CN115119853A - Chitosan-VC/nano-silver composite antibacterial material and preparation method thereof - Google Patents
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Abstract
The invention discloses a chitosan-VC/nano-silver composite antibacterial material and a preparation method thereof, wherein VC modified chitosan is used as a base material, silver nitrate is used as a load material, the chitosan-VC composite material is used as a reducing agent and a stabilizing agent, a sodium hydroxide solution is used as a pH value regulator, deionized water is used as a solvent, nitrogen is used as a protective gas, the chitosan-VC/nano-silver composite antibacterial agent powder is synthesized under the protection of heating, stirring, water bath and nitrogen, and is subjected to dialysis and freeze-drying to prepare the chitosan-VC/nano-silver composite antibacterial agent powder, wherein nano-silver is spherical particles, the diameter of the nano-silver is less than or equal to 29 nm, the antibacterial performance is excellent and can reach more than 99 percent, the preparation raw materials are environment-friendly and pollution-free, the chitosan-VC/nano-silver composite antibacterial agent powder can be used for antibacterial disinfection in the fields of food, freshness preservation, decontamination and medicine, the raw materials are easy to obtain, and are suitable for large-scale production.
Description
Technical Field
The invention relates to a preparation method of nano-silver, and particularly relates to a chitosan-VC/nano-silver composite antibacterial material and a preparation method thereof.
Background
In recent years, with the gradual increase of health requirements of people, silver has attracted extensive attention for antibacterial and bacteriostatic effects. The nano silver has a qualitative leap due to the fact that the particle size of the nano silver enters the nano level, and a very strong sterilization effect can be generated by using a very small amount of silver; and the high specific surface area has the characteristics of quick and lasting release, and is widely applied to the fields of food preservation, medical materials and the like.
At present, the preparation methods of nano-silver are many, and mainly include a chemical reduction method, a photoreduction method, a radiation method, a microemulsion method and the like. The chemical reduction method is mainly characterized in that silver ions or silver complexes are reduced into simple substance nano silver by silver salts (such as silver nitrate and silver sulfate) or silver complexes and proper reducing agents such as hydrazine hydrate, sodium citrate, glucose and the like in a liquid phase, and the nano silver is subjected to surface treatment by adopting surfactants (such as polyethylene glycol and polyvinylpyrrolidone PVP) in the preparation process to obtain the nano silver with various shapes which are uniformly dispersed and stably stored.
Although there are many methods for preparing nano silver, the cost is high, and toxic chemical reagents are often used. With the continuous improvement of environmental protection consciousness of people, a green and pollution-free method is urgently needed to be found for preparing the nano silver. Therefore, the development of a simple and green method for synthesizing silver nanoparticles with high stability, small particle size and different sizes is of great significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a chitosan-VC/nano-silver composite antibacterial material and a preparation method thereof, and the synthesized material has high antibacterial property and good stable dispersibility.
In order to solve the above technical problems, according to an aspect of the present invention, there is provided a method for preparing a chitosan-VC/nano silver composite antibacterial material, comprising the steps of:
step one, preparing a chitosan-VC template solution, and heating to 50-90 ℃; the molar ratio of the chitosan to the VC in the chitosan-VC template solution is 1 (0.5-1.3);
step two, preparing a sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH to 4-7;
thirdly, preparing a silver nitrate solution, and dropwise adding the silver nitrate solution into the chitosan-VC template solution for reaction at the temperature of 50-90 ℃;
and step four, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 3 to 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano silver composite antibacterial material.
Further, in the step one, the concentration of the prepared chitosan-VC template solution is 5-15 mg/mL.
Further, in the first step, the chitosan-VC template solution is dissolved overnight to form a uniform base solution, and then the uniform base solution is placed in a water bath and heated to 50-90 ℃.
Further, in the second step, the concentration of the prepared sodium hydroxide solution is 0.05-0.1M.
Further, in the third step, the concentration of the prepared silver nitrate solution is 0.7-1.7 ppm.
Furthermore, in the third step, the reaction time is 0.5-2 h.
According to another aspect of the present invention, there is provided a chitosan-VC/nano silver composite antibacterial material prepared by the above-described method.
According to another aspect of the invention, the application of the chitosan-VC/nano-silver composite antibacterial material as an antibacterial agent is provided.
In the invention, VC is introduced into a molecular chain of chitosan to obtain the chitosan-VC composite material, and the chitosan-VC/nano-silver composite antibacterial material is obtained by taking the chitosan-VC composite material as a reducing agent and a stable dispersing agent of silver nanoparticles. The particle size of the nano silver particles prepared by the method is within 29 nm, and the nano silver particles have good dispersibility.
The chitosan-VC/nano-silver composite antibacterial material prepared by the invention has excellent antibacterial performance and water solubility, has no precipitation within three months, has better stability, and can be used as an ideal antibacterial composite material for antibacterial disinfection in the fields of food, fresh keeping, decontamination and medicine.
The method has the advantages of simple preparation process, low cost, simple process and the like, has strong repeatability, and is suitable for large-scale production.
Drawings
FIG. 1 is a diagram of an ultraviolet absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material prepared in example 1.
FIG. 2 is a diagram of the UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material prepared in example 2.
FIG. 3 is a diagram of the UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material prepared in example 3.
FIG. 4 is a UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material prepared in example 4.
FIG. 5 is a UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material prepared in example 5.
FIG. 6 is a UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material prepared in example 6.
FIG. 7 is a UV absorption spectrum of the chitosan/nano-silver composite antibacterial material prepared in comparative example 1.
FIG. 8 is a scanning electron microscope image of the chitosan-VC/nano-silver composite antibacterial material prepared by the invention.
FIG. 9 is an EDS energy spectrum of the chitosan-VC/nano-silver composite antibacterial material prepared by the present invention.
FIG. 10 is a comparison graph of the colony counts of Escherichia coli and Staphylococcus aureus of the composite antibacterial material prepared by the present invention.
FIG. 11 is a comparison graph of the bacteriostatic rate of the composite antibacterial material prepared by the invention on Escherichia coli and Staphylococcus aureus.
Detailed Description
The preparation method of the chitosan-VC/nano-silver composite antibacterial material provided by the invention comprises the following steps:
step one, preparing a chitosan-VC template solution, and heating to 50-90 ℃; the molar ratio of the chitosan to the VC in the chitosan-VC template solution is 1 (0.5-1.3).
In the step, the concentration of the prepared chitosan-VC template solution is 5-15 mg/mL.
In the step, the chitosan-VC template solution is dissolved overnight to form uniform base solution, and then the uniform base solution is placed in a water bath and heated to 50-90 ℃.
And step two, preparing a sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 4-7.
In this step, the concentration of the prepared sodium hydroxide solution is 0.05-0.1M.
And step three, preparing a silver nitrate solution, and dropwise adding the silver nitrate solution into the chitosan-VC template solution for reaction at the temperature of 50-90 ℃.
In the step, the concentration of the prepared silver nitrate solution is 0.7-1.7 ppm, and the reaction time is 0.5-2 h.
And step four, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 3 to 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano silver composite antibacterial material.
The invention takes VC modified chitosan as a substrate material, silver nitrate as a load material, a chitosan-VC composite material as a reducing agent and a stabilizing agent, a sodium hydroxide solution as a pH value regulator, deionized water as a solvent and nitrogen as a protective gas, and the chitosan-VC/nano silver composite antibacterial agent is synthesized under the conditions of heating, stirring, water bath and nitrogen protection, and is dialyzed and freeze-dried to prepare the chitosan-VC/nano silver composite antibacterial agent powder, wherein nano silver is spherical particles, the diameter of the nano silver is less than or equal to 29 nm, and the antibacterial performance is excellent and can reach more than 99%.
The chitosan is a green and environment-friendly high polymer material, has a biodegradable function, is wide in source and low in price, and rich hydroxyl in chitosan molecules can form coordinate bonds with silver ions, so that the nano-silver can be effectively prevented from being agglomerated, but the reducibility of the hydroxyl is poor. Since VC contains a large amount of hydroxyl groups and is ionized in water to form ascorbic acid free radicals with strong reducibility, the reducibility of chitosan is increased while the water solubility of the chitosan is improved, silver ions are added into the aqueous solution of chitosan-VC, and the silver ions are attracted by the hydroxyl groups on the chitosan-VC in the aqueous solution due to electrostatic action and are reduced furtherIs Ag 0 And due to the long-chain property of the chitosan, the nano silver material with small particle size can be prepared by playing a certain stable dispersion role on the zero-valent nano silver simple substances.
The claimed solution is further illustrated by the following examples. However, the examples and comparative examples are intended to illustrate the embodiments of the present invention without departing from the scope of the subject matter of the present invention, and the scope of the present invention is not limited by the examples. Unless otherwise specifically indicated, the materials and reagents used in the present invention are available from commercial products in the art.
Example 1
Step one, preparing 5 mg/mL chitosan-VC template solution with a molar ratio of 1:1, dissolving overnight to form uniform base solution, then placing the base solution in a water bath kettle, and continuously heating to 60 ℃;
secondly, preparing 0.1M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 4;
thirdly, preparing 1.5 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at a constant speed under the protection of nitrogen at 60 ℃, and reacting for 1 h;
and fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano-silver composite antibacterial material with the particle size of 16-18 nm.
FIG. 1 is a diagram of an ultraviolet absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material obtained in example 1.
Example 2
Step one, preparing 5 mg/mL chitosan-VC template solution with a molar ratio of 1:1, dissolving overnight to form uniform base solution, then placing the base solution in a water bath kettle, and continuously heating to 60 ℃;
step two, preparing 0.1M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 4;
thirdly, preparing 0.5 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at a constant speed under the protection of nitrogen at 60 ℃, and reacting for 1 h;
and fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano-silver composite antibacterial material with the particle size of 23-25 nm.
FIG. 2 is a diagram of the UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material obtained in example 2.
Example 3
Step one, preparing 5 mg/mL chitosan-VC template solution with a molar ratio of 1:1, dissolving overnight to form uniform base solution, then placing the base solution in a water bath kettle, and continuously heating to 80 ℃;
secondly, preparing 0.1M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 4;
thirdly, preparing 1.5 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at 80 ℃ under the protection of nitrogen, and reacting for 1 h;
and fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano-silver composite antibacterial material with the particle size of 14-16 nm.
FIG. 3 is a diagram of the UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material obtained in example 3.
Example 4
Step one, preparing 5 mg/mL chitosan-VC template solution with a molar ratio of 1:1, dissolving overnight to form uniform base solution, then placing the base solution in a water bath kettle, and continuously heating to 50 ℃;
secondly, preparing 0.1M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 4;
thirdly, preparing 1.5 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at 50 ℃ under the protection of nitrogen, and reacting for 1 h;
and fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano-silver composite antibacterial material with the particle size of 18-20 nm.
FIG. 4 is a diagram of the ultraviolet absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material obtained in example 4 of the present invention.
Example 5
Step one, preparing 5 mg/mL chitosan-VC template solution with a molar ratio of 1:1, dissolving overnight to form uniform base solution, then placing the base solution in a water bath kettle, and continuously heating to 80 ℃;
secondly, preparing 0.1M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 4;
thirdly, preparing 1.1 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at 80 ℃ under the protection of nitrogen, and reacting for 2 hours;
and fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano-silver composite antibacterial material with the particle size of 12-14 nm.
FIG. 5 is a diagram of the UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material obtained in example 5.
Example 6
Step one, preparing 5 mg/mL chitosan-VC template solution with a molar ratio of 1:1, dissolving overnight to form uniform base solution, then placing the base solution in a water bath kettle, and continuously heating to 80 ℃;
step two, preparing 0.1M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 4;
thirdly, preparing 1.1 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at 80 ℃ under the protection of nitrogen, and reacting for 0.5 h;
and fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano-silver composite antibacterial material with the particle size of 21-23 nm.
FIG. 6 is a UV absorption spectrum of the chitosan-VC/nano-silver composite antibacterial material obtained in example 6.
Example 7
Step one, preparing a chitosan-VC template solution with a molar ratio of 1:1.3 of 15 mg/mL, dissolving overnight to form a uniform base solution, then placing the base solution in a water bath kettle, and continuously heating to 90 ℃;
secondly, preparing 0.05M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 5;
thirdly, preparing 0.7 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at a constant speed under the protection of nitrogen at 90 ℃, and reacting for 0.5 h;
fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freezing and drying the solution to obtain the chitosan-VC/nano-silver composite antibacterial material with the particle size of 25-27 nm.
Example 8
Step one, preparing 10 mg/mL chitosan-VC template solution with the molar ratio of 1:0.5, dissolving overnight to form uniform base solution, then placing the base solution in a water bath kettle, and continuously heating to 90 ℃;
step two, preparing 0.1M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 7;
thirdly, preparing 1.7 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at a constant speed under the protection of nitrogen at 90 ℃, and reacting for 2 hours;
and fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano-silver composite antibacterial material with the particle size of 25-29 nm.
Comparative example 1
Step one, preparing 5 mg/mL chitosan uniform solution, then placing the solution in a water bath kettle, and continuously heating the solution to 80 ℃;
secondly, preparing 0.1M sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH value to 4;
thirdly, preparing 1.5 ppm silver nitrate solution, slowly and uniformly dropping the silver nitrate solution into the chitosan-VC template solution at 80 ℃ under the protection of nitrogen, and reacting for 2 hours;
and fourthly, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the reaction solution with deionized water for 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan/nano-silver composite antibacterial material.
The grain size of the nano-silver prepared in the comparative example 1 is 38-40 nm, and fig. 7 is an ultraviolet absorption spectrogram of the chitosan/nano-silver composite antibacterial material obtained in the comparative example 4, wherein the peak intensity is obviously weaker and the peak position is larger.
The chitosan-VC/nano-silver composite antibacterial material synthesized by the invention has the following performance tests.
(1) And (4) SEM test: the synthesized chitosan-VC/nano silver composite antibacterial material is subjected to micro-morphology and EDS analysis, and the micro-morphology and the EDS analysis are shown in figures 8 and 9.
Fig. 8 is a microscopic morphology of the chitosan-VC/nano-silver composite antibacterial material, which clearly shows that the nano-silver particles of the small spherical particles are uniformly distributed on the surface of the chitosan-VC composite material, and the silver nanoparticles prepared by us are all proved to be within 29 nm by the uniform distribution of silver element in the EDS of fig. 9.
(2) And (3) testing antibacterial performance: the antibacterial performance of the chitosan, the chitosan/nano-silver composite antibacterial material and the chitosan-VC/nano-silver composite antibacterial material is evaluated by a colony counting method by taking gram-positive staphylococcus aureus and gram-negative escherichia coli as representative bacteria, which are shown in fig. 10 and fig. 11.
FIG. 10 is a diagram of the colony counting effect of the chitosan-VC/nano-silver composite antibacterial material, FIG. 11 is a diagram of the bacteriostatic rate of the chitosan-VC/nano-silver composite antibacterial material to Escherichia coli and Staphylococcus aureus, and it can be seen that the bacteriostatic rates of chitosan to Escherichia coli and Staphylococcus aureus are respectively 28.47% and 23.33%, which shows that the chitosan itself has very poor antibacterial performance, and the bacteriostatic rates of the chitosan/nano-silver composite material to Escherichia coli and Staphylococcus aureus are respectively 73.14% and 46.84%, which shows that the antibacterial effect of the chitosan/nano-silver composite material to Escherichia coli is stronger than that to Staphylococcus aureus, while the bacteriostatic rates of the chitosan-VC/nano-silver composite antibacterial material prepared in the invention to Escherichia coli and Staphylococcus aureus respectively reach 99.94% and 99.19%, shows that the chitosan-VC/nano-silver composite antibacterial material prepared by the invention has excellent antibacterial performance.
The test results take the chitosan-VC/nano-silver composite antibacterial material obtained in example 1 as an example, and the chitosan-VC/nano-silver composite antibacterial materials obtained in other examples also have the same antibacterial performance. The antibacterial materials obtained in examples 1 to 8 were free from precipitation within three months and had good stability.
Claims (8)
1. A preparation method of a chitosan-VC/nano-silver composite antibacterial material is characterized by comprising the following steps:
step one, preparing a chitosan-VC template solution, and heating to 50-90 ℃; the molar ratio of chitosan to VC in the chitosan-VC template solution is 1 (0.5-1.3);
step two, preparing a sodium hydroxide solution, dropwise adding the sodium hydroxide solution into the chitosan-VC template solution, and adjusting the pH to 4-7;
thirdly, preparing a silver nitrate solution, and dropwise adding the silver nitrate solution into the chitosan-VC template solution for reaction at the temperature of 50-90 ℃;
and step four, after the reaction is finished, putting the reaction solution into a dialysis bag, dialyzing the solution with deionized water for 3 to 7 days, removing silver ions which are not completely reacted in the solution, and then freeze-drying the solution to obtain the chitosan-VC/nano silver composite antibacterial material.
2. The method of claim 1, wherein: in the first step, the concentration of the prepared chitosan-VC template solution is 5-15 mg/mL.
3. The method of claim 2, wherein: in the first step, the chitosan-VC template solution is dissolved overnight to form uniform base solution, and then the uniform base solution is placed in a water bath kettle and heated to 50-90 ℃.
4. A method according to claim 1, 2 or 3, characterized in that: in the second step, the concentration of the prepared sodium hydroxide solution is 0.05-0.1M.
5. The method of claim 4, wherein: in the third step, the concentration of the prepared silver nitrate solution is 0.7-1.7 ppm.
6. The method of claim 5, wherein: in the third step, the reaction time is 0.5-2 h.
7. A chitosan-VC/nano-silver composite antibacterial material is characterized in that: prepared by the process of any one of claims 1 to 6.
8. Use of the chitosan-VC/nanosilver composite antibacterial material of claim 7 as an antibacterial agent.
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Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1653907A (en) * | 2005-01-27 | 2005-08-17 | 浙江大学 | Method for preparing nanometer silver solution and nanometer silver powder by using high polymer as stabilizer |
| CN101618047A (en) * | 2009-08-11 | 2010-01-06 | 聊城大学 | Preparation method and application of nanocomposite of silver, chitosan and/or derivative thereof |
| WO2012140520A2 (en) * | 2011-03-25 | 2012-10-18 | Indian Institute Of Technology | Sustained silver release composition for water purification |
| CN103785857A (en) * | 2014-02-25 | 2014-05-14 | 南开大学 | Nano-silver used for anti-microbial dressing and preparation method thereof |
| CN105345029A (en) * | 2015-12-11 | 2016-02-24 | 广东工业大学 | Method for preparing nano-silver gel through one-pot method |
| CN108329531A (en) * | 2018-02-06 | 2018-07-27 | 中山安康德美生物科技有限公司 | A kind of modification of chitosan nano silver composite material and preparation method thereof |
| CN108339977A (en) * | 2018-02-12 | 2018-07-31 | 太原理工大学 | A kind of preparation method and application of chitosan oligosaccharide nano silver composite antibacterial agent |
| CN108835125A (en) * | 2018-08-10 | 2018-11-20 | 湖州大本营科技有限公司 | A kind of preparation method and applications of micro-nano silver/chitosan compound anti-bacteria agent |
| CN109128211A (en) * | 2018-08-16 | 2019-01-04 | 山东大学 | The method of micro-nano silver particle is prepared in water solution system |
| CN109530716A (en) * | 2018-11-17 | 2019-03-29 | 赵兵 | A kind of nano-Ag particles and preparation method thereof based on Chitosan-Thiolated Polymers |
| CN110432320A (en) * | 2018-05-04 | 2019-11-12 | 天津科技大学 | A kind of preparation method of nano silver chitosan complex microsphere |
| RU2754738C1 (en) * | 2020-10-21 | 2021-09-06 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" | Method for obtaining food-grade film material based on chitosan |
| WO2022045916A1 (en) * | 2020-08-25 | 2022-03-03 | Общество С Ограниченной Ответственностью "Научно-Производственное Объединение "Минералика" | Nanocomposite coatings to protect underwater and coastal infrastructure objects from biofouling |
-
2022
- 2022-07-29 CN CN202210910028.3A patent/CN115119853A/en active Pending
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1653907A (en) * | 2005-01-27 | 2005-08-17 | 浙江大学 | Method for preparing nanometer silver solution and nanometer silver powder by using high polymer as stabilizer |
| CN101618047A (en) * | 2009-08-11 | 2010-01-06 | 聊城大学 | Preparation method and application of nanocomposite of silver, chitosan and/or derivative thereof |
| WO2012140520A2 (en) * | 2011-03-25 | 2012-10-18 | Indian Institute Of Technology | Sustained silver release composition for water purification |
| CN103785857A (en) * | 2014-02-25 | 2014-05-14 | 南开大学 | Nano-silver used for anti-microbial dressing and preparation method thereof |
| CN105345029A (en) * | 2015-12-11 | 2016-02-24 | 广东工业大学 | Method for preparing nano-silver gel through one-pot method |
| CN108329531A (en) * | 2018-02-06 | 2018-07-27 | 中山安康德美生物科技有限公司 | A kind of modification of chitosan nano silver composite material and preparation method thereof |
| CN108339977A (en) * | 2018-02-12 | 2018-07-31 | 太原理工大学 | A kind of preparation method and application of chitosan oligosaccharide nano silver composite antibacterial agent |
| CN110432320A (en) * | 2018-05-04 | 2019-11-12 | 天津科技大学 | A kind of preparation method of nano silver chitosan complex microsphere |
| CN108835125A (en) * | 2018-08-10 | 2018-11-20 | 湖州大本营科技有限公司 | A kind of preparation method and applications of micro-nano silver/chitosan compound anti-bacteria agent |
| CN109128211A (en) * | 2018-08-16 | 2019-01-04 | 山东大学 | The method of micro-nano silver particle is prepared in water solution system |
| CN109530716A (en) * | 2018-11-17 | 2019-03-29 | 赵兵 | A kind of nano-Ag particles and preparation method thereof based on Chitosan-Thiolated Polymers |
| WO2022045916A1 (en) * | 2020-08-25 | 2022-03-03 | Общество С Ограниченной Ответственностью "Научно-Производственное Объединение "Минералика" | Nanocomposite coatings to protect underwater and coastal infrastructure objects from biofouling |
| RU2754738C1 (en) * | 2020-10-21 | 2021-09-06 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ивановский государственный химико-технологический университет" | Method for obtaining food-grade film material based on chitosan |
Non-Patent Citations (2)
| Title |
|---|
| 辛宜聪: "纳米银_壳聚糖复合膜的制备及性能_", 《包装工程》 * |
| 黄晓飞: ""壳聚糖基载银材料的制备及其抗菌性能的研究"", 《中国博士学位论文全文数据库（电子期刊） 工程科技I辑》 * |
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