CN1328095A - Self-cleaning antibacterial coating composition and its preparing process and application - Google Patents
Self-cleaning antibacterial coating composition and its preparing process and application Download PDFInfo
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- CN1328095A CN1328095A CN 00109154 CN00109154A CN1328095A CN 1328095 A CN1328095 A CN 1328095A CN 00109154 CN00109154 CN 00109154 CN 00109154 A CN00109154 A CN 00109154A CN 1328095 A CN1328095 A CN 1328095A
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Abstract
A self-cleaning antibacterial coating composition contains photosemiconductor TiO2 particles (less than 50 nm) (0.25-10%) and H4TiO5 (0.13-4%), and is prepared through hydrolyzing Ti salt compound to prepare titanic acid, and reaction with hydrogen peroxide while heating and stirring. It can be coated on the surface of metal or ceramic and has sterilizing action under action of weak light.
Description
The present invention relates to a kind of self-cleaning antibacterial coating composition, particularly relate to a kind of colloidal solution preparation of self-cleaning antibacterial coating composition.The invention still further relates to a kind of preparation method and application of colloidal solution preparation of described self-cleaning antibacterial coating composition.
In recent years, various germ resistance life goods have become the focus of consuming on the market.The antimicrobial treatment of product surface adopts precious metal anti-biotic materials such as organic bactericide and silver more.Organic bactericide is not only to human body safety inadequately, and sterilant is dissolved easily and runs off and lose effect when washing, is not suitable for the goods that need such as pottery, glass, metal form through high-temperature firing.The precious metal anti-biotic material then has been subjected to considerable restraint because of lattice are expensive on using.
With TiO
2For the photosemiconductor material of representative is causing extensive concern in the applied research aspect the environment such as antibiotic, self-cleaning.This photosemiconductor material is under the effect of the UV-light about natural light or 360nm, and its surface can inspire unbound electron and form the hole of a positively charged simultaneously, and then causes a series of redox reactions, produces hydroxyl and active oxygen radical.These free radicals have very strong redox ability.It can decompose the various organic compound that are adsorbed in its surface, killing bacteria, and microorganisms such as virus play significant anti-microbial effect.
But attached to various material surfaces, strong, the robust problem of its activity is not resolved for a long time photosemiconductor.The method of prior art has sol-gel method, and chemistry is steaming method etc., manufacturing cost costliness not only, and a little less than the activity, on producing and using, be difficult to penetration and promotion.And to have the whole bag of tricks now with TiO
2The coating fluid of photosemiconductor particles dispersed in water all is difficult to form strong and have highly active filming.
It is strong that the present invention aims to provide a kind of film forming ability, active high, cheap, the self-cleaning antibacterial coating composition that the scope of application is extensive.
Self-cleaning antibacterial coating composition of the present invention is water miscible colloidal solution, contains the titanium dioxide (TiO of particle diameter less than 50nm
2) photosemiconductor particle and high metatitanic acid (H
4TiO
5).TiO
2Content is 0.25-10%, H
4TiO
5Content is 0.13-4%, TiO
2/ H
4TiO
5The content ratio is 0.3-6.
Among the present invention, TiO
2Preferred content be 1-4%, H
4TiO
5Preferred content be 0.5-2%, TiO
2/ H
4TiO
5The content ratio is preferably 1-4; Its optimum content is TiO
22%, H
4TiO
51%, TiO
2/ H
4TiO
5The content ratio is 2.
This TiO
2The photosemiconductor particle has the antibiosis and self-cleaning activity, and high metatitanic acid can improve the dispersed of colloidal solution and can improve the intensity and the sticking power of filming.TiO
2Content is lower than 0.25% does not almost have activity, and greater than 10% difficulty in preparation, the transparency of filming and sticking power are very poor.H
4TiO
5Content is dispersed easily bad less than 0.13% o'clock colloidal solution, can form the jelly shape because of viscosity is too high greater than 4% o'clock colloidal solution, loses use value.TiO
2/ H
4TiO
5The content ratio was less than 0.3 o'clock, and colloidal solution can be crossed the low practical value of not having because of activity.TiO
2/ H
4TiO
5The content ratio was greater than 6 o'clock, and colloidal solution precipitates in preparation and storage process easily, and film adhesive is very poor.
The preparation method of colloidal solution of the present invention is:
1. the titanium salt compound is prepared metatitanic acid through hydrolysis reaction;
2. the metatitanic acid and the aqueous solution that contains hydrogen peroxide are reacted, make the aqueous solution that contains metatitanic acid and high metatitanic acid;
3. heated and stirred is handled the above-mentioned aqueous solution, promotes the TiO of particle diameter less than 50nm
2The photosemiconductor particulate forms;
Described titanium salt compound can be from titanium sulfate, selects in the titanium tetrachloride, Titanium Nitrate and organic titanic compound etc.Described high metatitanic acid is the resultant behind metatitanic acid and the hydroperoxidation.
Germ resistance coating composition of the present invention is coated pottery, metal, glass, plastics and fiber and other material surface can form transparent, strong pottery and film after the drying.This filming, thickness can be brought into play significant sterilizing function usually between 0.1-0.5 μ m.Under faint natural light and artificial light effect, can produce automatic sterilizing and disinfectant effect to various bacteriums and inhibition breeding of virus generation intensive and killing actions such as intestinal bacteria, streptococcus aureus, Pseudomonas aeruginosas.
Below in conjunction with embodiment the present invention is done further detailed elaboration.
Embodiment 1
10% titanium sulfate aqueous solution 900ml adds 10%NaOH aqueous solution 500ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 35g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 2%TiO
2, 1%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 2.
The making of antimicrobial prod and effect assessment thereof
1. making method
The colloidal solution of embodiment 1 preparation is pressed 10mg/m
2Amount evenly coat glass, ceramic disc, glazing ceramic tile (entire body brick) surface respectively, dry back heat treated 30 minutes under 500 ℃ condition obtains to have three kinds of goods samples of antibacterial film coating.
2. coating strength is measured
1) with the powerful repeatedly friction of rubber 100 times, three kinds of goods samples all do not find to have filmed any obscission.
2) the determination of pencil hardness method of filming with coating is tested.The coating strength of three kinds of goods specimen surfaces of proof all reaches more than the 9H.
3. antibacterial tests one
1) three kinds of specimen surfaces evenly are coated with intestinal bacteria and Salmonellas mixed solution respectively.Also be coated with bacterium at the specimen surface of handling without filming simultaneously and compare group.
2) test group and control group all are placed under the 100W bulb and shone 2 hours.
3) at two groups of specimen surfaces with the sampling of disinfecting silk or cotton swabs, cultivate in 37 ℃ after being applied to plate.
4) observe contrast bacterial growth situation.
The result: three kinds of specimen surfaces of test group, 30% bacterium of all having an appointment is killed, and control group covers with by bacterium.
4. antibacterial tests two
Sample is basic identical with antibacterial tests one with test method, and only the 3rd of test the step was that two test group samples are placed irradiation 3 hours (placing angle is 45 degree, and the time is 9:00-12:00am) under the sunlight.
Result: the not long bacterium colony in entire body brick surface, sterilization effect 100%; Glass surface is a bacterium colony only, sterilization effect 99%; The not long bacterium colony in ceramic disc surface, sterilization effect 100%.
(antibacterial tests one, two) test unit: animal medicine microbial room of China Agricultural University
5. antibacterial tests three
Cultured e. coli jm109 is coated in respectively on the tableware and contrast tableware of the antibacterial film coating processing of crossing, under fine illumination and cloudy illumination, placed 1-4 hour with aseptic water washing.Use the physiological saline wash dining set, get washings 0.1ml and be coated with on the LB flat board, be placed on overnight incubation in 37 ℃ of thermostat containers, do the bacterium counting.The intestinal bacteria count results sees Table 1.
Table 1 germ resistance qualification result
| Minute | Antibacterial film coating is handled tableware | The contrast tableware | ||
| Fine | Cloudy day | Fine | Cloudy day | |
| 0 hour | ????0 | ????0 | ????0 | ????0 |
| 1 hour | Undetermined | ????0 | Undetermined | ????200 |
| 2 hours | ????16 | Undetermined | ????210 | Undetermined |
| 3 hours | ????0 | ????2 | ????37 | ????110 |
| 4 hours | Undetermined | ????2 | Undetermined | ????150 |
The tableware that antibacterial film coating is handled no matter fine illumination or cloudy diffusion light according under, the bacterium counting is seldom or aseptic; The contrast tableware does not have effect to intestinal bacteria.
Conclusion: the self-cleaning antibacterial coating of being tested has significant killing action with composition to intestinal bacteria.
Test unit: Institute of Microorganism, Academia Sinica.
6. chmice acute per os toxicity test
1) test sample: after the ceramic tile that colloidal solution was handled is pulverized, suspend, make the testing liquid of 255mg/ml with soybean salad oil.
2) experimental animal: three grades of Kunming mouses.
3) test method
Administration group and control group male and female are respectively with 10 mouse, fasting is 16 hours before the administration, and administration group male and female mouse is pressed the 10200mg/kg administration after the mensuration body weight, with oral administration of irrigation stomach device, administration volume 40ml/kg body weight, control group gives the solvent soybean salad oil with volume.
Observe once every day after the administration, and viewing duration is 7 days, measured body weight on the 1st, 3,5,7 day, carries out the t check, through the check there was no significant difference.Cut open inspection after the off-test.
4) result
Animal no abnormality seen reaction after the administration, body weight is in rising trend.Mouse is 10200mg/kg to the maximum tolerated dose of the ceramic tile gastric infusion that colloidal solution was handled.
Test unit: Nat'l Pharmaceutical ﹠ Biological Products Control Institute
Embodiment 2
10% titanium tetrachloride aqueous solution 720ml adds 10%NaOH aqueous solution 500ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 35g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 2%TiO
2, 1%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 2.
Embodiment 3
With 95g organic titanium salt compound Ti (OC
3H
7)
4Join 10%NaOH aqueous solution 500ml, the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.The aqueous hydrogen peroxide solution of 35g 30%, drops into behind this titanium hydroxide powder adding distil water again and adjusts to 1000ml to 500ml with distilled water diluting then, heated and stirred to solution transparent till.Acquisition contains 2%TiO
2, 1%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 2.
Embodiment 4
10% titanium sulfate aqueous solution 1800ml adds 10%NaOH aqueous solution 1000ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 70g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 4%TiO
2, 2%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 2.
Embodiment 5
10% titanium sulfate aqueous solution 450ml adds 10%NaOH aqueous solution 250ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 17.5g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 1%TiO
2, 0.5%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 2.
Embodiment 6
10% titanium sulfate aqueous solution 225ml adds 10%NaOH aqueous solution 125ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 8.8g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 0.5%TiO
2, 0.25%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 2.
Embodiment 7
10% titanium sulfate aqueous solution 2700ml adds 10%NaOH aqueous solution 1500ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 105g 30% with distilled water diluting to 500ml, drop into this titanium hydroxide powder after redistilled water adjust to 1000ml, through abundant heated and stirred.Acquisition contains 6%TiO
2, 3%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the translucent solution that is 2.
Embodiment 8
10% titanium sulfate aqueous solution 1101ml adds 10% NaOH aqueous solution 665ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 70g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 2%TiO
2, 2%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 1.
Embodiment 9
10% titanium sulfate aqueous solution 800ml adds 10%NaOH aqueous solution 445ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 17.5g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 2%TiO
2, 0.5%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 4.
Embodiment 10
10% titanium sulfate aqueous solution 750ml adds 10%NaOH aqueous solution 417ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 70g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 1%TiO
2, 2%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 0.5.
Embodiment 11
10% titanium sulfate aqueous solution 3670ml adds 10%NaOH aqueous solution 2038ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 87.5g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, through abundant heated and stirred.Acquisition contains 10%TiO
2, 2.5%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the opaque colloidal solution that is 4.
Embodiment 12
Doubly after the dilution, stirred 30 minutes with distilled water etc. implementing 4 colloidal solution.Acquisition contains 0.25%TiO
2, 0.13%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 2.
Embodiment 13
10% titanium sulfate aqueous solution 2200ml adds 10% NaOH aqueous solution 400ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 140g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, after the heated and stirred.Acquisition contains 4%TiO
2, 4%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the jelly shape dope that is 1.
Embodiment 14
10% titanium sulfate aqueous solution 970ml adds 10% NaOH aqueous solution 539ml, and the reaction 30 minutes that is hydrolyzed under constantly stirring filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 105g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, heated and stirred to solution transparent till.Acquisition contains 1%TiO
2, 3%H
4TiO
5, TiO
2/ H
4TiO
5Content is than the transparent colloidal solution that is 0.3.
Embodiment 15
10% titanium sulfate aqueous solution 2280ml adds 10%NaOH aqueous solution 1267ml, and the reaction 30 minutes that is hydrolyzed under stirring condition filters out the titanium hydroxide powder that reaction generates.Then with the aqueous hydrogen peroxide solution of 35g 30% with distilled water diluting to 500ml, drop into behind this titanium hydroxide powder again adding distil water and adjust to 1000ml, through abundant heated and stirred.Acquisition contains 6%TiO
2, 1%H
4TiO
5, TiO
2/ H
4TiO
5Content is placed and after 2 hours precipitation has been taken place than the translucent liquid solution that is 6.
The effect assessment of filming test
1. after the liquid composition of the various embodiments described above preparation evenly being coated microscope usefulness glass slide surface with writing brush respectively, drying is 1 hour under 100 ℃ of conditions.The test materials that has obtained to film and handled.
2. under aseptic technique, with each test materials and the control material handled of not filming be that the intestinal bacteria liquid of 1000/ml evenly is coated with concentration respectively.
3. under the condition of preserving moisture, each processing material through filming and control group were placed under the 15W black lamp 15cm place radiation treatment 2 hours.
4. wash towards each test materials surface with stroke-physiological saline solution, washing lotion is cultivated under 37 ℃ of conditions, measure sterilization effect.Test-results sees Table 2.
5. the residual situation of filming is observed in rubber powerful repeatedly friction 20 times on each test materials surface.The film adhesive measurement result sees Table 2.
Test unit: animal medicine microbial room of China Agricultural University
The various coating compositions of table 2 become to be grouped into and performance compares
*Excellent-no change of filming; Very-small quantities of powder shape cast arranged; In-a large amount of Powdered casts are arranged; Differ from-all come off
| Embodiment | ???TiO 2Content | ??H 4TiO 5% content | ??TiO 2/ ??H 4TiO 5 | The transparency | Dispersed | Sticking power * | Average bactericidal rate |
| ???1 | ????2％ | ????1％ | ????2 | Transparent | Well | Excellent | ????98％ |
| ???2 | ????2％ | ????1％ | ????2 | Transparent | Well | Excellent | ????95％ |
| ???3 | ????2％ | ????1％ | ????2 | Transparent | Well | Excellent | ????100％ |
| ???4 | ????4％ | ????2％ | ????2 | Transparent | Well | Excellent | ????100％ |
| ???5 | ????1％ | ????0.5％ | ????2 | Transparent | Well | Excellent | ????82％ |
| ???6 | ????0.5％ | ????0.25％ | ????2 | Transparent | Well | Excellent | ????51％ |
| ???7 | ????6％ | ????3％ | ????2 | Translucent | Well | Very | ????98％ |
| ???8 | ????2％ | ????2％ | ????1 | Transparent | Well | Excellent | ????78％ |
| ???9 | ????2％ | ????0.5％ | ????4 | Transparent | Well | Excellent | ????90％ |
| ???10 | ????1％ | ????2％ | ????0.5 | Transparent | Well | Excellent | ????42％ |
| ???11 | ????10％ | ????2.5％ | ????4 | Opaque | Bad | In | ????94％ |
| ???12 | ????0.25 | ????0.13％ | ????2 | Transparent | Well | Excellent | ????12％ |
| ???13 | ????4％ | ????4％ | ????1 | Translucent | The jelly shape | Difference | Undetermined |
| ???14 | ????1％ | ????3％ | ????0.3 | Transparent | Well | Excellent | ????5％ |
| ???15 | ????6％ | ????1％ | ????6 | Translucent | Precipitation | Difference | Undetermined |
Claims (5)
1. a self-cleaning antibacterial coating composition is characterized in that described composition is water miscible colloidal solution, contains the titanium dioxide (TiO of particle diameter less than 50nm
2) photosemiconductor particle, high metatitanic acid (H
4TiO
5); TiO wherein
2Content is 0.25-10%, H
4TiO
5Content is 0.13-4%, TiO
2/ H
4TiO
5The content ratio is 0.3-6.
2. the described self-cleaning antibacterial coating composition of claim 1 is characterized in that TiO
2Preferred content be 1-4%, H
4TiO
5Preferred content be 0.5-2%, TiO
2/ H
4TiO
5The preferred content ratio be 1-4; TiO in the said composition
2Optimum content be TiO
22%, H
4TiO
51%, TiO
2/ H
4TiO
5The optimum content ratio be 2.
3. the preparation method of the described self-cleaning antibacterial coating composition of claim 1 is characterized in that the preparation method is following steps:
(1) the titanium salt compound is being prepared metatitanic acid (H through after the hydrolysis under the alkaline condition
4TiO
4);
(2) metatitanic acid and the reactant aqueous solution that contains hydrogen peroxide are made the aqueous solution that contains metatitanic acid and high metatitanic acid;
(3) heated and stirred is handled the above-mentioned aqueous solution, promotes the TiO of particle diameter less than 50nm
2The photosemiconductor particulate forms.
4. the preparation method of the described self-cleaning antibacterial coating composition of claim 3, wherein said titanium salt compound can be from titanium sulfate, and titanium tetrachloride is selected in Titanium Nitrate and the organic titanic compound.
5. the application of the described self-cleaning antibacterial coating composition of claim 1 is characterized in that being used for the material surface processing of filming, thereby obtains antibiotic, self-cleaning function.
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|---|---|---|---|
| CN 00109154 CN1328095A (en) | 2000-06-13 | 2000-06-13 | Self-cleaning antibacterial coating composition and its preparing process and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00109154 CN1328095A (en) | 2000-06-13 | 2000-06-13 | Self-cleaning antibacterial coating composition and its preparing process and application |
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| Publication Number | Publication Date |
|---|---|
| CN1328095A true CN1328095A (en) | 2001-12-26 |
Family
ID=4579459
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100450364C (en) * | 2002-01-15 | 2009-01-14 | 崔光洙 | The liquid composition for promoting plant growth, which includes nano-particle titanium dioxide |
-
2000
- 2000-06-13 CN CN 00109154 patent/CN1328095A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100450364C (en) * | 2002-01-15 | 2009-01-14 | 崔光洙 | The liquid composition for promoting plant growth, which includes nano-particle titanium dioxide |
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