A novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions and its preparation method

Abstract

The present invention discloses a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions and a preparation method thereof. The specific preparation steps are: 1) the gauze is immersed in a graphene oxide solution, then rinsed and dried; a first layer of strengthening layer structure is formed on the surface of the gauze; 2) the gauze forming the first layer of strengthening layer structure is immersed in a stearic acid / organic silicon emulsion / vegetable oil mixed solution for hydrophobic modification to form a second layer of waterproof layer structure; 3) cold gas dynamic spraying is performed on the surface of the gauze to deposit nano silver particles to form a third layer of antibacterial layer structure; 4) it is light-proof packaged and irradiated and sterilized to obtain a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions, and the side with the silver coating is in direct contact with the wound during use. The gauze material of the present invention can achieve efficient prevention and treatment of wound infection, and the hydrophobic coating can effectively block external water and ensure breathability, which has important clinical significance for wound treatment.

Description

Technical Field

[0001] The present 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 a crucial emergency treatment measure at the scene of trauma. Timely and correct bandaging can achieve the goals of hemostasis, infection reduction, wound protection, pain relief, and the fixation of dressings and splints. Proper bandaging requires more than just technical skill. If the bandaging material possesses a certain degree of bioactivity, it can positively impact wound treatment, particularly infection and wound ulceration.

[0003] Currently, some wound dressings and gauze with anti-infection properties are commercially available. However, their complex manufacturing processes, suboptimal efficacy, and airtightness due to their multi-layered structures significantly limit their clinical use, resulting in less than satisfactory wound treatment outcomes. Furthermore, when using a dressing or gauze, patients inevitably come into contact with liquids such as water. Once exposed to liquids, the dressing or gauze itself has a certain water absorption capacity, which can directly contaminate the wound and worsen the patient's condition.

[0004] Therefore, to address the problems of existing gauze materials, such as poor antibacterial efficacy, poor air permeability, and lack of waterproofness, the present invention provides a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions and a method for preparing the same. Through a multi-step combined process, a reinforcing layer, a waterproof layer, and an antibacterial layer are sequentially introduced onto the surface of the gauze without affecting the good air permeability of the gauze itself, providing a new solution for wound treatment and infection prevention. Summary of the Invention

[0005] The present invention aims to address the problems of traditional gauze materials being neither waterproof nor anti-infective, by providing a novel composite multi-layer breathable gauze material with both waterproof and anti-infective properties and a method for preparing the same. This novel composite multi-layer breathable gauze material can effectively prevent and treat wound infections, with its hydrophobic coating effectively blocking external water while ensuring breathability, thus having 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 with both waterproof and anti-infection functions comprises the following steps:

[0008] 1) dipping the gauze in a graphene oxide (GO) solution, then rinsing and drying, and performing a dipping-rinsing-drying cycle several times to form a first reinforcement layer structure on the gauze surface;

[0009] 2) Dipping the gauze forming the first reinforcing layer into a stearic acid / organic silicone emulsion / vegetable oil mixed solution for hydrophobic modification, and after drying, forming a second waterproof layer structure, which is then flatly fixed on the template, ensuring 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 facing 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 material 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] Furthermore, in step 1), in the GO solution, the size of GO is 2-5 microns, the solution concentration is 0.05-0.1 wt %, the immersion time is 3-10 min, 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 30-60 minutes;

[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 using nitrogen drying for 6-12 hours at a temperature of 25-30°C.

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

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

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

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

[0025] A novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions is obtained by using 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 a combination process of cyclic impregnation-rinsing-drying, vacuum cold gas dynamic spraying, and nitrogen flushing to produce a novel 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 the GO on the gauze surface, the ordinary gauze is enhanced, laying a solid physical foundation for the subsequent vacuum cold gas dynamic spraying to introduce the nanosilver antibacterial layer; the second waterproof layer is made of a variety of raw materials with hydrophobic properties and high biocompatibility, including stearic acid, silicone emulsion, and vegetable oil. By 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 nanosilver layer. By vacuum cold gas dynamic spraying of nanosilver on the reinforcing layer, the physical embedding of nanosilver on the gauze surface is achieved, and the nanosilver that is not firmly bound to the surface 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, by circulating impregnation-rinsing-drying process, introduce strengthening layer as basis on gauze surface, and further in conjunction with vacuum cold gas power spraying nano silver antibacterial layer structure, successfully give gauze excellent infection prevention and control function. Because common gauze is not resistant to high temperatures, therefore can't use methods such as PVD or CVD to introduce antibacterial coating, and if use technology such as chemical reduction, then can introduce reducing agent in gauze, thereby bring biotoxicity, therefore in conjunction with the characteristics of gauze in the present invention, and meticulously design gentle processing parameter and build GO strengthening layer (by the physical protection barrier effect of GO, prevent that vacuum cold gas power spraying operation makes gauze break and damage), successfully by vacuum cold gas power spraying technology not destroying gauze mechanical property, and vacuum condition ensures on the basis that nano silver does not oxidize, by nitrogen, nano silver is sprayed onto gauze surface, make gauze surface occur strong plastic deformation and deposit and form coating, and utilize nitrogen flushing technology, rinse off in conjunction with loose nano silver particles, prevent that later stage gauze from nano silver coming off in use, finally successfully build antibacterial layer structure, give gauze with excellent infection prevention and control function. 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) novel composite gauze in the present invention has breathable, anti-infection, waterproof and water-absorbing function simultaneously. In the present invention, by introducing multiple raw materials with hydrophobic properties and high biocompatibility such as stearic acid, organosilicon emulsion, vegetable oil, gauze is given excellent hydrophobicity, prevent it from being wetted and causing pollution or infection in use, vacuum cold gas power is sprayed on the surface to form the nano silver antibacterial layer of micron level, the process of spraying can wash away the hydrophobic substance on the antibacterial layer one side surface, realize the efficient prevention and treatment to infection, and ensure the water-absorbing property of antibacterial layer one side. Simultaneously because above-mentioned modification is all based on micron or nanometer scale, the structure of gauze macroscopicity is not caused to obvious change, the air permeability of gauze itself is preserved intact, ensure the good ventilation demand of wound healing, not because gauze forms closed environment thereby causes infection and the pollution of wound, there is actual 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 2This is the 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 with reference to the accompanying drawings and specific embodiments.

[0036] Example 1:

[0037] 1) First, take conventional gauze and immerse it in a 0.1 wt% GO solution (GO size 2-5 microns) for 3 minutes. After removing it, use deionized water to rinse off the free GO on the surface. After drying at 60°C for 30 minutes, the first reinforcement layer structure is formed on the surface. This immersion-rinsing-drying process is repeated three times.

[0038] 2) The gauze was immersed in a mixed solution of 0.25 v / v% stearic acid / 3 v / v% hexadecyltriethoxysilane emulsion / 2 v / v% olive oil (the solvent was dichloromethane) for hydrophobic modification. The remaining solvent was removed using nitrogen gas drying at 25°C for 12 hours to form a second waterproof layer structure. The gauze was then fixed flatly on the template, ensuring that one side of the gauze was in close contact with the template.

[0039] 3) vacuum cold gas dynamic spraying (vacuum greater than 5 Pa, spraying pressure 0.5 MPa, nitrogen as the working gas, spraying distance 25 mm, temperature 60° C., cyclic scanning spray mode, 3 cycles of spraying) was performed on the gauze surface facing away from the template to deposit nanosilver particles (nanosilver particles with a size of approximately 2-3 nanometers and a purity of 99.99%) to form a third antibacterial layer structure. After completion, nitrogen gas flushing (nitrogen gas flushing pressure 0.3 MPa, flushing time 10 minutes) was performed to remove nanosilver particles that were not firmly attached to the surface;

[0040] 4) The material is light-proofed and packaged with aluminum foil, and then 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.

[0041] The contact angle of the composite gauze surface is about 158°. Figure 2 As shown; the extract of the composite gauze material was prepared and co-cultured 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 test. The results showed that the inhibition zone area was about 3.04 cm2 ,like Figure 3 As shown; combined with the rat skin wound infection model, the surface was sprayed 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] Example 2:

[0043] 1) First, conventional gauze was hydrophobically modified by dipping it in a mixture of 0.25 v / v% stearic acid / 3 v / v% hexadecyltriethoxysilane emulsion / 2 v / v% olive oil (solvent: dichloromethane). The remaining solvent was removed by nitrogen drying at 25°C for 12 hours to form a first waterproof layer. The gauze was then flatly fixed to a template, ensuring that one side of the gauze was in close contact with the template.

[0044] 2) vacuum cold gas dynamic spraying (vacuum greater than 5 Pa, spraying pressure 0.5 MPa, nitrogen as the working gas, spraying distance 25 mm, temperature 60° C., cyclic scanning spray mode, 3 cycles of spraying) was performed on the gauze surface facing away from the template to deposit silver nanoparticles (nanosilver particles with a size of approximately 2-3 nanometers and a purity of 99.99%) to form a second antibacterial layer structure. After completion, nitrogen gas flushing (nitrogen gas flushing pressure 0.3 MPa, flushing time 10 minutes) was performed to remove nanosilver particles that were not firmly attached 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 was reduced in this embodiment. The contact angle of the composite gauze surface was about 141°. The composite gauze material was used to prepare an extract. After co-culture with endothelial cells for 7 days, CCK-8 results showed that the cell survival rate was about 87%. The composite gauze (1 cm diameter disc) was subjected to an inhibition zone test, and the results showed that the inhibition zone area was about 3.27 cm. 2 Combined with the rat skin wound infection model, the surface was sprayed 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] Example 3:

[0048] 1) Conventional gauze was hydrophobically modified by dipping it in a mixture of 0.25 v / v% stearic acid / 3 v / v% hexadecyltriethoxysilane emulsion / 2 v / v% olive oil (solvent: dichloromethane). The remaining solvent was removed by nitrogen drying at 25°C for 12 hours to form a waterproof layer. The gauze was then flatly fixed to a mold, ensuring that one side of the gauze was in close contact with the mold.

[0049] 2) The composite gauze material is packaged and sterilized by irradiation to obtain a new type of composite gauze material with waterproof function.

[0050] Compared with Example 1, the GO reinforcement 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-cultured 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 test, 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] Example 4:

[0052] 1) First, take conventional gauze and immerse it in a 0.1 wt% GO solution (size 2-5 microns) for 3 minutes. After removing it, use deionized water to rinse off the free GO on the surface. After drying at 60°C for 30 minutes, the first reinforcement layer structure is formed on the surface. This immersion-rinsing-drying process is repeated three times.

[0053] 2) vacuum cold gas dynamic spraying (vacuum greater than 5 Pa, spraying pressure 0.5 MPa, nitrogen as the working gas, spraying distance 25 mm, temperature 60° C., cyclic scanning spray mode, 3 cycles of spraying) was performed on the gauze surface facing away from the template to deposit silver nanoparticles (nanosilver particles of approximately 2-3 nm in size and 99.99% purity) to form an antibacterial layer structure. After completion, nitrogen gas flushing (nitrogen gas flushing pressure 0.3 MPa, flushing time 10 minutes) was performed to remove nanosilver particles that were not firmly attached to the surface;

[0054] 3) 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 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, this embodiment reduces the waterproof layer. The contact angle of the composite gauze surface was about 18°. The composite gauze material was used to prepare an extract. After co-culture with endothelial cells for 7 days, CCK-8 results showed that the cell survival rate was about 90%. The composite gauze (1 cm diameter disc) was subjected to an inhibition zone test, and the results showed that the inhibition zone area was about 3.48 cm. 2 Combined with the rat skin wound infection model, the surface was sprayed with water at 0.5 ml / cm on day 1. 2 , 3 days later, the skin became severely infected and accompanied by ulceration symptoms.

Claims

1. A method for preparing a novel composite multi-layer breathable gauze material with both waterproof and anti-infection functions, characterized in that: The following steps are involved: 1) Immerse the gauze in graphene oxide (GO) solution, then rinse and dry; After the dipping-rinsing-drying process is cycled several times, a first strengthening layer structure is formed on the surface of the gauze; 2) Dipping the gauze forming the first reinforcing layer into a stearic acid / organic silicone emulsion / vegetable oil mixed solution for hydrophobic modification, and after drying, forming a second waterproof layer structure, which is then flatly fixed on the template, ensuring 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 facing 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 novel 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 0.05-0.1 wt %, the solvent is deionized water, and the immersion time is 3-10 min; The rinsing is performed with deionized water; During the drying process, the drying temperature is 50-60°C and the time is 30-60 minutes; 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) the stearic acid / organic silicone emulsion / vegetable oil mixed solution has a stearic acid concentration of 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 using 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 nanosilver 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 cyclic scanning spraying mode is adopted, and the spraying cycle is 2-3 times; The gas flushing uses nitrogen, the gas flushing pressure is 0.3-0.5 MPa, and the flushing time is 5-15 minutes.

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 as described in any one of claims 1 to 6.

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