CN1742582A - Photocatalyst-type anti-biotic material preparing method - Google Patents
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Abstract
The preparation method of photocatalytic type antimicrobial material includes the following steps: A. preparing antimicrobial solution and pretreating material surface; B. coating material surface with antimicrobial solution and forming antimicrobial film on the material surface; C. drying antimicrobial solution coated on the material surface; D. utilizing thermal treatment to accelerate the combination of antimicrobial layer and base body surface, at the same time making photocatalytic antimicrobial layer implement anatase crystalline conversion. The described antimicrobial solution is antimicrobial sol solution containing nano titanium dioxide or composite antimicrobial sol solution containing titanium dioxide and silver.
Description
[technical field]
The present invention relates to a kind of anti-biotic material preparation method, especially relate to a kind of photocatalyst-type anti-biotic material preparation method.
[background technology]
At present along with social development and growth in the living standard, people strengthen gradually to health, health, cleaning, fungi-proofing consciousness, market constantly increases for the demand of antimicrobial product, people are expecting that daily living article has the energy antibacterial functions, therefore antibacterial metal goods applying in life will be caused the new revolution of health field.
Especially the optically catalytic TiO 2 anti-microbial property is extensively approved, the preparation method of nano titanium oxide is also a lot, and the preparation method can be summed up as physical method and chemical method, and simple physics, chemical method have many defectives.Simultaneously, at present most the employing bought nano-titanium dioxide powders, adds dispersant again and forms the titania solution that disperses, and then it added in the powder such as inorganic material or liquid of coating, paint, ceramic glaze, fusion, after the stir process, it is central to play antibacterial effect to be blended in product.Yet also the existence dispersion is inhomogeneous, particle is easily reunited, separate out shortcomings such as difficulty and antibiotic cost increase continuously lastingly, causes the application of nano titanium oxide to be very restricted.
Particularly nano titanium oxide is added to when going in some organic or inorganic material systems as filler, the interaction force inorganic because of the very little meeting of nano particle and other or organic compound formation is stronger, even but the nano particle disperse is in inorganic solid solution or strong bonding polymerizable molecular chain, therefore its anti-microbial property can can't be moved to product surface continuously enduringly because of titanium dioxide nanoparticle when product uses, and makes the continuity of nanometer titanium dioxide antibiotic performance and persistence exist not enough.
Consider simultaneously and need illumination when using titanium dioxide, just can excite airborne oxygen and hydrone, negative oxygen base and hydroxyl free radical so that generation has superpower oxidability destroy the cell membrane of bacterium, cytoplasm is run off, play the activity that suppresses virus, the effect of removing bacterium in the air.For some daily life products, the sterilizing function of titanium dioxide is restricted when night, therefore, require under the stronger service condition for antibiotic, just need antibacterial product also bactericidal action will be arranged during night, only rely on antibiotic, the sterilization purpose that the titanium dioxide antibiotic composition promptly can't reach expection this moment.
[summary of the invention]
Technical problem to be solved by this invention is: a kind of photocatalyst-type anti-biotic material preparation method is provided, and the anti-microbial property continuity and the persistence of the anti-biotic material for preparing are strong.
The further technical problem to be solved of the present invention is: a kind of photocatalyst-type anti-biotic material preparation method is provided, and the anti-biotic material for preparing also can effectively antibiotic, sterilization under the night condition.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of photocatalyst-type anti-biotic material preparation method is provided, comprises the steps:
A, preparation process, it preparation antiseptic solution that comprises in no particular order order step by step with the material surface preliminary treatment step by step, wherein, the preparation antiseptic solution goes out antiseptic solution according to formulated step by step, and the material surface preliminary treatment is carried out preliminary treatment to material surface step by step to be made material surface cleaning and form activating area;
B, material surface apply the antiseptic solution step, antiseptic solution is adhered at material surface form one deck antibacterial film;
C, drying steps make the antiseptic solution drying that is coated on material surface by drying step;
D, solidify treatment step, promoting combining of antibiotic layer and matrix surface, and make the transformation of photocatalysis antibacterial layer generation anatase crystal by cooling behind the heat treatment mode elder generation heat tracing.
Further improvement in the technical proposal is: described antiseptic solution is for containing the nanometer titanium dioxide antibiotic sol solution, described contain in the nanometer titanium dioxide antibiotic sol solution each composition and corresponding content as follows:
Butyl titanate: 17%～20% (volumn concentration);
Distilled water: 1.1～1.5% (volumn concentrations);
Acetic acid: 4%～6% (volumn concentration);
Ethanol: solvent;
Stabilizing agent: 2～3%;
Bonding agent: 2～4g/L;
Film forming agent: 0.5～1% (volumn concentration);
Distilled water: 1.3～2.0%;
Wherein, stabilizing agent can be selected three any one in hydramine, ethylene glycol, ethylene glycol amine, acetylacetone,2,4-pentanedione, the citric acid; Bonding agent is PEG400 or PEG600.
Further improvement in the technical proposal is: when preparation contains the nanometer titanium dioxide antibiotic sol solution, at first metatitanic acid fourth fat is mixed forming ethanolic solution with 50% volume of ethanol, under 40～50 ℃ of conditions, heating, stirring are so that fully dissolving; Then, acetic acid is joined in the residue 50% volume ethanol solution, stir and splash into respectively the mixed solution of an amount of distilled water and stabilizing agent, film forming agent and bonding agent, then under 60～80 ℃ of conditions the heating and stirred 1～5 hour, pH value is controlled at 3～4, to form the sol solution of micro emulsion yellow, the sol solution ageing promptly forms the yellowish nanometer titanium dioxide antibiotic gel solution that contains after 1～2 day.
Further improvement in the technical proposal is: described antiseptic solution is the composite antibiosis sol solution that contains nano titanium oxide and silver, it is slowly joined volume and is not more than in the silver-colored particle solution that contains the nano titanic oxide sol liquor capacity by a certain amount of nano titanic oxide sol solution that contains, fully stirred 1～2 hour, and it is about 7.5～8.5 that adding ammoniacal liquor makes the pH value of solution, can obtain the described composite antibiosis solution that contains nano titanium oxide and silver.
Further improvement in the technical proposal is: each main component of described silver-colored particle solution and content thereof are as follows respectively:
Silver nitrate: 1 * 10
-2～1 * 10
-3Mol/L;
Reductant: (3～5) * 10
-2～1 * 10
-3Mol/L;
Surfactant: 0.1～0.01mol/L;
Bonding agent: 0.1～0.3g/L;
Ethanol: solvent;
Wherein, described reductant can be selected any one in potassium borohydride, sodium borohydride, hydrogen peroxide, the sodium hypophosphite; Surfactant can be selected any one in lauryl sodium sulfate, dodecyl sodium sulfate, the polyvinylpyrrolidone; Bonding agent is PEG400 or PEG600.
Owing to adopt technique scheme, the present invention has following beneficial effect: the antiseptic solution that the present invention adopts is to adopt containing the nanometer titanium dioxide antibiotic sol solution or containing nano titanium oxide and the composite antibiosis sol solution of silver of Prepared by Sol Gel Method, antiseptic solution is coated in stainless steel, aluminium alloy, plastics, substrate material surfaces such as glass, it is strong to generate adhesion with the thermal treatment heating, the anti-nano titanium oxide of scrubbing or silver-colored particle-titanium dioxide antibiotic functional layer, the disperse of antibacterial granule phase is evenly distributed in the substrate material surface layer, the antibiotic phase titanic oxide power that combines with matrix is stronger, is distributed in the surface at least in the following superficial layer of 3um.Can penetrate down in illumination, make the material surface of rich titanium dioxide exposed outside the time, the bacterioprotein sex change that contact with the surface, effective killing bacteria, sterilizing rate can reach more than 90%.The antibacterial functions layer that contains silver-colored particle simultaneously also can play antibacterial action under the condition on night, and product can be realized sterilization in 24 hours.
[description of drawings]
Fig. 1 is the preparation process schematic diagram of a kind of photocatalyst-type anti-biotic material preparation method of the present invention.
[embodiment]
As shown in Figure 1, the invention provides a kind of photocatalyst-type anti-biotic material preparation method, it mainly comprises following each step:
A, preparation process;
B, material surface apply the antiseptic solution step;
C, drying steps;
D, curing treatment step.
Next, respectively each step is elaborated:
A, preparation process
Preparation process mainly is to prepare for follow-up material surface applies antiseptic solution, its comprise again the preparation antiseptic solution step by step and the material surface preliminary treatment two step by step step by step, two not sequencing differences step by step, in can advanced Xingqi any one step by step, even two carried out step by step simultaneously.
A1, preparation antiseptic solution are step by step
Antiseptic solution of the present invention mainly contains two kinds: contain the nanometer titanium dioxide antibiotic sol solution and contain nano titanium oxide and the composite antibiosis sol solution of silver, when concrete preparation photocatalysis antibacterial material, can adopt wherein any one.Promptly be elaborated respectively below at the preparation of above-mentioned two kinds of antiseptic solutions.
1, contains the preparation of nanometer titanium dioxide antibiotic sol solution
It is as follows to contain each composition and the corresponding content thereof that contain in the nanometer titanium dioxide antibiotic sol solution:
Butyl titanate: 17%～20% (volumn concentration);
Distilled water: 1.1～1.5% (volumn concentrations);
Acetic acid: 4%～6% (volumn concentration);
Ethanol: solvent;
Stabilizing agent: 2～3%;
Bonding agent: 2～4g/L;
Film forming agent: 0.5～1% (volumn concentration);
Distilled water: 1.3～2.0%;
Wherein, stabilizing agent can be selected any one in three hexanol amine, ethylene glycol, ethylene glycol amine, acetylacetone,2,4-pentanedione, the citric acid; Bonding agent is PEG400 or PEG600.The invention provides two concrete prescriptions that contain the nanometer titanium dioxide antibiotic sol solution, be respectively table 1 as showing:
Table 1 contains nanometer titanium dioxide antibiotic sol solution prescription
| Composition | Prescription 1 | Prescription 2 |
| Butyl titanate | 17ml | 20ml |
| Distilled water | 1.3ml | 2.0ml |
| Acetic acid | 4ml | 6ml |
| Solvent: ethanol | 78ml | 68ml |
| Stabilizing agent: three hexanol amine | 2.0ml | 3ml |
| Bonding agent: PEG400 | 0.2g | 0.4g |
| Film forming agent | 0.5ml | 1.0ml |
When preparation contains the nanometer titanium dioxide antibiotic sol solution, at first, metatitanic acid fourth fat is mixed the formation ethanolic solution with about 50% volume of ethanol, under 40～50 ℃ of conditions, heating, stirring are so that fully dissolving; Then, acetic acid is joined in the residue 50% volume ethanol solution, stir and splash into respectively the mixed solution of an amount of distilled water and stabilizing agent, film forming agent and bonding agent, then under 60～80 ℃ of conditions the heating and stirred 1～5 hour, pH value is controlled at 3～4, to form the sol solution of micro emulsion yellow, the sol solution ageing promptly forms the yellowish nanometer titanium dioxide antibiotic gel solution that contains after 1～2 day.This antiseptic solution can be coated in and reach the purpose that realizes antibiotic layer on the clean surface of base materials such as metal, glass, plastics.
2, contain the preparation of the composite antibiosis sol solution of nano titanium oxide and silver
At first, dispose silver-colored particle solution, each main component of silver-colored particle solution and content thereof are as follows respectively:
Silver nitrate: 1 * 10
-2～1 * 10
-3Mol/L;
Reductant: (3～5) * 10
-2～1 * 10
-3Mol/L;
Surfactant: 0.1～0.01mol/L;
Bonding agent: 0.1～0.3g/L.
Wherein, described reductant can be selected any one in potassium borohydride, sodium borohydride, hydrogen peroxide, the sodium hypophosphite; Surfactant can be selected any one in citric acid, lauryl sodium sulfate, dodecyl sodium sulfate, the polyvinylpyrrolidone; Bonding agent is PEG400.The present invention has equally also provided two silver-colored particle solution and specifically filled a prescription, and is as shown in table 2:
Table 2 silver particle solution prescription
| Composition | Prescription 1 | Prescription 2 |
| Silver nitrate | 1×10 -2mol/L | 1×10 -3mol/L |
| Reductant: potassium borohydride | 3×10 -2mol/L | 5×10 -3mol/L |
| Surfactant: citric acid | 0.1mol/L | 0.01mol/L |
| Bonding agent: PEG400 | 0.3g/L | 0.1g/L |
When concrete preparation, at first, silver nitrate is mixed the formation ethanolic solution with surfactant (citric acid); Then, above-mentioned solution joined in the ethanolic solution that reductant (potassium borohydride) and bonding agent (PEG400) form go, after fully stirring, promptly forming silver-colored particle solution.
Then, under stirring action, a certain amount of nano titanic oxide sol solution that contains is slowly joined silver-colored particle solution, and need control silver-colored particle and titanium dioxide molar ratio, general silver may be selected to be 1: 10 with the mol ratio of titanium～1: 20 scope in, mixing time was generally 1～2 hour, and adding ammoniacal liquor, to make the pH value of solution be in 7.5～8.5 scopes, can obtain containing the composite antibiosis solution of nano titanium oxide and silver.Promptly can be used for being sprayed directly into solid material surface and carry out antimicrobial treatment.
A2, material surface preliminary treatment are step by step
It mainly is to adopt diverse ways at different materials, makes material surface cleaning, and can effectively carry out antimicrobial treatment.Surface preparation mode at some common used materials is as follows:
Ferrous metal material product: adopt 5%～10% sulfuric acid solution and water to clean;
Aluminum metallic material goods: adopt 10～30% salpeter solution and water cleaning;
Goods such as glass, pottery: adopt 5%～10% sulfuric acid solution and ethanol to clean.
B, material surface apply the antiseptic solution step
Antiseptic solution adopted lift or mode such as spraying is adhered at material surface and formed one deck antibacterial film.When adopting czochralski method, pull rate is controlled at 4～7cm/min, and pull rate is directly proportional with the viscosity of solution, and solution viscosity is big more, and pull rate is fast more.
C, drying steps
Its main purpose is to make the antiseptic solution that is coated on material surface dry as early as possible by drying step, common drying step has natural seasoning and heated-air drying, for example: the method that can adopt natural seasoning for small-sized thin part, and when selecting the heated-air drying mode for use, hot blast temperature generally is controlled at 70～90 ℃.
D, curing treatment step
The purpose of this step is by solidify to handle promoting combining of antibiotic layer and matrix surface, and the curing mode that adopts is a heat treatment mode usually, and at different materials, and the heat treatment temperature and the type of cooling be also institute's difference all.The heat treatment temperature and the type of cooling for some common used materials are as follows:
D1, ferrous metal material: at first, be warming up to 150 ℃ with 3～6 ℃/min speed, keep 10～20min time at 150 ℃ then, then, be rapidly heated 450～550 ℃ with 4～8 ℃/min again, after arriving 450～550 ℃, be incubated 2～5 hours, last, cool off fast, the type of cooling is air cooling or water-cooled;
D2, aluminum metal: at first, be warming up to 150 ℃ with 3～6 ℃/min speed, keep 10～20min time at 150 ℃ then, then, be warmed up to 450～550 ℃ with 4～8 ℃/min speed, and last 450～550 ℃ of insulations 0.5～2 hour, to cool off fast, the type of cooling is air cooling or water-cooled;
D3, glass: at first, be warming up to 150 ℃, keep 20～40min time at 150 ℃ then with 3～6 ℃/min speed, then, be warmed up to 350～550 ℃ with 4～8 ℃/min speed, and in the time of 350～550 ℃, keep 20～30min time, carry out slowly cooling in the stove at last;
D4, pottery, at first, be warming up to 150 ℃ with 3～6 ℃/min speed, keep 10～20min time at 150 ℃ then, then, being warming up to 700～1000 ℃ of high temperature with the speed of 10～15 ℃/min heat-treats, when rising to default maximum temperature, insulation 1～2h, last, cool off, the type of cooling is the air cooling.
The antiseptic solution that the present invention adopts is to adopt containing the nanometer titanium dioxide antibiotic sol solution or containing nano titanium oxide and the composite antibiosis sol solution of silver of Prepared by Sol Gel Method, antiseptic solution is coated in stainless steel, aluminium alloy, plastics, substrate material surfaces such as glass, it is strong to generate adhesion with the thermal treatment heating, the anti-nano titanium oxide of scrubbing or silver-colored particle-titanium dioxide antibiotic functional layer, the disperse of antibacterial granule phase is evenly distributed in the superficial layer of matrix material, the antibiotic phase titanic oxide power that combines with matrix is stronger, is distributed in the surface at least in the following superficial layer of 3um.Can penetrate down in illumination, make the material surface of rich titanium dioxide exposed outside the time, the bacterioprotein sex change that contact with the surface gets final product effective killing bacteria, and sterilizing rate can reach more than 90%.For also playing antibacterial action under the condition on night under the condition of the antibacterial agent that contains silver-colored particle, product can be realized sterilization in 24 hours simultaneously.
Claims (10)
1, a kind of photocatalyst-type anti-biotic material preparation method comprises the steps:
A, preparation process, it preparation antiseptic solution that comprises in no particular order order step by step with the material surface preliminary treatment step by step, wherein, the preparation antiseptic solution goes out antiseptic solution according to formulated step by step, and the material surface preliminary treatment is carried out preliminary treatment to material surface step by step to be made material surface cleaning and form activating area;
B, material surface apply the antiseptic solution step, antiseptic solution is adhered at material surface form one deck antibacterial film;
C, drying steps make the antiseptic solution drying that is coated on material surface by drying step;
D, solidify treatment step, promoting combining of antibiotic layer and matrix surface, and make the transformation of photocatalysis antibacterial layer generation anatase crystal by cooling behind the heat treatment mode elder generation heat tracing.
2, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 1 is characterized in that: described antiseptic solution is for containing the nanometer titanium dioxide antibiotic sol solution, described contain in the nanometer titanium dioxide antibiotic sol solution each composition and corresponding content as follows:
Butyl titanate: 17%～20% (volumn concentration)
Distilled water: 1.1～1.5% (volumn concentrations);
Acetic acid: 4%～6% (volumn concentration);
Ethanol: solvent;
Stabilizing agent: 2～3%;
Bonding agent: 2～4g/L;
Film forming agent: 0.5～1% (volumn concentration);
Distilled water: 1.3～2.0%;
Wherein, stabilizing agent can be selected any one in three hexanol amine, ethylene glycol, ethylene glycol amine, acetylacetone,2,4-pentanedione, the citric acid; Bonding agent is polyethylene glycol PEG400 or PEG600.
3, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 2, it is characterized in that: when preparation contains the nanometer titanium dioxide antibiotic sol solution, at first, metatitanic acid fourth fat is mixed the formation ethanolic solution with 50% volume of ethanol, under 40～50 ℃ of conditions, heating, stirring are so that fully dissolving; Then, acetic acid is joined in the residue 50% volume ethanol solution, stir and splash into respectively the mixed solution of an amount of distilled water and stabilizing agent, film forming agent and bonding agent, then under 60～80 ℃ of conditions the heating and stirred 1～5 hour, pH value is controlled at 3～4, to form the sol solution of micro emulsion yellow, the sol solution ageing promptly forms the yellowish nanometer titanium dioxide antibiotic gel solution that contains after 1～2 day.
4, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 1, it is characterized in that: described antiseptic solution is the composite antibiosis sol solution that contains nano titanium oxide and silver, it is slowly joined volume and is not more than in the silver-colored particle solution that contains the nano titanic oxide sol liquor capacity by a certain amount of nano titanic oxide sol solution that contains, fully stirred 1～2 hour, and it is 7.5～8.5 that adding ammoniacal liquor makes the pH value of solution, can obtain the described composite antibiosis solution that contains nano titanium oxide and silver.
5, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 4 is characterized in that: each main component of described silver-colored particle solution and content thereof are as follows respectively:
Silver nitrate: 1 * 10
-2～1 * 10
-3Mol/L;
Reductant: (3～5) * 10
-2～1 * 10
-3Mol/L;
Surfactant: 0.1～0.01mol/L;
Bonding agent: 0.1～0.3g/L;
Ethanol: solvent;
Wherein, described reductant can be selected any one in potassium borohydride, sodium borohydride, hydrogen peroxide, the sodium hypophosphite; Surfactant can be selected any one in citric acid, lauryl sodium sulfate, dodecyl sodium sulfate, the polyvinylpyrrolidone; Bonding agent is polyethylene glycol PEG400 or PEG600.
6, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 1, it is characterized in that: described material is a kind of in ferrous metal, aluminum metal, glass or the pottery, and in the material surface pre-treatment step, when material is ferrous metal, adopt 5%～10% sulfuric acid solution and water to clean; When material is aluminum metal, adopt 10～30% salpeter solution and water cleaning; When material is glass or plastics, adopt 5%～10% sulfuric acid solution and ethanol to clean.
7, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 1, it is characterized in that: the mode that material surface applies antiseptic solution can be to lift or spraying method, when lifting mode, pull rate is controlled at 4～7cm/min, and pull rate is directly proportional with the viscosity of solution.
8, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 1, it is characterized in that: described drying step is natural seasoning or heated-air drying, the hot blast temperature during heated-air drying is controlled at 70～90 ℃.
9, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 1 is characterized in that: described material is ferrous metal or aluminum metal, in solidifying treatment step, when material is ferrous metal, at first, be warming up to 150 ℃, keep 10～20min time at 150 ℃ then with 3～6 ℃/min speed, then, be rapidly heated 450～550 ℃ with 4～8 ℃/min again, after arriving 450～550 ℃, be incubated 0.5～5 hour, last, cool off fast, the type of cooling is air cooling or water-cooled.
10, a kind of photocatalyst-type anti-biotic material preparation method as claimed in claim 1 is characterized in that: material is glass or pottery, in solidifying treatment step, when material is glass, at first, be warming up to 150 ℃, keep 20～40min time at 150 ℃ then with 3～6 ℃/min speed, then, be warmed up to 350～550 ℃ with 4～8 ℃/min speed, and in the time of 350～550 ℃, keep 0.5～1.0 hour time, last, cool off, the type of cooling has stove cold; When material is pottery, at first, be warming up to 150 ℃ with 3～6 ℃/min speed, keep 10～20min time at 150 ℃ then, then, being warming up to 700～1000 ℃ of high temperature with the speed of 10～15 ℃/min heat-treats, when rising to default maximum temperature, insulation 1～2h, last, cool off, the type of cooling is the air cooling.
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2005
- 2005-09-29 CN CN 200510105656 patent/CN1742582A/en active Pending
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