CN101659773A - Nano TiO2-polystyrene microsphere compound and preparation method and application thereof - Google Patents
Nano TiO2-polystyrene microsphere compound and preparation method and application thereof Download PDFInfo
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- CN101659773A CN101659773A CN200910152763A CN200910152763A CN101659773A CN 101659773 A CN101659773 A CN 101659773A CN 200910152763 A CN200910152763 A CN 200910152763A CN 200910152763 A CN200910152763 A CN 200910152763A CN 101659773 A CN101659773 A CN 101659773A
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Abstract
The invention discloses a nano TiO2-polystyrene microsphere compound and a preparation method and application thereof. The nano TiO2-polystyrene microsphere compound comprises polystyrene microspherewith positive charge and nano TiO2, wherein the polystyrene microsphere with positive charge is a carrier, the nano TiO2 is attached on the surface of the polystyrene microsphere, and the mass percentage of the nano TiO2 to the polystyrene microsphere is 0.5 to 5 percent; the structural formula of the polystyrene microsphere is shown as above, wherein R1 is -H or -CH-CH2-; and R2 is -CH3 or -CH2CH3. An agent made from the nano TiO2-polystyrene microsphere compound has excellent antibiosis performance and has the advantages of quickness, high-efficiency, broad spectrum, long-term use and non-tolerance and the like, thus overcoming the defects of an inorganic antibiotic agent that sterilization speed is slow and color is apt to change, and defects of an organic antibiotic agent that heat-resistance is poor and effective time is limited; and the invention has bright market prospect and can be popularized.
Description
Technical field:
The present invention relates to the antibacterial material of a kind of photochemical catalysis, particularly a kind of with nano-TiO
2Be the antibacterial material of photocatalyst, metal nanometer material technical field.
Background technology
Once the SARS that wreaks havoc in Beijing and other cities still made us remember clearly, and it has seized some life, and it is frightened to bring the secular psychology of people, in the whole nation so that the whole world caused fear to SARS.And current, the multinational Influenza A H1N1 epidemic situation that takes place with the area in the world is the continuation spreading trend.The appearance of China's Guangzhou Influenza A H1N1 secondary case shows that the risk that new type influenza generation interpersonal communication and community propagate continues to increase, and China's prevention and control epidemic situation work is faced with more arduous complicated situation.In the face of the continuous appearance of these highly pathogenic viruses, and the gesture of wreaking havoc is arranged in the world, and the variability that virus exists has produced resistance to a certain degree to more existing medicines.This makes people begin the concern for the environment health and it is had higher requirement.Threaten at these, we need set about developing novel treatment antibody drug on the one hand; On the other hand, the prevention anti-biotic material of development of new also is subjected to people's attention day by day.Research and development has that sterilization power is strong, good endurance, good stability, do not have the antibacterial material of characteristics such as secondary pollution to become the emphasis of current research.
Present antibacterial material mainly contains following several by use-pattern: (1) filters antibacterial material, utilizes suitable filtration unit, removes microorganism by filtering.Because filtering layer is thinner, will soon be saturated in adsorption process, lose effect.Activated carbon promptly is typical example.(2) adsorb antibacterial material, promptly bacterium is adsorbed on the material, play cleaning action with the concentration that reduces bacterium in the air by adsorption.(3) the antibacterial material of photochemical catalysis can destroy the cytolemma of various bacteriums under the effect of light, solidify the protein of various viruses.Current, using more is to filter antibacterial material and the antibacterial material of absorption, the weak point but this two classes material ubiquity bacteriostasis property is held time, and effect is lower, and has the possible characteristics of secondary pollution.And there is higher requirement in public places such as hospital, school to bacteriostasis property usually, as than higher sterilization rate, can not have secondary pollution, antibacterial time long etc.The composite bactericidal agent is emerging in recent years a kind of antiseptic-germicide, and its performance had both overcome the limitation and the easy wash-out of organic antibacterial agent of inorganic antiseptic antimicrobial spectrum, the shortcoming that thermotolerance is bad; Combine prompt effect, the persistence of organic system again, characteristics such as the security of inorganic system, discoloration-resistant.
Nano-TiO
2Having stable, the strong oxidation capacity of chemical property, indissoluble, characteristics such as nontoxic, is the ideal photocatalyst.Chinese patent CN1463790, CN1459331, CN1448214, CN1450123 disclose nano-TiO
2Has good photocatalysis performance.Under illumination condition, its light-catalyzed reaction can thoroughly be degraded into carbonic acid gas, water or other inorganics with organic and part inorganic pollutant, bacterium and virus.But nano-TiO
2Because the non-selectivity of its oxidation makes its carrier major limitation in inorganic materials such as glass, ceramic stainless steel and gacs, and because it is difficult for organic bonding, make TiO
2And only simple physics absorption or igneous fusion process between these carriers.Application facet at anti-biotic material is very restricted.
Summary of the invention
Technical problem to be solved by this invention provides a kind of nano-TiO
2-polystyrene microsphere compound and preparation method thereof.
Though nano-TiO
2Though have good antimicrobial property, make its anti-microbial property be effectively played, must make nano-TiO
2Can effectively contact with bacterium, and nano-TiO
2It is unsatisfactory to catch the bacterium ability.This just need adsorb and enrichment bacterium by other materials.
Inventive concept of the present invention is: utilize the electronegative characteristic of cytolemma of bacterium, use positively charged carrier can make bacterium in its surface adsorption and enrichment; Then utilize nano-TiO
2Strong oxidation capacity, bacterium is carried out deactivation and decomposition.
For solving technical problem to be solved by this invention, the technical solution adopted in the present invention is: use the easy dispersive nano-TiO of sol-gel method synthesis modification by butyl (tetra) titanate earlier
2Colloidal sol; 500 ℃ calcine anatase type nano TiO
2, handle through NaOH and 3-aminopropyl trimethoxysilane, make the easy dispersive nano-TiO of modification
2By required consumption styrene monomer, dimethylaminoethyl acrylate methyl (or second) amido ethyl ester and methacryloxypropyl trimethoxy silane (KH-570) coupling agent are got all the ready, contained the polystyrene microsphere of positive charge by precipitation polymerization method preparation surface.Add certain amount of nano TiO
2Colloidal sol passes through nano-TiO
2With the interaction of silane coupling agent, with nano-TiO
2Be adsorbed on the polystyrene microsphere surface, form nano-TiO
2-polystyrene microsphere compound.
Specifically, technical scheme of the present invention is as follows:
Nano-TiO of the present invention
2-polystyrene microsphere compound mainly comprises positively charged polystyrene microsphere and nano-TiO
2, described positively charged polystyrene microsphere is a carrier, described nano-TiO
2Be adsorbed on this polystyrene microsphere surface, described nano-TiO
2Mass percent with respect to polystyrene microsphere is 0.5～5%, and the structural formula of described polystyrene microsphere is as follows:
In the formula, R
1For-H or-CH-CH
2-; R
2For-CH
3Or-CH
2CH
3
Further, nano-TiO of the present invention
2With respect to nano-TiO
2The mass percent of-polystyrene microsphere compound is 2～5%.
Prepare nano-TiO of the present invention
2The method of-polystyrene microsphere compound mainly comprises the steps,
Step 1: with butyl (tetra) titanate 500 ℃ calcine anatase type nano TiO
2, handle through NaOH and 3-aminopropyl trimethoxysilane, make the easy dispersive nano-TiO of modification
2
Step 2: take by weighing styrene monomer, acrylic amine base class monomer and silane coupling agent by following mass percent, wherein
Styrene monomer 80-90%,
Acrylic amine base class monomer 5-10%,
Silane coupling agent 5-10%,
Be that initiator, dehydrated alcohol are that the polyreaction that reaction flux carried out 2 hours obtains the positively charged polystyrene microsphere in surface again with the Diisopropyl azodicarboxylate;
Step 3: add nano-TiO with respect to described polystyrene microsphere quality 0.5-5%
2, pass through nano-TiO
2With the interaction of silane coupling agent, with nano-TiO
2Be adsorbed on the polystyrene microsphere surface, form nano-TiO
2-polystyrene microsphere compound.
Further, the styrene monomer in the above-mentioned preparation method's of the present invention the step 2 is a styrene monomer or to the benzene diene monomers.
Further, the acrylic amine base class monomer in the above-mentioned preparation method's of the present invention the step 2 is Dimethylaminoethyl Methacrylate or methacrylic acid diethylin ethyl ester.
Further, the silane coupling agent in the above-mentioned preparation method's of the present invention the step 2 is a methacryloxypropyl trimethoxy silane.
Nano-TiO of the present invention
2-polystyrene microsphere compound can be used for eliminating intestinal bacteria as antibacterial material.
Compared with prior art, advantage of the present invention is: because nano-TiO
2Be adsorbed on described polystyrene microsphere surface, therefore nano-TiO of the present invention
2-polystyrene microsphere compound had both overcome the limitation and the easy wash-out of organic antibacterial agent of inorganic antiseptic antimicrobial spectrum, the shortcoming that thermotolerance is bad; Combine the advantage of the two again: have prompt effect, the persistence of organic system, characteristics such as the security of inorganic system, discoloration-resistant.Combine simultaneously nano-TiO again
2Excellent photocatalysis performance, and have itself the peculiar small-size effect of nanoparticle, surface interface effect and quantum size effect etc.Nano-TiO of the present invention
2-polystyrene microsphere compound is not the simple superposition of different materials, because nano-TiO
2Combine on molecular level with other elements, have extremely strong synergistic effect, its sterilizing ability and efficient are improved greatly.Nano-TiO of the present invention
2-polystyrene microsphere compound has fast, efficient, wide spectrum, lasting, advantage such as have no drug resistance, and overcome short shortcoming of slow, the easy to change and organic antibacterial agent poor heat resistance of inorganic antiseptic sterilization speed, working lipe.
Description of drawings
Fig. 1 is a nano-TiO of the present invention
2Nano-TiO in the-polystyrene microsphere compound
2Size distribution figure;
Fig. 2 is a nano-TiO of the present invention
2Nano-TiO in the-polystyrene microsphere compound
2X-ray diffractogram;
Fig. 3 is a nano-TiO of the present invention
2The antibacterial comparison diagram as a result of-polystyrene microsphere composite antibiosis microballoon A, B and C and poly-(vinylbenzene-co-methacryloxypropyl trimethoxy silane-co-Dimethylaminoethyl Methacrylate) organic microballoon D.
Embodiment
Be described in further detail the present invention below in conjunction with embodiment, but the present invention is not limited only to described embodiment.
Embodiment 1:
(1) nano-TiO
2Preparation
At room temperature, add 20mL dehydrated alcohol, 2mL acetone successively, slowly drip 6mL butyl (tetra) titanate and 400mL deionized water.Dehydrated alcohol dissolves butyl (tetra) titanate as solvent fully, solution is the water white transparency shape, adds deionized water, and butyl (tetra) titanate begins hydrolysis, solution is gradually by original colourless white shape that becomes, and adding acetone simultaneously, to suppress its hydrolysis reaction too fast and be unfavorable for the carrying out of testing.In ice-water bath, after violent constant speed stirred 1-2h, the pH value that adds an amount of concentrated nitric acid regulator solution was about at 1 o'clock and prepares gel, continued to stir 2h in 70 ℃～80 ℃ oil baths, and solution presents the colloidal solution that omits transparence and have micro emulsion white gradually; After 4h is left standstill in cooling, obtain TiO
2Sol solution.Remove solvent through rotary evaporation, products therefrom is through vacuum-drying, obtain the white powder product 500 ℃ of high-temperature calcinations.Adopt above-mentioned sol-gel method synthetic nano-TiO
2Colloidal sol, the TiO of gained
2The nanoparticle size-grade distribution is more even, the about 10nm of particle diameter (as shown in Figure 1); Nano-TiO through high-temperature calcination
2Be Detitanium-ore-type crystal (as shown in Figure 2), with the 2.0g nano-TiO of high-temperature calcination
2Ultra-sonic dispersion is 2h in the 50%NaOH of 20mL solution; Be dispersed in after the back centrifugation in the 40mL ethanol; Add 40 μ L 3-aminopropyl trimethoxysilane again,, make the easy dispersive nano-TiO of modification at 70 ℃ of ultrasonic reaction 24h
2Suspension liquid.
(2) nano-TiO
2The preparation of-polystyrene microsphere compound
In exsiccant 150mL flask, add 80mL dehydrated alcohol, 18g vinylbenzene, 1g methacryloxypropyl trimethoxy silane coupling agent, 1g Dimethylaminoethyl Methacrylate; get the 0.04g Diisopropyl azodicarboxylate and be dissolved in the 20mL dehydrated alcohol until pouring in the flask after the dissolving fully; violent constant speed stirring is also led to nitrogen protection; thermostatically heating after in 30min, rising to 70 ℃ rapidly; behind reaction 5～10min, solution presents oyster white.Behind the reaction 2h, obtain the positively charged polystyrene microsphere in surface.With the 2.0mL nano-TiO
2Suspension liquid (nano-TiO
2Mass percent with respect to the organic microballoon of polystyrene is 0.5%) slowly be added dropwise in the flask, continue reaction 3～4h, obtain layering solution, the upper strata is little yellow stillness of night of clear, lower floor is a yellow particle shape material.After reaction finishes to leave standstill for some time, remove unnecessary solvent through rotatory evaporator under 65 ℃, and at 50 ℃ of following vacuum-drying 24h.Obtain flaxen nano-TiO after the oven dry
2-polystyrene complex microsphere.
(3) bacteriostatic experiment
Cultured colibacillary slant culture is hung a little lawn down with transfering loop, makes 5mL bacterium liquid with sterilized nutrient broth medium then.It is standby with 10 times of nutrient broth dilutions to get this bacterium liquid 0.1mL.With the above-mentioned intestinal bacteria bacteria suspension 1mL that has made; Add the nutrient broth agar substratum that is cooled to about 50 ℃ then, being diluted to concentration is 1 * 10
7The solution of CFU/mL shakes up, and is fully standby after the condensation.Accurately take by weighing present embodiment gained nano-TiO
2-polystyrene complex 1.0g adds sterile purified water 100mL, and ultrasonic concussion 30min draws the 2mL nano-TiO
2-polystyrene complex microsphere suspension drops on the diameter 2.5cm sterile petri dish, makes it to be evenly distributed in the culture dish, with 1 * 10
7The bacterium liquid of CFU/mL adds culture dish, uses 15-W 365nm ultra violet lamp then, and the intensity of UV-light (365nm) is 0.63mW/cm
2The bacterium liquid of therefrom getting 20 μ L at regular intervals is distributed in the 1mL phosphoric acid salt buffered soln, this solution is distributed to contains on solid culture element (Luria-Bertani (LB) agar) sheet glass, in incubator, cultivate 24h then under 37 ℃, cultivate and finish the number that bacterium family on sheet glass is calculated in the back, calculate the variation of bacterial concentration in the culture dish again by this number.
Shown in the curve A of Fig. 3, present embodiment gained nano-TiO
2-polystyrene complex sterilization rate to intestinal bacteria 24h under λ=365nm action of ultraviolet light reaches more than 80.5%.
Embodiment 2:
(1) nano-TiO
2Preparation
As embodiment 1 preparation nano-TiO
2Suspension liquid is standby.
(2) nano-TiO
2The preparation of-polystyrene complex
In exsiccant 150mL flask, add 80mL dehydrated alcohol, 16g vinylbenzene, 2g methacryloxypropyl trimethoxy silane coupling agent, 2g methylacryoyloxyethyl trimethyl ammonium chloride; get the 0.04g Diisopropyl azodicarboxylate and be dissolved in the 20mL dehydrated alcohol until pouring in the flask after the dissolving fully; logical nitrogen protection; thermostatically heating; in 30min, rise to 70 ℃ rapidly; behind reaction 5～10min, solution presents oyster white.Behind the reaction 4h, with the 8.0mL nano-TiO of above-mentioned system
2Suspension liquid (nano-TiO
2Mass percent with respect to the organic microballoon of polystyrene is 2.0%) slowly be added dropwise in the flask, continue reaction 2h, obtain pale yellow solution.After reaction finishes to leave standstill for some time, remove unnecessary solvent through rotatory evaporator under 65 ℃, and at 50 ℃ of following vacuum-drying 24h.Obtain faint yellow nano-TiO after the oven dry
2-polystyrene complex microsphere.
(3) bacteriostatic experiment
Method according to embodiment 1 is carried out bacteriostatic experiment, shown in the curve B of Fig. 3, and present embodiment gained nano-TiO
2-polystyrene complex microsphere sterilization rate to intestinal bacteria 24h under λ=365nm action of ultraviolet light can reach 95.6%.
Embodiment 3:
(1) nano-TiO
2Preparation
As embodiment 1 preparation nano-TiO
2Suspension liquid is standby.
(2) nano-TiO
2The preparation of-polystyrene complex
In exsiccant 150mL flask, add 80mL dehydrated alcohol, 17g to benzene diene, 1.5g methacryloxypropyl trimethoxy silane coupling agent, 1.5g methacrylic acid diethylin ethyl ester; get the 0.04g Diisopropyl azodicarboxylate and be dissolved in the 20mL dehydrated alcohol until pouring in the flask after the dissolving fully; logical nitrogen protection; thermostatically heating; in 30min, rise to 70 ℃ rapidly; behind reaction 5～10min, solution presents oyster white.Behind the reaction 4h, with the 20.0mL nano-TiO of above-mentioned preparation
2Suspension liquid (nano-TiO
2Mass percent with respect to the organic microballoon of polystyrene is 5.0%) slowly be added dropwise in the flask, continue reaction 2h, obtain pale yellow solution.After reaction finishes to leave standstill for some time, remove unnecessary solvent through rotatory evaporator under 65 ℃, and at 50 ℃ of following vacuum-drying 24h.Obtain faint yellow nano-TiO after the oven dry
2-polystyrene complex microsphere.
(3) bacteriostatic experiment
Method according to embodiment 1 is carried out bacteriostatic experiment, shown in the curve C of Fig. 3, and present embodiment gained nano-TiO
2-polystyrene complex sterilization rate to intestinal bacteria 24h under λ=365nm action of ultraviolet light can reach 100%.
Claims (7)
1. nano-TiO
2-polystyrene microsphere compound is characterized in that: it comprises positively charged polystyrene microsphere and nano-TiO
2, described positively charged polystyrene microsphere is a carrier, described nano-TiO
2Be adsorbed on this polystyrene microsphere surface, described nano-TiO
2Mass percent with respect to polystyrene microsphere is 0.5～5%, and the structural formula of described polystyrene microsphere is as follows:
In the formula, R
1For-H or-CH-CH
2-; R
2For-CH
3Or-CH
2CH
3
2. nano-TiO according to claim 1
2-polystyrene microsphere compound is characterized in that: described nano-TiO
2With respect to nano-TiO
2The mass percent of-polystyrene microsphere compound is 2～5%.
3. nano-TiO for preparing claim 1
2The method of-polystyrene microsphere compound is characterized in that comprising the steps,
Step 1: with butyl (tetra) titanate 500 ℃ calcine anatase type nano TiO
2, handle through NaOH and 3-aminopropyl trimethoxysilane, make the easy dispersive nano-TiO of modification
2
Step 2: take by weighing styrene monomer, acrylic amine base class monomer and silane coupling agent by following mass percent, wherein
Styrene monomer 80-90%,
Acrylic amine base class monomer 5-10%,
Silane coupling agent 5-10%,
Be that initiator, dehydrated alcohol are that the polyreaction that reaction flux carried out 2 hours obtains the positively charged polystyrene microsphere in surface again with the Diisopropyl azodicarboxylate;
Step 3: add nano-TiO with respect to described polystyrene microsphere quality 0.5-5%
2, pass through nano-TiO
2With the interaction of silane coupling agent, with nano-TiO
2Be adsorbed on the polystyrene microsphere surface, form nano-TiO
2-polystyrene microsphere compound.
4. preparation nano-TiO according to claim 3
2The method of-polystyrene microsphere compound is characterized in that: the styrene monomer in the described step 2 is a styrene monomer or to the benzene diene monomers.
5. preparation nano-TiO according to claim 3
2The method of-polystyrene microsphere compound is characterized in that: the acrylic amine base class monomer in the described step 2 is Dimethylaminoethyl Methacrylate or methacrylic acid diethylin ethyl ester.
6. preparation nano-TiO according to claim 3
2The method of-polystyrene microsphere compound is characterized in that: the silane coupling agent in the described step 2 is a methacryloxypropyl trimethoxy silane.
7. nano-TiO
2-polystyrene microsphere compound is characterized in that as the purposes of antibacterial material: this nano-TiO
2-polystyrene microsphere compound is used to eliminate intestinal bacteria.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102613176A (en) * | 2012-03-06 | 2012-08-01 | 苏州百馥生化科技有限公司 | Mildewproof spray |
| CN104907093A (en) * | 2015-05-06 | 2015-09-16 | 杭州云界生物科技有限公司 | Nanometer titanium dioxide preparation method |
| CN106632787A (en) * | 2016-11-30 | 2017-05-10 | 上海纳米技术及应用国家工程研究中心有限公司 | Optical transparent polymer-titanium dioxide core-shell microspheres as well as preparation and application |
| TWI709419B (en) * | 2019-05-31 | 2020-11-11 | 國立虎尾科技大學 | Structure antibacterial film, its preparation method and application |
| CN114643077A (en) * | 2022-03-02 | 2022-06-21 | 湖北大学 | Microporous polymer with photocatalytic activity and preparation method thereof |
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| CN1569948A (en) * | 2004-05-08 | 2005-01-26 | 武汉大学 | Light degradable TiO2- polystyrene composite plastic preparation method |
| CN100503448C (en) * | 2006-05-23 | 2009-06-24 | 中国科学院理化技术研究所 | Method for synthesizing anatase type crystallizing titanium dioxide nano nuclear-shell or shell structure material by water phase one-step method |
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| CN102613176A (en) * | 2012-03-06 | 2012-08-01 | 苏州百馥生化科技有限公司 | Mildewproof spray |
| CN104907093A (en) * | 2015-05-06 | 2015-09-16 | 杭州云界生物科技有限公司 | Nanometer titanium dioxide preparation method |
| CN104907093B (en) * | 2015-05-06 | 2017-12-15 | 杭州云界生物科技有限公司 | A kind of preparation method of nano titanium oxide |
| CN106632787A (en) * | 2016-11-30 | 2017-05-10 | 上海纳米技术及应用国家工程研究中心有限公司 | Optical transparent polymer-titanium dioxide core-shell microspheres as well as preparation and application |
| TWI709419B (en) * | 2019-05-31 | 2020-11-11 | 國立虎尾科技大學 | Structure antibacterial film, its preparation method and application |
| CN114643077A (en) * | 2022-03-02 | 2022-06-21 | 湖北大学 | Microporous polymer with photocatalytic activity and preparation method thereof |
| CN114643077B (en) * | 2022-03-02 | 2023-09-26 | 湖北大学 | Microporous gel polymer with photocatalytic activity and preparation method thereof |
| CN115486443A (en) * | 2022-09-16 | 2022-12-20 | 中国科学院赣江创新研究院 | Cerium-doped titanium dioxide-polystyrene microsphere composite antibacterial material and preparation method and application thereof |
| CN115486443B (en) * | 2022-09-16 | 2023-11-10 | 中国科学院赣江创新研究院 | Cerium doped titanium dioxide-polystyrene microsphere composite antibacterial material and preparation method and application thereof |
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