CN104145993A - Method for preparing complex antimicrobial agent by blending chitosan and silver copper - Google Patents
Method for preparing complex antimicrobial agent by blending chitosan and silver copper Download PDFInfo
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- CN104145993A CN104145993A CN201410379214.4A CN201410379214A CN104145993A CN 104145993 A CN104145993 A CN 104145993A CN 201410379214 A CN201410379214 A CN 201410379214A CN 104145993 A CN104145993 A CN 104145993A
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- silver
- chitosan
- shitosan
- copper
- nitrate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention relates to a method for preparing a complex antimicrobial agent by blending chitosan and silver copper. The method comprises the following steps: silver nitrate and cupric nitrate are blended according to the concentration ratio of 1:30 to 1:80, and then are blended with chitosan. Therefore, a light blue antibacterial agent powder is prepared. According to the method provided by the invention, the usage amount of silver is reduced, the chitosan is also used as a reducing agent, chemical reagents are no longer added, and the toxicity of an antibacterial agent is reduced. Due to the change of technological conditions, the oxidation-reduction reaction of the chitosan and the cupric nitrate can be performed sufficiently, an aldehyde group (-CHO) is generated in the reaction, Ag<+> is enabled to be completely reduced to elemental silver, Cu<2+> is hibernated in a chitosan basal body, so as to play a synergistic antibacterial effect, a remarkable inhibiting effect on escherichia coli and staphylococcus aureus is detected through an inhibition ring test, an inhibition ring which is equal to or greater than 10 mm is formed under a culture condition of 37 DEG C, a remarkable bacteriostatic effect is played, materials used cause no harm to human body, the price is low, and the novel complex antimicrobial agent is green and environment-friendly.
Description
Technical field
The present invention relates to a kind of preparation method of complex antimicrobials, especially a kind of preparation method of the complex antimicrobials for the employing shitosan of weaving and silver-bearing copper blend.
Background technology
The antibacterial Ag that conventionally adopts that existing preparation has the shitosan class of anti-microbial property exists as main antibacterial.
Shitosan is a large amount of a kind of natural green alkaline polysaccharides that exist in biosphere, has a large amount of hydroxyls and amino isoreactivity group, is easy to metal ion and stings and close.And there are unique biocompatibility, biological degradability, antibiotic property, avirulence, biologically active and physico chemical property and cause and people's attention have wide practical use in chemical industry, weaving, printing and dyeing, papermaking and medicine and other fields.
Publication number is CN's 101297654 patent of invention of " a kind of preparation method of silver-loaded silica-chitosan compound anti-bacteria agent ", this patent is taking silica as inorganic raw material, taking polymer chitosan as Organic Ingredients, taking deionized water, silver nitrate, ammoniacal liquor, KH-550, glacial acetic acid, watery hydrochloric acid, glutaraldehyde, absolute ethyl alcohol as reagent, react by water-soluble synthetic chemistry, finally obtain white powder.This method technological process is short, and use equipment is few.But this patent is used more acids chemical reagent in preparation process, increases cost, also make to be restricted in medical material application aspect, easily health is produced and threatened.
The Hu Zongzhi of SanXia University, the good grade of forest of Zhongshan University has been inquired into taking natural polymer chitosan as raw material, carry out solution blending and it is carried out to toughening modifying with polyvinyl alcohol, in this blend film, shitosan and polyvinyl alcohol have good compatibility between the two, toughness has obtained obvious improvement, but its heat endurance declines to some extent with tensile strength, does not embody the anti-microbial property that shitosan has simultaneously.
The Wei Liqiao of Institutes Of Technology Of Taiyuan has inquired into the composite antibacterial latex of chitosan-loaded silver, this invention is taking polymer chitosan as Organic Ingredients, taking deionized water, silver nitrate, sodium borohydride, absolute ethyl alcohol etc. as reagent, react by water-soluble synthetic chemistry, finally obtain the antibacterial latex of brown, this method technological process is short, and use equipment is few.But this patent has been used the reagent such as borane reducing agent sodium hydride in preparation process, this is because shitosan is weak reductant, can not be simple substance silver by silver nitrate reduction, and the silver nitrate amount that preparation process is used is larger, has increased the cost of commercial Application.
Summary of the invention
The present invention adopts the mantle plate of shitosan as antibacterial agent, and silver-bearing copper blend is obtained to a kind of complex antimicrobials, makes it have good and safe anti-microbial property.Add copper to solve in existing product silver-colored usage amount, in preparation process, do not need the chemical reagent such as additional reducing agent, obtain the green NEW TYPE OF COMPOSITE antibacterial agent that anti-microbial property is good and cost is low, thereby provide a kind of shitosan and silver-bearing copper blend to prepare the method for complex antimicrobials.
Above-mentioned purpose is achieved through the following technical solutions.
A method for complex antimicrobials is prepared in shitosan and silver-bearing copper blend, and described in it, method follows these steps to carry out:
(1) be that the ratio that 1:30-1:80, volume ratio are 1:1-1:5 adds agitator by liquor argenti nitratis ophthalmicus and copper nitrate solution in concentration ratio;
(2) agitator is slowly heated up, and control temperature and stir 1h at 35 DEG C-45 DEG C, control temperature and stir 1h at 52 DEG C-58 DEG C; Rear standing half an hour;
(3) be again warmed up to 60 DEG C-68 DEG C, add 0.5g shitosan, after stirring 0.5 h, generate after light blue suspension, leave standstill;
(4) after suspension is cooling in circulating vavuum pump suction filtration, obtain light blue powder, put it in 60 DEG C of drying boxes dry;
(5) dried powder is ground, obtain the complex antimicrobials powder of shitosan and silver-bearing copper blend.
Wherein, described silver nitrate and copper nitrate solution are pressed concentration ratio further for 1:50; Be further 1:3 by volume; After described silver nitrate is reduced, be simple substance silver.
Technique scheme is on the basis of this seminar project research, according to chemical reaction mechanism, further investigated silver nitrate, copper nitrate and shitosan liquid and liquid, solid-state and solid-state, liquid and solid-state between in the course of reaction of uniform temperature, adopt reverse thinking, through lot of experiments, adopt and first liquor argenti nitratis ophthalmicus is mixed in proportion with copper nitrate solution, and then add solid chitosan to react, obtained unforeseeable effect, its unforeseeable effect is:
This method adopts the mantle plate of shitosan as antibacterial agent, and silver and copper blend are obtained to a kind of complex antimicrobials, makes it have long-acting lasting, safe anti-microbial property.Add copper to solve in existing product silver-colored usage amount, in preparation process, do not need the chemical reagent such as additional reducing agent, obtain anti-microbial property good, and the green NEW TYPE OF COMPOSITE antibacterial agent that cost is low, the preparation method's of the complex antimicrobials of shitosan of the present invention and silver-bearing copper blend main technological features is:
(1) the prepared antibacterial agent of forefathers is all first to add shitosan to prepare antibacterial latex, and the present invention is inverted this preparation method, finally adds shitosan and prepares pulverous antibacterial agent, and its antibacterial effect is better.
(2) in the time of liquor argenti nitratis ophthalmicus and copper nitrate solution blend, adopt the heating stirring means heating up gradually, make that its solution mixes better evenly, after being conducive to shitosan and adding, do not produce agglomeration.
(3) shitosan adding is pressed powder instead of chitosan solution, and the Powdered antibacterial agent generating is like this more excellent than the anti-microbial property of antibacterial colloidal sol.
The complex antimicrobials of the shitosan that this method is prepared and silver-bearing copper blend detects through antibacterial ring test: Escherichia coli and staphylococcus aureus are had to significant bacteriostasis, the antibacterial ring of formed under the condition of culture of 37 DEG C >=10mm, as accompanying drawing 4 and accompanying drawing 5; Heat endurance after shitosan and silver-bearing copper blend is better than shitosan and silver, makes its application wider; And this method is easy and simple to handle, fast, get rid of the use of poisonous chemical reagent, ensure personal health, can be safely for medical domain and textile industry, and material price is cheap, and economical and practical, natural stable for manufacturing, harmless biological medical polymer material provides a kind of new way.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of shitosan of the present invention and silver-bearing copper complex antimicrobials.By the obviously visible shitosan surface structure densification of figure, be bulk sheet, and on the matrix of shitosan, exist uniformly some granular materials, and produce the lamellar structure that multilayer covers, in the antibacterial agent of equal quality, be more conducive to adhering to of metal grain, the antibacterial of bringing into play antibacterial action is increased.
Fig. 2 is the infrared spectrogram of shitosan of the present invention and silver-colored complex antimicrobials.In figure, see 3429 cm
-1the strong peak at place belongs to amino (NH in CTS molecule
2) and the stretching vibration absworption peak of light base (0H), 1556 cm
-1the characteristic peak of the corresponding Nano Silver of characteristic absorption peak occurring.
Fig. 3 is the infrared spectrogram of shitosan of the present invention and silver-bearing copper complex antimicrobials.The position of seeing the absworption peak of CTS/Ag/Cu antibiotic complex entirety in figure does not change substantially, and characteristic absorption peak still exists, but at 3429 cm
-1, 2974 cm
-1, 2934 cm
-1, 1631 cm
-1, 1396 cm
-1, 1085cm
-1, 1046 cm
-1, 885 cm
-1locate corresponding absorption peak strength and weaken, at 1425 cm
-1, 1320cm
-1the stretching vibration absworption peak of the C-N at place disappears, and explanation is above more-NH of CTS
2with Ag
+there is complexation reaction; Meanwhile, 1087 cm
-1with 1025 cm
-1the C-0 stretching vibration absworption peak of corresponding secondary alcohol and primary alconol does not become substantially, illustrates that the primary alconol of CTS and the light base of secondary alcohol do not have and the raw complexation reaction of silver hair.
Fig. 4 is the colibacillary antibacterial ring test figure of shitosan of the present invention and silver-bearing copper complex antimicrobials.In figure, see: blank sample around overgrows with colibacillary bacterium colony, the antibacterial ring of formed around the complex antimicrobials of shitosan and silver-bearing copper blend >=10mm, proves that this antibacterial agent has anti-microbial property.
Fig. 5 is the antibacterial ring test figure of the staphylococcus aureus of the complex antimicrobials of shitosan of the present invention and silver-bearing copper blend.In figure, see that blank sample around overgrows with the bacterium colony of staphylococcus aureus, the antibacterial ring of formed around the complex antimicrobials of shitosan and silver-bearing copper blend >=10mm, proves that this antibacterial agent has anti-microbial property.
Embodiment
The preparation method of the complex antimicrobials of shitosan of the present invention and silver-bearing copper blend stirs for 1:3 is made into blend solution silver nitrate and copper nitrate by volume by its composition and content proportioning in agitator, to be mixedly add shitosan after evenly, solution becomes light blue suspension, cooled suspension is carried out to suction filtration, dry, grinding, finally obtain light blue pulverous complex antimicrobials.
Further describe the specific embodiment of the present invention below by specific embodiment.
Embodiment 1
(1) 0.004g silver nitrate is dissolved in 25ml deionized water, 0.94g copper nitrate is dissolved in 100ml deionized water, and its concentration ratio is 1:50, by volume for 1:3 mixes;
(2) solution of mixing is placed in to thermostatic mixer, at 40 DEG C, under the rotating speed of 25r/min, stirs 1h, temperature is raised to 50 DEG C, under the rotating speed of 25r/min, stir again 1h;
(3) temperature is raised to 60 DEG C, under the rotating speed of 25r/min, adds 0.5g shitosan solid to stir 0.5h, generate light blue suspension;
(4) after cooling, suspension is carried out to suction filtration, in 60 DEG C of insulating boxs dry completely, grind, obtain light blue pulverous complex antimicrobials.
Obtaining being made up of shitosan and silver nitrate and copper nitrate by above-mentioned preparation method, is that silver nitrate is 1:50 with the ratio of the concentration of copper nitrate by its content proportioning, and the ratio of volume is 1:3, the complex antimicrobials of generating chitosan and silver-bearing copper blend.
Embodiment 2
According to the process of embodiment 1, the difference of embodiment 2 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:50, and its volume ratio becomes 1:2, the complex antimicrobials of generating chitosan and silver-bearing copper blend.Known through antibacterial ring test, inhibition zone diameter is 8 mm, and its fungistatic effect can not show a candle to embodiment 1.
Embodiment 3
According to the process of embodiment 1, the difference of embodiment 3 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:50, and its volume ratio becomes 1:1, the complex antimicrobials of generating chitosan and silver-bearing copper blend.Known through antibacterial ring test, inhibition zone diameter is 7 mm, and its fungistatic effect can not show a candle to embodiment 1.
Embodiment 4
According to the process of embodiment 1, the difference of embodiment 4 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:50, and its volume ratio is 1:3.Be raised to 60 DEG C in temperature, under the rotating speed of 25r/min, add 0.5g chitosan solution to stir 0.5h, generate the complex antimicrobials of light blue colloidal sol blend.Known through antibacterial ring test, inhibition zone diameter is 6 mm, without antibiotic property.
Embodiment 5
According to the process of embodiment 1, the difference of embodiment 5 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:50, and its volume ratio is 1:3.After mixing, solution at 60 DEG C of constant temperature, stirs 2h, temperature constant, the complex antimicrobials of generating chitosan and silver-bearing copper blend in thermostatic mixer.Known through antibacterial ring test, inhibition zone diameter is 11 mm, and its fungistatic effect is the same with embodiment 1, but cost is high, and power consumption is large.
Embodiment 6
According to the process of embodiment 1, the difference of embodiment 6 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:40, and its volume ratio becomes 1:3, the complex antimicrobials of generating chitosan and silver-bearing copper blend.Known through antibacterial ring test, inhibition zone diameter is 8 mm, and its fungistatic effect can not show a candle to embodiment 1.
Embodiment 7
According to the process of embodiment 1, the difference of embodiment 7 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:50, and its volume ratio is 1:3.Be raised to 60 DEG C in temperature, under the rotating speed of 25r/min, add 0.5g chitosan solution to stir 0.5h, drip gradually sodium borohydride solution, generate the blend of black suspension.Known through antibacterial ring test, inhibition zone diameter is 6 mm, and without antibiotic property, and antibacterial agent color is also a drawback.
Embodiment 8
According to the process of embodiment 1, the difference of embodiment 8 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:50, and its volume ratio is 1:3.0.5g shitosan is dissolved in 25ml deionized water in thermostatic mixer to 60 DEG C, under the rotating speed of 25r/min, stirs, add silver nitrate and copper nitrate mixed solution simultaneously, form colloidal sol blend.Continue to stir 2h, the complex antimicrobials of generating chitosan and silver-bearing copper blend.Known through antibacterial ring test, inhibition zone diameter is 7 mm, and its fungistatic effect can not show a candle to embodiment 1.
Embodiment 9
According to the process of embodiment 1, the difference of embodiment 9 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:50, and its volume ratio is 1:3.0.5g shitosan is dissolved in 25ml deionized water in thermostatic mixer to 60 DEG C, under the rotating speed of 25r/min, stirs, add silver nitrate and copper nitrate mixed solution simultaneously, form colloidal sol blend.Continue to stir 2h, then drip gradually sodium borohydride solution, generate yellowish-brown colloidal sol blend.Known through antibacterial ring test, inhibition zone diameter is 9 mm, and its fungistatic effect is not as embodiment 1.
Embodiment 10
According to the process of embodiment 1, the difference of embodiment 10 is: the concentration proportioning of silver nitrate and copper nitrate solution is 1:50, and its volume ratio is 1:3.The blue suspension generating carries out after suction filtration, at air drying, can becoming the blend of black powder shape.Known through antibacterial ring test, inhibition zone diameter is 5 mm, and its fungistatic effect can not show a candle to embodiment 1.
Claims (4)
1. a method for complex antimicrobials is prepared in shitosan and silver-bearing copper blend, and described in it, method follows these steps to carry out:
(1) be that the ratio that 1:30-1:80, volume ratio are 1:1-1:5 adds agitator by liquor argenti nitratis ophthalmicus and copper nitrate solution in concentration ratio;
(2) agitator is slowly heated up, and control temperature and stir 1h at 35 DEG C-45 DEG C, control temperature and stir 1h at 52 DEG C-58 DEG C; Rear standing half an hour;
(3) be again warmed up to 60 DEG C-68 DEG C, add 0.5g shitosan, after stirring 0.5 h, generate after light blue suspension, leave standstill;
(4) after suspension is cooling in circulating vavuum pump suction filtration, obtain light blue powder, put it in 60 DEG C of drying boxes dry;
(5) dried powder is ground, obtain the complex antimicrobials powder of shitosan and silver-bearing copper blend.
2. preparation method as claimed in claim 1, described in it, silver nitrate and copper nitrate solution are pressed concentration ratio further for 1:50.
3. preparation method as claimed in claim 1 or 2, described in it, silver nitrate and copper nitrate solution are further 1:3 by volume.
4. the preparation method as described in claim 1 or 2 or 3, described in it, silver nitrate is simple substance silver after being reduced.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104863007A (en) * | 2015-04-03 | 2015-08-26 | 华南理工大学 | Chitin crystal bar-based nano-silver composite antibacterial paper, and preparation method and application thereof |
| CN105696112A (en) * | 2016-03-08 | 2016-06-22 | 安徽微美纳米技术有限公司 | Copper-ion antibacterial socks |
| CN106106522A (en) * | 2016-06-23 | 2016-11-16 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | A kind of nano zine oxide carries silver chitosan compound anti-bacteria agent and preparation method thereof |
| CN106674982A (en) * | 2016-12-12 | 2017-05-17 | 成都育芽科技有限公司 | Polyurethane antibacterial biomedical composite material and preparation method thereof |
| CN106857658A (en) * | 2017-03-30 | 2017-06-20 | 安徽省银锂子生物科技发展有限公司 | It is a kind of carry with, the Nano Silver table-ware disinfection liquid of efficient quick sterilization |
| CN107518004A (en) * | 2016-06-21 | 2017-12-29 | 张家港市山牧新材料技术开发有限公司 | A kind of preparation method of Nanometer Copper antibacterial granule |
| CN106942274B (en) * | 2017-03-30 | 2018-03-20 | 安徽省银锂子生物科技发展有限公司 | A kind of high-effective broad-spectrum fungicide of low content Nano silver solution |
| CN109912982A (en) * | 2019-03-21 | 2019-06-21 | 山西大医院（山西医学科学院） | A kind of bio-medical silicon rubber with antibiotic property |
| CN110812948A (en) * | 2019-10-18 | 2020-02-21 | 东莞市亿茂滤材有限公司 | Multifunctional filtering material and preparation method thereof |
| CN111840630A (en) * | 2020-07-21 | 2020-10-30 | 华南农业大学 | Bacteriostatic absorbable medical soft tissue suture line and preparation method and application thereof |
| CN114711253A (en) * | 2021-01-06 | 2022-07-08 | 合肥杰事杰新材料股份有限公司 | Antibacterial agent, preparation method thereof and antibacterial composition |
| CN115216964A (en) * | 2022-08-30 | 2022-10-21 | 全小强 | Washable antibacterial fabric and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104863007A (en) * | 2015-04-03 | 2015-08-26 | 华南理工大学 | Chitin crystal bar-based nano-silver composite antibacterial paper, and preparation method and application thereof |
| CN104863007B (en) * | 2015-04-03 | 2017-04-19 | 华南理工大学 | Chitin crystal bar-based nano-silver composite antibacterial paper, and preparation method and application thereof |
| CN105696112A (en) * | 2016-03-08 | 2016-06-22 | 安徽微美纳米技术有限公司 | Copper-ion antibacterial socks |
| CN105696112B (en) * | 2016-03-08 | 2017-12-26 | 安徽微美纳米技术有限公司 | A kind of copper ion antibacterial socks |
| CN107518004A (en) * | 2016-06-21 | 2017-12-29 | 张家港市山牧新材料技术开发有限公司 | A kind of preparation method of Nanometer Copper antibacterial granule |
| CN106106522A (en) * | 2016-06-23 | 2016-11-16 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | A kind of nano zine oxide carries silver chitosan compound anti-bacteria agent and preparation method thereof |
| CN106106522B (en) * | 2016-06-23 | 2019-05-14 | 中国人民解放军军事医学科学院卫生学环境医学研究所 | A kind of nano zine oxide-load silver chitosan compound anti-bacteria agent and preparation method thereof |
| CN106674982A (en) * | 2016-12-12 | 2017-05-17 | 成都育芽科技有限公司 | Polyurethane antibacterial biomedical composite material and preparation method thereof |
| CN106942274B (en) * | 2017-03-30 | 2018-03-20 | 安徽省银锂子生物科技发展有限公司 | A kind of high-effective broad-spectrum fungicide of low content Nano silver solution |
| CN106857658A (en) * | 2017-03-30 | 2017-06-20 | 安徽省银锂子生物科技发展有限公司 | It is a kind of carry with, the Nano Silver table-ware disinfection liquid of efficient quick sterilization |
| CN109912982A (en) * | 2019-03-21 | 2019-06-21 | 山西大医院（山西医学科学院） | A kind of bio-medical silicon rubber with antibiotic property |
| CN109912982B (en) * | 2019-03-21 | 2021-06-29 | 山西大医院（山西医学科学院） | Antibacterial biomedical silicone rubber |
| CN110812948A (en) * | 2019-10-18 | 2020-02-21 | 东莞市亿茂滤材有限公司 | Multifunctional filtering material and preparation method thereof |
| CN111840630A (en) * | 2020-07-21 | 2020-10-30 | 华南农业大学 | Bacteriostatic absorbable medical soft tissue suture line and preparation method and application thereof |
| CN114711253A (en) * | 2021-01-06 | 2022-07-08 | 合肥杰事杰新材料股份有限公司 | Antibacterial agent, preparation method thereof and antibacterial composition |
| CN114711253B (en) * | 2021-01-06 | 2024-02-20 | 合肥杰事杰新材料股份有限公司 | Antibacterial agent, preparation method thereof and antibacterial composition |
| CN115216964A (en) * | 2022-08-30 | 2022-10-21 | 全小强 | Washable antibacterial fabric and preparation method thereof |
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