CN101940222B - Method for preparing titanium sol carrier zinc and copper ion-adsorbing antibacterial agent by microwave heating - Google Patents
Method for preparing titanium sol carrier zinc and copper ion-adsorbing antibacterial agent by microwave heating Download PDFInfo
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- CN101940222B CN101940222B CN2010102511605A CN201010251160A CN101940222B CN 101940222 B CN101940222 B CN 101940222B CN 2010102511605 A CN2010102511605 A CN 2010102511605A CN 201010251160 A CN201010251160 A CN 201010251160A CN 101940222 B CN101940222 B CN 101940222B
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Abstract
The invention relates to a method for preparing a titanium sol carrier zinc and copper ion-adsorbing antibacterial agent by microwave heating. The method comprises the following steps of: dripping 8mL of butyl titanate into 20mL of ethanol for uniformly mixing under certain condition, and adding 2mL of glacial acetic acid to prepare solution A; stirring 60mL of ethanol and 2mL of distilled water and adding nitric acid to regulate the pH value to be 2-3 so as to prepare solution B; dripping the solution B into the solution A at a dripping speed of 50 to 60 drops per minute, stirring, regulating the pH value to be 2-3, and heating the solution in a microwave oven for 20 to 90 seconds so as to prepare titanium sol; dripping 0.3mol/L solution of copper nitrate and zinc nitrate into the titanium sol, stirring for 1 to 2 hours at the temperature of 30 DEG C, and performing microwave heating for 20 to 50 seconds so as to prepare titanium gel for absorbing the zinc and copper ions, wherein the ion addition is 8:100 (the molar ratio of total ions to the butyl titanate) and the molar ratio of zinc ions to copper ions is 2:1; drying, grinding and calcining the gel, keeping the temperature at 450 DEG C for 30 to 60 minutes, and finally taking the product out so as to prepare the needed antibacterial agent. Researches prove that: the antibacterial agent has excellent performance, and simultaneously solves the problems that a silver antibacterial agent has high cost and an antibacterial material changes color and has single function.
Description
Technical field:
The present invention relates to the technology of preparing of powder, relate in particular to a kind of method that adopts heating using microwave to prepare titanium sol vehicle absorption zinc, copper ion antibacterial agent.
Background technology:
The research that the research of inorganic antiseptic at present both at home and abroad mainly concentrates on single antibacterial agent with use, like the research and the application of the antibiotic or self-cleaning action of single silver system or single titanium system.The product effect of being developed is single, uses to be limited to, and the antibacterial effect of anti-biotic material is also not ideal, as the titanium based material night unglazed according to the time do not have antibiotic self-cleaning action and occur, and night bacterial reproduction peak period just.In addition; Silver is that anti-biotic material and titanium are that antibiosis and self-cleaning material itself also exists many shortcomings; Like silver is the high problem of oxidation stain problem, cost of anti-biotic material, and titanium is that the activity of antibiosis and self-cleaning material improves problem and visible light-responded problem and load technology problem etc. all await carrying out deep research.The present invention prepares titanium sol vehicle absorption zinc, copper ion antibacterial agent under the condition of heating using microwave, be intended to Zn
2+, Cu
2+Sterilization, bacteriostasis and TiO
2Collaborative being combined with each other of two kinds of antibiotic self-cleanings effect; To solve the monistic problem of present anti-biotic material effect; Make traditional anti-biotic material and goods not only have antibacterial functions but also have self-cleaning function, thereby widen range of application, raising antibiosis and self-cleaning performance and the effect of anti-biotic material.
Summary of the invention:
The present invention under the condition of heating using microwave, is a carrier with titanium colloidal sol first, absorption zinc, copper ion, and preparation possesses composite granules antibiotic, two kinds of effects of automatically cleaning.Characteristics of the present invention are:
1. the cost height of silver-series antibacterial agent and the discoloration problem of anti-biotic material have been solved.
2. through adopting microwave heating method, optimized synthesis condition, made the antibacterial agent particle diameter little and even, anti-microbial property improves.
3. with Zn
2+, Cu
2+Sterilization, bacteriostasis and TiO
2Collaborative being combined with each other of two kinds of antibiotic self-cleanings effect, solved the monistic problem of present anti-biotic material effect.
Its preparation method is following:
1. with 8mL butyl titanate (Ti (OBu)
4) under 50 ℃ of stirring conditions, be added drop-wise in the 20mL ethanol and mix, add the 2mL glacial acetic acid again and obtain solution A.Distilled water with 60mL ethanol and 2mL under agitation adds nitre acid for adjusting pH value to 2～3 then, obtains solution B.The speed of solution B with 50～60 of per minutes is added drop-wise in the solution A, stirs and also to regulate pH value to 2～3, placing power is can obtain flaxen transparent titanium colloidal sol after the micro-wave oven of 500～900W heats 20～90s.
2. drip copper nitrate and the zinc nitrate solution of 0.3mol/L to colloidal sol; The ion addition is 8: 100 (mol ratio of population of ions and butyl titanate); It is 1.5g ion/100mL butyl titanate; The mol ratio of zinc-copper ion is 2: 1,30 ℃ with stirring 1～2h, heating using microwave 20～50s makes the titanium gel of absorption zinc-copper ion then.
3. place drying box dry prepared gel, 100 ℃ of baking temperatures obtain loose xerogel, grind to be placed on and put into the stove calcining in the crucible then, and at 450 ℃ of insulation 30～60min, promptly get required antibacterial agent after the taking-up.
It is as shown in Figure 1 that the titanium colloidal sol of preparation absorption zinc, copper ion antibacterial agent carry out the inhibition zone test as stated above; Can find out by Fig. 1; In the inhibition zone test of titanium colloidal sol composite granule of absorbing copper zinc ion gained under different adsorption conditionses, the antibacterial effect of heating using microwave is better than magnetic agitation heats.Though analyze former, can promote the effect of titanium colloidal sol adion, but its heats and dispersibility are different because the two all has heating function.Heating using microwave is from inside to outside to heat, and the instantaneous temperature of its generation is higher, ion is adsorbed on the colloid apace, thereby antibacterial effect is relatively good.
Fig. 2 composes at the XRD figure of 450 ℃ of insulation 60min gained powders for the titanium dry gel powder of absorption zinc, copper ion.The diffraction maximum that occurs copper zinc in the collection of illustrative plates can know that by XRD analysis its content is less, can judge that the two is the adsorbate of titanium colloidal sol.For principal crystalline phase titanium dioxide, TiO
2The peak position of low angle diffraction maximum is about 25 °, and warp can know that with the standard diagram card comparison of titanium dioxide crystal titanium dioxide crystal mainly is an anatase crystal.
Fig. 3 can find out the TiO of Detitanium-ore-type for the titanium colloidal sol absorption zinc of heating using microwave preparation, the electromicroscopic photograph of copper ion antibacterial agent from figure
2Particle is tridimensional network, TiO
2Shorter on the crystal one dimension direction, longer on the two-dimensional directional, be interlaced with one another together, form a lot of spaces.This is because TiO
2Powder is made by sol-gal process, and titanium colloidal sol belongs to colloidal dispersion, has very big interface; Titanium colloidal sol obtains gel through evaporating solvent; Colloidal solid is assembled each other in this process, makes gel have " card " shape structure, is interlaced with one another; Form a lot " cavity ", so obtain TiO through dry, calcining by gel
2Crystal also has a lot of spaces.TiO just
2Have a lot of spaces, just can make its with ionic adsorption in these spaces.From figure, it can also be seen that, at column TiO
2Adsorbing some particles on the particle, these particles have be ellipticity, have be spherical, can judge that titanium colloidal sol has adsorbed the zinc-copper ion.
Description of drawings:
Fig. 1 is the titanium colloidal sol absorption zinc of preparation under heating using microwave and the magnetic agitation heating condition, the inhibition zone of copper ion antibacterial agent
Fig. 2 adsorbs the XRD figure spectrum of the titanium dry gel powder of zinc, copper ion at 450 ℃ of insulation 60min gained powders
Fig. 3 is the SEM photo of the antibiotic composite granule that adopts heating using microwave and make
Embodiment:
Embodiment 1
With 8mL butyl titanate (Ti (OBu)
4) under 50 ℃ of stirrings, be added drop-wise in the 20mL ethanol and mix, add the 2mL glacial acetic acid again and obtain solution A.Distilled water with 60mL ethanol and 2mL under agitation adds nitre acid for adjusting pH value to 1～2 then, obtains solution B.The speed of solution B with 50～60 of per minutes is added drop-wise in the solution A, and the distilled water with 60mL ethanol and 2mL under agitation adds nitre acid for adjusting pH value to 2～3 then, obtains solution B.The speed of solution B with 50～60 of per minutes is added drop-wise in the solution A, stirs and also to regulate pH value to 2～3, placing power is can obtain flaxen transparent titanium colloidal sol after the micro-wave oven of 500～900W heats 20～90s.
Embodiment 2
Drip copper nitrate and the zinc nitrate solution of 0.3mol/L to colloidal sol; The ion addition is 8: 100 (mol ratio of population of ions and butyl titanate); It is 1.5g ion/100mL butyl titanate; The mol ratio of zinc-copper ion is 2: 1, stirs 2h at 30 ℃, and heating using microwave 20～50s obtains adsorbing the titanium gel of zinc-copper ion then.Place drying box dry prepared gel then, obtain loose xerogel, grind to be placed on to put in the crucible under 450 ℃ in the stove and calcine and be incubated 30～60min, promptly get required antibacterial agent after the taking-up.
Claims (1)
1. one kind is adopted heating using microwave to prepare the method that the titanium sol vehicle is adsorbed zinc, copper ion antibacterial agent; It is characterized in that this antimicrobial powder is with Zn
2+, Cu
2+Sterilization, bacteriostasis and TiO
2Collaborative being combined with each other of two kinds of antibiotic self-cleanings effect, concrete preparation method is: 1. at first the 8mL butyl titanate is added drop-wise in the 20mL ethanol under 50 ℃ of stirrings and mixes, add the 2mL glacial acetic acid again and obtain solution A; Distilled water with 60mL ethanol and 2mL under agitation adds nitre acid for adjusting pH value to 2～3 then, obtains solution B; B is dripped among the A with the speed of 50～60 of per minutes, stir and also to regulate pH value to 2～3, can obtain titanium colloidal sol after placing micro-wave oven to heat 20～90s; 2. in titanium colloidal sol, drip copper nitrate and the zinc nitrate solution of 0.3mol/L; The ion addition is 8: 100; This ratio is the mol ratio of population of ions and butyl titanate, i.e. 1.5g ion/100mL butyl titanate, and the mol ratio of zinc-copper ion is 2: 1; Stir 1～2h at 30 ℃, heating using microwave 20～50s makes the titanium gel of absorption zinc-copper ion then; Place drying box dry prepared gel then, 100 ℃ of baking temperatures obtain loose xerogel, grind to be placed on and put into 450 ℃ of calcinings of stove in the crucible again, and be incubated 30～60min, take out at last and promptly get required antibacterial agent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010102511605A CN101940222B (en) | 2010-08-12 | 2010-08-12 | Method for preparing titanium sol carrier zinc and copper ion-adsorbing antibacterial agent by microwave heating |
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| CN2010102511605A CN101940222B (en) | 2010-08-12 | 2010-08-12 | Method for preparing titanium sol carrier zinc and copper ion-adsorbing antibacterial agent by microwave heating |
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| CN101940222B true CN101940222B (en) | 2012-05-23 |
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| CN104526806B (en) * | 2014-12-05 | 2016-09-28 | 中南林业科技大学 | The preparation method of bamboo wood mould preservative |
| CN108064882A (en) * | 2017-12-11 | 2018-05-25 | 刘凡领 | A kind of preparation method of long-acting antibiotic agent |
| CN115874350A (en) * | 2021-09-28 | 2023-03-31 | 江苏青昀新材料有限公司 | Mildew-proof polyethylene fabric and production method and application thereof |
| CN114946879A (en) * | 2022-06-02 | 2022-08-30 | 江苏美百加电器科技有限公司 | Preparation method of titanium oxide aerogel loaded zinc oxide antibacterial material |
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| CN1228240C (en) * | 2003-09-10 | 2005-11-23 | 河北工业大学 | Tourmaline/titanium dioxide composite collosol and preparing method and use thereof |
| CN101258856B (en) * | 2008-04-21 | 2012-06-20 | 河北理工大学 | Method for preparing antimicrobial agent with carrier for adsorbing copper and zinc ion by microwave heating |
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