CN101322497A - Active stephanoporate mineral TiO2-doped composite catalytic antimicrobial material preparation and using method - Google Patents
Active stephanoporate mineral TiO2-doped composite catalytic antimicrobial material preparation and using method Download PDFInfo
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- CN101322497A CN101322497A CN 200810045513 CN200810045513A CN101322497A CN 101322497 A CN101322497 A CN 101322497A CN 200810045513 CN200810045513 CN 200810045513 CN 200810045513 A CN200810045513 A CN 200810045513A CN 101322497 A CN101322497 A CN 101322497A
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Abstract
The invention discloses a preparation and using method of multiple active porous mineral doped nano-TiO2 composite catalytic anti-bacterial materials, and the preparation and using method belongs to the technical field of new material. The main technical key point of the invention is to combine the anti-bacterial mechanism of the ion modified porous minerals and the photo-catalytic anti-bacterial mechanism of the element doped nano-TiO2 to realize the synergistic anti-bacterial role, the modification of the porous minerals by the metal anti-bacterial ion (one of Ag<+>, Cu<2+>, Zn<2+> and Fe<3+>) and the rare earth ion and the nano-TiO2 doped synchronous composite process technology by the metal anti-bacterial ion and the rare earth ion are realized during the preparation process, thereby obtaining the composite catalytic anti-bacterial composite materials which are characterized by broad-spectrum, long-acting effect and safety, etc. The composite catalytic anti-bacterial products prepared by adopting the method and the technical process have low cost, anti-bacterial and long-acting effects, broad-spectrum and good synergistic anti-bacterial effect, the preparation process of the materials has the advantages of simpleness and strong operationality, and the like, so the preparation and using method can be widely applied in anti-bacterial coating, putty, fabric and other industries.
Description
(1) technical field
The present invention relates to a kind of compound urging and change antibiotic functional material, belong to the anti-biotic material technical field.Be specifically related to antibacterial metal ions Ag
+, Cu
2+, Zn
2+, Fe
3+In one or more, rare earth ion is to porous mineral material modification and nano-TiO
2Doping is the compound method for preparing anti-biotic material and use thereof synchronously.
(2) background technology
Along with the raising day by day of people's living standard, various daily necessities healthization have become the trend of current social development.The product that comprises a lot of fields such as household electrical appliances, daily living article is at present all made all kinds of consumer goods with antibacterial functions at the application anti-biotic material as additive.As antimicrobial refrigerator, antibiotic plastic packing, antibacterial fabric etc.Inorganic antiseptic is difficult for producing outstanding features such as drug resistance with its broad-spectrum antibacterial property, persistence, chemical stability, weather resistance, warm tolerance, safety, bacterium, become the glad class antibacterial agent of selecting of potentialization and people.
Inorganic antiseptic is made up of antibacterial activity composition and carrier, antibacterial activity mainly is a metal ion, using maximum antibacterial metal ions at present is silver, zinc, copper etc., carrier is a zeolite, attapulgite, sepiolite, vermiculite and montmorillonite, active carbon, Woelm Alumina, porous silicon, the charcoal fiber, apatite etc., its mesolite, attapulgite, sepiolite, mineral such as vermiculite and montmorillonite are the natural minerals of cation exchange capacity maximum, what research application at present was more is the commutative characteristic of utilizing in these mineral structures of cation, different metal antibacterial ion exchange is prepared the novel inorganic anti-biotic material to mineral structure, through having more than 160 (domestic) in last inquiry patent in this respect.Disclosing a kind of vermiculite as Chinese patent CN1271523A is inorganic antiseptic of carrier and preparation method thereof, and this method is to utilize ion exchange principle, and copper ion is implanted between vermiculite layers, makes the anti-biotic material of cupric 0.5-8.5%; It is the inorganic antiseptic and preparation method thereof of carrier with the palygorskite that Chinese patent CN1339257A discloses a kind of, and this method is at first handled palygorskite with acid activation, makes by the silver ion or the copper ion of absorption as antibacterial components then; Chinese patent CN02129370 discloses a kind of silver-carried fluor apatite antimicrobials and preparation method thereof, this method at first prepares amorphous nano silver-carrying fluor-apatite powder with coprecipitation, and then strengthen its year of silver-colored effect by high-temperature calcination, obtain silver-carried fluor apatite antimicrobials.Above ionic antibacterial agent mainly is that the metal ion that will have antibacterial action is carried on certain carrier, and by slow release metal ions performance antibacterial action, but its shortcoming is also obvious, and a little less than mildew-resistant, compound antifungic action, cost is higher, and is easy to change etc.
Another kind of inorganic antiseptic is with TiO
2Antibacterial agent for representative with photocatalysis.The photocatalysis characteristic of photocatalysis material of titanium dioxide and antibacterial characteristics all need exciting of ultraviolet light, and less because of the content of ultraviolet light in sunshine on the one hand, titanium dioxide is low to the availability of sunshine, causes photocatalysis efficiency low; Limited the titanium dioxide catalysis material in indoor application indoor because no ultraviolet light exists on the other hand, perhaps will join ultraviolet source in addition, given to be suitable for and make troubles.And the patent of application mainly to concentrate on nanometer two titaniums be carrier, prepare photocatalysis antibacterial material at its surface absorption antibacterial metal ions, perhaps utilize rare earth, transition metal, element such as nonmetal that nano titanium oxide is mixed to change the photocatalysis respective wavelength, preparation has the photocatalysis antibacterial material of anti-microbial property at visible light.
To sum up, based on porous mineral ion modification (antibacterial metal ions, rare earth element) and antibacterial metal ions or contain can rare earth doped nano-TiO
2The patent of preparation of composite catalytic antimicrobial functional material and application facet yet there are no report.Modified porous mineral antibacterial agent and nano-TiO
2Technology of preparing will with low cost, broad spectrum activity, long-lasting be target, with the nano-TiO of tool high light catalytic antimicrobial performance under modified porous mineral functional material with good antibacterial performance, the visible light
2Emphasis as research.In conjunction with and utilize have good antibacterial performance, modified porous mineral and the high dopen Nano TiO of photocatalysis efficiency cheaply
2It also will be the important thinking of promoting this type of functional material extensive use.Therefore, the present invention adopt metal antibacterial ion and rare earth element to porous mineral modification and rare earth element to TiO
2The synchronous compound preparation photocatalysis antibacterial functional material that mixes, and its photocatalysis composite antibiosis performance carried out system research, on this basis, be applied in the industries such as coating, fabric, plastics, rubber, latex.
(3) summary of the invention
1, goal of the invention
Technical problem to be solved by this invention is to avoid existing problem in the above-mentioned antibacterial agent material prior art, provides a kind of raw materials consumption few, and technology is simple, and production cost is low, and has more excellent physicochemical property.The porous mineral that has ion-exchange performance with zeolite, attapulgite, sepiolite, expanded vermiculite etc. is a preparing carriers composite catalytic antimicrobial material.Key problem in technology is to have realized in the antibacterial agent preparation process metal antibacterial ion (Ag of porous mineral
+, Cu
2+, Zn
2+, Fe
3+In one or more), rare earth ion doped and antibacterial metal ions loaded with nano TiO
2Composite technology is realized antibiotic mechanism of modified porous mineral ion type and rare earth mixing with nano TiO synchronously
2(or nano SnO
2, nano-ZnO) the synergetic antibacterial effect that combines of composite catalytic antimicrobial mechanism.Thereby obtain the composite catalytic antimicrobial functional material with safety, antibiotic wide spectrum, long-acting performance of use under environment (intensity of illumination, humidity), and prepared goods such as composite photocatalyst antibacterial functions coating, fabric, plastics, rubber, latex.
2, technical scheme
1. active porous mineral dopen Nano TiO
2The composite catalytic antimicrobial material preparation
With metal antibacterial ion (Ag
+, Cu
2+, Zn
2+, Fe
3+In one or more), rare earth ion (La
3+, Ce
3+, Pr
3+, Eu
3+, Sm
3+, Gd
3+In one or more) and hydrolysis inhibitor (acetylacetone,2,4-pentanedione) join in the absolute ethyl alcohol together, and stir, then with butyl titanate by volume (butyl titanate: absolute ethyl alcohol is 1: 3) slowly join in the above-mentioned solution, stir fast while dripping, after stirring certain hour again, add a certain amount of deionized water, promptly form colloidal sol, (liquid-solid ratio 1: 1) adds a certain amount of through fragmentation more according to a certain percentage, grinding is to the porous mineral (zeolite of-0.074mm, montmorillonite, sepiolite, palygorskite, in the expanded vermiculite a kind of or wherein a kind of with another or multiple), it is even to continue dispersed with stirring, slowly drop to a certain amount of nitric acid and absolute ethyl alcohol in the suspension simultaneously, at last, slowly drip deionized water and make sol-hydrolysis, gel.Promptly obtain predecessor after said process gained mixture being placed 120 ℃ baking oven oven dry, at last with gel in 550 ℃ of calcining 2h down, promptly finish porous mineral modification and rare earth ion doped nano-TiO
2Compound synchronously, prepare modified porous mineral dopen Nano TiO
2The composite photocatalyst antibiotic functional material, wherein metal antibacterial ion and the rare earth ion content in antibiotic functional material is controlled at 0.6～60mg/g and 0.5～30mg/g respectively.
2. active porous mineral doped Ti O
2The preparation of composite photocatalyst antibiotic paint
To be ground to-the active porous mineral doped Ti O of 0.074mm
2Composite catalytic antimicrobial material (3 parts), commercial coating (97 parts) mix, and after high-speed stirred is uniformly dispersed, promptly prepare the coating with photocatalysis antibacterial function.
3. active porous mineral doped Ti O
2The preparation of composite photocatalyst antibiotic fabric
Active porous mineral doped Ti O with preparation
2The composite catalytic antimicrobial material grinds (granularity d
90For about-0.049mm), mix the back spinning with spinning slurry according to the content of 0.5～1.0% (mass percent), be processed into fabric.
4. active porous mineral doped Ti O
2The preparation of composite photocatalyst antibacterial functions composite plastic
Active porous mineral doped Ti O with preparation
2Composite catalytic antimicrobial material grinding is to-0.049mm, and the content according to 0.5～5.0% is made with the plastics extruding and is processed into mother particles of antibacterial plastics, and the composite plastic with anti-microbial property is promptly prepared in further processing.
5. active porous mineral doped Ti O
2The preparation of composite photocatalyst antibacterial rubber
Active porous mineral doped Ti O with preparation
2Composite catalytic antimicrobial material grinding is to-0.049mm, after content according to 0.1～5.0% and rubber are mixing, adds promoter again, vulcanizing agent can be prepared antibacterial rubber.
6. active porous mineral doped Ti O
2The preparation of composite photocatalyst antibacterial latex
Active porous mineral doped Ti O with preparation
2Composite catalytic antimicrobial material grinding is to-0.049mm, and the content according to 1.0～5.0% joins in the latex, after high-speed stirred is uniformly dispersed, promptly prepares antibacterial latex.
3. the key technical indexes
1. each composition (is mainly porous mineral and nano-TiO in the composite catalytic antimicrobial material
2) be evenly distributed, no one-component is gathered into larger particles phenomenon, TiO
2Particle diameter is a nanoscale.Price is lower than nano-TiO
2The market price of photochemical catalyst, the bacteriostasis rate to Escherichia coli, staphylococcus aureus under different condition (intensity of illumination, humidity) all is higher than 99%, MIC is lower than 40 μ g/mL, satisfy as the coating additive requirement, whiteness be not less than 95 degree (°).
2. the composite catalytic antimicrobial functional paint satisfies the construction requirement under the different condition, has long-acting, broad-spectrum antiseptic characteristics, and to nontoxic, harmless (the acute oral toxicity LD of human body
50＞5000mg), the bacteriostasis rate of Escherichia coli, staphylococcus aureus all is higher than 95%, meet the GB/9756-2001 standard when using as interior wall coating.
3. the composite catalytic antimicrobial function fabric characteristics that have that long-actingly, water-fast wash, spectrum is antibiotic etc. meet textile industry standard FZ/T 73023-2006, and to advantages such as human body safety.Bacteriostasis rate to Escherichia coli, staphylococcus aureus all is higher than 95%, and function fabric bacteriostasis rate after washing 30 times is not less than 90%.
4. composite photocatalyst antibacterial functions plastics have long-actingly, water-fast wash, characteristics that spectrum is antibiotic, meet antibiotic composite plastic industry standard QB/T 2591-2003, to human body safety, bacteriostasis rate to Escherichia coli, staphylococcus aureus all is higher than 95%, uses that bacteriostasis rate is not less than 90% after 365 days.
5. composite photocatalyst antibacterial functions rubber have long-actingly, water-fast wash, characteristics that spectrum is antibiotic, to human body safety, the bacteriostasis rate of Escherichia coli, staphylococcus aureus is higher than 95%, use that bacteriostasis rate is not less than 90% after 365 days.
6. composite photocatalyst antibacterial functions latex have long-actingly, water-fast wash, characteristics that spectrum is antibiotic, to human body safety, the bacteriostasis rate of Escherichia coli, staphylococcus aureus is higher than 95%, bacteriostasis rate is not less than 90% after washing 30 times.
(4) description of drawings
Fig. 1 is active porous mineral doped Ti O
2The preparation flow of composite catalytic antimicrobial material; Fig. 2 is the preparation flow figure of composite catalytic antimicrobial coating; Fig. 3 is the preparation flow figure of composite catalytic antimicrobial fabric; Fig. 4 is the preparation flow of composite catalytic antimicrobial plastics; Fig. 5 is the preparation flow of composite catalytic antimicrobial rubber; The preparation flow of Fig. 6 composite catalytic antimicrobial latex.
(5) embodiment
Be several concrete embodiment of the present invention below.
1, preparation active porous mineral doped Ti O
2The embodiment of composite catalytic antimicrobial material
1. contain Zn
2+, La
3+The base and doped TiO of activated zeolite
2The composite catalytic antimicrobial material
Annotate: Zn in the material
2+And La
3+Content is respectively 0.6mg/g and 0.5mg/g; A is Detitanium-ore-type TiO
2, R is rutile TiO
2
2. contain Cu
2+, Ce
3+The base and doped TiO of activated zeolite
2The composite catalytic antimicrobial material
Annotate: Cu in the material
2+And Ce
3+Content is respectively 10mg/g and 10mg/g; A is Detitanium-ore-type TiO
2, R is rutile TiO
2
3. partially porous mineral doped Ti O
2The composite catalytic antimicrobial material property
2, the embodiment of functional paint
Annotate: the addition (mass percent) of composite catalytic antimicrobial material in coating is 3%.
3, the embodiment of antibiotic fabric
4, the embodiment of antibiotic plastic
5, the embodiment of antibacterial rubber
6, the embodiment of antibacterial latex
Can prepare the product that reaches the object of the invention by the various embodiments described above and according to aforementioned production method.Embodiments of the invention all can be implemented, and the invention is not restricted to these embodiment.
Claims (9)
1, a kind of active porous mineral doped Ti O
2The composite catalytic antimicrobial preparation methods is characterized in that, with active porous mineral material ion antibacterial mechanism and rare earth ion doped nano-TiO
2The photocatalysis antibacterial mechanism realization synergetic antibacterial effect that combines, in preparation process, realize metal antibacterial ion, rare earth ion to the activity of porous mineral with to nano-TiO
2The synchronous composite technology that mixes, thus obtain to have wide spectrum and characteristics antibacterial functions composite such as long-lasting.
2, porous mineral doped Ti O according to claim 1
2The composite catalytic antimicrobial preparation methods, it is characterized in that, described porous mineral purity all is higher than 80%, is mainly one or more the mixed mineral in zeolite, sepiolite, palygorskite, the expanded vermiculite, the porous mineral powder that obtains to-the 0.074mm through broken, grinding.
3, porous mineral loaded with nano TiO according to claim 1
2The composite catalytic antimicrobial preparation methods is characterized in that, described metal antibacterial ion or doping ion are Ag
+, Cu
2+, Zn
2+, Fe
3+In one or more; Described doping ion is that metal antibacterial ion or rare earth ion are La
3+, Ce
3+, Pr
3+, Eu
3+, Sm
3+, Gd
3+In one or more, part ion wherein can ion for containing.
4, porous mineral doped Ti O according to claim 1 and 2
2The composite catalytic antimicrobial preparation methods is characterized in that, the preparation of described composite antibacterial material is to pass through TiO with metal antibacterial ion and rare earth ion that concentration is respectively 0.6～60mg/g and 0.5～30mg/g
2Element doping and will carry out a kind of in zeolite, sepiolite, palygorskite, the expanded vermiculite or two or more the priority of ion activity in same reaction system of heterogeneous mineral powder wherein, realize the synthetic synchronously composite antibacterial material that obtains; Composite antibacterial material all is higher than 99% to the bacteriostasis rate of Escherichia coli and staphylococcus aureus.
5, utilize the described porous mineral doped Ti of claim 1 O
2The method of composite catalytic antimicrobial material preparation antibiotic paint is characterized in that, with the base and doped TiO of active porous mineral of preparation
2Composite catalytic antimicrobial material grinding is to-0.074mm, and the content according to 1.0～5.0% joins in the commercially available exterior coating, after high-speed stirred is uniformly dispersed, promptly prepares antibiotic paint.
6, utilize the described porous mineral doped Ti of claim 1 O
2The method of composite catalytic antimicrobial material preparation antibiotic fabric is characterized in that the active porous mineral doped Ti O with preparation
2Composite catalytic antimicrobial material grinding is to-0.049mm, and the content according to 0.5～1.0% mixes spinning afterwards with spinning slurry, promptly prepare antibiotic fabric after the processing.
7, utilize the described porous mineral doped Ti of claim 1 O
2The method of composite catalytic antimicrobial material preparation antibiotic plastic is characterized in that the active porous mineral doped Ti O with preparation
2Composite catalytic antimicrobial material grinding is to-0.049mm, and the content according to 0.5～5.0% is made with the plastics extruding and is processed into mother particles of antibacterial plastics, and antibiotic plastic is promptly prepared in further processing.
8, utilize the described porous mineral doped Ti of claim 1 O
2The method of composite catalytic antimicrobial material preparation antibiotic fabric is characterized in that the active porous mineral doped Ti O with preparation
2Composite catalytic antimicrobial material grinding is to-0.049mm, after content according to 0.1～5.0% and rubber are mixing, adds promoter again, vulcanizing agent can be prepared antibacterial rubber.
9, utilize the described porous mineral doped Ti of claim 1 O
2The method of composite catalytic antimicrobial material preparation antibiotic fabric is characterized in that the active porous mineral doped Ti O with preparation
2Composite catalytic antimicrobial material grinding is to-0.049mm, and the content according to 1.0～5.0% joins in the latex, after high-speed stirred is uniformly dispersed, promptly prepares antibacterial latex.
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