A preparation process of antibacterial silver-loaded dressing

Abstract

The invention discloses a preparation process of an antibacterial silver-loaded dressing. The invention comprises the following steps: providing a chitosan raw material, dissolving the chitosan raw material in a 5% concentration acetic acid aqueous solution, filtering and defoaming to prepare a spinning stock solution with viscosity; preparing a mixed solution of a silane coupling agent and distilled water of 1%wt, weighing 5%wt of a nanometer powder of silver-loaded zirconium phosphate, adding the mixed solution to the mixed solution and stirring evenly, then adding a polytetrafluoroethylene fine powder, stirring at a low speed for 30 minutes, so that the nanometer silver-loaded zirconium phosphate is uniformly attached to the surface of polytetrafluoroethylene suspended particles, and obtaining an antibacterial solution; slowly adding the antibacterial solution to the spinning stock solution, weighing 22%wt of a waterproof polyether-modified silicone oil, stirring at a low speed for more than 60 minutes, pumping the oil into a metering pump, extruding the oil from a spinneret of a spinning machine, and passing through a coagulation bath to coagulate into an antibacterial solid fiber; sending the antibacterial solid fiber into a stretching machine, and undergoing multi-pass stretching to obtain an antibacterial chitosan fiber filament; and washing the antibacterial chitosan fiber filament with clean water and sending the antibacterial chitosan fiber filament into a braiding machine to be braided into an antibacterial chitosan fiber cloth. The silver-loaded zirconium phosphate of the present invention has excellent antibacterial properties and can quickly "kill" microbial slime attached to the surface of the membrane pores, avoiding clogging of the membrane pores and increased membrane resistance. At the same time, it is combined with polytetrafluoroethylene to spin chitosan fibers to enhance their waterproofness and avoid wound erosion, thereby avoiding the problem that the non-woven fabrics of previous dressings are unevenly distributed after post-treatment with antibacterial agents, which is easy to overflow and leads to reduced antibacterial effects.

Description

Technical Field

[0001] The invention belongs to the technical field of antibacterial dressings, and in particular relates to a preparation process of an antibacterial silver-loaded dressing. Background Art

[0002] As people's living standards improve, their awareness of self-health is increasing, and the antibacterial requirements for daily hygiene products are getting higher and higher. Nanosilver is a new type of antibacterial agent with strong antibacterial and bactericidal effects and broad-spectrum antibacterial activity, good durability, no drug resistance and high safety. It is widely used in textiles, coatings, medical treatment, environmental protection and other fields.

[0003] The method for preparing antibacterial dressings generally adopted at present is: through the process of post-finishing, the nano silver antibacterial agent is arranged on the dressing non-woven fabric to make it have antibacterial activity. The above preparation method can effectively control the relevant parameters of the nano silver antibacterial agent, and it is easy to meet different antibacterial requirements. However, the antibacterial agent directly post-finished is a chemical powder material, which is attached to the dressing non-woven fabric with a short durability, and its antibacterial rate and sterilization rate are not ideal. In addition, since the surface area and surface energy of the antibacterial powder material are very large during the production process, it is easy to adsorb each other and reunite. The nano silver antibacterial agent that is easy to reunite and unevenly dispersed will make the non-woven surface antibacterial effect uneven, and even partially lose the antibacterial effect, which seriously affects the product quality. Summary of the invention

[0004] In view of this, the technical problem to be solved by the present invention is to provide a preparation process for an antibacterial silver-loaded dressing, so as to avoid the problem that the non-woven fabric of the dressing is unevenly distributed after post-treatment with an antibacterial agent, which is easy to overflow and leads to reduced antibacterial effect.

[0005] In order to solve the above technical problems, the present invention discloses a process for preparing an antibacterial silver-loaded dressing, comprising: Step a. providing chitosan raw material, dissolving it in a 5% concentration of acetic acid aqueous solution, filtering and degassing to prepare a spinning solution having viscosity; Step b. Prepare a mixed solution of 1%wt of a silane coupling agent and distilled water, weigh 5%wt of a zirconium phosphate silver nanopowder, add it to the mixed solution and stir evenly, then add a polytetrafluoroethylene fine powder, stir at a low speed for 30 minutes, so that the nano-scale zirconium phosphate silver is evenly attached to the surface of the polytetrafluoroethylene suspended particles to obtain an antibacterial solution; Step c. Slowly adding the antibacterial solution to the spinning solution, and weighing 22% wt of waterproof polyether modified silicone oil, stirring at low speed for more than 60min, pumping into a metering pump, extruding from the spinneret of the spinning machine, and passing through a coagulation bath to coagulate into an antibacterial solid fiber; Step d. feeding the antibacterial solid fiber into a stretching machine and undergoing multiple stretching steps to obtain antibacterial chitosan fiber filaments; Step e: The antibacterial chitosan fiber filaments are washed with clean water and then fed into a weaving machine to be woven into an antibacterial chitosan fiber cloth.

[0006] According to one embodiment of the present invention, the silane coupling agent in the above step b is selected from at least one of KH550, KH560 or KH570.

[0007] According to one embodiment of the present invention, the nanometer powder of silver supported by zirconium phosphate in the above step b has a layered crystal structure and an average particle size of less than 80 nm.

[0008] According to one embodiment of the present invention, the weight ratio of the nano-powder of silver supported by zirconium phosphate in the above step b is in the range of 1%-5%.

[0009] According to one embodiment of the present invention, the mass ratio of the antibacterial solution to the spinning solution is 1:15.

[0010] According to one embodiment of the present invention, in the above step e, the washing with clean water is followed by drying, the drying temperature is 70-90° C., and the drying time is 3-4 hours.

[0011] According to one embodiment of the present invention, the antibacterial solution in the above step b is a polytetrafluoroethylene composite powder solution containing 2.0%wt of zirconium phosphate-supported silver modified.

[0012] Compared with the prior art, the present invention can achieve the following technical effects: The layered structure of zirconium phosphate-supported silver is similar to the structure of graphene and can improve the mechanical properties of chitosan fiber nonwoven fabrics; Silver-loaded zirconium phosphate has excellent antibacterial properties and can quickly "kill" microbial slime attached to the surface of membrane pores, avoiding clogging of membrane pores and increased membrane resistance. At the same time, it is combined with polytetrafluoroethylene-blended chitosan fiber spinning to enhance its waterproofness and avoid wound erosion.

[0013] Of course, any product implementing the present invention does not necessarily need to achieve all of the above-mentioned technical effects at the same time. DETAILED DESCRIPTION

[0014] The following will describe the implementation methods of the present invention in detail with reference to examples, so that the implementation process of how the present invention applies technical means to solve technical problems and achieve technical effects can be fully understood and implemented accordingly.

[0015] The invention discloses a preparation process of an antibacterial silver-loaded dressing, comprising: Step a. providing chitosan raw material, dissolving it in a 5% concentration of acetic acid aqueous solution, filtering and degassing to prepare a spinning solution having viscosity; Step b. Prepare a mixed solution of 1%wt of a silane coupling agent and distilled water, weigh 5%wt of a zirconium phosphate silver-loaded nanopowder, add it to the mixed solution and stir evenly, then add a polytetrafluoroethylene fine powder, stir at a low speed for 30 minutes, so that the nano-scale zirconium phosphate silver-loaded nanoparticles are evenly attached to the surface of the polytetrafluoroethylene suspended particles to obtain an antibacterial solution; wherein the silane coupling agent is selected from at least one of KH550, KH560 or KH570; Step c. slowly adding the antibacterial solution to the spinning solution, and weighing 22% wt of waterproof polyether modified silicone oil, stirring at a low speed for more than 60 minutes, pumping into a metering pump, extruding from the spinneret of the spinning machine, and passing through a coagulation bath to coagulate into an antibacterial solid fiber; the mass ratio of the antibacterial solution to the spinning solution is 1:15; Step d. feeding the antibacterial solid fiber into a stretching machine and undergoing multiple stretching steps to obtain antibacterial chitosan fiber filaments; Step e: The antibacterial chitosan fiber filaments are washed with clean water and then fed into a weaving machine to be woven into an antibacterial chitosan fiber cloth. Example 1

[0016] Step a. providing chitosan raw material, dissolving it in a 5% concentration of acetic acid aqueous solution, filtering and degassing to prepare a spinning solution having viscosity; Step b. The spinning solution is pumped into a metering pump, extruded from the spinneret of the spinning machine, and coagulated into a solid fiber through a coagulation bath; Step c. feeding the solid fiber into a stretching machine and stretching the chitosan fiber filaments through multiple passes; Step d. The chitosan fiber filaments are washed with clean water and then fed into a braiding machine to be woven into chitosan fiber cloth. Example 2

[0017] Step a. providing chitosan raw material, dissolving it in a 5% concentration of acetic acid aqueous solution, filtering and degassing to prepare a spinning solution having viscosity; Step b. The spinning solution is pumped into a metering pump, extruded from the spinneret of the spinning machine, and coagulated into a solid fiber through a coagulation bath; Step c. feeding the solid fiber into a stretching machine and stretching the chitosan fiber filaments through multiple passes; Step d. The chitosan fiber filaments are washed with clean water and then fed into a braiding machine to be woven into a chitosan fiber cloth; Step e: pre-immersing the chitosan fiber cloth in a solution containing a nano antibacterial agent, and drying the solution to obtain the antibacterial chitosan fiber cloth. Example 3

[0018] Step a. providing chitosan raw material, dissolving it in a 5% concentration of acetic acid aqueous solution, filtering and degassing to prepare a spinning solution having viscosity; Step b. Prepare a mixed solution of 1%wt of a silane coupling agent and distilled water, weigh 5%wt of a zirconium phosphate silver-loaded nanopowder, add it to the mixed solution and stir evenly, then add a polytetrafluoroethylene fine powder, stir at a low speed for 30 minutes, so that the nano-scale zirconium phosphate silver-loaded nanoparticles are evenly attached to the surface of the polytetrafluoroethylene suspended particles to obtain an antibacterial solution; wherein the silane coupling agent is selected from at least one of KH550, KH560 or KH570; Step c. Slowly adding the antibacterial solution to the spinning solution, and weighing 22% wt of waterproof polyether modified silicone oil, stirring at low speed for more than 60min, pumping into a metering pump, extruding from the spinneret of the spinning machine, and passing through a coagulation bath to coagulate into an antibacterial solid fiber; Step d. feeding the antibacterial solid fiber into a stretching machine and undergoing multiple stretching steps to obtain antibacterial chitosan fiber filaments; Step e: The antibacterial chitosan fiber filaments are washed with clean water and then fed into a weaving machine to be woven into an antibacterial chitosan fiber cloth. Example 4

[0019] Step a. providing chitosan raw material, dissolving it in a 5% concentration of acetic acid aqueous solution, filtering and degassing to prepare a spinning solution having viscosity; Step b. Prepare a 1%wt mixed solution of a silane coupling agent and distilled water, and then weigh 5%wt of zirconium phosphate silver nanopowder, add it to the mixed solution and stir to obtain an antibacterial solution; Step c. Slowly adding the antibacterial solution to the spinning solution, and weighing 22% wt of waterproof polyether modified silicone oil, stirring at low speed for more than 60min, pumping into a metering pump, extruding from the spinneret of the spinning machine, and passing through a coagulation bath to coagulate into an antibacterial solid fiber; Step d. feeding the antibacterial solid fiber into a stretching machine and undergoing multiple stretching steps to obtain antibacterial chitosan fiber filaments; Step e: The antibacterial chitosan fiber filaments are washed with clean water and then fed into a weaving machine to be woven into an antibacterial chitosan fiber cloth.

[0020] The chitosan fiber cloth prepared in Example 1-4 was washed and immersed in a suspension of Staphylococcus aureus, and cultured in a 37°C incubator for 18 hours for a control test. The colony count was observed and the sterilization rate was calculated. The performance and experimental results are shown in the following table:

[0021] In summary, the antibacterial chitosan fiber cloth prepared in Example 3 has the best antibacterial effect, and the polytetrafluoroethylene suspended particles can enhance the adhesion of zirconium phosphate-loaded silver particles, thereby maintaining high antibacterial properties.

[0022] The nanometer powder of zirconium phosphate loaded with silver in step b is a layered crystal structure with an average particle size of less than 80 nm, and can improve the mechanical properties of the chitosan fiber nonwoven fabric.

[0023] In step b, the weight ratio of the zirconium phosphate-supported silver nanopowder added is in the range of 1%-5%, which can be fully adsorbed by the polytetrafluoroethylene suspended particles.

[0024] Step e: After washing with clean water, drying is performed at a temperature of 70-90°C and a drying time of 3-4 hours to complete the cleaning.

[0025] The antibacterial solution in step b is a polytetrafluoroethylene composite powder solution containing 2.0%wt of zirconium phosphate-supported silver modified. At this time, nano-scale zirconium phosphate-supported silver is uniformly attached to the surface of the polytetrafluoroethylene suspended particles with good uniformity, and is finally mixed with the spinning solution to improve the antibacterial function.

[0026] In summary, the silver-loaded zirconium phosphate of the present invention has excellent antibacterial properties and can quickly "kill" the microbial slime attached to the surface of the membrane pores, avoiding clogging of the membrane pores and increasing the membrane resistance. At the same time, it is combined with polytetrafluoroethylene to blend chitosan fiber spinning to enhance its waterproofness and avoid wound erosion. It also avoids the problem that the non-woven fabric of the previous dressing is unevenly distributed after the antibacterial agent is post-treated, which is easy to overflow and leads to the trouble of reduced antibacterial effect.

[0027] The above description shows and describes several preferred embodiments of the present invention, but as mentioned above, it should be understood that the present invention is not limited to the form disclosed herein, and should not be regarded as excluding other embodiments, but can be used in various other combinations, modifications and environments, and can be modified within the scope of the invention concept described herein through the above teachings or the technology or knowledge of the relevant field. Changes and variations made by those skilled in the art do not depart from the spirit and scope of the present invention, and should be within the scope of protection of the claims attached to the present invention.

Claims

1. A process for preparing an antibacterial silver-loaded dressing, characterized in that: include: Step a. providing chitosan raw material, dissolving it in a 5% concentration of acetic acid aqueous solution, filtering and degassing to prepare a spinning solution having viscosity; Step b. Prepare a mixed solution of 1%wt of a silane coupling agent and distilled water, weigh 5%wt of a zirconium phosphate silver nanopowder, add it to the mixed solution and stir evenly, then add a polytetrafluoroethylene fine powder, stir at a low speed for 30 minutes, so that the nano-scale zirconium phosphate silver is evenly attached to the surface of the polytetrafluoroethylene suspended particles to obtain an antibacterial solution; Step c. Slowly adding the antibacterial solution to the spinning solution, and weighing 22% wt of waterproof polyether modified silicone oil, stirring at low speed for more than 60min, pumping into a metering pump, extruding from the spinneret of the spinning machine, and passing through a coagulation bath to coagulate into an antibacterial solid fiber; Step d. feeding the antibacterial solid fiber into a stretching machine and undergoing multiple stretching steps to obtain antibacterial chitosan fiber filaments; Step e: The antibacterial chitosan fiber filaments are washed with clean water and then fed into a weaving machine to be woven into an antibacterial chitosan fiber cloth.

2. The process for preparing the antibacterial silver-loaded dressing according to claim 1, characterized in that: The silane coupling agent in step b is selected from at least one of KH550, KH560 or KH570.

3. The process for preparing the antibacterial silver-loaded dressing according to claim 1, characterized in that: The nanometer powder of silver-loaded zirconium phosphate in step b is a layered crystal structure with an average particle size of less than 80 nm.

4. The process for preparing the antibacterial silver-loaded dressing according to claim 1, characterized in that: The weight ratio of the nanometer powder of silver-loaded zirconium phosphate added in step b is in the range of 1%-5%.

5. The process for preparing the antibacterial silver-loaded dressing according to claim 1, characterized in that: The mass ratio of the antibacterial solution to the spinning solution is 1:

15.

6. The process for preparing the antibacterial silver-loaded dressing according to claim 1, characterized in that: In step e, the washing is followed by drying at a temperature of 70-90° C. for 3-4 hours.

7. The process for preparing the antibacterial silver-loaded dressing according to claim 1, characterized in that: The antibacterial solution in step b is a polytetrafluoroethylene composite powder solution containing 2.0%wt of zirconium phosphate-supported silver modified.

Images