CN101151967A - Nano antimicrobial powder body with shell powder as carrier and method for preparing the same - Google Patents
Nano antimicrobial powder body with shell powder as carrier and method for preparing the same Download PDFInfo
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- CN101151967A CN101151967A CNA2006101224575A CN200610122457A CN101151967A CN 101151967 A CN101151967 A CN 101151967A CN A2006101224575 A CNA2006101224575 A CN A2006101224575A CN 200610122457 A CN200610122457 A CN 200610122457A CN 101151967 A CN101151967 A CN 101151967A
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Abstract
The invention discloses a nanometer antibacterial powder body which takes shell powder as a carrier and a preparation method of the antibacterial powder body. The antibacterial powder body includes 80-98 percent (weight) of shell powder carrier (optimum selection of 85-97 percent) and 2-20 percent (weight) of nanometer antibacterial active components (optimum selection of 3-15 percent) which firmly absorb inner cavity of the shell powder with grain diameter of 1-100 nanometer. The invention is characterized by small grain diameter, sound compatibility with materials, safety, innocuity, extensive antimicrobial spectrum, high antibacterial efficiency, sound stability and no color fade, which can be used in fields of plastics, rubber, fiber, coating, home appliance, ceramic ware, water treatment and medical products. In the respects of material source and production process, the invention overcomes defections of generally high prices of mass antibacterial products, which not only lowers production costs of antibacterial agents, but also is beneficial for governing increasingly serious environment pollutions and has great significance of the environmental protection.
Description
Technical field:
The present invention relates to a kind of antiseptic nano powder and preparation method thereof, particularly relating to a kind of is the antiseptic nano powder and preparation method thereof of carrier with the conch meal, the metal nanometer material technical field.
Background technology:
1996, the 0-157 that Japan takes place infected incident, is once once causing global fear.And comprise cholera, pneumonia, malaria, tuberculosis and the hepatitis etc. that cause because of bacterial infection in the whole world cause human death to be seen in report especially again and again, and are startling.For this reason, control and growth of elimination harmful microbe and breeding are one of most important in the current new and high technology.Wherein, adding antibacterial agent, to prepare antibiotic functional material in material be a kind of efficient ways.
The used antibacterial agent of antibacterial product is divided into natural, organic and inorganic three big series.Though natural antibacterial agent has tight security, but its antibacterial effect is bad, poor heat resistance, mass marketization not as yet at present; Organic antibacterial agent because of its efficiently 1 characteristic of sterilization fast obtain market cream and look at, in industries such as food production, medical environment, breed, use in a large number.But, along with improving constantly of people's living standard, degree of concern to health is also more and more higher, green and environmental protection becomes focus, recognize that a large amount of use organic antibacterial agents have certain negative effect to human body and environment, easily produce drug resistance and cause secondary pollution, its consumption begins to be restricted; Simultaneously, market constantly enlarges the demand field of anti-biotic material, products such as fiber, plastics, pottery, glass, coating, rubber have been proposed antibiotic requirement, and organic antibacterial agent can not satisfy market demands because of himself characteristics poor chemical stability, poor heat resistance.In recent years, inorganic new material development is rapid, and the especially appearance of nano material is for the rise of inorganic antiseptic is taken a firm foundation.The nano inorganic antimicrobial agent report is a lot, is to go up loaded with nano level silver, zinc, copper etc. at inorganic carrier material (as zeolite, montmorillonite etc.) mostly.When contacting with bacterium, metal ion slowly releases, because metal ion has oxidation-reducibility, can react with organic matter (thio group, carboxyl, hydroxyl), and can combine with bacterial cell membrane and memebrane protein, destroy its structure, enter the enzyme that destroys electron transport system behind the cell and with the DNA reaction, reach the sterilization purpose.Test shows, because zeolite and montmorillonite are natural minerals, preliminary treatment is difficulty relatively, be difficult to disperse, poor with the compatibility of material, can influence the performance and the processing characteristics of material itself, the antibiotic persistence of material of preparation is poor, and the antibacterial agent consumption is big, uses to be restricted equally.In recent years, surfaces externally and internally by porous material is that main body is carried out the self assembly of nanoparticle and the research focus that the load synthetic technology has become field of nanometer material technology. Chinese invention patent 01110767 " aggregation-preventing nanometer wide-spectrum antibacterial silve powder and inductrial production process " discloses a kind of aggregation-preventing nanometer wide-spectrum antibacterial silve powder and inductrial production process, nano silver powder securely on the vegetable material attached to some natural porous, is made that Nano Silver type antimicrobial product is on the high side.
The present invention is from raw material sources, production technology, overcome the general higher shortcoming of numerous antimicrobial product prices on the current market, this not only greatly reduces the production cost of antibacterial agent, and helps administering serious environmental pollution problem day by day, has very big environment protection significance.The invention provides a kind of is the antiseptic nano powder of carrier with the conch meal, because characteristics such as conch meal porous, light weight, thereby make antimicrobial powder have better broad-spectrum antiseptic function, this antiseptic nano powder does not contain organic solvent, environmentally safe during use, waste of material is few, is a kind of environmental type new material.
Summary of the invention:
The object of the present invention is to provide with the conch meal is the antiseptic nano powder of carrier, and reduces the production cost of antiseptic nano powder.This antimicrobial powder has characteristics such as particle diameter is little, good with material compatibility, safety non-toxic, has a broad antifungal spectrum, antimicrobial efficiency height, good stability, nondiscolouring.Another object of the present invention is to provide the preparation method of above-mentioned antiseptic nano powder.The nano-antibacterial active component (preferred 3-15%) that contains conch meal carrier (preferred 85-97%) and the 2-20% (weight) of 80-98% (weight) in this antimicrobial powder, in the micropore of conch meal, firmly adsorbing the nano-antibacterial active component, its particle diameter is the 1-100 nanometer, and wherein the antibacterial activity component is the blending ingredients of silver or silver and copper, nickel or zinc.Described conch meal is oyster shell powder, spiral shell shell powder, Concha Meretricis Seu Cyclinae powder, conch meal.
The preparation method who with the conch meal is the antiseptic nano powder of carrier has three kinds:
(1) preparation AgNO
3(concentration is 0.001-0.010molL to solution
-1), conch meal soak (agitation as appropriate or with frequency be the ultrasonic of 40-200kHz handle to make antimicrobial component is loaded on the carrier), separation cleaning, oven dry, comminution by gas stream, illumination, cleaning, oven dry make product.Wherein separate to clean and adopt centrifugation to clean, wash number is 2 times, and light application time is 30-60min.
(2) preparation AgNO
3(concentration is 0.001-0.010molL to solution
-1), conch meal soak (agitation as appropriate or with frequency be the ultrasonic of 40-200kHz handle to make antimicrobial component is loaded on the carrier), separate clean, immersion one hour in reductant solution, separate and washing, oven dry and comminution by gas stream make product again, and wherein reductant can be selected formaldehyde, ascorbic acid, oxalic acid, hydrazine hydrate or glucose solution etc. for use.
(3) preparation silver ammino ion solution, conch meal soak (agitation as appropriate or with frequency be the ultrasonic of 40-200kHz handle to make antimicrobial component is loaded on the carrier), separate cleaning, in reductant solution, reaction is 2-3 hour under 60-80 ℃ of condition, add copper nitrate, nickel nitrate or zinc nitrate solution again, under 60-80 ℃ of condition (agitation as appropriate or with frequency be the ultrasonic of 40-200kHz handle to make antimicrobial component is loaded on the carrier) reaction 3-5 hour, washing, dry, comminution by gas stream make product.
The present invention is that the antiseptic nano powder of carrier has following performance characteristics with the conch meal:
(1) has a broad antifungal spectrum, antimicrobial efficiency height: can prevent the growth of the bacterium (as Escherichia coli, staphylococcus aureus, Pseudomonas aeruginosa, bud pole bacterium, Candida albicans, hemolytic streptococcus, Friedlander etc.) in the environment.
(2) tight security: nontoxic, can be added in the material of contact food, as packaging material for food and tableware, by the index of toxicological test (as acute toxicity experience, Ames experiment and skin irritation test), be nontoxic antiseptic nano powder.
(3) good stability: do not have volatilization, do not dissolve, the heat resisting temperature height can not make the goods variable color in the adding goods.
(4) compatibility with material is good: can be added on intermediate preparation antibiotic functional materials such as plastics, rubber, fiber, coating, paper, adhesive, pottery and glass.
(5),, therefore have nano particle distinctive 1 so end article can reach nanoscale because this antibacterial agent is to make of solwution method, and the antibacterial activity component enters in the carrier with ionic condition) small-size effect; 2) surface interface effect; 3) quantum effect.Antiseptic nano powder excellent performance of the present invention has quick, efficient, durable antibiotic bactericidal effect.
Product of the present invention can be used as the skin infection material of treatment traumatic patient, have broad spectrum antibacterial, long-lasting, kill excellent properties such as drug resistance. from raw material sources, production technology, overcome the general higher shortcoming of numerous antimicrobial product prices on the current market, this not only greatly reduces the production cost of silver type antibacterial agent, and help administering serious environmental pollution problem day by day, have very big environment protection significance.Therefore, the present invention not only has very high economic benefit, and can obtain the huge social benefit.
Figure of description:
Accompanying drawing is that the present invention is the process chart of the antiseptic nano powder of carrier with the conch meal
Embodiment
At this is that example elaborates preparation process with the oyster shell powder.
Embodiment 1
(1), takes by weighing 0.102gAgNO
3, be dissolved in the 100ml deionized water, obtaining concentration is 0.006molL
-1AgNO
3Solution; (2), take by weighing the oyster shell powder of 2.0g drying, put into AgNO
3Soak agitation as appropriate or be that the ultrasonic of 40kHz handles that oyster shell powder is soaked is thorough in the solution with frequency; (3), centrifugation AgNO
3Solution and oyster shell powder are poured out upper strata AgNO
3Behind the solution, add proper amount of deionized water at once, centrifugation more immediately after shaking up, according to said method cleaning process wants fast, avoids the AgNO that will adsorb in the oyster shell powder
3Wash-out comes out; (4), above-mentioned separating obtained sample is dried (can adopt atomized drying in batches) under about 80-100 ℃ condition; (5), with the suitable comminution by gas stream of dried sample; (6), with the sample placement of in vessel, making thinner, with solar radiation sample 30-60min, in the illumination process, suitably stir sample and make illumination even, just formed the nano-Ag particles that is evenly distributed in the oyster shell powder after the illumination; (7), use the washed with de-ionized water sample, wash residual AgNO
3Deng; (8), oven dry and comminution by gas stream, promptly prepare antiseptic nano powder of the present invention, sealing is preserved then.Experimental result sees Table one.
Embodiment 2
(1), takes by weighing 0.102g AgNO
3, be dissolved in the 100ml deionized water, obtaining concentration is 0.006 molL
-1AgNO
3Solution; (2), take by weighing the oyster shell powder of 2.0g drying, put into AgNO
3Soak agitation as appropriate or be that the ultrasonic of 40kHz handles that oyster shell powder is soaked is thorough in the solution with frequency; (3), separate AgNO
3Solution and oyster shell powder are poured out upper strata AgNO
3Behind the solution, add proper amount of deionized water at once, centrifugation more immediately after shaking up, then according to said method again with washed with de-ionized water once, it is fast that cleaning process is wanted, and avoids the AgNO that adsorbs in the oyster shell powder
3Come out; (4), add an amount of formaldehyde and soak sample, about 1 hour of soak time, formaldehyde makes the AgNO of absorption in the oyster shell powder
3In Ag
+Reduction forms nano-Ag particles; (5), again adopt centrifugation, and use the washed with de-ionized water sample; (6), oven dry and comminution by gas stream, promptly prepare antiseptic nano powder of the present invention, sealing is preserved then.Experimental result sees Table one.
Embodiment 3
The oyster shell powder carrier is made into 20% suspension 1L, adds 1.4molL
-1Silver nitrate aqueous solution 80ml stirs or is ultrasonic processing reaction 1-3 hour of 40kHz with frequency at 60 ℃, adds 1molL then
-1Reductant oxalic acid solution 30-100mL 60-80 ℃ of reaction 2-3 hour, with product washing, drying and comminution by gas stream, promptly prepares antiseptic nano powder of the present invention, and sealing is preserved then.Experimental result as shown in Table 1.
Embodiment 4
The oyster shell powder carrier is made into 20% suspension 1L, adds 2molL
-1Zn (NO
3)
2Solution 100ml stirs or is ultrasonic processing reaction 2-3 hour of 40kHz with frequency at 70 ℃, with product washing, drying and comminution by gas stream, promptly prepares antiseptic nano powder of the present invention, sealing preservation then.Experimental result sees Table one.
Embodiment 5-6
During reaction kinetic, respectively with Cu (NO
3)
2, Ni (NO
3)
2Replace Zn (NO
3)
2, other and embodiment 4 with, experimental result sees Table one.
Embodiment 7
The oyster shell powder carrier is made into 10% suspension 1L, adds 0.5molL
-1AgNO
3Solution 100ml adds 1molL then
-1Ascorbic acid reductant 50-100mL stirs or is ultrasonic processing reaction 2-3 hour of 40kHz with frequency at 60-80 ℃.Add 2molL again
-1Zn (NO
3)
2Solution 80ml stirs or is the ultrasonic processing reaction 3 hours of 40kHz with frequency at 70 ℃, and with the product washing, drying and comminution by gas stream are promptly prepared antiseptic nano powder of the present invention, sealing preservation then.Experimental result sees Table
Embodiment 8-9
During reaction kinetic respectively with Cu (NO
3)
2, Ni (NO
3)
2Replace Zn (NO
3)
2, other is identical with embodiment 7, and experimental result sees Table one.
Embodiment 10
The oyster shell powder carrier is made into 20% suspension 1L, adds 1molL
-1Silver ammino ion 10-50mL, stir or be ultrasonic processing reaction 3-5 hour of 40kHz at 50-70 ℃ with frequency, add 1molL then
-1Hydrazine hydrate reduction agent 30-100mL 60-80 ℃ of reaction 2-3 hour, adds 2molL again
-1Cn (NO
3)
2And 2molL
-1Zn (NO
3)
2Each 80ml of solution stirs or is the ultrasonic processing reaction 3 hours of 40kHz with frequency at 70 ℃, and with product cleaning, drying and comminution by gas stream are promptly prepared antiseptic nano powder of the present invention, sealing preservation then.Experimental result sees Table one.
The experimental result of table one antiseptic nano powder powder
| Embodiment | Average grain diameter (nm) | Antibacterial metal constituent content (%) | Minimum inhibitory concentration (ppm) | Toxicological experiment | |||
| Escherichia coli | Staphylococcus aureus | Acute toxicity testing LD 50(mg/kg) | The mutagenesis experiment | Skin primary stimulation test | |||
| 1 | 49 | 3.7(Ag) | 50 | 74 | ＞10000 | Negative | Non-stimulated |
| 2 | 46 | 3.7(Ag) | 50 | 74 | ＞10000 | Negative | Non-stimulated |
| 3 | 50 | 3.7(Ag) | 50 | 74 | ＞10000 | Negative | Non-stimulated |
| 4 | 51 | 6.2(Zn) | 1950 | 1960 | ＞10000 | Negative | Non-stimulated |
| 5 | 44 | 6.0(Cu) | 1600 | 1500 | ＞10000 | Negative | Non-stimulated |
| 6 | 47 | 5.9(Ni) | 2000 | 2000 | ＞10000 | Negative | Non-stimulated |
| 7 | 70 | 2.6(Ag)，4.7(Zn) | 75 | 100 | ＞10000 | Negative | Non-stimulated |
| 8 | 54 | 2.9(Ag)，4.5(Cu) | 75 | 99 | ＞10000 | Negative | Non-stimulated |
| 9 | 80 | 2.5(Ag)，4.5(Ni) | 75 | 100 | ＞10000 | Negative | Non-stimulated |
| 10 | 56 | 2.0(Ag)， 3.7(Zn)，4.0(Cu) | 75 | 100 | ＞10000 | Negative | Non-stimulated |
Annotate: 1. by the analyses metal element content;
2. colibacillary test strain is ATCC25922, and the test strain of staphylococcus aureus is ATCC6538;
3. acute toxicity experience is to measure white mouse oral dose LD
50
4. the skin irritatin reaction is an experimental animal with the rabbit;
5. the mutagenesis experiment is an experimental animal with the white mouse;
6. measure its particle diameter by high magnification TEM method.
Embodiment 11
Embodiment 1 prepared antiseptic nano powder is added plastics such as PE, PP, ABS respectively, manage to be uniformly dispersed, adopt the anti-microbial property after film adherence method is surveyed its contact 24h, experimental result as shown in Table 2.
The anti-microbial property of table two plastic sheet
| The antibiotic plastic matrix | Antimicrobial powder addition (% (wt)) | Anti-microbial property | |
| Escherichia coli (%) | Staphylococcus aureus (%) | ||
| PE | 0.5 | 92.3 | 94.0 |
| PE | 1 | 99.8 | 99.8 |
| PP | 0.5 | 91.0 | 92.4 |
| PP | 1 | 99.4 | 99.6 |
| ABS | 0.5 | 90.7 | 91.2 |
| ABS | 1 | 98.8 | 99.0 |
Embodiment 12
The PP resin that will contain the antiseptic nano powder (embodiment 1 preparation) of 1% (wt) is spun into 90 purpose fibers, measures its anti-microbial property, the result as shown in Table 3:
The anti-microbial property of table three anti-bacterial fibre
| Fiber | Anti-microbial property | |
| Escherichia coli (%) | Staphylococcus aureus (%) | |
| Do not add antimicrobial powder | 0 | 0 |
| 1% (wt) antimicrobial powder | 99.0 | 99.6 |
Embodiment 13
Embodiment 1 prepared antiseptic nano powder is added under the ceramic glaze, and addition is 2%, fully is uniformly dispersed, and makes antibiotic ceramic tile, adopts the anti-microbial property after film adherence method is surveyed its contact 24h, and experimental result sees Table four.
The anti-microbial property of the antibiotic ceramic tile of table four
| Ceramic tile | Anti-microbial property | |
| Escherichia coli (%) | Staphylococcus aureus (%) | |
| Blank ceramic tile | 60.6 | 55 |
| 2% (wt) antimicrobial powder ceramic tile | 99.3 | 99.8 |
Claims (16)
1. one kind is the antiseptic nano powder of carrier with the conch meal, it is characterized in that containing in the antimicrobial powder nano-antibacterial active component of conch meal carrier and the 2-20% (weight) of 80-98% (weight).It is characterized in that firmly adsorbing in the micropore of conch meal the nano-antibacterial particle, its particle diameter is the 1-100 nanometer.
2. antiseptic nano powder according to claim 1 is characterized in that described conch meal is oyster shell powder, spiral shell shell powder, Concha Meretricis Seu Cyclinae powder, conch meal.
3. antiseptic nano powder according to claim 1 is characterized in that containing the nano-antibacterial active component of conch meal carrier and the 3-15% (weight) of 85-97% (weight).
4. antiseptic nano powder according to claim 1 is characterized in that described antibacterial activity component is one or more in silver, copper, nickel or the zinc.
5. the preparation method of antiseptic nano powder according to claim 1 is characterized in that comprising preparation AgNO
3Solution, conch meal soak (agitation as appropriate or with frequency be the ultrasonic of 40-200kHz handle to make antimicrobial component is loaded on the carrier), separation cleaning, oven dry, comminution by gas stream, illumination, cleaning, oven dry make product.
6. the preparation method of antiseptic nano powder according to claim 1 is characterized in that comprising preparation AgNO
3Solution, conch meal soak (agitation as appropriate or with frequency be the ultrasonic of 40-200kHz handle to make antimicrobial component is loaded on the carrier), separate and clean, in reductant solution, soak, separate also and clean, dry again and make product.
7. the preparation method of antiseptic nano powder according to claim 1, it is characterized in that comprising preparation silver ammino ion solution, conch meal soak (agitation as appropriate or with frequency be the ultrasonic of 40-200kHz handle to make antimicrobial component is loaded on the carrier), separate cleaning, in reductant solution, react, add again the reaction of copper nitrate, nickel nitrate or zinc nitrate solution (agitation as appropriate or with frequency be the ultrasonic processing of 40-200kHz make antimicrobial component is loaded on the carrier), washing, dry, comminution by gas stream promptly make product.
8. the preparation method of antiseptic nano powder according to claim 5 is characterized in that light application time is 30-60min.
9. according to the preparation method of claim 5 or 6 described antiseptic nano powders, it is characterized in that described separation cleaning employing centrifugation cleaning, wash number is 2 times.
10. according to the preparation method of claim 5 or 6 described nanometer Hangzhoupro bacterium powders, it is characterized in that AgNO
3The concentration of solution is 0.001-0.01molL
-1
11., it is characterized in that reductant is formaldehyde, ascorbic acid, oxalic acid, hydrazine hydrate or glucose solution according to the preparation method of claim 6 or 7 described antiseptic nano powders.
12. the preparation method of antiseptic nano powder according to claim 7 is characterized in that adding the reductant reaction after 2-3 hour, added copper nitrate, nickel nitrate or zinc nitrate solution again and reacted 3-5 hour.
13. the preparation method of antiseptic nano powder according to claim 7 is characterized in that reaction temperature is 60-80 ℃.
14. the preparation method of antiseptic nano powder according to claim 7, it is characterized in that described antibacterial activity component except that comprising silver ion, also should comprise at least a in copper, zinc, nickel ion and corresponding copper sulphate thereof, copper chloride, zinc sulphate, zinc chloride, nickel nitrate, the nickel chloride salt compounds.
15. according to the preparation method of claim 5,6 or 7 described antiseptic nano powders, the ultrasonic frequency that it is characterized in that handling described nanometer conch meal and antimicrobial component is 40-80kHz.
16. antiseptic nano powder according to claim 1 is characterized in that prepared antiseptic nano powder is added suitable medicinal adjuvant or excipients can make pulvis, tablet, paste, creme, film, gel, patch, injection, aqua, spray or biological medicine chip.
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