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CN113599564B - Novel non-woven fabric wound dressing and preparation method and application thereof - Google Patents

Novel non-woven fabric wound dressing and preparation method and application thereof
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CN113599564B
CN113599564BCN202110854030.9ACN202110854030ACN113599564BCN 113599564 BCN113599564 BCN 113599564BCN 202110854030 ACN202110854030 ACN 202110854030ACN 113599564 BCN113599564 BCN 113599564B
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chitosan
fiber
modified
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spinning
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CN113599564A (en
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李喆
杜柘彬
徐畅
吕向国
孙卫华
陈俭
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Jiangsu Guowang High Technique Fiber Co ltd
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Jiangsu Guowang High Technique Fiber Co ltd
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Abstract

The invention discloses a novel non-woven fabric wound dressing and a preparation method and application thereof, wherein the wound dressing is prepared from modified polyester fibers, modified chitosan fibers and modified calcium alginate fibers through a spunlace or needle-punching non-woven processing procedure; wherein, calculated by weight portion, 20-40 portions of modified polyester fiber, 10-20 portions of modified chitosan fiber and 10-40 portions of modified calcium alginate fiber; the modified polyester fiber contains 5-10wt% of nano silver, the modified chitosan fiber contains 0.1-1wt% of copper ions, and the modified calcium alginate fiber contains 0.1-2wt% of zinc ions; and the application of the novel non-woven fabric wound dressing in the skin wound covering dressing; the wound dressing provided by the invention not only can enable the antibacterial effect to run through the whole process of wound healing, but also has the effects of promoting angiogenesis, promoting re-epithelization and the like, so that the wound dressing can play a role in effectively promoting or assisting in accelerating the wound healing process.

Description

Novel non-woven fabric wound dressing and preparation method and application thereof
Technical Field
The invention relates to the technical field of wound dressings, in particular to a novel non-woven fabric wound dressing and a preparation method and application thereof.
Background
The skin is the largest organ of a human body, people inevitably encounter various wounds in production and life, and the method of wound care for covering exposed wounds by using the dressing is a common method for clinical wound care, and the dressing which is widely applied at present is the traditional cotton gauze; however, with the development of science and technology and the improvement of living standard, people put forward higher requirements on medical dressings, the traditional cotton gauze is difficult to meet actual requirements, and the traditional cotton gauze is increasingly replaced by novel medical dressings, for example, the conventional medical dressings contain silver ions, so that the novel medical dressings with antibacterial efficacy are obtained, the invention of China is CN109453409A, which discloses an antibacterial medical dressing, which is prepared by the following method: mixing medical sterile dressing and dopamine hydrochloride in trihydroxymethyl aminomethane solution, adding AgNO3 The silver-carrying antibacterial medical dressing is prepared from the aqueous solution at normal temperature and in a dark place under the stirring condition. Meanwhile, the ideal wound dressing not only can have partial functions of skin, provide a moist environment which is beneficial to wound healing, even play a role in protecting and preventing bacterial invasion, but also can accelerate or assist wound epithelization or transition to reconstruction of a permanent skin barrier.
Disclosure of Invention
The invention aims to overcome one or more defects in the prior art, and provides an improved non-woven fabric wound dressing capable of effectively promoting or assisting to accelerate wound healing.
The invention also provides a preparation method of the non-woven fabric wound dressing.
The invention also provides application of the non-woven fabric wound dressing in a skin wound covering dressing.
In order to achieve the purpose, the invention adopts a technical scheme that:
a novel non-woven fabric wound dressing is prepared by modified polyester fibers, modified chitosan fibers and modified calcium alginate fibers through a spunlace or needle-punching non-woven processing procedure; wherein, calculated by weight portion, 20-40 portions of modified polyester fiber, 10-20 portions of modified chitosan fiber and 10-40 portions of modified calcium alginate fiber; the modified polyester fiber contains 5-10wt% of nano silver, the modified chitosan fiber contains 0.1-1wt% of copper ions, and the modified calcium alginate fiber contains 0.1-2wt% of zinc ions.
According to some preferred aspects of the present invention, the nano silver has a particle size of 80 to 120nm.
According to some specific and preferred aspects of the present invention, the modified polyester fiber has a length of 35 to 150mm and a fineness of 0.3 to 10dtex.
According to some specific and preferred aspects of the present invention, the modified chitosan fiber has a fiber length of 35 to 150mm and a fineness of 0.5 to 5dtex, wherein the chitosan deacetylation degree is greater than 95%.
According to some specific and preferred aspects of the present invention, the modified calcium alginate fibers have a fiber length of 35 to 150mm and a titer of 0.5 to 5dtex.
According to some preferred aspects of the invention, the modified polyester fiber is prepared by melt spinning after mixing nano silver and polyester, nano silver particles and polyester are melt spun, and the particles are not easy to fall off in a fiber matrix during use, so that the durability and effectiveness of the antibacterial property are prolonged.
According to some preferred aspects of the invention, the modified chitosan fiber is prepared by mixing mother liquor containing copper ions with chitosan spinning solution, spinning, solidifying and stretching; wherein the mother liquor containing copper ions is obtained by dissolving copper sulfate or copper acetate in 1-6wt% of vinegar acid solution, and the copper ion content in the mother liquor containing copper ions is 0.1-0.5mol/L; the chitosan spinning solution is obtained by dissolving chitosan for spinning in 1-6wt% of acid-vinegar aqueous solution, wherein the content of the chitosan is 3-10wt%, and the deacetylation degree of the chitosan is more than 95%; the mixing ratio of the mother liquor containing copper ions to the chitosan spinning solution is 1:3-10.
According to some preferred aspects of the invention, the modified calcium alginate fiber is prepared by filtering and defoaming a sodium alginate aqueous solution to prepare a spinning solution, then spinning, entering a coagulating bath, washing with water, and stretching; wherein the coagulating bath is a mixed water solution of calcium ions and zinc ions, the concentration of the calcium ions is 0.1-0.5mol/L, and the concentration of the zinc ions is 0.05-0.2mol/L. In the spinning process of alginic acid, sodium alginate can rapidly generate ion exchange reaction with calcium ions and zinc ions; when the sodium alginate water solution is extruded into the coagulating bath from the spinneret orifice through the metering pump under the action of pressure, the sodium alginate liquid flow is rapidly coagulated and finally converted into calcium alginate fibers containing zinc ions.
The invention provides another technical scheme that: the preparation method of the novel non-woven fabric wound dressing comprises the following steps:
(1) Preparing modified polyester fiber: the nano silver/polyester fiber composite material is prepared by melt spinning after mixing nano silver and polyester chips;
preparing modified chitosan fiber: the copper ion-containing mother liquor and the chitosan spinning solution are mixed and then are spun, solidified and stretched to prepare the copper ion-containing chitosan fiber; wherein the mother liquor containing copper ions is obtained by dissolving copper sulfate or copper acetate in 1-6wt% of vinegar acid solution, and the copper ion content in the mother liquor containing copper ions is 0.1-0.5mol/L; the chitosan spinning solution is obtained by dissolving chitosan for spinning in 1-6wt% of acid-vinegar aqueous solution, wherein the content of chitosan is 3-10wt%, and the deacetylation degree of chitosan is more than 95%; the mixing ratio of the mother liquor containing copper ions to the chitosan spinning solution is 1:3-10;
preparing modified calcium alginate fibers: filtering and defoaming a sodium alginate aqueous solution to prepare a spinning solution, then spraying the spinning solution, feeding the spinning solution into a coagulating bath, washing with water, and stretching to prepare the composite material; wherein the coagulating bath is a mixed water solution of calcium ions and zinc ions, the concentration of the calcium ions is 0.1-0.5mol/L, and the concentration of the zinc ions is 0.05-0.2mol/L;
(2) According to the weight ratio, the modified polyester fiber, the modified chitosan fiber and the modified calcium alginate fiber are made into the wound dressing through the spunlace or needle-punching non-woven processing procedure.
The invention provides another technical scheme that: the novel non-woven fabric wound dressing has good antibacterial performance when applied to a skin wound covering dressing, and the sterilization rate of the novel non-woven fabric wound dressing to escherichia coli, staphylococcus aureus, candida albicans and pseudomonas aeruginosa is over 98% within 7-10 days.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
based on the problems that the existing medical dressing has single function, is difficult to effectively realize antibacterial effect, simultaneously has effect on the aspects of angiogenesis, wound epithelization and the like of a wound, and cannot obviously and effectively promote the healing of the wound, the invention innovatively provides a non-woven fabric wound dressing prepared by mixing modified polyester fibers, modified calcium alginate fibers and modified chitosan fibers containing different trace elements, wherein the adopted degradable calcium alginate fibers and chitosan fibers contain copper ions, the calcium alginate fibers contain calcium ions and zinc ions, and the two degradable materials can be used for quickly releasing the copper ions, the calcium ions and the zinc ions, so that the expression of a vascular endothelial growth factor can be induced, angiogenesis is promoted, and the stability of collagen is maintained; meanwhile, the re-epithelialization can be promoted in the early stage of wound healing, the structural integrity of protein and the expression of regulatory genes are maintained in the stages of proliferation and maturation processes, the regulation of immunity, cell growth and migration is involved, and a key role is played in wound healing; the degradable polyester fiber which is difficult to degrade is adopted to match with the degradable fiber, on one hand, the polyester fiber is utilized to bear silver ions, on the other hand, the material is difficult to degrade, so that the problem that nano silver is quickly released when the material is mixed with a biodegradable material is solved, researches prove that the wound dressing disclosed by the invention has effective antibacterial performance of more than 7 days, the antibacterial rate of common wound bacteria is more than 95%, and meanwhile, the angiogenesis and wound epithelization of wounds are promoted, and the healing of infected wounds is effectively accelerated.
Drawings
FIG. 1 is a schematic structural view of a novel nonwoven fabric wound dressing made in example 1 of the present invention;
FIG. 2 is a graph of wound area as a function of time in an animal experiment showing the healing of a wound according to an embodiment of the present invention.
Detailed Description
The above scheme is further explained by combining with specific embodiments; it is to be understood that these embodiments are provided to illustrate the general principles, essential features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.
In the following, all starting materials are either commercially available or prepared according to methods conventional in the art, unless otherwise specified.
Example 1
The embodiment provides a novel non-woven fabric wound dressing and a preparation method thereof, the wound dressing is prepared by modified polyester fiber, modified chitosan fiber and modified calcium alginate fiber through a spunlace or needle-punching non-woven processing procedure, and the structural schematic diagram is shown in figure 1; the modified polyester fiber is prepared from 40 parts by mass of modified polyester fiber, 10 parts by mass of modified chitosan fiber and 10 parts by mass of modified calcium alginate fiber.
The preparation method comprises the following steps:
(1) Preparing modified polyester fiber: uniformly mixing nano silver and polyester chips, and carrying out melt spinning to obtain the nano silver-polyester fiber; the melt spinning process parameters are as follows: controlling the water content to be 50-100 ppm (mass content), the spinning temperature to be 275-285 ℃, and the length of the prepared modified polyester fiber to be 150mm, and the titer to be: 0.3 dtex; the grain diameter of the nano silver is 80nm, and the addition amount of the nano silver accounts for 10wt% of the total weight of the nano silver and the polyester chip;
preparing modified chitosan fiber: the modified chitosan fiber is prepared by mixing mother liquor containing copper ions and chitosan spinning solution, and then spinning, solidifying and stretching, wherein the length of the prepared modified chitosan fiber is 150mm, and the titer is as follows: 0.5dtex; wherein the mother liquor containing copper ions is obtained by dissolving copper sulfate in 6wt% of vinegar acid aqueous solution, and the copper ion content in the mother liquor containing copper ions is 0.5mol/L; the chitosan spinning solution is obtained by dissolving chitosan for spinning in 6wt% of acid-vinegar aqueous solution, wherein the content of chitosan is 10wt%, and the deacetylation degree of chitosan is 97%; the mixing volume ratio of the mother liquor containing copper ions to the chitosan spinning solution is 1:3; measuring that the prepared modified chitosan fiber contains 1wt% of copper ions;
preparing modified calcium alginate fibers: filtering and defoaming a sodium alginate aqueous solution to obtain a spinning solution, then spraying, feeding into a coagulating bath, washing with water, and stretching to prepare the modified calcium alginate fiber with the fiber length of 120 mm and the titer of 0.5dtex; wherein the spinning speed is 20m/s, the drawing multiple is 5 times, the coagulating bath is a mixed aqueous solution of calcium ions and zinc ions, the concentration of the calcium ions is 0.1mol/L, and the concentration of the zinc ions is 0.05 mol/L; the prepared modified calcium alginate fiber is measured to contain 0.1 weight percent of zinc ions;
(2) According to the weight ratio, the modified polyester fiber, the modified chitosan fiber and the modified calcium alginate fiber are made into the wound dressing through the spunlace non-woven processing procedure.
Example 2
The present invention provides a novel non-woven fabric wound dressing and a preparation method thereof, wherein the wound dressing is prepared from modified polyester fibers, modified chitosan fibers and modified calcium alginate fibers through a spunlace or needle-punching non-woven processing procedure; wherein, calculated by mass portion, 30 portions of modified polyester fiber, 20 portions of modified chitosan fiber and 20 portions of modified calcium alginate fiber.
The preparation method comprises the following steps:
(1) Preparing modified polyester fiber: uniformly mixing nano silver and polyester chips, and carrying out melt spinning to obtain the nano silver-polyester fiber; the melt spinning process parameters are as follows: controlling the water content to be 50-100 ppm (mass content), the spinning temperature to be 255-275 ℃, and the length of the prepared modified polyester fiber to be 65mm, and the titer to be: 3.0dtex; the grain diameter of the nano silver is 100nm, and the adding amount of the nano silver accounts for 8wt% of the total weight of the nano silver and the polyester chip;
preparing modified chitosan fiber: the modified chitosan fiber is prepared by mixing mother liquor containing copper ions and chitosan spinning solution, and then spinning, solidifying and stretching, wherein the length of the prepared modified chitosan fiber is 65mm, and the titer is as follows: 2 dtex; wherein the mother liquor containing copper ions is obtained by dissolving copper sulfate in 6wt% of vinegar acid aqueous solution, and the copper ion content in the mother liquor containing copper ions is 0.2mol/L; the chitosan spinning solution is obtained by dissolving chitosan for spinning in 6wt% of acid-vinegar aqueous solution, wherein the content of chitosan is 8wt%, and the deacetylation degree of chitosan is 99%; the mixing volume ratio of the mother liquor containing copper ions to the chitosan spinning solution is 1:5; measuring that the prepared modified chitosan fiber contains 0.5wt% of copper ions;
preparing modified calcium alginate fibers: filtering and defoaming a sodium alginate aqueous solution to obtain a spinning solution, then spinning, feeding into a coagulating bath, washing with water, and stretching to prepare the modified calcium alginate fiber with the fiber length of 60 mm and the titer of 3 dtex; wherein the spinning speed is 20m/s, the drawing multiple is 4 times, the coagulating bath is a mixed aqueous solution of calcium ions and zinc ions, the concentration of the calcium ions is 0.3mol/L, and the concentration of the zinc ions is 0.1mol/L; the prepared modified calcium alginate fiber is measured to contain 1 weight percent of zinc ions;
(2) According to the weight ratio, the wound dressing is prepared by the modified polyester fiber, the modified chitosan fiber and the modified calcium alginate fiber through the spunlace non-woven processing procedure.
Example 3
The present invention provides a novel non-woven fabric wound dressing and a preparation method thereof, wherein the wound dressing is prepared from modified polyester fibers, modified chitosan fibers and modified calcium alginate fibers through a spunlace or needle-punching non-woven processing procedure; the modified polyester fiber is prepared from 40 parts by mass of modified polyester fiber, 10 parts by mass of modified chitosan fiber and 30 parts by mass of modified calcium alginate fiber.
The preparation method comprises the following steps:
(1) Preparing modified polyester fiber: uniformly mixing nano silver and polyester chips, and carrying out melt spinning to obtain the nano silver-polyester fiber; the melt spinning process parameters are as follows: controlling the water content to be 50-100 ppm (mass content), the spinning temperature to be 235-245 ℃, and the length of the prepared modified polyester fiber to be 38mm, and the titer to be: 10dtex; the particle size of the nano silver is 120nm, and the addition amount of the nano silver accounts for 5wt% of the total weight of the nano silver and the polyester chip;
preparing modified chitosan fiber: the modified chitosan fiber is prepared by mixing mother liquor containing copper ions and chitosan spinning solution, and then spinning, solidifying and stretching, wherein the length of the prepared modified chitosan fiber is 35 mm, and the titer is as follows: 5dtex; wherein the mother liquor containing copper ions is obtained by dissolving copper sulfate in 6wt% of vinegar acid aqueous solution, and the copper ion content in the mother liquor containing copper ions is 0.1mol/L; the chitosan spinning solution is obtained by dissolving chitosan for spinning in 6wt% of acid-vinegar aqueous solution, wherein the content of chitosan is 10wt%, and the deacetylation degree of chitosan is 98%; the mixing volume ratio of the mother liquor containing copper ions to the chitosan spinning solution is 1:10; the prepared modified chitosan fiber is measured to contain 0.1wt% of copper ions;
preparing modified calcium alginate fibers: the modified calcium alginate fiber is prepared by filtering and defoaming a sodium alginate aqueous solution to obtain a spinning solution, then spinning, entering a coagulating bath, washing with water and stretching, wherein the fiber length of the prepared modified calcium alginate fiber is 38mm, and the titer is 5dtex; wherein the spinning speed is 20m/s, the drawing multiple is 2 times, the coagulating bath is a mixed aqueous solution of calcium ions and zinc ions, the concentration of the calcium ions is 0.5mol/L, and the concentration of the zinc ions is 0.2mol/L; measuring that the prepared modified calcium alginate fiber contains 2wt% of zinc ions;
(2) According to the weight ratio, the wound dressing is prepared by the modified polyester fiber, the modified chitosan fiber and the modified calcium alginate fiber through the spunlace non-woven processing procedure.
Application test: a series of experiments comprise the safety and effectiveness evaluation of the novel non-woven fabric wound dressing prepared by the patent. Wherein the safety evaluation is carried out according to the requirements of the biological evaluation of GB/T16886 medical instruments. The effectiveness evaluation includes antibacterial performance, water vapor permeability and zoology evaluation.
Testing the biocompatibility:
the novel nonwoven fabric wound dressing prepared in this patent (as in example 1) was evaluated for cytotoxicity, delayed contact sensitization of guinea pigs, skin irritation, and the like, respectively, with reference to biological evaluation of GB/T16886 medical devices.
Intracellular toxicity test according to GB/T16886-5, part 5 of the biological evaluation of medical devices: in vitro cytotoxicity test "; guinea pig delayed contact sensitization test according to GB/T16886-10,part 10 of the biological evaluation of medical devices: stimulation and delayed type hypersensitivity tests were performed using the Magnusson and Kligman methods of maximum test. Skin irritation test according to GB/T16886-10,part 10 of the biological evaluation of medical devices: stimulation and delayed hypersensitivity tests.
The results show that: the novel non-woven fabric wound dressing prepared in the embodiment 1 is less thangrade 2 in cytotoxicity, free of skin sensitization reaction and skin irritation reaction and good in biosafety.
Test for antibacterial Property
The novel non-woven fabric wound dressing sample of the example 1 is tested for antibacterial performance by adopting AATCC-100, and the antibacterial rate is 99%; after 7 days of continuous use, the antibacterial performance of the product is tested by adopting AATCC-100, and the antibacterial rate is 95 percent.
Water vapor transmission rate test
According to YY/T0471.2-2004part 2 of the contact wound dressing test method: breathable film dressing Water vapor Transmission Rate test the water vapor transmission rate of the novel nonwoven fabric wound dressing sample of example 1 was measured to have a water vapor transmission rate (MVTR) of 1800 grams per square meter per 24 hours (g.m)-2 •24h-1 )。
Wound healing conditions animal experiments:
a full-layer skin wound surface is established on two sides of the back of a New Zealand white rabbit, staphylococcus aureus is planted on the wound surface, and a rabbit infected wound model is established. The two side wound surfaces are respectively treated by the novel non-woven fabric wound dressing (experimental group) in the patent example 1 and a clinical common dressing (a comparison group is an antibacterial medical dressing, the specific material is that the novel non-woven fabric wound dressing is prepared from nano-silver-containing antibacterial medical non-woven fabric and a net-shaped PE film, and the novel non-woven fabric wound dressing is suitable for blank groups of large-area ulcers, skin injury wounds, anti-infection healing promotion treatment of skin supply area wounds and skin grafting area wounds and no treatment. Ondays 2, 7, 10, 14 and 17, the wound size was imaged and the wound area was calculated from the photographs.
The results show that the healing rate of the experimental group is obviously higher than that of the control group and the blank group: on day 17, the experimental group had a wound area of 5.2%, indicating that substantial healing had occurred; the control group had a wound area of 34.3%; the wound area in the blank group was 52.5%, as shown in particular in fig. 2.
The above embodiments are only for illustrating the technical idea and features of the present invention, and the purpose of the present invention is to enable those skilled in the art to understand the content of the present invention and implement the present invention, and not to limit the protection scope of the present invention by this means. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (4)

CN202110854030.9A2021-07-282021-07-28Novel non-woven fabric wound dressing and preparation method and application thereofActiveCN113599564B (en)

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