CN102578148A - 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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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 antibacterial agent preparation methods, relate in particular to four acicular type zinc oxide crystal whisker complex antimicrobials preparation methods.
Background technology
Noxious bacteria is present in the various occasions around us, like housing floor, the metope of living, the furniture of use, household electrical appliances, clothing and articles for daily use etc.1996, the national infection incident of O-157 Escherichia coli of Japanese large tracts of land outburst was not only seized many people's life, and caused that the whole world is panic.According to statistics, the whole world is annual because of bacterial infection causes dead number near 2,000 ten thousand, accounts for more than 30% of dead sum; The intersection bacterial infection rate of each hospital surpasses 10%.Will prevent effectively that bacterium from producing and grow, using anti-biotic material is the most simple and efficient method.Anti-biotic material is meant one type of new function material with sterilization and bacteria growing inhibiting function.Wherein inorganic antiseptic is because it is long-lasting, stability and be difficult for causing that pesticide resistance has obtained extensive use.
Inorganic antiseptic adopts the physical adsorption ion-exchange process, and metals such as silver, copper, zinc are carried on porous material surface, utilizes the antibacterial action of metal ion, reaches the purpose of long-acting bacteriostatic through slow releasing function.Inorganic antiseptic does not produce drug resistance and safety is good, and particularly its outstanding warm tolerance (＞600 ℃) has very big advantage in the application of multiple antibacterial product.
Existing inorganic antiseptic is main with silver and zinc ion mainly; Wherein best with the antibacterial effect of silver ion; But silver ion antimicrobial agent exists and to be prone to be reduced and variable color (being grey black) and cost high two big shortcomings, and simple substance is silver-colored to be lost or weaken its antibacterial effect greatly owing to becoming after reducing.At present, have and report that much nano material has antibiotic property, but simple nano material has very big surface area because particle diameter is too little, be difficult in use fully disperse, even can't disperse.Coat processing so all will carry out the surface before using to it.The result who coats greatly reduces the performance of nano effect and antibacterial action on the one hand, and this on the other hand processing procedure also is very loaded down with trivial details.Moreover, more existing nano-powder materials are (like nano-TiO
2) will rely on photocatalysis just to show certain antibacterial effect.
(spy opens flat 5-912 to Japan Patent; Te Kaiping 8-133918) report is compound with four acicular type zinc oxide crystal whisker and silver salt; Prepared inorganic antiseptic and obtained in different materials and environment to use that (Te Kaiping-93365, spy open flat 5-78498, and the spy opens flat 78218 with excellent antibacterial effect; Te Kaiping 6-140731 etc.); The spicule activated centre and the point effect of the techniques make use ZnOw of these Japan Patent reports activate airborne water and oxygen repeatedly, produce hydroxyl radical free radical (OH) and active oxygen ion (O
2 -), destroy bacteria live and multiplication capacity and make bacterial death, and reach antibacterial effect.But owing to use 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, and in order to improve its antibacterial effect, one of its method is to add silver ion (like ZL 200510115039.9), yet the doping process of silver ion is complicated, and product cost is high, and receives the restriction of this resource of silver.So necessary exploitation is a kind of to improve the four acicular type zinc oxide crystal whisker anti-microbial property, and antibacterial agent allochroic, not with low cost.
Summary of the invention
The purpose of this invention is to provide a kind of method that improves the four acicular type zinc oxide crystal whisker anti-microbial property, the four acicular type zinc oxide crystal whisker bactericidal power of handling with this method is stronger, and nondiscolouring and with low cost in the 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 the four acicular type zinc oxide crystal whisker anti-microbial property the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery joined in the aqueous solution of sodium potassium tartrate tetrahydrate and form pasty state or suspension; Stirred 10～30 minutes; The mol ratio of described sodium potassium tartrate tetrahydrate and four acicular type zinc oxide crystal whisker is 0.1～1: 100, and the amount of described potassium tartrate sodium water solution also can form the amount of scattered paste shape more than or equal to ability submergence four acicular type zinc oxide crystal whisker; Under stirring, slowly add the aqueous solution again with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 30～60 minutes; At last, through filtering, wash, drying, get the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits the nanometer cupric tartrate;
B, the composite powder that the A step is obtained are warming up to 270～300 ℃ of insulations 15～60 minutes in hydrogen atmosphere, be 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:
In solution, evenly adsorb potassium tartrate sodium through four acicular type zinc oxide crystal whisker; Then in the process that drips the equivalent copper chloride; Copper chloride and sodium potassium tartrate tetrahydrate reaction generate the nanometer cupric tartrate, thereby have 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 the cupric tartrate thermolysis be nano simple substance copper, thereby obtain the four acicular type zinc oxide crystal whisker of surperficial uniform deposition nano simple substance copper.
Through above distinctive nanometer copper in-situ deposition modified technique, the present invention has realized that nano copper particle evenly and stably is deposited on the four acicular type zinc oxide crystal whisker surface, and the nanometer shot copper directly is about 20nm; Sterilizing rate had brought up to 98.5%～99.9% by 68.0% in 4 hours, had obviously improved its antibacterial effect.
With respect to the Ag deposition and the doping of costliness, the nanometer copper of this method deposition, it is cheap; And the nanometer copper nondiscolouring in use of deposition, more welcome, promote easily, have more wide application prospect.
Above-mentioned washing is to use washing earlier, washes with alcohol again.
Washing can be washed unnecessary inorganic ions the most simply and easily off, avoids in subsequent processes, forming impurity, makes the purity that makes thing high, and sterilizing ability is strong; Add alcohol and wash the dispersiveness that to remove organic impurities and improve powder, further improve the sterilizing ability of prepared product.
Below in conjunction with accompanying drawing and embodiment the present invention is made further detailed description.
Description of drawings
Fig. 1 is the close-up view that use emission surface sweeping Electronic Speculum is amplified the nanometer copper modification four acicular type zinc oxide crystal whisker that 80,000 times of observed embodiment 1 obtain.
Fig. 2 is the spicule surface local shape appearance figure that use emission surface sweeping Electronic Speculum is amplified the nanometer copper modification four acicular type zinc oxide crystal whisker that 160,000 times of observed embodiment 1 obtain.
Fig. 3 is the surperficial X-ray photoelectron spectroscopic analysis result of nanometer copper modification four acicular type zinc oxide crystal whisker that embodiment 1 obtains.
Fig. 4 is the close-up view that use emission surface sweeping Electronic Speculum is amplified the nanometer copper modification four acicular type zinc oxide crystal whisker that 40,000 times of observed embodiment 3 obtain.
Fig. 5 is the spicule surface local shape appearance figure that use emission surface sweeping Electronic Speculum is amplified the nanometer copper modification four acicular type zinc oxide crystal whisker that 160,000 times of observed embodiment 3 obtain.
Fig. 6 is that the four acicular type zinc oxide crystal whisker of the nanometer copper modification that obtains of embodiment 1～5 is to the design sketch of Escherichia coli sterilization after 4 hours.(a)～(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 among the figure, and (f) component is the antibacterial effect figure without the four acicular type zinc oxide crystal whisker of nanometer copper modification.
Embodiment
Embodiment 1
A kind of method that improves the four acicular type zinc oxide crystal whisker anti-microbial property the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery joined in the potassium tartrate sodium water solution form pasty state, stirred 30 minutes, the mol ratio of described sodium potassium tartrate tetrahydrate and four acicular type zinc oxide crystal whisker is 1: 100; Under stirring, slowly add the aqueous solution (mole of the copper chloride that promptly contains in this aqueous solution equates with sodium potassium tartrate tetrahydrate) again with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 60 minutes; At last, through filtering, wash, drying, get the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits the nanometer cupric tartrate;
B, the composite powder that the A step is obtained are warming up to 270 ℃ of insulations 60 minutes in hydrogen atmosphere, be 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 emission surface sweeping Electronic Speculum is amplified the nanometer copper modification four acicular type zinc oxide crystal whisker that 80,000 times of observed examples obtain, and is all adhering to tiny particle uniformly on four pins of four needle-like oxidisability whiskers.Fig. 2 is that 160,000 times of observed results are amplified on the spicule surface of whisker, and the equally distributed nano particle diameter in whisker surface is about 20nm.
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 the collection of illustrative plates, explains that there is the existence of copper on four acicular type zinc oxide crystal whisker surface that this example prepares.
Embodiment 2
A kind of method that improves the four acicular type zinc oxide crystal whisker anti-microbial property the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery joined in the potassium tartrate sodium water solution form pasty state, stirred 30 minutes, the mol ratio of described sodium potassium tartrate tetrahydrate and four acicular type zinc oxide crystal whisker is 0.8: 100; Under stirring, slowly add the aqueous solution again with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 60 minutes; At last, through filtering, wash, drying, get the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits the nanometer cupric tartrate;
B, the composite powder that the A step is obtained are warming up to 270 ℃ of insulations 40 minutes in hydrogen atmosphere, be cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition nanometer copper.
A kind of method that improves the four acicular type zinc oxide crystal whisker anti-microbial property the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery joined in the aqueous solution of sodium potassium tartrate tetrahydrate and form suspension, stirred 20 minutes, the mol ratio of described sodium potassium tartrate tetrahydrate and four acicular type zinc oxide crystal whisker is 0.6: 100; Under stirring, slowly add the aqueous solution again with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 50 minutes; At last, through filtering, wash, drying, get the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits the nanometer cupric tartrate;
B, the composite powder that the A step is obtained are warming up to 270 ℃ of insulations 30 minutes in hydrogen atmosphere, be 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 emission surface sweeping Electronic Speculum is amplified the nanometer copper modification four acicular type zinc oxide crystal whisker that 40,000 times of observed examples prepare, and is all adhering to tiny particle uniformly on four pins of four needle-like oxidisability whiskers.160,000 times of observed results are amplified on the spicule surface of Fig. 5 nanometer copper modification four acicular type zinc oxide crystal whisker that to be use emission surface sweeping Electronic Speculum prepare this example, and the equally distributed nano particle diameter in whisker surface is about 20nm.Fig. 5 and Fig. 2 compared to find 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 kind of method that improves the four acicular type zinc oxide crystal whisker anti-microbial property the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery joined in the aqueous solution of sodium potassium tartrate tetrahydrate and form pasty state, stirred 20 minutes, the mol ratio of described sodium potassium tartrate tetrahydrate and four acicular type zinc oxide crystal whisker is 0.4: 100; Under stirring, slowly add the aqueous solution again with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 40 minutes; At last, through filtering, wash, drying, get the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits the nanometer cupric tartrate;
B, the composite powder that the A step is obtained are warming up to 280 ℃ of insulations 30 minutes in hydrogen atmosphere, be cooled to room temperature, obtain the four acicular type zinc oxide crystal whisker powder of surface deposition nanometer copper.
Embodiment 5
A kind of method that improves the four acicular type zinc oxide crystal whisker anti-microbial property the steps include:
A, the four acicular type zinc oxide crystal whisker of powdery joined in the aqueous solution of sodium potassium tartrate tetrahydrate and form suspension, stirred 10 minutes, the mol ratio of described sodium potassium tartrate tetrahydrate and four acicular type zinc oxide crystal whisker is 0.1: 100; Under stirring, slowly add the aqueous solution again with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 30 minutes; At last, through filtering, wash, drying, get the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits the nanometer cupric tartrate;
B, the composite powder that the A step is obtained are warming up to 300 ℃ of insulations 15 minutes in hydrogen atmosphere, be 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 make it form pasty state or suspension with four acicular type zinc oxide crystal whisker.Because the amount of sodium potassium tartrate tetrahydrate confirms that the amount of potassium tartrate sodium water solution is promptly confirmed 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.
The antibacterial experiment result:
The four acicular type zinc oxide crystal whisker of the nanometer copper modification (surface deposition nanometer copper) that above embodiment 1～5 is made is with its sterilizing rate rate of concussion method test, with same procedure the sterilizing rate without the four acicular type zinc oxide crystal whisker of nanometer copper modification also tested simultaneously.
The specific practice of test is: every liter of Escherichia coli suspension that contains five gram four acicular type zinc oxide crystal whiskers is cultivated 4h through concussion, the Escherichia coli before and after the experiment are counted, draw 4 hours sterilizing rates.The 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 are merely 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)～(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 among the figure, 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 the four acicular type zinc oxide crystal whisker anti-microbial property the steps include:
A, be that the four acicular type zinc oxide crystal whisker of white powdery joins in the aqueous solution of sodium potassium tartrate tetrahydrate and forms pasty state or suspension, stirred 10～30 minutes that the mol ratio of described sodium potassium tartrate tetrahydrate and four acicular type zinc oxide crystal whisker is 0.1～1: 100 with outward appearance; Under stirring, slowly add the aqueous solution again with sodium potassium tartrate tetrahydrate equimolar amounts copper chloride; Afterwards, continue to stir 30～60 minutes; At last, through filtering, wash, drying, get the four acicular type zinc oxide crystal whisker composite powder that surface in situ deposits the nanometer cupric tartrate;
B, the composite powder that the A step is obtained are warming up to 270～300 ℃ of insulations 15～60 minutes in hydrogen atmosphere, be 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 the four acicular type zinc oxide crystal whisker anti-microbial property according to claim 1 is characterized in that: described washing, is washed with alcohol with washing for earlier again.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103276476A (en) * | 2013-04-09 | 2013-09-04 | 西南交通大学 | Method for preparing nano-carbon fibers by T-ZnOw surface in-situ polymerization |
| CN105475354A (en) * | 2015-11-25 | 2016-04-13 | 航天神舟生物科技集团有限公司 | Carbon nanotube/tetrapod-shaped zinc oxide 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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