CN102120043B - Absorbent cotton gauze containing nanometer silver and chitosan, preparation device as well as method thereof - Google Patents
Absorbent cotton gauze containing nanometer silver and chitosan, preparation device as well as method thereof Download PDFInfo
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- CN102120043B CN102120043B CN 201110044108 CN201110044108A CN102120043B CN 102120043 B CN102120043 B CN 102120043B CN 201110044108 CN201110044108 CN 201110044108 CN 201110044108 A CN201110044108 A CN 201110044108A CN 102120043 B CN102120043 B CN 102120043B
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Abstract
The invention discloses absorbent cotton gauze containing nanometer silver and chitosan, a preparation device as well as a method thereof, belonging to the technical field of medical dressing biological material preparation. The absorbent cotton gauze contains cation polysaccharide having excellent antibiosis and nanometer silver, wherein the chitosan is combined with the medical absorbent cottongauze by using the method of soaking and freeze drying, and the nanometer silver is absorbed on the gauze under the mutual action between nanometer silver grain and chitosan amino. The absorbent cotton gauze containing nanometer silver and chitosan provided by the invention has excellent air permeability and mechanical property, has lasting and efficient sterilization effect, can be conveniently used due to the excellent mechanical property, and is beneficial to the wound recovering.
Description
Technical field
The invention belongs to medical dressing biomaterial preparing technical field, be specifically related to a kind of degreasing cotton gauze and preparation facilities and method that contains nanometer silver and chitosan.
Background technology
Nano material with highly-breathable and antibacterial characteristics is beneficial to growth and the regeneration of wound tissue Cellular respiration, epithelial tissue, thereby significantly to promote the recovery of wound.
Chitosan is the unique cationic polysaccharide of nature, has the good cell compatibility and histocompatibility.Has stronger antibacterial activity simultaneously.Silver uses the history [Carbohydrate Research 344 (2009) 2375-2382] that has several centuries as antibacterial, and the development of nanotechnology makes silver have potential advantage and broad application as the use of antibacterial.Each have its shortcoming again when the two uses separately at that time, for example the fragility of chitosan film is bigger, uses operation inconvenience.The less stable of nanometer silver solution, thereby and solid when using nano-particle can reunite and lose the characteristic of nanometer together.The present invention contains the degreasing cotton gauze of chitosan and nanometer silver, overcomes these shortcomings thereby both are combined well.
Summary of the invention
The object of the present invention is to provide a kind of degreasing cotton gauze that contains nanometer silver and chitosan.
The present invention also aims to provide a kind of preparation facilities that contains nanometer silver and chitosan degreasing cotton gauze.
The present invention also aims to provide a kind of preparation method that contains nanometer silver and chitosan degreasing cotton gauze.
A kind of degreasing cotton gauze that contains nanometer silver and chitosan is characterized in that, this bundle contains the chitosan of mass fraction 20-70% and the nanometer silver of mass fraction 2-50%; The particle diameter of nanometer silver is 2-50nm.
A kind of preparation facilities that contains the degreasing cotton gauze of nanometer silver and chitosan is characterized in that described device is made of container, perforated baffle, force (forcing) pump, peristaltic pump and tank; Perforated baffle is positioned at opening inverted container centre position; Force (forcing) pump, peristaltic pump and the container side of remaining silent communicates; Tank communicates with peristaltic pump; Liquid level is higher than the tank liquid level in the container.
A kind of preparation method that contains the degreasing cotton gauze of nanometer silver and chitosan is characterized in that, comprises the steps:
(1) takes by weighing chitosan it is dissolved in the acetic acid solution of 1%-3%, stir until whole dissolvings, be prepared into the acetic acid solution that mass concentration is the 1%-5% chitosan;
(2) the medical absorbent cotton gauze is immersed in the acetic acid solution of chitosan 1-12 hour, place under-10~-196 ℃ of conditions its taking-up freezing, be placed on lyophilization in the freezer dryer after regular hour, it is immersed in 0.25% the glutaraldehyde solution takes out after 30 minutes, be immersed in 1% the sodium borohydride solution more than 12 hours, then it is soaked in 1% the NaOH solution and removed acetic acid in 1-3 hour, with a large amount of water flushing back secondary pre-freeze and lyophilizations, make the degreasing cotton gauze that contains chitosan;
(3) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, then it is inserted in the ice bath and cools off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution;
(4) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container, the 50-500mL nanometer silver solution is poured in the container, nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
Beneficial effect of the present invention: the procedure of the present invention degreasing cotton gauze that contains nanometer silver and chitosan simple and preparation has controlled permeability, and contained chitosan component and nanometer silver component all have good antibacterial performance.The degreasing cotton gauze that contains nanometer silver and chitosan of the present invention has lastingly, the characteristics that sterilize efficiently, has the good mechanical performance simultaneously, and is easy and simple to handle during use.
Description of drawings
Fig. 1 preparation contains the device sketch map of nanometer silver and chitosan degreasing cotton gauze;
Wherein, 1-perforated baffle, 2-contain degreasing cotton gauze, 3-nanometer silver solution, 4-force (forcing) pump, 5-peristaltic pump, 6-tank, the 7-container of chitosan.
The specific embodiment
Further specify the present invention below in conjunction with the drawings and specific embodiments.
Below implement used main raw material of chitosan (deacetylation 95% molecular weight 200,000), polyvinylpyrrolidone, silver nitrate, sodium borohydride, acetic acid, sodium hydroxide and be chemical pure; Gauze adopts the medical absorbent cotton gauze.
The used device that contains nanometer silver and chitosan degreasing cotton gauze of following examples is device shown in Figure 1, and this device is made of container, perforated baffle, force (forcing) pump, peristaltic pump and tank; Perforated baffle is positioned at opening inverted container centre position; Force (forcing) pump, peristaltic pump and the container side of remaining silent communicates; Tank communicates with peristaltic pump; Liquid level is higher than the tank liquid level in the container.
Embodiment 1
(1) the preparation mass percent concentration is 1% acetic acid solution 50ml, takes by weighing the 1g chitosan and dissolves in wherein that magnetic agitation 20min fully dissolves it, and the mass concentration of preparation is 2% chitosan solution.
(2) degreasing cotton gauze is immersed in the chitosan solution 6 hours.
(3) will insert under-60 ℃ of temperature pre-freeze 12 hours through the degreasing cotton gauze that step (2) is handled.
(4) pre-freeze is good degreasing cotton gauze placed the freezer dryer lyophilization 48 hours.
(5) place the sodium hydroxide solution of 2% (wt) to soak 4h the degreasing cotton gauze that contains after the lyophilizing, remove residual acetic acid.The sodium borohydride solution that is placed on 2% (wt) behind the deionized water rinsing again soaks 3h, washes, is dipped to neutrality repeatedly with deionized water, and secondary freeze drying is made the degreasing cotton gauze that contains chitosan.
(6) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, it is inserted in the ice bath cooled off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution.
(7) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container shown in Figure 1, and the 50ml nanometer silver solution is poured into wherein.Nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, remove polyvinylpyrrolidone, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
(1) the preparation mass percent concentration is 1% acetic acid solution 50ml, takes by weighing the 1g chitosan and dissolves in wherein that magnetic agitation 20min fully dissolves it, and the mass concentration of preparation is 2% chitosan solution.
(2) degreasing cotton gauze is immersed in the chitosan solution 6 hours.
(3) will insert under-60 ℃ of temperature pre-freeze 12 hours through the degreasing cotton gauze that step (2) is handled.
(4) pre-freeze is good degreasing cotton gauze placed the freezer dryer lyophilization 48 hours.
(5) place the sodium hydroxide solution of 2% (wt) to soak 4h the degreasing cotton gauze that contains after the lyophilizing, remove residual acetic acid.The sodium borohydride solution that is placed on 2% (wt) behind the deionized water rinsing again soaks 3h, washes, is dipped to neutrality repeatedly with deionized water, and secondary freeze drying is made the degreasing cotton gauze that contains chitosan.
(6) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, it is inserted in the ice bath cooled off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution.
(7) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container shown in Figure 1, and the 100ml nanometer silver solution is poured into wherein.Nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, remove polyvinylpyrrolidone, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
(1) the preparation mass percent concentration is 1% acetic acid solution 50ml, takes by weighing the 1g chitosan and dissolves in wherein that magnetic agitation 20min fully dissolves it, and the mass concentration of preparation is 2% chitosan solution.
(2) degreasing cotton gauze is immersed in the chitosan solution 6 hours.
(3) will insert under-60 ℃ of temperature pre-freeze 12 hours through the degreasing cotton gauze that step (2) is handled.
(4) pre-freeze is good degreasing cotton gauze placed the freezer dryer lyophilization 48 hours.
(5) place the sodium hydroxide solution of 2% (wt) to soak 4h the degreasing cotton gauze that contains after the lyophilizing, remove residual acetic acid.The sodium borohydride solution that is placed on 2% (wt) behind the deionized water rinsing again soaks 3h, washes, is dipped to neutrality repeatedly with deionized water, and secondary freeze drying is made the degreasing cotton gauze that contains chitosan.
(6) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, it is inserted in the ice bath cooled off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution.
(7) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container shown in Figure 1, and the 500ml nanometer silver solution is poured into wherein.Nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, remove polyvinylpyrrolidone, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
Embodiment 4
(1) the preparation mass percent concentration is 1% acetic acid solution 50ml, takes by weighing the 2g chitosan and dissolves in wherein that magnetic agitation 20min fully dissolves it, and the mass concentration of preparation is 4% chitosan solution.
(2) degreasing cotton gauze is immersed in the chitosan solution 6 hours.
(3) will insert under-60 ℃ of temperature pre-freeze 12 hours through the degreasing cotton gauze that step (2) is handled.
(4) pre-freeze is good degreasing cotton gauze placed the freezer dryer lyophilization 48 hours.
(5) place the sodium hydroxide solution of 2% (wt) to soak 4h the degreasing cotton gauze that contains after the lyophilizing, remove residual acetic acid.The sodium borohydride solution that is placed on 2% (wt) behind the deionized water rinsing again soaks 3h, washes, is dipped to neutrality repeatedly with deionized water, and secondary freeze drying is made the degreasing cotton gauze that contains chitosan.
(6) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, it is inserted in the ice bath cooled off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution.
(7) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container shown in Figure 1, and the 100ml nanometer silver solution is poured into wherein.Nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, remove polyvinylpyrrolidone, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
Embodiment 5
(1) being adjusted into the preparation mass percent concentration is 1% acetic acid solution 50ml, takes by weighing the 0.5g chitosan and dissolves in wherein that magnetic agitation 20min fully dissolves it, and the mass concentration of preparation is 1% chitosan solution.
(2) degreasing cotton gauze is immersed in the chitosan solution 6 hours.
(3) will insert under-60 ℃ of temperature pre-freeze 12 hours through the degreasing cotton gauze that step (2) is handled.
(4) pre-freeze is good degreasing cotton gauze placed the freezer dryer lyophilization 48 hours.
(5) place the sodium hydroxide solution of 2% (wt) to soak 4h the degreasing cotton gauze that contains after the lyophilizing, remove residual acetic acid.The sodium borohydride solution that is placed on 2% (wt) behind the deionized water rinsing again soaks 3h, washes, is dipped to neutrality repeatedly with deionized water, and secondary freeze drying is made the degreasing cotton gauze that contains chitosan.
(6) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, it is inserted in the ice bath cooled off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution.
(7) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container shown in Figure 1, and the 100ml nanometer silver solution is poured into wherein.Nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, remove polyvinylpyrrolidone, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
Embodiment 6
(1) the preparation mass percent concentration is 1% acetic acid solution 50ml, takes by weighing the 1g chitosan and dissolves in wherein that magnetic agitation 20min fully dissolves it, and the mass concentration of preparation is 2% chitosan solution.
(2) degreasing cotton gauze is immersed in the chitosan solution 6 hours.
(3) will insert-20 ℃ of pre-freezes 12 hours through the degreasing cotton gauze that step (2) is handled.
(4) pre-freeze is good degreasing cotton gauze placed the freezer dryer lyophilization 48 hours.
(5) place the sodium hydroxide solution of 2% (wt) to soak 4h the degreasing cotton gauze that contains after the lyophilizing, remove residual acetic acid.The sodium borohydride solution that is placed on 2% (wt) behind the deionized water rinsing again soaks 3h, washes, is dipped to neutrality repeatedly with deionized water, and secondary freeze drying is made the degreasing cotton gauze that contains chitosan.
(6) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, it is inserted in the ice bath cooled off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution.
(7) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container shown in Figure 1, and the 100ml nanometer silver solution is poured into wherein.Nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, remove polyvinylpyrrolidone, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
Embodiment 7
(1) the preparation mass percent concentration is 1% acetic acid solution 50ml, takes by weighing the 1g chitosan and dissolves in wherein that magnetic agitation 20min fully dissolves it, and the mass concentration of preparation is 2% chitosan solution.
(2) degreasing cotton gauze is immersed in the chitosan solution 6 hours.
(3) will place liquid nitrogen pre-freeze through the degreasing cotton gauze that step (2) is handled.
(4) pre-freeze is good degreasing cotton gauze placed the freezer dryer lyophilization 48 hours.
(5) place the sodium hydroxide solution of 2% (wt) to soak 4h the degreasing cotton gauze that contains after the lyophilizing, remove residual acetic acid.The sodium borohydride solution that is placed on 2% (wt) behind the deionized water rinsing again soaks 3h, washes, is dipped to neutrality repeatedly with deionized water, and secondary freeze drying is made the degreasing cotton gauze that contains chitosan.
(6) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, it is inserted in the ice bath cooled off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution.
(7) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container shown in Figure 1, and the 100ml nanometer silver solution is poured into wherein.Nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, remove polyvinylpyrrolidone, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
Claims (2)
1. a preparation facilities that contains the degreasing cotton gauze of nanometer silver and chitosan is characterized in that, described device is made of container, perforated baffle, force (forcing) pump, peristaltic pump and tank; Perforated baffle is positioned at opening inverted container centre position; Force (forcing) pump, peristaltic pump and the container side of remaining silent communicates; Tank communicates with peristaltic pump; Liquid level is higher than the tank liquid level in the container.
2. a preparation method that contains the degreasing cotton gauze of nanometer silver and chitosan is characterized in that, comprises the steps:
(1) takes by weighing chitosan it is dissolved in the acetic acid solution of 1%-3%, stir until whole dissolvings, be prepared into the acetic acid solution that mass concentration is the 1%-5% chitosan;
(2) the medical absorbent cotton gauze is immersed in the acetic acid solution of chitosan 1-12 hour, place under-10~-196 ℃ of conditions its taking-up freezing, be placed on lyophilization in the freezer dryer after regular hour, it is immersed in 0.25% the glutaraldehyde solution takes out after 30 minutes, be immersed in 1% the sodium borohydride solution more than 12 hours, then it is soaked in 1% the NaOH solution and removed acetic acid in 1-3 hour, with a large amount of water flushing back secondary pre-freeze and lyophilizations, make the degreasing cotton gauze that contains chitosan;
(3) a certain amount of silver nitrate is dissolved in the polyvinylpyrrolidonesolution solution, forming concentration is the silver nitrate solution of 1mM, then it is inserted in the ice bath and cools off 10 minutes, adds excessive sodium borohydride and stirring then therein, after solution becomes glassy yellow, stop to stir, make nanometer silver solution;
(4) degreasing cotton gauze that will contain chitosan is inserted on the perforated baffle in the container, the 50-500mL nanometer silver solution is poured in the container, nanometer silver solution is slowly permeated through containing the degreasing cotton gauze of chitosan, regulate the seepage velocity that the pressure on liquid level upper strata in the container is regulated nanometer silver solution by force (forcing) pump, again add in container by peristaltic pump the nanometer silver penetrating fluid simultaneously, the degreasing cotton gauze that the nanometer silver penetrating fluid is penetrated repeatedly contain chitosan repeatedly, then gauze is taken out from container the ultra-pure water flushing for several times, last secondary freeze drying obtains to contain the degreasing cotton gauze of nanometer silver and chitosan.
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