Novel composite multilayer breathable gauze material with waterproof and anti-infection functions and preparation method thereof

Abstract

The invention discloses a novel composite multilayer breathable gauze material with waterproof and anti-infection functions and a preparation method thereof. The preparation method comprises the following specific preparation steps: 1) dipping gauze in a graphene oxide solution, and then washing and drying; forming a first reinforced layer structure on the surface of the gauze; 2) dipping the gauze forming the first reinforced layer structure in a stearic acid / organic silicon emulsion / vegetable oil mixed solution for hydrophobic modification to form a second waterproof layer structure; 3) performing cold gas dynamic spraying on the surface of the gauze to deposit nano-silver particles so as to form a third antibacterial layer structure; and 4) carrying out light-proof packaging and irradiation sterilization to obtain the novel composite multi-layer breathable gauze material with waterproof and anti-infection functions. When the novel composite multi-layer breathable gauze material is used, the side with the silver coating is in direct contact with a wound. The gauze material can achieve efficient prevention and treatment of wound infection, the hydrophobic coating can effectively block external water and guarantee breathability, and the gauze material has important clinical significance on wound treatment.

Description

Technical Field

[0001] The invention relates to a preparation technology of a gauze material, and in particular to a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions and a preparation method thereof. Background Art

[0002] Bandaging is one of the important measures for emergency treatment of trauma. Timely and correct bandaging can achieve the purpose of compression hemostasis, reduce infection, protect wounds, reduce pain, and fix dressings and splints. Correct bandaging not only requires bandaging technology, but also has certain biological activity, which will have a positive effect on wound treatment, especially infection and wound ulceration.

[0003] At present, some wound dressings and gauze with anti-infection functions are on the market, but their complex preparation process, poor effect, and airtightness caused by the multi-layer structure have greatly limited their clinical use, resulting in unsatisfactory wound treatment effects. More importantly, when patients use dressings or gauze, they often inevitably come into contact with liquids such as water. Once in contact with liquid, the dressing or gauze itself has a certain water absorption capacity, which causes direct contamination of the wound and worsens the patient's condition.

[0004] Therefore, in view of the problems of poor antibacterial effect, poor air permeability and non-waterproofness of the above-mentioned gauze materials, the present invention provides a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions and a preparation method thereof. A reinforcing layer, a waterproof layer and an antibacterial layer structure are sequentially introduced on the surface of the gauze through a multi-step combined process, and the good air permeability of the gauze itself is not affected, providing a new solution strategy for the treatment of wounds and the prevention and treatment of infections. Summary of the invention

[0005] The purpose of the present invention is to provide a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions and a preparation method thereof in view of the problems that traditional gauze materials are not waterproof and do not have anti-infection functions. The novel composite multi-layer breathable gauze material can achieve efficient prevention and treatment of wound infection, and the hydrophobic coating can effectively block external water and ensure air permeability, which has important clinical significance for wound treatment.

[0006] The present invention is implemented by the following technical solution, which specifically includes the following steps:

[0007] A method for preparing a novel composite multi-layer breathable gauze material having both waterproof and anti-infection functions, comprising the following steps:

[0008] 1) dipping the gauze in a graphene oxide (GO) solution, then rinsing and drying, and forming a first reinforcement layer structure on the surface of the gauze after the dipping-rinsing-drying process is cycled several times;

[0009] 2) The gauze forming the first reinforcing layer structure is immersed in a mixed solution of stearic acid / organic silicon emulsion / vegetable oil for hydrophobic modification, and after drying, a second waterproof layer structure is formed, which is then flatly fixed on the template to ensure that one side of the gauze is in close contact with the template;

[0010] 3) vacuum cold gas dynamic spraying is performed on the gauze surface away from the template to deposit nanosilver particles to form a third antibacterial layer structure, followed by gas flushing;

[0011] 4) After the gas flushing is completed, the gauze is packaged in a light-proof manner and sterilized by irradiation to obtain a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions. When used, the side with the silver antibacterial layer structure is in direct contact with the wound.

[0012] Further, in step 1), in the GO solution, the size of GO is 2-5 microns, the solution concentration is 0.05-0.1wt%, the immersion time is 3-10min, and the solvent is deionized water;

[0013] The rinsing is performed with deionized water;

[0014] During the drying process, the drying temperature is 50-60°C and the time is 30-60min;

[0015] The dipping-rinsing-drying process was cycled 2-3 times.

[0016] Furthermore, in the stearic acid / organic silicon emulsion / vegetable oil mixed solution of step 2), the concentration of stearic acid is 0.05-0.5 v / v%;

[0017] The silicone emulsion is one or more of polydiethylsiloxane, dodecyltriethylsilane, polymethyltrifluoropropylsiloxane, polymethylvinylsiloxane, hexadecyltriethoxysilane, polydimethylsiloxane, hexadecyltrimethoxysilane, and methyltriethoxysilane, with a concentration of 1-5 v / v%;

[0018] The vegetable oil is one or more of olive oil, soybean oil, and sesame oil, with a concentration of 0.5-2 v / v%;

[0019] The solvent is one of dichloromethane, acetone, and trichloroethane;

[0020] The drying is carried out by nitrogen drying for 6-12 hours at a temperature of 25-30°C.

[0021] Furthermore, in step 3), the size of the nano silver particles is 1-5 nanometers, and the purity is above 99.99%.

[0022] Furthermore, in the vacuum cold gas power spraying process, the vacuum degree is greater than 5Pa, the spraying pressure is 0.5-1MPa, nitrogen is used as the working gas, the spraying distance is 20-45mm, the temperature is 60-80°C, and the cycle scanning spraying mode is adopted, and the cycle spraying is repeated 2-3 times;

[0023] The gas flushing uses nitrogen, the gas flushing pressure is 0.3-0.5MPa, and the flushing time is 5-15min.

[0024] Furthermore, in step 4), aluminum foil is used as the packaging material for light-proof packaging, and vacuum is drawn during packaging.

[0025] A novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions is obtained by adopting any of the above-mentioned preparation methods.

[0026] Compared with the prior art, the present invention has the following advantages:

[0027] 1) The present invention uses ordinary gauze, GO, stearic acid, silicone emulsion, vegetable oil, nanosilver, etc. as raw materials, and combines cyclic impregnation-washing-drying, vacuum cold gas dynamic spraying, nitrogen flushing and other combined processes to prepare a new composite multi-layer breathable gauze material with both waterproof and anti-infection functions. The above raw material selection and process combination are original to the present invention.

[0028] 2) The novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions in the present invention has a first reinforcing layer, a second waterproof layer and a third antibacterial layer structure. In the present invention, the first reinforcing layer is a GO layer introduced on the gauze surface by a cyclic impregnation-rinsing-drying process. By wrapping GO on the gauze surface, the ordinary gauze is enhanced, and a solid physical foundation is laid for the subsequent vacuum cold gas dynamic spraying to introduce the nano-silver antibacterial layer; the second waterproof layer is made of stearic acid, silicone emulsion, vegetable oil and a variety of raw materials with hydrophobic properties and high biocompatibility. Through the adsorption of the above raw materials on the gauze surface, the hydrophobicity of the above materials is transferred to the gauze, which can prevent the gauze from being wetted by the solution during use, causing wound contamination, infection, etc.; the third antibacterial layer structure is a nano-silver layer, and the nano-silver is physically embedded on the gauze surface by vacuum cold gas dynamic spraying of nano-silver on the reinforcing layer, and the nano-silver with loose surface bonding is removed by nitrogen flushing, etc., to obtain a stable antibacterial layer structure, which can achieve efficient prevention and treatment of wound infection.

[0029] 3) In the present invention, a reinforcing layer is introduced on the gauze surface as a basis by a circulating impregnation-rinsing-drying process, and further in combination with a vacuum cold gas power spraying nano silver antibacterial layer structure, the gauze is successfully endowed with excellent infection prevention and control functions. Since ordinary gauze is not resistant to high temperatures, it is impossible to use methods such as PVD or CVD to introduce antibacterial coatings, and if technologies such as chemical reduction are used, a reducing agent will be introduced into the gauze, thereby bringing biological toxicity, so in the present invention, in combination with the characteristics of gauze, and gentle process parameters and a GO reinforcing layer are carefully designed (by the physical protective barrier effect of GO, the vacuum cold gas power spraying operation is prevented from causing the gauze to break and be damaged), the vacuum cold gas power spraying technology is successfully used without destroying the mechanical properties of the gauze, and the vacuum condition ensures that the nano silver is not oxidized. On the basis, the nano silver is sprayed onto the gauze surface by nitrogen, so that the gauze surface undergoes strong plastic deformation and is deposited to form a coating, and the nitrogen flushing technology is used to flush out the nano silver particles that are not firmly bonded, and prevent the nano silver from falling off during use of the later gauze, and finally successfully construct an antibacterial layer structure, giving the gauze with excellent infection prevention and control functions. The above structural design and process selection are designed by the applicant in combination with the preparation requirements of the gauze material of the present invention, realizing a new application of the old process.

[0030] 4) The novel composite gauze in the present invention has the functions of air permeability, anti-infection, waterproof and water absorption at the same time. In the present invention, the gauze is given excellent hydrophobicity by introducing various raw materials with hydrophobic properties and high biocompatibility such as stearic acid, silicone emulsion, vegetable oil, etc., to prevent it from being wetted and causing pollution or infection during use, and vacuum cold gas power spraying forms a nano silver antibacterial layer of micron level on the surface, and the process of spraying can wash away the hydrophobic substance on the surface of one side of the antibacterial layer, so as to achieve efficient prevention and treatment of infection, and ensure the water absorption performance of one side of the antibacterial layer. At the same time, because the above-mentioned modification is all based on micron or nanometer scale, the macroscopic structure of the gauze is not significantly changed, so that the air permeability of the gauze itself is well preserved, and the good air permeability demand of wound healing is guaranteed, and the infection and pollution of the wound are not caused by the formation of a closed environment by the gauze, which has practical clinical application significance.

[0031] 5) The combined process used in the present invention is universal, and the controllable construction of the above-mentioned multiple composite functional layer structure can be achieved on any gauze base surface, thereby giving the gauze excellent breathability, anti-infection and waterproof functions, which has important clinical significance for the functional innovation and upgrading of traditional gauze. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 This is a schematic diagram of the preparation process of the novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions of the present invention;

[0033] Figure 2The contact angle result of a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions according to an embodiment of the present invention (Example 1);

[0034] Figure 3 This is the antibacterial zone result of a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions according to an embodiment of the present invention (Example 1). DETAILED DESCRIPTION

[0035] The technical solution of the present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments.

[0036] Embodiment 1:

[0037] 1) First, take a conventional gauze and immerse it in a GO solution with a concentration of 0.1wt% (GO size is 2-5 microns) for 3 minutes. After taking it out, use deionized water to rinse off the free GO on the surface, and then dry it at 60°C for 30 minutes to form the first strengthening layer structure on the surface. The above immersion-rinsing-drying process is repeated 3 times;

[0038] 2) The gauze is immersed in a mixed solution of 0.25 v / v% stearic acid / 3 v / v% hexadecyl triethoxysilane emulsion / 2 v / v% olive oil (the solvent is dichloromethane) for hydrophobic modification, and the residual solvent is removed by nitrogen drying at 25°C for 12 hours to form a second waterproof layer structure, and then it is flatly fixed on the template to ensure that one side of the gauze is in close contact with the template;

[0039] 3) vacuum cold gas power spraying (vacuum degree greater than 5Pa, spraying pressure 0.5MPa, nitrogen as working gas, spraying distance 25mm, temperature 60°C, cyclic scanning spraying mode, cyclic spraying 3 times) is performed on the gauze surface away from the template to deposit nanosilver particles (the size of the nanosilver particles is about 2-3 nanometers, purity 99.99%) to form a third antibacterial layer structure, and then nitrogen gas is used for gas flushing (nitrogen gas flushing pressure is 0.3MPa, flushing time is 10min) to remove the nanosilver particles that are not firmly bound to the surface;

[0040] 4) The material is packaged in a light-proof manner using aluminum foil, and then sterilized by irradiation after vacuuming to obtain a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions. When used, the side with the silver antibacterial layer structure is in direct contact with the wound.

[0041] The contact angle of the composite gauze surface is about 158°. Figure 2 As shown; the composite gauze material was used to prepare an extract, and after co-culture with endothelial cells for 7 days, the CCK-8 results showed that the cell survival rate was about 89%; the composite gauze (1 cm diameter disc) was subjected to an inhibition zone experiment, and the results showed that the area of ​​the inhibition zone was about 3.04 cm2 ,like Figure 3 As shown; combined with the rat skin wound infection model, the surface was sprinkled with water 0.5ml / cm on day 1. 2 , after 7 days the skin began to scab over and the infection was effectively treated.

[0042] Embodiment 2:

[0043] 1) First, take a conventional gauze and immerse it in a mixed solution of 0.25v / v% stearic acid / 3v / v% hexadecyl triethoxysilane emulsion / 2v / v% olive oil (the solvent is dichloromethane) for hydrophobic modification, and use nitrogen to dry for 12 hours at 25°C to remove the residual solvent to form a first waterproof layer structure, and then fix it flatly on the template to ensure that one side of the gauze is in close contact with the template;

[0044] 2) vacuum cold gas power spraying (vacuum degree greater than 5Pa, spraying pressure 0.5MPa, nitrogen as working gas, spraying distance 25mm, temperature 60°C, cyclic scanning spraying mode, cyclic spraying 3 times) is performed on the gauze surface away from the template to deposit nanosilver particles (the size of the nanosilver particles is about 2-3 nanometers, and the purity is 99.99%) to form a second antibacterial layer structure, and then nitrogen gas is used for gas flushing (nitrogen gas flushing pressure is 0.3MPa, and the flushing time is 10min) to remove the nanosilver particles that are not firmly bound to the surface;

[0045] 3) The material is packaged in a light-proof manner using aluminum foil, and then sterilized by irradiation after vacuuming to obtain a composite multi-layer breathable gauze material with both waterproof and anti-infection functions without a GO reinforcement layer. When used, the side with the silver antibacterial layer structure is in direct contact with the wound.

[0046] Compared with Example 1, the GO reinforcement layer is reduced in this embodiment. The contact angle of the composite gauze surface is about 141°; the composite gauze material is used to prepare an extract, and after co-culture with endothelial cells for 7 days, the CCK-8 results show that the cell survival rate is about 87%; the composite gauze (1 cm diameter disc) is subjected to an antibacterial zone experiment, and the results show that the antibacterial zone area is about 3.27 cm 2 Combined with the rat skin wound infection model, the surface was sprinkled with water at 0.5 ml / cm on day 1. 2 After 7 days, the skin began to scab and the infection was effectively treated. However, due to the disappearance of the GO reinforcement layer, the gauze fibers were significantly damaged, which affected the strength and appearance of the gauze.

[0047] Embodiment 3:

[0048] 1) Taking traditional gauze and dipping it in a mixed solution of 0.25v / v% stearic acid / 3v / v% hexadecyl triethoxysilane emulsion / 2v / v% olive oil (the solvent is dichloromethane) for hydrophobic modification, using nitrogen to dry for 12 hours at 25°C to remove the residual solvent to form a waterproof layer structure, and then fixing it flatly on the template to ensure that one side of the gauze is tightly fitted to the mold;

[0049] 2) Packing the gauze and sterilizing it by irradiation to obtain a new type of composite gauze material with waterproof function.

[0050] Compared with Example 1, the GO strengthening layer and the nanosilver antibacterial layer were reduced in this embodiment. The contact angle of the composite gauze surface was about 163°; the composite gauze material was prepared by extracting liquid, and after co-culture with endothelial cells for 7 days, the CCK-8 results showed that the cell survival rate was about 92%; the composite gauze (1 cm diameter disc) was subjected to an inhibition zone experiment, and the results showed that no inhibition zone was formed; combined with the rat skin wound infection model, the surface was sprinkled with water 0.5 ml / cm on day 1. 2 , 3 days later, the skin became severely infected and ulcerated.

[0051] Embodiment 4:

[0052] 1) First, take a conventional gauze and immerse it in a GO solution (size 2-5 microns) with a concentration of 0.1wt% for 3 minutes, then use deionized water to rinse off the free GO on the surface, and dry it at 60°C for 30 minutes to form the first strengthening layer structure on the surface. The above immersion-rinsing-drying process is repeated 3 times;

[0053] 2) vacuum cold gas power spraying (vacuum degree greater than 5Pa, spraying pressure 0.5MPa, nitrogen as working gas, spraying distance 25mm, temperature 60°C, cyclic scanning spraying mode, cyclic spraying 3 times) is performed on the gauze surface away from the template to deposit nanosilver particles (the size of the nanosilver particles is about 2-3 nanometers, purity 99.99%) to form an antibacterial layer structure, and then nitrogen gas is used for gas flushing (nitrogen gas flushing pressure is 0.3MPa, flushing time is 10min) to remove the nanosilver particles that are not firmly bound to the surface;

[0054] 3) The material is packaged in a light-proof manner using aluminum foil, and then evacuated and irradiated for sterilization to obtain a novel composite multilayer gauze material with anti-infection function. When used, the side with the silver antibacterial layer structure is in direct contact with the wound.

[0055] Compared with Example 1, the waterproof layer is reduced in this example. The contact angle of the composite gauze surface is about 18°; the composite gauze material is used to prepare an extract, and after co-culture with endothelial cells for 7 days, the CCK-8 results show that the cell survival rate is about 90%; the composite gauze (1 cm diameter disc) is subjected to an antibacterial zone test, and the results show that the antibacterial zone area is about 3.48 cm 2 Combined with the rat skin wound infection model, the surface was sprinkled with water at 0.5 ml / cm on day 1. 2 , and on the 3rd day, the skin became severely infected and accompanied by ulceration symptoms.

Claims

1. A method for preparing a novel composite multi-layer breathable gauze material having both waterproof and anti-infection functions, characterized in that: The following steps are involved: 1) Immersing the gauze in a graphene oxide (GO) solution, then rinsing and drying; After the immersion-rinsing-drying process is cycled several times, a first strengthening layer structure is formed on the surface of the gauze; 2) The gauze forming the first reinforcing layer structure is immersed in a mixed solution of stearic acid / organic silicon emulsion / vegetable oil for hydrophobic modification, and after drying, a second waterproof layer structure is formed, which is then flatly fixed on the template to ensure that one side of the gauze is in close contact with the template; 3) vacuum cold gas dynamic spraying is performed on the gauze surface away from the template to deposit nanosilver particles to form a third antibacterial layer structure, followed by gas flushing; 4) After the gas flushing is completed, the product is packaged in a light-proof manner and sterilized by irradiation to obtain a new composite multi-layer breathable gauze material with both waterproof and anti-infection functions.

2. The method for preparing the novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions according to claim 1, characterized in that: Step 1) In the GO solution, the size of GO is 2-5 microns, the solution concentration is 0.05-0.1wt%, the solvent is deionized water, and the immersion time is 3-10min; The rinsing is performed with deionized water; In the drying process, the temperature is 50-60°C and the time is 30-60min; The dipping-rinsing-drying process was cycled 2-3 times.

3. The method for preparing the novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions according to claim 1, characterized in that: Step 2) in the stearic acid / organic silicon emulsion / vegetable oil mixed solution, the stearic acid concentration is 0.05-0.5 v / v%; The silicone emulsion is one or more of polydiethylsiloxane, dodecyltriethylsilane, polymethyltrifluoropropylsiloxane, polymethylvinylsiloxane, hexadecyltriethoxysilane, polydimethylsiloxane, hexadecyltrimethoxysilane, and methyltriethoxysilane, with a concentration of 1-5 v / v%; The vegetable oil is one or more of olive oil, soybean oil, and sesame oil, with a concentration of 0.5-2 v / v%; The solvent is one of dichloromethane, acetone, and trichloroethane; The drying is carried out by nitrogen drying for 6-12 hours at a temperature of 25-30°C.

4. The method for preparing the novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions according to claim 1, characterized in that: In step 3), the size of the nano silver particles is 1-5 nanometers, and the purity is above 99.99%.

5. The method for preparing the novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions according to claim 1, characterized in that: During the vacuum cold gas dynamic spraying process, the vacuum degree is greater than 5Pa, the spraying pressure is 0.5-1MPa, nitrogen is used as the working gas, the spraying distance is 20-45mm, the temperature is 60-80℃, and the cycle scanning spraying mode is adopted, and the cycle spraying is repeated 2-3 times; The gas flushing uses nitrogen, the gas flushing pressure is 0.3-0.5MPa, and the flushing time is 5-15min.

6. The method for preparing the novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions according to claim 1, characterized in that: In step 4), aluminum foil is used as the packaging material for light-proof packaging, and vacuum is applied during packaging.

7. A novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions, characterized in that: The method is adopted as claimed in any one of claims 1 to 6.

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