CN102578148B - Method for improving antibacterial property of tetrapod-like zinc oxide whisker - Google Patents
Method for improving antibacterial property of tetrapod-like zinc oxide whisker Download PDFInfo
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- CN102578148B CN102578148B CN201210005760.2A CN201210005760A CN102578148B CN 102578148 B CN102578148 B CN 102578148B CN 201210005760 A CN201210005760 A CN 201210005760A CN 102578148 B CN102578148 B CN 102578148B
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Abstract
A method for improving the antibacterial property of a tetrapod-like zinc oxide whisker comprises the steps of A. adding the tetrapod-like zinc oxide whisker taking the shape of white powder in an aqueous solution of potassium sodium tartrate to form paste or suspension and stirring for 10-30 minutes, wherein the mole ratio of the potassium sodium tartrate to the tetrapod-like zinc oxide whisker is (0.1-1):100; then under the state of stirring, slowly adding an aqueous solution of copper chloride with the same molar weight as the potassium sodium tartrate; later continuing stirring for 30-60 minutes; at last, conducting filtering, washing and drying, thus obtaining tetrapod-like zinc oxide whisker compound powder with nanometer cupric tartrate in-situ deposited on the surface; and B. increasing the temperature of the compound powder to 270-300 DEG C, keeping the temperature for 15-60 minutes, and conducting cooling to room temperature, thus obtaining the tetrapod-like zinc oxide whisker with strong antibacterial property. The powder obtained by the method has strong antibacterial capability, sterilizing rate of 98.5%-99.9%, low cost, does not change color when in use and is easy to popularize.
Description
Technical field
The present invention relates to a kind of preparation method of antibacterial agent material, relate in particular to the preparation method of four acicular type zinc oxide crystal whisker composite antibiosis agent material.
Background technology
Noxious bacteria is present in the various occasions of ours around, as housing floor, the metope of living, the furniture of use, household electrical appliances, clothing and articles for daily use etc.1996, the national infection event of O-157 Escherichia coli of Japanese large area outburst, not only seized many people's life, and caused that the whole world is panic.According to statistics, the whole world causes dead number to approach 2,000 ten thousand because bacterium infects every year, accounts for the more than 30% of dead sum; The intersection infection of each hospital surpasses 10%.Will effectively prevent that bacterium from producing and growing, using anti-biotic material is the most simple and efficient method.Anti-biotic material refers to a class new function material with sterilization and bacteria growing inhibiting function.Wherein inorganic antiseptic because it is long-lasting, stability and be difficult for causing that pesticide resistance is widely applied.
Inorganic antiseptic adopts physical adsorption ion-exchange process, and the Metal Supporteds such as silver, copper, zinc, in porous material surface, are utilized to the antibacterial action of metal ion, reaches the object of long-acting bacteriostatic by slow releasing function.Inorganic antiseptic does not produce drug resistance and safety is good, and particularly its outstanding warm tolerance (600 ℃ of >) has very large advantage in the application of multiple antibacterial product.
Existing inorganic antiseptic mainly take silver and zinc ion as main, wherein best with the antibacterial effect of silver ion, but silver ion antimicrobial agent exists and to be easily reduced and variable color (being grey black) and the large shortcoming of cost high two, and simple substance is silver-colored to be lost or greatly weakens its antibacterial effect owing to becoming after reducing.At present, have and much report that nano material has antibiotic property, but simple nano material is because particle diameter is too little, has very large surface area, be difficult in use fully disperse, even cannot disperse.So all will carry out the coated processing in surface to it before using.Coated result greatly reduces the performance of nano effect and antibacterial action on the one hand, and this processing procedure is also very loaded down with trivial details on the other hand.Moreover, more existing nano-powder materials are (as nano-TiO
2) will rely on photocatalysis just to show certain antibacterial effect.
Japan Patent (Unexamined Patent 5-912, Unexamined Patent 8-133918) report is compound with four acicular type zinc oxide crystal whisker and silver salt, prepared and there is the inorganic antiseptic of excellent antibacterial effect and in different materials and environment, obtain application (Unexamined Patent-93365, Unexamined Patent 5-78498, Unexamined Patent 78218, Unexamined Patent 6-140731 etc.), the technology of these Japan Patent reports is utilized spicule activated centre and the point effect of ZnOw, repeatedly activate airborne water and oxygen, produce hydroxyl radical free radical (OH) and active oxygen ion (O
2 -), destroy bacteria live and multiplication capacity and make bacterium dead, and reach antibacterial effect.But owing to using common four acicular type zinc oxide crystal whisker, its whisker length reaches 30～100 μ m, and root diameter (RD) slightly reaches 0.1～10 μ m.Its spicule activated centre is few, and most advanced and sophisticated nano effect is poor, in order to improve its antibacterial effect, one of its method is to add silver ion (as ZL 200510115039.9), yet the doping process of silver ion is complicated, and product cost is high, and be subject to silver this resource restriction.So necessary exploitation is a kind of can improve antibacterial property of tetrapod-like zinc oxide whisker, and antibacterial agent allochroic, not with low cost.
Summary of the invention
The object of this invention is to provide a kind of method that improves antibacterial property of tetrapod-like zinc oxide whisker, the four acicular type zinc oxide crystal whisker bactericidal power of processing by this method is stronger, and nondiscolouring and with low cost in use is easy to promote.
The technical solution adopted for the present invention to solve the technical problems is that a kind of method that improves antibacterial property of tetrapod-like zinc oxide whisker, the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery is joined in the aqueous solution of sodium potassium tartrate tetrahydrate and form pasty state or suspension, stir 10～30 minutes, described sodium potassium tartrate tetrahydrate and the mol ratio of four acicular type zinc oxide crystal whisker are 0.1～1: 100, and the amount of described potassium tartrate sodium water solution is more than or equal to and can also can forms the amount of scattered paste shape by submergence four acicular type zinc oxide crystal whisker; Under stirring, slowly add again the aqueous solution with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 30～60 minutes; Finally, after filtration, washing, dry, obtain the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits nanometer cupric tartrate;
B, the composite powder that A step is obtained are warming up to 270～300 ℃ of insulations 15～60 minutes in hydrogen atmosphere, are cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition Nanometer Copper.
Compared with prior art, beneficial effect of the present invention:
By four acicular type zinc oxide crystal whisker, in solution, evenly adsorb sodium potassium tartrate tetrahydrate, then in dripping the process of equivalent copper chloride, copper chloride reacts with sodium potassium tartrate tetrahydrate and generates nanometer cupric tartrate, thereby has realized the surface in situ deposition of nanometer cupric tartrate at four acicular type zinc oxide crystal whisker.Again in hydrogen atmosphere high temperature treatment to make cupric tartrate thermolysis be nano simple substance copper, thereby obtain the four acicular type zinc oxide crystal whisker of surface uniform deposition nano simple substance copper.
By above distinctive Nanometer Copper in-situ deposition modified technique, the present invention has realized nano copper particle and evenly and has stably been deposited on four acicular type zinc oxide crystal whisker surface, and Nanometer Copper particle diameter is 20nm left and right; Within 4 hours, sterilizing rate has brought up to 98.5%～99.9% by 68.0%, has obviously improved its antibacterial effect.
With respect to expensive Ag deposition and doping, the Nanometer Copper of this method deposition, it is cheap; And the in use nondiscolouring of Nanometer Copper of deposition, more welcome, promote easily, there is more wide application prospect.
Above-mentioned washing is for first washing with water, then washes with alcohol.
Washing can be washed unnecessary inorganic ions the most simply and easily off, avoids in subsequent processes, forming impurity, and the purity that makes to make thing is high, and sterilizing ability is strong; Add alcohol and wash the dispersiveness that can remove organic impurities and improve powder, further improve the sterilizing ability of prepared product.
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is the close-up view that use transmitting surface sweeping Electronic Speculum is amplified the Nanometer Copper modification four acicular type zinc oxide crystal whisker that 80,000 times of embodiment that observe 1 obtain.
Fig. 2 is the spicule surface local shape appearance figure that use transmitting surface sweeping Electronic Speculum is amplified the Nanometer Copper modification four acicular type zinc oxide crystal whisker that 160,000 times of embodiment that observe 1 obtain.
Fig. 3 is the X-ray photoelectron spectroscopic analysis result on the Nanometer Copper modification four acicular type zinc oxide crystal whisker surface that obtains of embodiment 1.
Fig. 4 is the close-up view that use transmitting surface sweeping Electronic Speculum is amplified the Nanometer Copper modification four acicular type zinc oxide crystal whisker that 40,000 times of embodiment that observe 3 obtain.
Fig. 5 is the spicule surface local shape appearance figure that use transmitting surface sweeping Electronic Speculum is amplified the Nanometer Copper modification four acicular type zinc oxide crystal whisker that 160,000 times of embodiment that observe 3 obtain.
Fig. 6 be the four acicular type zinc oxide crystal whisker of the Nanometer Copper modification that obtains of embodiment 1～5 to Escherichia coli sterilization the design sketch after 4 hours.(a) in figure～(e) component is respectively the antibacterial effect figure of the Nanometer Copper modification four acicular type zinc oxide crystal whisker that embodiment 1～5 obtains, and (f) component is the antibacterial effect figure without the four acicular type zinc oxide crystal whisker of Nanometer Copper modification.
Embodiment
A method that improves antibacterial property of tetrapod-like zinc oxide whisker, the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery is joined in potassium tartrate sodium water solution and forms pasty state, stir 30 minutes, described sodium potassium tartrate tetrahydrate and the mol ratio of four acicular type zinc oxide crystal whisker are 1: 100; Under stirring, slowly add again the aqueous solution (mole of the copper chloride containing in this aqueous solution equates with sodium potassium tartrate tetrahydrate) with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 60 minutes; Finally, after filtration, washing, dry, obtain the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits nanometer cupric tartrate;
B, the composite powder that A step is obtained are warming up to 270 ℃ of insulations 60 minutes in hydrogen atmosphere, are cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition Nanometer Copper.
Fig. 1 is the close-up view that use transmitting surface sweeping Electronic Speculum is amplified the Nanometer Copper modification four acicular type zinc oxide crystal whisker that 80,000 times of these examples of observing obtain, and on four pins of four needle-like oxidisability whiskers, is all adhering to uniformly tiny particle.Fig. 2 is that 160,000 times of results of observing are amplified on the spicule surface of whisker, and the nano particle diameter that whisker surface uniform distributes is in 20nm left and right.
Fig. 3 is the X-ray photoelectron spectroscopic analysis result on the Nanometer Copper modification four acicular type zinc oxide crystal whisker surface that obtains of this example, has occurred the characteristic peak of Cu 2p orbital electron in collection of illustrative plates, illustrates that there is the existence of copper on four acicular type zinc oxide crystal whisker surface that this example prepares.
Embodiment 2
A method that improves antibacterial property of tetrapod-like zinc oxide whisker, the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery is joined in potassium tartrate sodium water solution and forms pasty state, stir 30 minutes, described sodium potassium tartrate tetrahydrate and the mol ratio of four acicular type zinc oxide crystal whisker are 0.8: 100; Under stirring, slowly add again the aqueous solution with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 60 minutes; Finally, after filtration, washing, dry, obtain the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits nanometer cupric tartrate;
B, the composite powder that A step is obtained are warming up to 270 ℃ of insulations 40 minutes in hydrogen atmosphere, are cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition Nanometer Copper.
A method that improves antibacterial property of tetrapod-like zinc oxide whisker, the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery is joined in the aqueous solution of sodium potassium tartrate tetrahydrate and form suspension, stir 20 minutes, described sodium potassium tartrate tetrahydrate and the mol ratio of four acicular type zinc oxide crystal whisker are 0.6: 100; Under stirring, slowly add again the aqueous solution with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 50 minutes; Finally, after filtration, washing, dry, obtain the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits nanometer cupric tartrate;
B, the composite powder that A step is obtained are warming up to 270 ℃ of insulations 30 minutes in hydrogen atmosphere, are cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition Nanometer Copper.
Fig. 4 is the close-up view that use transmitting surface sweeping Electronic Speculum is amplified the Nanometer Copper modification four acicular type zinc oxide crystal whisker that 40,000 times of these examples of observing prepare, and on four pins of four needle-like oxidisability whiskers, is all adhering to uniformly tiny particle.Fig. 5 is that 160,000 times of results of observing are amplified on the spicule surface of use transmitting surface sweeping Electronic Speculum Nanometer Copper modification four acicular type zinc oxide crystal whisker that this example is prepared, and the nano particle diameter that whisker surface uniform distributes is in 20nm left and right.Fig. 5 and Fig. 2 are compared and can be found when the mol ratio of sodium potassium tartrate tetrahydrate and copper chloride and whisker reduced to 0.6: 100 by 1: 100, the nano particle of whisker surface attachment close corresponding reduction that distribute.
Embodiment 4
A method that improves antibacterial property of tetrapod-like zinc oxide whisker, the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery is joined in the aqueous solution of sodium potassium tartrate tetrahydrate and form pasty state, stir 20 minutes, described sodium potassium tartrate tetrahydrate and the mol ratio of four acicular type zinc oxide crystal whisker are 0.4: 100; Under stirring, slowly add again the aqueous solution with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 40 minutes; Finally, after filtration, washing, dry, obtain the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits nanometer cupric tartrate;
B, the composite powder that A step is obtained are warming up to 280 ℃ of insulations 30 minutes in hydrogen atmosphere, are cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition Nanometer Copper.
Embodiment 5
A method that improves antibacterial property of tetrapod-like zinc oxide whisker, the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery is joined in the aqueous solution of sodium potassium tartrate tetrahydrate and form suspension, stir 10 minutes, described sodium potassium tartrate tetrahydrate and the mol ratio of four acicular type zinc oxide crystal whisker are 0.1: 100; Under stirring, slowly add again the aqueous solution with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 30 minutes; Finally, after filtration, washing, dry, obtain the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits nanometer cupric tartrate;
B, the composite powder that A step is obtained are warming up to 300 ℃ of insulations 15 minutes in hydrogen atmosphere, are cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition Nanometer Copper.
The amount of the aqueous solution of mesotartaric acid potassium sodium of the present invention be more than or equal to can submergence four acicular type zinc oxide crystal whisker and can with the amount of its formation pasty state; When the quantity not sufficient of the aqueous solution of sodium potassium tartrate tetrahydrate, in the time of can not forming pasty state, can add water and can form pasty state or suspension with four acicular type zinc oxide crystal whisker.Because the amount of sodium potassium tartrate tetrahydrate is determined, the amount of potassium tartrate sodium water solution is determined by its concentration; When the concentration of potassium tartrate sodium water solution is 0.2mmol/L, can form scattered paste shape with four acicular type zinc oxide crystal whisker.
Antibacterial experiment result:
The four acicular type zinc oxide crystal whisker of the Nanometer Copper modification that above embodiment 1～5 is made (surface deposition Nanometer Copper) is tested its sterilizing rate rate by concussion method, by same procedure, the sterilizing rate of the four acicular type zinc oxide crystal whisker without Nanometer Copper modification is also tested simultaneously.
The specific practice of test is: every liter of Escherichia coli suspension containing five grams of four acicular type zinc oxide crystal whiskers is cultivated to 4h through concussion, the Escherichia coli before and after experiment are counted, draw 4 hours sterilizing rates.Result shows: 4 hours sterilizing rates of the four acicular type zinc oxide crystal whisker of the Nanometer Copper modification that embodiment 1～5 makes (surface deposition Nanometer Copper) are respectively 99.9%, 99.9%, 99.7%, 99.3%, 98.5%, and is only 68.0% without 4 hours sterilizing rates of the four acicular type zinc oxide crystal whisker of Nanometer Copper modification.
Fig. 6 is the design sketch of the Nanometer Copper modification four acicular type zinc oxide crystal whisker that obtains of embodiment 1～5 after to Escherichia coli sterilization in 4 hours.(a) in figure～(e) component is respectively the antibacterial effect figure of the Nanometer Copper modification four acicular type zinc oxide crystal whisker that embodiment 1～5 obtains, and (f) component is the antibacterial effect figure without the four acicular type zinc oxide crystal whisker of Nanometer Copper modification.
Above experimental result shows: the antibacterial effect of the four acicular type zinc oxide crystal whisker after the modification of the inventive method Nanometer Copper has obtained significant lifting.And in the inventive method along with the minimizing of the addition of sodium potassium tartrate tetrahydrate and copper chloride, the corresponding slight reduction of its sterilizing rate.
Claims (2)
1. a method that improves antibacterial property of tetrapod-like zinc oxide whisker, the steps include:
A, the four acicular type zinc oxide crystal whisker that is white powdery by outward appearance join in the aqueous solution of sodium potassium tartrate tetrahydrate and form pasty state or suspension, stir 10～30 minutes, and described sodium potassium tartrate tetrahydrate and the mol ratio of four acicular type zinc oxide crystal whisker are 0.1～1: 100; Under stirring, slowly add again the aqueous solution with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 30～60 minutes; Finally, after filtration, washing, dry, obtain the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits nanometer cupric tartrate;
B, the composite powder that A step is obtained are warming up to 270～300 ℃ of insulations 15～60 minutes in hydrogen atmosphere, are cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition Nanometer Copper.
2. a kind of method that improves antibacterial property of tetrapod-like zinc oxide whisker according to claim 1, is characterized in that: described washing is for first washing with water, then washes with alcohol.
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| CN103276476B (en) * | 2013-04-09 | 2015-03-25 | 西南交通大学 | Method for preparing nano-carbon fibers by T-ZnOw surface in-situ polymerization |
| CN105475354B (en) * | 2015-11-25 | 2018-03-02 | 航天神舟生物科技集团有限公司 | A kind of CNT/four acicular type zinc oxide crystal whisker composite antibacterial material and preparation method thereof |
| CN107174949A (en) * | 2017-05-27 | 2017-09-19 | 郭强 | A kind of indoor air purification compound formulation and preparation method thereof |
| CN112251115A (en) * | 2020-11-04 | 2021-01-22 | 杭州吉邦综合服务有限公司 | Concrete steel structure anticorrosive paint and production process thereof |
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| CN1771807A (en) * | 2005-07-29 | 2006-05-17 | 西南交通大学 | Inorganic antiseptic of zinc oxide lattice carried silver and its prepn |
| CN101181755A (en) * | 2007-12-17 | 2008-05-21 | 中国铝业股份有限公司 | Method for preparing nano Cu/ZnO composite material |
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| CN101974740A (en) * | 2010-10-29 | 2011-02-16 | 北京矿冶研究总院 | Preparation method of zinc oxide whisker loaded copper and silver |
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| JP3381274B2 (en) * | 1992-07-30 | 2003-02-24 | 松下電器産業株式会社 | Algae-proofing composition and algae-proofing agent for ornamental fish using the present composition |
| JPH06100403A (en) * | 1992-09-22 | 1994-04-12 | Hakusui Chem Ind Ltd | Antimicrobial and mildewproofing composition |
| JPH08133918A (en) * | 1994-11-11 | 1996-05-28 | Matsushita Electric Ind Co Ltd | Inorganic antimicrobial agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1771807A (en) * | 2005-07-29 | 2006-05-17 | 西南交通大学 | Inorganic antiseptic of zinc oxide lattice carried silver and its prepn |
| CN101181755A (en) * | 2007-12-17 | 2008-05-21 | 中国铝业股份有限公司 | Method for preparing nano Cu/ZnO composite material |
| CN101302710A (en) * | 2008-06-16 | 2008-11-12 | 中南大学 | Inorganic coating anti-bacterial fiber and preparation thereof |
| CN101974740A (en) * | 2010-10-29 | 2011-02-16 | 北京矿冶研究总院 | Preparation method of zinc oxide whisker loaded copper and silver |
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