in 70% absolute ethyl alcohol and fully be mixed to get mixed solution, then, to the neodymium nitrate that adds mixed solution quality 1.5% in mixed solution, then fully stir to obtain the former liquid that drives;
2) preparation dropping liquid
By volume 12% distilled water is joined in 88% absolute ethyl alcohol, be stirred to and fully be mixed to get dropping liquid;
3) prepare nano-TiO
2colloidal sol
Under vigorous stirring, splash into dropping liquid to former driving in liquid, continue strong 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 to ultrasonic cleaning, dry, then it is immersed in strong base solution, carry out again afterwards ultrasonic cleaning, dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed to nano-TiO
2in colloidal sol, vacuum impregnation is also dried, and the high silica optical fiber after drying is placed in to muffle furnace with 600 ℃ of temperature calcinings 6 hours, obtains the high silica optical fiber of load neodymium-doped nano titanium oxide.
Embodiment 5:
1) prepare the former liquid that drives
By volume the diethanol amine of 16% butyl titanate and 4% is joined in 80% absolute ethyl alcohol and fully be mixed to get mixed solution, then, to the neodymium nitrate that adds mixed solution quality 2.5% in mixed solution, then fully stir to obtain the former liquid that drives;
2) preparation dropping liquid
By volume 13% distilled water is joined in 86% absolute ethyl alcohol, be stirred to and fully be mixed to get dropping liquid;
3) prepare nano-TiO
2colloidal sol
Under vigorous stirring, splash into dropping liquid to former driving in liquid, continue strong 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 to ultrasonic cleaning, dry, then it is immersed in strong base solution, carry out again afterwards ultrasonic cleaning, dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed to nano-TiO
2in colloidal sol, vacuum impregnation is also dried, and the high silica optical fiber after drying is placed in to muffle furnace with 570 ℃ of temperature calcinings 6.5 hours, obtains 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, because selected high silica fiber has higher specific area, therefore greatly improved nano-TiO
2the amount of carry applying; Due to the photoconduction performance of carrier material high silica fiber, farthest utilize the initiating power of light to catalyst, thereby improve nano-TiO
2photocatalysis performance.The photocatalysis performance methyl orange of taking to degrade is tested, by 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 and survey its absorbance after ultra violet lamp 2h, calculate both degradation rates to methyl orange, found 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 comprising the following steps:
1) prepare the former liquid that drives
By volume the diethanol amine of 16%～23% butyl titanate and 4%～7% is joined in 70%～80% absolute ethyl alcohol and fully be mixed to get mixed solution, to the neodymium nitrate that adds mixed solution quality 1%～3% in mixed solution, then fully stir to obtain the former liquid that drives again;
2) preparation dropping liquid
By volume 8%～15% water is joined in 85%～92% absolute ethyl alcohol, be stirred to and fully be mixed to get dropping liquid;
3) prepare nano-TiO
2colloidal sol
Under vigorous stirring, splash into dropping liquid to former driving in liquid, continue strong 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 to ultrasonic cleaning, dry, then it is immersed in strong base solution, carry out again afterwards ultrasonic cleaning, dry;
5) coating nanometer TiO
2
High silica optical fiber is immersed to nano-TiO
2in colloidal sol, vacuum impregnation is also dried, and the high silica optical fiber after drying is placed in to muffle furnace with 450～600 ℃ of temperature calcinings 6～8 hours, obtains 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, it is characterized in that: described water is deionized water or distilled water.
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| CN102895972B (en) * | 2012-10-17 | 2014-04-16 | 陕西科技大学 | Method for preparing negative ion material used for organic pollutant and sewage treatment and having photo-catalysis performance |
| 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 |
| 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 |
| US11673831B2 (en) * | 2019-10-01 | 2023-06-13 | The Hong Kong University Of Science And Technology | Method for preparing optical fibers with high-particle-coated porous polymeric outer coating layers |
| 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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| FI115134B (en) * | 2002-06-28 | 2005-03-15 | Liekki Oy | A method for producing doped glass material |
| CN1772372A (en) * | 2005-10-31 | 2006-05-17 | 东南大学 | Prepn process of diffuse fiber supported nanometer photocatalytic titania film |
| CN101181678B (en) * | 2007-10-26 | 2011-02-09 | 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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