CN103599800A - Preparation method of glass fiber loaded silver-silver bromide-titanium oxide composite material - Google Patents
Preparation method of glass fiber loaded silver-silver bromide-titanium oxide composite material Download PDFInfo
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- CN103599800A CN103599800A CN201310597479.7A CN201310597479A CN103599800A CN 103599800 A CN103599800 A CN 103599800A CN 201310597479 A CN201310597479 A CN 201310597479A CN 103599800 A CN103599800 A CN 103599800A
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Abstract
The invention provides a preparation method of a glass fiber loaded silver-silver bromide-titanium oxide composite material. The method comprises the following steps: with an organic or inorganic titanium compound as a titanium source and glass fibers as a carrier, obtaining a spherical titanium dioxide (TiO2) nano particle loaded threaded glass fiber composite material by a hydrolysis method under an acidic condition; impregnating the composite material in an ethylene glycol solution containing silver nitrate, and subsequently, adding dropwise an ethylene glycol solution containing potassium bromide to generate an AgBr-TiO2/glass fiber composite material; and finally, reducing partial Ag<+1> in the AgBr-TiO2/glass fiber composite material into metal Ag, thus obtaining an Ag-AgBr-TiO2/glass fiber composite photocatalyst. The method provided by the invention realizes even loading of a nano-material having visible light catalytic activity on the surface of the threaded glass fibers by a two-step method; the method has the advantages of simple and convenient operation, easy large-scale production and the like; the obtained Ag-AgBr-TiO2/glass fiber composite material has relatively high visible light catalytic activity.
Description
Technical field
The invention belongs to environmentally conscious materials field, be specifically related to a kind of have visible light photocatalysis active, the glass fiber loaded Ag-AgBr-TiO of renewable screw-like
2the preparation method of composite.
Background technology
It is the large problem that the current mankind are concerned about most that environmental contaminants are administered, and the green technology of Development of Novel practicality is one of heat subject of numerous scientific research personnel's research always.Adopt the methods such as catalytic combustion, chemical oxidation, biodegradation can realize the removal of pollutant in environment, but said method all has certain limitation: as equipment and operating cost is high, removal efficiency is low, easily produce secondary pollution etc. in processing procedure, so these conventional methods are difficult to meet pollutant removal requirement technically and economically.In recent decades people study find Photocatalytic Oxidation With Semiconductors technology remove have that energy consumption is low, oxidability is strong, reaction condition is gentle aspect pollutant, easy and simple to handle, can reduce the outstanding features such as secondary pollution, become one of practical industrialization technology.Common semiconductor light-catalyst mostly is metal oxide, as ZnO, TiO
2, Fe
2o
3deng.From people such as Cary in 1976, reported successively TiO under UV-irradiation
2since labile organic compound, TiO
2because it is inexpensive, nontoxic, catalytic activity is high, good stability, be easy to the character such as recovery and favored, be considered to desirable photochemical catalyst and obtain broad research.Nowadays, photocatalysis has developed into an emerging chemical frontier branch of science.Utilize TiO
2semi-conducting material carries out photocatalytic degradation to organic pollution and becomes just gradually industrialization technology, and at soil, the pollution control aspect of water quality and atmosphere shows very bright application prospect.
Visible ray utilization rate is low is restriction nano-TiO
2practical principal element.TiO
2greater band gap (>3.2eV), can only be by ultraviolet excitation, and sunshine medium ultraviolet light proportion is less than 5%, so nano-TiO
2directly utilize sunshine very low as the efficiency of the organic pollution in light source light catalytic degradation environment.To utilize on a large scale nano-TiO
2light-catalyzed reaction, must expand daylighting area to increase luminous intensity, or adopt artificial ultraviolet source, this can increase Design and manufacture cost undoubtedly.If can widen nano-TiO
2spectrum utilize scope, just can greatly reduce the cost of photocatalysis technology, its degradation of organic substances in natural environment is polluted becomes possibility.Noble metal nano particles (Au, Pt, Ag) is owing to having surface plasmon resonance effect, thereby visible ray is had to stronger absorption.Patent CN101543780 is by the synthetic Ag-TiO of conventional solvent-thermal method
2-montmorillonite Composite photochemical catalyst, under black light irradiates, this Ag-TiO
2surface plasma catalysis material has shown excellent photocatalysis performance.In order further to expand the visible light activity scope of photochemical catalyst, need to be metal nanoparticle Direct precipitation the surface at catalysis material.Like this, the near-field effect of noble metal nano particles will further be strengthened by active substrate.For example contain the TiO of a small amount of Ag-AgBr
2material has stronger visible absorption and photocatalytic activity, be mainly because: 1) Ag-AgBr has very high speed at visible region, can make TiO
2have visible light-responded; 2) Ag-AgBr can with TiO
2form heterogeneous semiconductor junction structure, thereby effectively suppress right compound in light induced electron-hole, improve Ti0
2visible light catalysis activity.But AgBr and TiO in above-mentioned material
2between combined efficiency lower, the photogenerated charge producing under visible ray condition is difficult to be used effectively.Patent CN102500402A has reported that employing class microemulsion system synthesizes AgBr-TiO
2the method of nano-photocatalyst, it has solved AgBr-TiO
2the poor problem of different materials Compound Degree in nano-heterogeneous structure, but the method production cost is high, technique is wayward, is unfavorable for practical application.
In addition TiO,
2photochemical catalyst, in actual application, particularly, in water pollution control, adopts the suspension system of nano particle mostly.Commercial TiO
2particle is tiny and proportion is lower, is difficult for precipitation, in fluid not only separation difficulty, be difficult to recycle, and easily there is cohesion and reduce active.By TiO
2be fixed on certain carrier, can overcome suspended phase TiO
2the shortcoming of photochemical catalyst, solves the problem of separation and recovery of catalyst difficulty, and can select different carriers and immobilization technology according to the difference of photo catalysis reactor structure.The advantages such as glass fiber material has good insulating, heat resistance is strong, elastic modelling quantity is large, plastic deformation is little, mechanical strength is high, cheap and easy to get, are widely used in preparing fibre reinforced composites, and become one of most important material in modern project field.Unique filamentary structure and workability can (as forms such as single fiber, short fiber, bunchy, nonwoven, felts) make glass fiber material become desirable loaded with nano TiO
2carrier.
Summary of the invention:
The object of the invention is, a kind of preparation method of glass fiber loaded silver-silver bromide-titanium oxide composite material is provided, the method be take organic or inorganic titanium compound as titanium source, glass fibre is carrier, under acid condition, by Hydrolyze method, obtain the composite of the glass fiber loaded spherical tio2 nano particle of screw-like, again composite is joined in the ethylene glycol solution that contains silver nitrate and flooded, drip the ethylene glycol solution that contains KBr, generated AgBr-TiO
2/ glass fiber compound material, then by AgBr-TiO
2part Ag in/glass fiber compound material
+photo-reduction is metal A g, obtains Ag-AgBr-TiO
2/ glass fibre composite photo-catalyst.Method provided by the invention has been realized and will have been had the Ag-AgBr-TiO of visible light photocatalysis active by two-step method
2uniform load is at screw-like fiberglass surfacing, and that method has is easy and simple to handle, be easy to the advantages such as scale.The novel surface plasma Ag-AgBr-TiO of gained
2/ glass fiber compound material combines the characteristic of surface plasmon resonance effect, metal-semiconductor contact and the conductor photocatalysis of noble metal, has effectively solved TiO
2catalysis material combined efficiency is low, be difficult for the deficiencies such as reuse, has higher visible light photocatalysis performance.
The preparation method of a kind of glass fiber loaded silver-silver bromide-titanium oxide composite material of the present invention, follows these steps to carry out:
A. 0.02-0.2M titanium source is joined in 1M sulfuric acid solution, mix;
B. by adding 3g glass fibre in step a gained solution, be warming up to 110 ℃, react after 6 hours, with concentrated ammonia solution adjust pH to 7, ageing, after 12 hours, is cleaned, dry, obtains composite;
C. polyvinylpyrrolidone is joined in the ethylene glycol solution that 0.05M contains silver nitrate, obtain mixed solution, the composite obtaining in step b is impregnated in mixed solution, then the ethylene glycol solution that adds 0.05M to contain KBr, after mixing, be heated to temperature 40-150 ℃, insulation 1-6 hour, products therefrom replaces after washed product with deionized water and ethanol, can obtain glass fiber loaded AgBr-TiO
2composite photocatalyst material;
D. again by glass fiber loaded AgBr-TiO
2after the chemical reduction method of composite material by adopting routine or the reduction of the method for photo-reduction, products therefrom, with after deionized water washing, is dried to 3 hours at temperature 60 C, obtains glass fiber loaded Ag-AgBr-TiO
2composite photocatalyst material.
In step a, titanium source is potassium fluotitanate, ammonium titanium fluoride, isopropyl titanate or titanium tetrachloride.
In step b, glass fibre is A-glass fibre, E-glass fibre, C-glass fibre or AR-glass fibre.
Selected A-glass fibre, E-glass fibre, C-glass fibre or AR-glass fibre are single fiber, short fiber, bunchy or nonwoven form.
Reducing agent in steps d chemical reduction method is sodium borohydride, ascorbic acid, citric acid.
Accompanying drawing explanation
Fig. 1 be the embodiment of the present invention 2 synthesizeds there is the glass fiber loaded Ag-AgBr-TiO of having of regular screw-like
2the scanning electron microscope (SEM) photograph of composite;
Fig. 2 be the embodiment of the present invention 2 synthesizeds there is the glass fiber loaded Ag-AgBr-TiO of having of regular screw-like
2the electron energy scattering spectra (EDS) of composite, wherein
Fig. 3 be the embodiment of the present invention 2 synthesizeds there is the glass fiber loaded Ag-AgBr-TiO of regular screw-like
2composite photocatalyst material under visible ray (wavelength 420nm) condition to 20mgL
-1the degradation curve of methyl orange solution, wherein 1 is 0min, 2 is 10min, 3 is 20min, 4 is 30min, 5 is 40min, 6 is 50min, 7-is 60min, 8 is 70min, 9 is 80min, 10 is 90min, 11 is 100min.
The specific embodiment
The present embodiment is to implement under prerequisite in technical solution of the present invention, provided detailed embodiment and concrete operating process, but the present invention is not limited only to following embodiment:
Embodiment 1
A. 0.05M isopropyl titanate is joined in 1M sulfuric acid solution, mix;
B. by adding 3g short fiber form E-glass fibre in step a gained solution, be warming up to 110 ℃, react after 6 hours, with concentrated ammonia solution adjust pH to 7, ageing, after 12 hours, is cleaned, dry, obtains composite;
C. 0.6g polyvinylpyrrolidone is joined in the ethylene glycol solution that 0.05M contains silver nitrate, obtain mixed solution, the composite obtaining in step b is impregnated in mixed solution, then the ethylene glycol solution that adds 0.05M to contain KBr, after mixing, be heated to temperature 50 C, be incubated 3 hours, products therefrom replaces after washed product with deionized water and ethanol, can obtain the glass fiber loaded AgBr-TiO of screw-like
2composite photocatalyst material;
D. again by the glass fiber loaded AgBr-TiO of screw-like
2composite is dispersed in ethanolic solution, adds the ascorbic acid of 0.5M, and temperature 60 C reaction 2 hours, products therefrom was with after deionized water washing, and dry 3 hours of temperature 60 C, obtains the glass fiber loaded surface plasma Ag-AgBr-TiO of screw-like
2composite photocatalyst material.
A. 0.15M titanium tetrachloride is joined in 1M sulfuric acid solution, mix;
B. by adding 3g bunchy form C-glass fibre in step a gained solution, be warming up to 110 ℃, react after 6 hours, with concentrated ammonia solution adjust pH to 7, ageing, after 12 hours, is cleaned, dry, obtains composite;
C. 2g polyvinylpyrrolidone is joined in the ethylene glycol solution that 0.05M contains silver nitrate, obtain mixed solution, the composite that step b is obtained is impregnated in mixed solution, then the ethylene glycol solution that adds 0.05M to contain KBr, after mixing, be heated to 80 ℃ of temperature, be incubated 2 hours, products therefrom replaces after washed product with deionized water and ethanol, can obtain the glass fiber loaded AgBr-TiO of screw-like
2composite photocatalyst material;
D. again by the glass fiber loaded AgBr-TiO of screw-like
2composite is dispersed in ethanolic solution, is placed in reduction 30min under 300W xenon lamp (wavelength 420nm), and products therefrom, with after deionized water washing, is dried 3 hours at temperature 60 C, obtains the glass fiber loaded surface plasma Ag-AgBr-TiO of screw-like
2under the xenon lamp that composite photocatalyst material is 420nm in wavelength X irradiates, composite photocatalyst material has excellent degradation effect to methyl orange solution, can be by 20mgL in 100 minutes
-1methyl orange solution degradable.
Embodiment 3
A. 0.02M ammonium titanium fluoride is joined in 1M sulfuric acid solution, mix;
B. by adding 3g nonwoven form AR-glass fibre in step a gained solution, be warming up to 110 ℃, react after 6 hours, with concentrated ammonia solution adjust pH to 7, ageing, after 12 hours, is cleaned, dry, obtains composite;
C. 3g polyvinylpyrrolidone is joined in the ethylene glycol solution that 0.05M contains silver nitrate, obtain mixed solution, the composite obtaining in step b is impregnated in mixed solution, then the ethylene glycol solution that adds 0.05M to contain KBr, after mixing, be heated to 150 ℃ of temperature, be incubated 1 hour, products therefrom replaces after washed product with deionized water and ethanol, can obtain the glass fiber loaded AgBr-TiO of screw-like
2composite photocatalyst material;
D. again by the glass fiber loaded AgBr-TiO of screw-like
2composite is dispersed in ethanolic solution, adds the sodium borohydride of 0.5M, and temperature 60 C reaction 2 hours, products therefrom was with after deionized water washing, and dry 3 hours of temperature 60 C, obtains the glass fiber loaded surface plasma Ag-AgBr-TiO of screw-like
2composite photocatalyst material.
Embodiment 4
A. 0.2M ammonium titanium fluoride is joined in 1M sulfuric acid solution, mix;
B. by adding 3g single fiber form A-glass fibre in step a gained solution, be warming up to 110 ℃, react after 6 hours, with concentrated ammonia solution adjust pH to 7, ageing, after 12 hours, is cleaned, dry, obtains composite;
C. 0.2g polyvinylpyrrolidone is joined in the ethylene glycol solution that 0.05M contains silver nitrate, obtain mixed solution, the composite obtaining in step b is impregnated in mixed solution, then the ethylene glycol solution that adds 0.05M to contain KBr, after mixing, be heated to 40 ℃ of temperature, be incubated 6 hours, products therefrom replaces after washed product with deionized water and ethanol, can obtain the glass fiber loaded AgBr-TiO of screw-like
2composite photocatalyst material;
D. again by the glass fiber loaded AgBr-TiO of screw-like
2composite is dispersed in ethanolic solution, adds the citric acid of 0.5M, and temperature 60 C reaction 2 hours, products therefrom was with after deionized water washing, and dry 3 hours of temperature 60 C, obtains the glass fiber loaded surface plasma Ag-AgBr-TiO of screw-like
2composite photocatalyst material.
Embodiment 5
By conventional characterization method electron scattering power spectrum, synthesized sample in embodiment has been carried out to the research that element forms, find to have comprised the elements such as Ag, Ti, Br, O in sample, in conjunction with SEM data, illustrate that the present invention has successfully synthesized the glass fiber loaded Ag-AgBr-TiO of screw-like
2composite photocatalyst material.
Claims (5)
1. a preparation method for glass fiber loaded silver-silver bromide-titanium oxide composite material, is characterized in that following these steps to carrying out:
A. 0.02-0.2 M titanium source is joined in 1 M sulfuric acid solution, mix;
B. by adding 3 g glass fibres in step a gained solution, be warming up to 110 ℃, react after 6 hours, with concentrated ammonia solution adjust pH to 7, ageing, after 12 hours, is cleaned, dry, obtains composite;
C. polyvinylpyrrolidone is joined in the ethylene glycol solution that 0.05 M contains silver nitrate, obtain mixed solution, the composite obtaining in step b is impregnated in mixed solution, then the ethylene glycol solution that adds 0.05 M to contain KBr, after mixing, be heated to temperature 40-150 ℃, insulation 1-6 hour, products therefrom replaces after washed product with deionized water and ethanol, can obtain glass fiber loaded AgBr-TiO
2composite photocatalyst material;
D. again by glass fiber loaded AgBr-TiO
2after the chemical reduction method of composite material by adopting routine or the reduction of the method for photo-reduction, products therefrom, with after deionized water washing, is dried to 3 hours at temperature 60 C, obtains glass fiber loaded Ag-AgBr-TiO
2composite photocatalyst material.
2. method according to claim 1, is characterized in that in step a, titanium source is potassium fluotitanate, ammonium titanium fluoride, isopropyl titanate or titanium tetrachloride.
3. method according to claim 1, is characterized in that in step b, glass fibre is A-glass fibre, E-glass fibre, C-glass fibre or AR-glass fibre.
4. method according to claim 3, is characterized in that selected A-glass fibre, E-glass fibre, C-glass fibre or AR-glass fibre are single fiber, short fiber, bunchy or nonwoven form.
5. method according to claim 1, is characterized in that the reducing agent in steps d chemical reduction method is sodium borohydride, ascorbic acid, citric acid.
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| CN109534696A (en) * | 2019-01-25 | 2019-03-29 | 重庆化工职业学院 | Load the preparation method of the glass fiber material of silicon carbide |
| CN111604068A (en) * | 2020-06-21 | 2020-09-01 | 安徽理工大学 | Ag-AgBr/TiO2Method for preparing nano-rod composite array film |
| CN114405524A (en) * | 2022-01-29 | 2022-04-29 | 中国科学院东北地理与农业生态研究所 | P-n heterojunction type Pt/TiO2Preparation method of/AgBr/Ag composite photocatalyst |
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