CN1784973A - Method for preparing composite photocatalytic germicide - Google Patents
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Abstract
A composite photocatalytic antibacterial agent contains proportionally TiO2, SiO2 and Ag is prepared through preparing the alcohol solution of tetrabutyl titanate and the mixture of deionized water and alcohol, dripping said mixture in said alcohol solution while stirring to obtain TiO2 sol, preparing the alcohol solution of ethyl silicate and the mixture of deionized water and alcohol, dripping said mixture in said alcohol solution while stirring to obtain SiO2 sol, mixing TiO2 sol with SiO2 sol, preparing aqueous solution of silver nitrate, dripping it in the sol mixture while stirring to obtain gel, ageing, drying, grinding and calcining.
Description
Technical field
What the present invention relates to is a kind of method of chemical technology field, specifically is a kind of preparation method of composite photocatalitic germicide.
Background technology
Nano-TiO
2Under ultraviolet irradiation, electronics transits on the conduction band from valence band, forms hole-electron pair, and absorption is dissolved in nano-TiO
2The oxygen trapped electron on surface forms active oxygen O
2 -, the hole then will be adsorbed on nano-TiO
2The OH on surface
-And H
2O is oxidized to free radical HO
The active oxygen O that generates
2 -With free radical HO
Can penetrate the cell wall of bacterium, enter thalline, stop the transmission of film forming matter, block its respiratory system and electric transmission system, thus effective kill bacteria.Nano-TiO
2Another advantage of sterilization is the noxious material that its energy bacterium for degrading discharges when dead.Free radical HO
Has very high oxidability, effectively degradation of organic substances and environmental contaminants.Common photocatalitic germicide has wide spectrum, durable, safe characteristics, obtains extensive use aspect textile, amenities, but nano-TiO
2Can only absorb excitation wavelength is that the following light of 385nm (ultraviolet wavelength) reacts, thereby common photocatalitic germicide must be at ultraviolet irradiation competence exertion antibacterial action, and this makes the application of common photocatalitic germicide be subjected to certain limitation.
Find through literature search prior art, the article that is published in the 34th the 1st phase of volume of " application chemical industry " January in 2005 " carries the research of silver-colored titanium oxide photocatalysis disinfectant performance ", this article will be in the deficiency of competence exertion antibacterial action under the ultraviolet irradiation in order to overcome nano titanium oxide, with the metatitanic acid is presoma, flood certain density liquor argenti nitratis ophthalmicus, prepare year silver-colored titanium dioxide with the heat deposition method, and the anti-microbial property of silver-colored titanium dioxide is carried in research.But year silver-colored titanium dioxide particle diameter that adopts the heat deposition method to prepare is thicker, the photocatalysis antibacterial poor-performing; Titanium dioxide surface does not pass through modification, can not be used to prepare fiber and textile with anti-microbial property.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method of composite photocatalitic germicide is provided, make the composite photocatalitic germicide of its preparation, overcoming common photocatalitic germicide will be in the limitation of competence exertion antibacterial action under the ultraviolet irradiation, the antibacterial agent of the present invention's preparation has good antibiotic, antifouling, deodorization functions, can be used to prepare have textile and amenities antibiotic, antifouling, deodorization functions.
The present invention is achieved by the following technical solutions, composite photocatalitic germicide of the present invention, and each component and percentage by weight thereof are: TiO
273.7 ~ 87.0%, SiO
210.7 ~ 22.6%, Ag 2.3 ~ 3.7%, its preparation method may further comprise the steps:
(1) preparation TiO 2 sol.
Metatitanic acid four fourth liposoluble are gone in the absolute ethyl alcohol, the preparation weight percent concentration is 10 ~ 20% metatitanic acid four fourth fat ethanolic solutions, ratio preparation deionized water in 1: 1 ~ 5, alcohol mixeding liquid, splash into a small amount of glacial acetic acid, with deionized water, the pH value of alcohol mixeding liquid transfers to 4 ~ 5, deionized water with equal volume, alcohol mixeding liquid splashes in the metatitanic acid four fourth fat ethanolic solutions, stir while splashing into, solution temperature remains on 15 ~ 35 ℃, treat deionized water, after alcohol mixeding liquid adds metatitanic acid four fourth fat ethanolic solutions fully, continue to stir 4 ~ 6 hours, obtain the TiO 2 sol of homogeneous transparent.
(2) preparation silicon dioxide gel.
Tetraethoxysilance is dissolved in the absolute ethyl alcohol, the preparation weight percent concentration is 10 ~ 20% tetraethoxysilance ethanolic solution, ratio preparation deionized water, alcohol mixeding liquid in 1: 1 ~ 3, deionized water, the alcohol mixeding liquid of equal volume are splashed in the tetraethoxysilance ethanolic solution, stir while splashing into, solution temperature remains on 15 ~ 35 ℃.After treating that deionized water, alcohol mixeding liquid add the tetraethoxysilance ethanolic solution fully, stirred 8 ~ 16 hours, obtain the silicon dioxide gel of homogeneous transparent.
(3) TiO 2 sol is mixed with silicon dioxide gel.
TiO 2 sol, silicon dioxide gel are mixed, and the volume ratio of TiO 2 sol, silicon dioxide gel is 4 ~ 10: 1, and collosol temperature remains on 15 ~ 35 ℃, stirs 2 ~ 4 hours, obtains the mixed sols of homogeneous transparent.
(4) mix silver.
The preparation weight percent concentration is 2.5% silver nitrate aqueous solution, silver nitrate aqueous solution is splashed in the mixed sols, and the volume of silver nitrate aqueous solution is 1.8 ~ 4% of titanium dioxide, a silica mixed sols, stirs while splash into, collosol temperature remains on 15 ~ 35 ℃, stirs 1 ~ 2 hour.Form and do not have a gel of flowability.
(5) ageing, drying, grinding, roasting
Through the gel that step (4) obtains, put only 3 days, under vacuum, be warming up to 100 ℃, programming rate is 1 ℃/min, be incubated 12 hours, after the grinding, in air atmosphere, be warming up to 600 ℃, programming rate is 3 ℃/min, is incubated 3 hours, obtains the composite photo catalyst antimicrobial powder.
Among the present invention, TiO
2, SiO
2Be nanoscale with the size of Ag.SiO
2Be coated on TiO
2Nanoparticle surface forms the special perforated membrane of one deck, has overcome TiO
2The agglomeration traits of nano particle in polymer improved TiO
2The dispersiveness of nano particle in polymer, thus make this composite photocatalitic germicide can be used to prepare antibiotic macromolecular material and textile.Ag itself has very strong anti-microbial property, and it meets water can stripping Ag
+, attract strongly in the bacterium body and the thin base of breathing relevant zymoprotein, and lump together by chemical bonded refractory, its respiratory metabolism is obstructed, make bacterium death, thereby make this composite photocatalitic germicide not have also have good antibacterial performance under the situation of ultraviolet irradiation.Ag can promote TiO
2Change mutually to rutile from anatase, and the anatase that contains certain proportion rutile phase has higher catalytic activity, thereby Ag can improve the anti-microbial property of photocatalitic germicide.
The composite photo catalyst antimicrobial powder particle diameter distribution uniform of the present invention's preparation, particle diameter is less than 100nm, under ultraviolet irradiation, to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate greater than 99%, do not having under the ultraviolet irradiation, to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate greater than 90%.Composite photocatalitic germicide preparation method technology provided by the invention is simple, does not need special installation, and industrialization prospect is good.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.Following examples only are used to the present invention is described and are not used in restriction the present invention.
Embodiment 1:
Metatitanic acid four fourth liposoluble are gone in the absolute ethyl alcohol, the metatitanic acid four fourth fat ethanolic solutions of preparation 10%, ratio preparation deionized water, alcohol mixeding liquid in 1: 5, splashing into a small amount of glacial acetic acid, to make the pH value of deionized water, alcohol mixeding liquid be 4, isopyknic deionized water, alcohol mixeding liquid are splashed into metatitanic acid four fourth fat ethanolic solutions, stir while splashing into, solution temperature remains on 15 ℃.After treating that deionized water, alcohol mixeding liquid add metatitanic acid four fourth fat ethanolic solutions, stirred 6 hours, obtain the TiO 2 sol of homogeneous transparent.
Tetraethoxysilance is dissolved in the absolute ethyl alcohol, the tetraethoxysilance ethanolic solution of preparation 10%, prepare deionized water, alcohol mixeding liquid in 1: 3 ratio, isopyknic deionized water, alcohol mixeding liquid are splashed into the tetraethoxysilance ethanolic solution, stir while splashing into, solution temperature remains on 15 ℃, stirs 16 hours, obtains the silicon dioxide gel of homogeneous transparent.With volume ratio is that 10: 1 TiO 2 sol, silicon dioxide gel mixes, and stirs 4 hours, and collosol temperature remains on 15 ℃, obtains the mixed sols of homogeneous transparent.
The preparation weight percent concentration is 2.5% liquor argenti nitratis ophthalmicus, and the silver nitrate aqueous solution of mixed sols volume 1.8% is splashed in the mixed sols, stirs while splash into, and collosol temperature remains on 15 ℃, stirs 2 hours.Form and do not have behind the gel of flowability, put only 3 days, be warming up to 100 ℃ under vacuum, programming rate is 1 ℃/min, be incubated 12 hours, after the grinding, in air atmosphere, be warming up to 600 ℃, programming rate is 3 ℃/min, is incubated 3 hours, obtains the composite photo catalyst antimicrobial powder.
The component of this composite photo catalyst antimicrobial powder and percentage by weight thereof are: TiO
2(87.0%), SiO
2(10.7%) and Ag (2.3%), under ultraviolet irradiation, to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate is 99.99%, not having under the ultraviolet irradiation, is 90.5% to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate.
Embodiment 2:
Metatitanic acid four fourth liposoluble are gone in the absolute ethyl alcohol, the metatitanic acid four fourth fat ethanolic solutions of preparation 15%, ratio preparation deionized water, alcohol mixeding liquid in 1: 3, splashing into a small amount of glacial acetic acid, to make the pH value of deionized water, alcohol mixeding liquid be 4.5, isopyknic deionized water, alcohol mixeding liquid are splashed into metatitanic acid four fourth fat ethanolic solutions, stir while splashing into, solution temperature remains on 25 ℃, after treating that deionized water, alcohol mixeding liquid add metatitanic acid four fourth fat ethanolic solutions, stirred 5 hours, and obtained the TiO 2 sol of homogeneous transparent.
Tetraethoxysilance is dissolved in the absolute ethyl alcohol, the tetraethoxysilance ethanolic solution of preparation 15%, prepare deionized water, alcohol mixeding liquid in 1: 2 ratio, isopyknic deionized water, alcohol mixeding liquid are splashed into the tetraethoxysilance ethanolic solution, stir while splashing into, solution temperature remains on 25 ℃, stirs 12 hours, obtains the silicon dioxide gel of homogeneous transparent.With volume ratio is that 6: 1 TiO 2 sol, silicon dioxide gel mixes, and stirs 3 hours, and collosol temperature remains on 25 ℃, obtains the mixed sols of homogeneous transparent.
The preparation weight percent concentration is 2.5% liquor argenti nitratis ophthalmicus, and the silver nitrate aqueous solution of mixed sols volume 2.8% is added dropwise in the mixed sols, stirs while add, and collosol temperature remains on 25 ℃, stirs 1.5 hours.Form and do not have behind the gel of flowability, put only 3 days, be warming up to 100 ℃ under vacuum, programming rate is 1 ℃/min, be incubated 12 hours, after the grinding, in air atmosphere, be warming up to 600 ℃, programming rate is 3 ℃/min, is incubated 3 hours, obtains the composite photo catalyst antimicrobial powder.
The component of this composite photo catalyst antimicrobial powder and percentage by weight thereof are: TiO
2(81.1%), SiO
2(16.6%) and Ag (2.4%), under ultraviolet irradiation, to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate is 99.99%, not having under the ultraviolet irradiation, is 90.8% to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate.
Embodiment 3:
Metatitanic acid four fourth liposoluble are gone in the absolute ethyl alcohol, the metatitanic acid four fourth fat ethanolic solutions of preparation 20%, ratio preparation deionized water, alcohol mixeding liquid in 1: 1, splashing into a small amount of glacial acetic acid, to make the pH value of deionized water, alcohol mixeding liquid be 5, isopyknic deionized water, alcohol mixeding liquid are splashed into metatitanic acid four fourth fat ethanolic solutions, stir while splashing into, solution temperature remains on 35 ℃, after treating that deionized water, alcohol mixeding liquid add metatitanic acid four fourth fat ethanolic solutions, stirred 4 hours, and obtained the TiO 2 sol of homogeneous transparent.
Tetraethoxysilance is dissolved in the absolute ethyl alcohol, the tetraethoxysilance ethanolic solution of preparation 20%, prepare deionized water, alcohol mixeding liquid in 1: 1 ratio, isopyknic deionized water, alcohol mixeding liquid are splashed into the tetraethoxysilance ethanolic solution, stir while splashing into, solution temperature remains on 35 ℃, stirs 8 hours, obtains the silicon dioxide gel of homogeneous transparent.With volume ratio is that 4: 1 TiO 2 sol, silicon dioxide gel mixes, and stirs 2 hours, and collosol temperature remains on 35 ℃, obtains the mixed sols of homogeneous transparent.
The preparation weight percent concentration is 2.5% liquor argenti nitratis ophthalmicus, and the silver nitrate aqueous solution of mixed sols volume 4% is added dropwise in the mixed sols, stirs while add, and collosol temperature remains on 35 ℃, stirs 1 hour.Form and do not have behind the gel of flowability, put only 3 days, be warming up to 100 ℃ under vacuum, programming rate is 1 ℃/min, be incubated 12 hours, after the grinding, in air atmosphere, be warming up to 600 ℃, programming rate is 3 ℃/min, is incubated 3 hours, obtains the composite photo catalyst antimicrobial powder.
The component of this composite photo catalyst antimicrobial powder and percentage by weight thereof are: TiO
2(74.9%), SiO
2(22.6%) and Ag (2.5%), under ultraviolet irradiation, to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate is 99.99%, not having under the ultraviolet irradiation, is 91.6% to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate.
Embodiment 4:
Metatitanic acid four fourth liposoluble are gone in the absolute ethyl alcohol, the metatitanic acid four fourth fat ethanolic solutions of preparation 10%, ratio preparation deionized water, alcohol mixeding liquid in 1: 3, splashing into a small amount of glacial acetic acid, to make the pH value of deionized water, alcohol mixeding liquid be 4.5, isopyknic deionized water, alcohol mixeding liquid are splashed into metatitanic acid four fourth fat ethanolic solutions, stir while splashing into, solution temperature remains on 25 ℃, after treating that deionized water, alcohol mixeding liquid add metatitanic acid four fourth fat ethanolic solutions, stirred 5 hours, and obtained the TiO 2 sol of homogeneous transparent.
Tetraethoxysilance is dissolved in the absolute ethyl alcohol, the tetraethoxysilance ethanolic solution of preparation 10%, prepare deionized water, alcohol mixeding liquid in 1: 3 ratio, isopyknic deionized water, alcohol mixeding liquid are splashed into the tetraethoxysilance ethanolic solution, stir while splashing into, solution temperature remains on 25 ℃, stirs 12 hours, obtains the silicon dioxide gel of homogeneous transparent.With volume ratio is that 6: 1 TiO 2 sol, silicon dioxide gel mixes, and stirs 3 hours, and collosol temperature remains on 25 ℃, obtains the mixed sols of homogeneous transparent.
The preparation weight percent concentration is 2.5% liquor argenti nitratis ophthalmicus, and the silver nitrate aqueous solution of mixed sols volume 2.3% is added dropwise in the mixed sols, stirs while add, and collosol temperature remains on 25 ℃, stirs 1.5 hours.Form and do not have behind the gel of flowability, put only 3 days, be warming up to 100 ℃ under vacuum, programming rate is 1 ℃/min, be incubated 12 hours, after the grinding, in air atmosphere, be warming up to 600 ℃, programming rate is 3 ℃/min, is incubated 3 hours, obtains the composite photo catalyst antimicrobial powder.
The component of this composite photo catalyst antimicrobial powder and percentage by weight thereof are: TiO
2(80.6%), SiO
2(16.5%) and Ag (2.9%), under ultraviolet irradiation, to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate is 99.99%, not having under the ultraviolet irradiation, is 96.6% to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate.
Embodiment 5:
Metatitanic acid four fourth liposoluble are gone in the absolute ethyl alcohol, the metatitanic acid four fourth fat ethanolic solutions of preparation 10%, ratio preparation deionized water, alcohol mixeding liquid in 1: 3, splashing into a small amount of glacial acetic acid, to make the pH value of deionized water, alcohol mixeding liquid be 5, isopyknic deionized water, alcohol mixeding liquid are splashed into metatitanic acid four fourth fat ethanolic solutions, stir while splashing into, solution temperature remains on 35 ℃, after treating that deionized water, alcohol mixeding liquid add metatitanic acid four fourth fat ethanolic solutions, stirred 4 hours, and obtained the TiO 2 sol of homogeneous transparent.
Tetraethoxysilance is dissolved in the absolute ethyl alcohol, the tetraethoxysilance ethanolic solution of preparation 10%, prepare deionized water, alcohol mixeding liquid in 1: 3 ratio, isopyknic deionized water, alcohol mixeding liquid are splashed into the tetraethoxysilance ethanolic solution, stir while splashing into, solution temperature remains on 35 ℃, stirs 8 hours, obtains the silicon dioxide gel of homogeneous transparent.With volume ratio is that 4: 1 TiO 2 sol, silicon dioxide gel mixes, and stirs 2 hours, and collosol temperature remains on 35 ℃, obtains the mixed sols of homogeneous transparent.
The preparation weight percent concentration is 2.5% liquor argenti nitratis ophthalmicus, and the silver nitrate aqueous solution of mixed sols volume 3% is added dropwise in the mixed sols, stirs while add, and collosol temperature remains on 35 ℃, stirs 1 hour.Form and do not have behind the gel of flowability, put only 3 days, be warming up to 100 ℃ under vacuum, programming rate is 1 ℃/min, be incubated 12 hours, after the grinding, in air atmosphere, be warming up to 600 ℃, programming rate is 3 ℃/min, is incubated 3 hours, obtains the composite photo catalyst antimicrobial powder.
The component of this composite photo catalyst antimicrobial powder and percentage by weight thereof are: TiO
2(73.7%), SiO
2(22.6%) and Ag (3.7%), under ultraviolet irradiation, to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate is 99.99%, not having under the ultraviolet irradiation, is 99.5% to Escherichia coli, staphylococcus aureus, bacillus megaterium, hay bacillus (48 hours) antibiotic rate.
Claims (10)
1, a kind of preparation method of composite photocatalitic germicide is characterized in that, described composite photocatalitic germicide, and each component and percentage by weight thereof are :/TiO
273.7 ~ 87.0%, SiO
210.7 ~ 22.6%, Ag2.3 ~ 3.7%, its preparation method may further comprise the steps:
(1) preparation TiO 2 sol: prepare metatitanic acid four fourth fat ethanolic solutions and deionized water, alcohol mixeding liquid respectively, deionized water, the alcohol mixeding liquid of equal volume are splashed in the metatitanic acid four fourth fat ethanolic solutions, stir while splashing into, obtain the TiO 2 sol of homogeneous transparent;
(2) preparation silicon dioxide gel: prepare tetraethoxysilance ethanolic solution and deionized water, alcohol mixeding liquid respectively, deionized water, the alcohol mixeding liquid of equal volume are splashed in the tetraethoxysilance ethanolic solution, stir while splashing into, obtain the silicon dioxide gel of homogeneous transparent;
(3) TiO 2 sol is mixed with silicon dioxide gel: TiO 2 sol, silicon dioxide gel are mixed, and insulated and stirred obtains the mixed sols of homogeneous transparent;
(4) mix silver: the preparation silver nitrate aqueous solution, silver nitrate aqueous solution is splashed in the mixed sols, stir while splash into, form gel;
(5) ageing, drying, grinding, roasting.
2, the preparation method of composite photocatalitic germicide according to claim 1, it is characterized in that, in the described step (1), prepare metatitanic acid four fourth fat ethanolic solutions and deionized water, alcohol mixeding liquid respectively, be meant: metatitanic acid four fourth liposoluble are gone in the absolute ethyl alcohol, and the preparation weight percent concentration is 10 ~ 20% metatitanic acid four fourth fat ethanolic solutions, ratio preparation deionized water, alcohol mixeding liquid in 1: 1 ~ 5, splash into a small amount of glacial acetic acid, the pH value of deionized water, alcohol mixeding liquid is transferred to 4 ~ 5.
3, according to the preparation method of claim 1 or 2 described composite photocatalitic germicides, it is characterized in that, in the described step (1), while splashing into when stirring, solution temperature remains on 15 ~ 35 ℃, after treating that deionized water, alcohol mixeding liquid add metatitanic acid four fourth fat ethanolic solutions fully, continue to stir 4 ~ 6 hours, obtain the TiO 2 sol of homogeneous transparent.
4, the preparation method of composite photocatalitic germicide according to claim 1, it is characterized in that, in the described step (2), prepare tetraethoxysilance ethanolic solution and deionized water, alcohol mixeding liquid respectively, be meant: tetraethoxysilance is dissolved in the absolute ethyl alcohol, the preparation weight percent concentration is 10 ~ 20% tetraethoxysilance ethanolic solution, ratio preparation deionized water, alcohol mixeding liquid in 1: 1 ~ 3.
5, according to the preparation method of claim 1 or 4 described composite photocatalitic germicides, it is characterized in that, in the described step (2), while splashing into when stirring, solution temperature remains on 15 ~ 35 ℃, after treating that deionized water, alcohol mixeding liquid add the tetraethoxysilance ethanolic solution fully, stirred 8 ~ 16 hours, obtain the silicon dioxide gel of homogeneous transparent.
6, the preparation method of composite photocatalitic germicide according to claim 1 is characterized in that, in the described step (3), the volume ratio that TiO 2 sol, silicon dioxide gel mix is 4 ~ 10: 1.
According to the preparation method of claim 1 or 6 described composite photocatalitic germicides, it is characterized in that 7, in the described step (3), insulated and stirred is meant: the mixed sols temperature remains on 15 ~ 35 ℃, stirs 2 ~ 4 hours.
8, the preparation method of composite photocatalitic germicide according to claim 1, it is characterized in that, described step (4), the preparation weight percent concentration is 2.5% silver nitrate aqueous solution, silver nitrate aqueous solution is splashed in the mixed sols, and the volume of silver nitrate aqueous solution is 1.8 ~ 4% of titanium dioxide, a silica mixed sols volume, stirs while splash into, collosol temperature remains on 15 ~ 35 ℃, stirs 1 ~ 2 hour.
9, the preparation method of composite photocatalitic germicide according to claim 1 is characterized in that, described step (5), be specially: with the gel that step (4) obtains, put only 3 days, be incubated 12 hours, after the grinding, be incubated 3 hours, obtain the composite photo catalyst antimicrobial powder.
According to the preparation method of claim 1 or 9 described composite photocatalitic germicides, it is characterized in that 10, described step (5) was put 3 days only, was warming up to 100 ℃ under vacuum, programming rate is 1 ℃/min; After the grinding, be warming up to 600 ℃ in air atmosphere, programming rate is 3 ℃/min.
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