Antibacterial durable silk quilt and preparation method thereof

Abstract

The invention belongs to the technical field of silk products, and particularly relates to an antibacterial durable silk quilt and a preparation method thereof. The antibacterial durable silk quilt is prepared from the following raw materials in parts by weight: 60 to 70 parts of mulberry silk, 25 to 35 parts of filler, 3 to 5 parts of chitosan and 0.5 to 1 part of lavender essential oil. The filler is prepared from HAP, poplar powder and an AgNO3 solution through the steps of pretreatment, composite forming and the like, silver ions released by Ag-HAP can directly destroy bacterial structures, the porous structure of carbonized pine powder can adsorb bacteria and metabolites thereof, after the bacteria are killed by the silver ions, the carbonized pine powder quickly adsorbs residues, and secondary pollution caused by dead bacteria decomposition is avoided; ag-HAP and carbonized poplar powder are stably combined by a silane coupling agent through chemical bonds, so that rapid loss of silver ions is avoided, it is ensured that an adsorption channel of carbonized pine powder is not blocked, and the antibacterial property is kept stable in long-term use.

Description

Technical Field

[0001] The invention belongs to the technical field of silk products, and particularly relates to an antibacterial and durable silk quilt and a preparation method thereof. Background Art

[0002] As a high-end home textile product, silk quilts are highly sought after by consumers due to the silk fiber's natural lightness, softness, breathability, and skin-friendly properties. The natural sericin and amino acids contained in silk not only provide a comfortable sleep experience but also have certain moisturizing and skin-care benefits. Therefore, they are widely used in various settings, such as homes and hotels. However, traditional silk quilts still face some urgent problems during long-term use. On the one hand, although silk fiber itself has certain natural antibacterial properties, these antibacterial effects gradually weaken in humid environments or after long-term use, making it easy for bacteria, mold, and other microorganisms to grow. This can cause the silk quilt to develop an unpleasant odor, mildew, and even cause health problems such as skin allergies. This problem is particularly prominent in humid southern regions or during the rainy season.

[0003] While some existing technologies have attempted to enhance the performance of silk quilts by adding antimicrobial agents or improving the weaving process, most suffer from issues such as the easy loss of antimicrobial agents, which can affect the natural properties of silk, or complex and costly processes. Therefore, developing a silk quilt and its preparation method that combines high-efficiency, long-lasting antimicrobial properties with excellent durability without compromising the natural advantages of silk has become an important research direction in the home textile field, with significant practical application value. Summary of the Invention

[0004] In response to the deficiencies in the prior art, the present invention provides an antibacterial and durable silk quilt and a preparation method thereof; wherein, the raw material filler for the preparation of the antibacterial and durable silk quilt is prepared from HAP, poplar wood powder and AgNO3 through the steps of pretreatment, composite molding, etc., the silver ions released by Ag-HAP can directly destroy the bacterial structure, and the porous structure of the carbonized pine wood powder can adsorb bacteria and their metabolites, and after the silver ions kill the bacteria, the carbonized pine wood powder quickly adsorbs the residues to avoid secondary pollution caused by the decomposition of dead bacteria; the silane coupling agent stably combines Ag-HAP and carbonized pine wood powder through chemical bonds, which not only avoids the rapid loss of silver ions, but also ensures that the adsorption channel of the carbonized pine wood powder is not blocked, so that the antibacterial performance remains stable during long-term use, not only achieves efficient inhibition of common bacteria, improves the mechanical properties and washing resistance of the silk quilt, but also balances the antibacterial property and skin-friendliness, prolongs the duration of the tranquilizing effect, solves the problems of traditional silk quilts such as weak antibacterial properties, easy breakage, single function and insufficient skin-friendliness, and has significant technical advantages and practical value.

[0005] The present invention provides an antibacterial and durable silk quilt, which comprises the following raw materials in parts by weight: 60-70 parts of mulberry silk, 25-35 parts of filler, 3-5 parts of chitosan, 1-2 parts of hyaluronic acid, and 0.5-1 part of lavender essential oil; The filler includes the following raw materials: HAP (hydroxyapatite), poplar wood powder, pine wood powder and AgNO3 solution; The preparation method of the filler comprises the following preparation steps: (1) Poplar wood powder was taken, passed through a 100-mesh sieve, washed with deionized water to remove impurities, and vacuum-dried at 60 °C to form pretreated poplar wood powder. The pretreated poplar wood powder was added to a 4% sulfuric acid solution, stirred in a constant temperature water bath at 45 °C for 2 h, centrifuged, washed until neutral, and then subjected to high-pressure homogenization circulation treatment to obtain a nanocellulose suspension; (2) HAP was dispersed in a 0.1 mol / L AgNO3 solution at a ratio of 1 g HAP to 100 mL. The mixture was stirred in the dark for 24 h, and the precipitate was collected by centrifugation and dried in vacuo to obtain Ag-HAP powder. (3) Take pine wood powder, place it in a tube furnace, introduce nitrogen to exclude air, heat it to 300 °C at a heating rate of 5 °C / min at room temperature, keep it warm for 2 h for pyrolysis, cool it naturally to room temperature, pass it through a 200-mesh sieve, soak it in 10% hydrochloric acid for 2 h to remove ash, wash it with deionized water until it is neutral, and dry it at 60 °C to obtain carbonized pine wood powder; (4) Nanocellulose suspension, Ag-HAP powder and carbonized pine wood powder were mixed in a mass ratio of 5:3:2 to form a mixture. Silane coupling agent KH-570 was added at 1% of the total mass of the mixture. The mixture was ultrasonically dispersed for 30 min and then freeze-dried. The mixture was hot-pressed at 80 °C with a pressure of 0.1 MPa for 10 min to obtain a filler.

[0006] The present invention also provides a method for preparing an antibacterial and durable silk quilt, which specifically comprises the following preparation steps: S1, degumming of mulberry silk: immersing the mulberry silk in an aqueous solution containing 0.5% Na2CO3 and 0.1% neutral protease at a bath ratio of 1:30, stirring, and treating at a constant temperature of 85°C for 1 h, rinsing with deionized water until neutral, vacuum drying at 60°C for 4 h, and mechanically opening to obtain degummed mulberry silk; S2, cross-linking of mulberry silk fibers: a 5% PEGDA (polyethylene glycol diacrylate) aqueous solution was prepared, and a 0.5% photoinitiator Irgacure 2959 was added to form a photocrosslinking solution. The degummed mulberry silk was immersed in the photocrosslinking solution for 10 min, irradiated with 365 nm UV light for 10 min, and dried at 60°C for curing to obtain pretreated mulberry silk. S3, essential oil composite spinning: β-cyclodextrin and lavender essential oil were mixed in a molar ratio of 1:1, deionized water was added, and the mixture was stirred at 40°C for 2 h. The mixture was freeze-dried to obtain an essential oil composite. The essential oil composite was then mixed with a filler in a mass ratio of 1:10 to form a mixed system. 0.1% of polyoxyethylene sorbitan monolaurate dispersant, based on the total mass of the mixed system, was added, and a composite fiber web was prepared by electrospinning. S4, finishing silk cotton: chitosan and composite fiber web were mixed in a mass ratio of 1:10, then added to a 1% acetic acid solution, stirred at 50°C for 30 minutes to form a finishing solution, the pretreated mulberry silk was immersed in the finishing solution with a bath ratio of 1:20, shaken in a constant temperature water bath at 45°C for 30 minutes, squeezed, dried at 100°C, carded into a web, cross-laid to a thickness of 5-10 cm, and hot air-set at 80°C to obtain silk cotton; S5, assemble to obtain an antibacterial and durable silk quilt: take hyaluronic acid, add deionized water to prepare a hyaluronic acid solution with a mass concentration of 3%, take mulberry silk fabric, immerse and roll it in the hyaluronic acid solution, and vacuum dry it to form a fabric, take mulberry silk and carbonized pine wood powder in a mass ratio of 9:1 to blend into a non-woven fabric, magnetron sputter a 20 nm thick TiO2 film on the surface to form a lining, sandwich silk cotton between the fabric and the lining, seal it after filling, and lightly press and shape it at 80°C to prepare an antibacterial and durable silk quilt.

[0007] Compared with the prior art, the present invention has the following beneficial effects: The present invention uses mulberry silk, fillers, lavender essential oil and other raw materials to prepare antibacterial and durable mulberry silk. The silver ions released by the Ag-HAP powder in the filler can directly destroy the bacterial structure, while the porous structure of the carbonized pine wood powder can adsorb bacteria and their metabolites. After the silver ions kill the bacteria, the carbonized pine wood powder quickly adsorbs the residue, avoiding secondary pollution caused by the decomposition of dead bacteria and effectively inhibiting drug-resistant bacteria. Compared with a single component, the antibacterial effect is more comprehensive and longer-lasting. The added silane coupling agent chemically bonds the Ag-HAP powder with the silane coupling agent. The stable combination of carbonized pine wood powder prevents the rapid loss of silver ions and ensures that the carbonized pine wood powder's adsorption channels remain unobstructed, maintaining stable antibacterial properties over long-term use. The long-chain structure of nanocellulose entangles silk fibers, providing flexible support, while the rigid particles of Ag-HAP powder and the fibrous structure of carbonized pine wood powder act as rigid nodes to disperse external impacts, allowing the silk quilt to maintain appropriate elasticity while also resisting stretching and tearing. This resolves the contradiction between traditional silk quilts being "soft but fragile, yet tough but stiff." The entanglement of nanocellulose prevents fiber slippage, the carbonized pine wood powder fills gaps and reduces voids, and the Ag-HAP particles provide enhanced local support. Together, these elements ensure that the silk quilt maintains its fluffy shape and avoids compaction even after repeated use and washing. This morphological stability far exceeds the reinforcing effect of a single component. The flexible chain segments of PEGDA are grafted onto the surface of silk through UV curing, which not only enhances the bonding strength between fibers but also retains the natural air permeability of silk. Its hydrogen bonding with chitosan can also fix the antibacterial components, and the antibacterial rate remains at a high level after multiple washings. The essential oil complex and filler are made into a fiber mesh through electrospinning. The nanofibers formed under high pressure can evenly wrap the filler and lavender essential oil inclusion complex, and its porous structure can ensure that Ag + The controlled release of essential oils and the physical constraints of the fiber network prevent the volatilization of essential oils, which significantly prolongs the retention time of the fragrance. At the same time, the entanglement of the fiber network and silk enhances the stability of the overall structure. During the preparation process, hot air setting fixes the initial shape through hydrogen bonds between fibers to avoid the inactivation of functional components caused by high temperature; the final light pressure setting promotes the fusion of the interfaces of each layer through appropriate pressure, which not only ensures the fluffiness of the silk cotton, but also enhances the bonding between the quilt shell and the filling core. The degumming treatment of mulberry silk can effectively remove impurities and retain the fiber structure; PEGDA cross-linking enhances the fiber bonding, taking into account durability and skin-friendliness; essential oil composite spinning achieves stable retention and uniform distribution of functional ingredients; the silk cotton finishing process integrates antibacterial and structural stability properties; and finally, an antibacterial and durable silk quilt is prepared, which achieves synergistic improvement in antibacterial, durability, skin-friendliness, and calming effects of the silk quilt, making it not only suitable for the general population, but also meeting the needs of special groups such as infants and sensitive skin, thus expanding the application scenarios. BRIEF DESCRIPTION OF THE DRAWINGS

[0008] Figure 1 This is a flow chart for preparing the antibacterial and durable silk quilt of the present invention; Figure 2 This is the SEM image of the filler prepared in the present invention. DETAILED DESCRIPTION

[0009] In order to enable those skilled in the art to better understand the technical solution of the present invention and to make the above-mentioned features, purposes and advantages of the present invention more clearly understood, the present invention is further described below in conjunction with examples. The examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention.

[0010] Unless otherwise defined, all technical and scientific terms used herein have the same meanings as those familiar to those skilled in the art. Furthermore, any methods and materials similar or equivalent to those described herein can be applied to the present invention. The preferred embodiments and materials described herein are for illustrative purposes only and are not intended to limit the scope of this application.

[0011] In the following examples, unless otherwise specified, conventional methods are used; the materials used in the following examples, unless otherwise specified, are all new materials purchased from the market.

[0012] according to Figure 1 The process flow chart for preparing the antibacterial and durable silk quilt of the present invention is shown, and the following examples are carried out: Example 1: This example provides an antibacterial and durable silk quilt, which comprises the following raw materials in parts by weight: 60 parts of mulberry silk, 25 parts of filler, 3 parts of chitosan, 1 part of hyaluronic acid, and 0.5 parts of lavender essential oil; The filler includes the following raw materials: HAP, poplar wood powder, pine wood powder and AgNO3 solution; The preparation method of the filler comprises the following preparation steps: (1) Take 25 parts of poplar wood powder, pass it through a 100-mesh sieve, wash it with deionized water to remove impurities, and vacuum dry it at 60 °C to form pretreated poplar wood powder. The pretreated poplar wood powder is added to a 4% sulfuric acid solution in a ratio of 1 g:10 mL. Stir in a constant temperature water bath at 45 °C for 2 h, centrifuge, wash until neutral, and then high-pressure homogenize and cycle for 5 times to obtain a nanocellulose suspension. (2) Disperse 3 portions of HAP in 0.1 mol / L AgNO3 solution at a ratio of 1 g HAP to 100 mL. Stir in dark place for 24 h, collect the precipitate by centrifugation, and dry in vacuum to obtain Ag-HAP powder. (3) Take 18 parts of pine wood powder, place them in a tube furnace, introduce nitrogen at a flow rate of 50 mL / min, exclude air, and heat to 300 °C at a heating rate of 5 °C / min at room temperature. Keep warm for 2 h for pyrolysis, cool naturally to room temperature, pass through a 200-mesh sieve, soak in 10% hydrochloric acid for 2 h to remove ash, wash with deionized water until neutral, and dry in a vacuum at 60 °C to obtain carbonized pine wood powder; (4) Nanocellulose suspension, Ag-HAP powder and carbonized pine wood powder were mixed in a mass ratio of 5:3:2 to form a mixture. Silane coupling agent KH-570 was added at 1% of the total mass of the mixture. The mixture was ultrasonically dispersed for 30 min and then freeze-dried. The mixture was hot-pressed at 80 °C with a pressure of 0.1 MPa for 10 min to obtain a filler.

[0013] This embodiment also provides a method for preparing an antibacterial and durable silk quilt, which specifically includes the following preparation steps: S1, degumming of mulberry silk: immersing the mulberry silk in an aqueous solution containing 0.5% Na2CO3 and 0.1% neutral protease at a bath ratio of 1:30, stirring, and treating at a constant temperature of 85°C for 1 h, rinsing with deionized water until neutral, vacuum drying at 60°C for 4 h, and mechanically opening to obtain degummed mulberry silk; S2, cross-linking of mulberry silk fibers: a 5% PEGDA aqueous solution was prepared, and a 0.5% photoinitiator Irgacure 2959 was added. The degummed mulberry silk was immersed in the solution for 10 min, irradiated with 365 nm UV light for 10 min, and dried at 60°C for curing to obtain pretreated mulberry silk. S3, essential oil composite spinning: β-cyclodextrin and 0.5 parts of lavender essential oil were mixed in a molar ratio of 1:1, deionized water was added, and the mixture was stirred at 40°C for 2 h. The mixture was freeze-dried to obtain an essential oil composite. The essential oil composite was then mixed with 25 parts of a filler in a mass ratio of 1:10, and 0.1% polyoxyethylene sorbitan monolaurate dispersant was added. The composite fiber web was prepared by electrospinning at a voltage of 18 kV, a receiving distance of 20 cm, and a flow rate of 0.8 mL / h. S4, finishing silk cotton: 3 parts of chitosan and composite fiber web were mixed in a mass ratio of 1:10, then added to a 1% acetic acid solution, stirred at 50°C for 30 minutes to form a finishing solution, and the pretreated mulberry silk was immersed in the finishing solution with a bath ratio of 1:20, shaken in a constant temperature water bath at 45°C for 30 minutes, squeezed out, with a squeeze rate of 70%, dried at 100°C, carded into a web, cross-laid, with a thickness of 5 cm, and hot air-set at 80°C to obtain silk cotton; S5, assemble to obtain an antibacterial and durable silk quilt: take 1 part of hyaluronic acid, add deionized water to prepare a hyaluronic acid solution with a mass concentration of 3%, take mulberry silk fabric, immerse and roll it in the hyaluronic acid solution, and vacuum dry it to form a fabric, take mulberry silk and carbonized pine wood powder in a mass ratio of 9:1 to blend into a non-woven fabric, magnetron sputter a 20 nm thick TiO2 film on the surface to form a lining, sandwich silk cotton between the fabric and the lining, fill and seal, and lightly press and shape for 2 minutes at 80°C and a pressure of 0.1 MPa to prepare an antibacterial and durable silk quilt.

[0014] Example 2: This example provides an antibacterial and durable silk quilt, which comprises the following raw materials in parts by weight: 65 parts of mulberry silk, 30 parts of filler, 4 parts of chitosan, 1.5 parts of hyaluronic acid, and 0.8 parts of lavender essential oil; The filler includes the following raw materials: HAP, poplar wood powder, pine wood powder and AgNO3 solution; The preparation method of the filler comprises the following preparation steps: (1) Take 30 parts of poplar wood powder, pass it through a 100-mesh sieve, wash it with deionized water to remove impurities, and vacuum dry it at 60 °C to form pretreated poplar wood powder. The pretreated poplar wood powder is added to a 4% sulfuric acid solution in a ratio of 1 g:15 mL. Stir in a constant temperature water bath at 45 °C for 2 h, centrifuge, wash until neutral, and then high-pressure homogenize and cycle for 5 times to obtain a nanocellulose suspension. (2) Disperse 5 portions of HAP in 0.1 mol / L AgNO3 solution, stir in the dark for 24 h, collect the precipitate by centrifugation, and vacuum dry to obtain Ag-HAP powder; (3) Take 20 parts of pine wood powder, place them in a tube furnace, introduce nitrogen at a flow rate of 50 mL / min, exclude air, and heat from room temperature to 300 °C at a heating rate of 5 °C / min, keep warm for 2 h, perform pyrolysis, cool naturally to room temperature, pass through a 200-mesh sieve, soak in 10% hydrochloric acid for 2 h to remove ash, wash with deionized water until neutral, and vacuum dry at 60 °C to obtain carbonized pine wood powder; (4) Nanocellulose suspension, Ag-HAP powder and carbonized pine wood powder were mixed in a mass ratio of 5:3:2 to form a mixture. Silane coupling agent KH-570 was added at 1% of the total mass of the mixture. The mixture was ultrasonically dispersed for 30 min and then freeze-dried. The mixture was hot-pressed at 80 °C with a pressure of 0.1 MPa for 10 min to obtain a filler.

[0015] This embodiment also provides a method for preparing an antibacterial and durable silk quilt, which specifically includes the following preparation steps: S1, degumming of mulberry silk: immersing the mulberry silk in an aqueous solution containing 0.5% Na2CO3 and 0.1% neutral protease at a bath ratio of 1:30, stirring, and treating at a constant temperature of 85°C for 1 h, rinsing with deionized water until neutral, vacuum drying at 60°C for 4 h, and mechanically opening to obtain degummed mulberry silk; S2, cross-linking of mulberry silk fibers: a 5% PEGDA aqueous solution was prepared, and a 0.5% photoinitiator Irgacure 2959 was added. The degummed mulberry silk was immersed in the solution for 10 min, irradiated with 365 nm UV light for 10 min, and dried at 60°C for curing to obtain pretreated mulberry silk. S3, essential oil composite spinning: β-cyclodextrin and 0.8 parts of lavender essential oil were mixed in a molar ratio of 1:1, deionized water was added, and the mixture was stirred at 40°C for 2 h. The mixture was freeze-dried to obtain an essential oil composite. The essential oil composite was then mixed with 30 parts of filler in a mass ratio of 1:10, and 0.1% polyoxyethylene sorbitan monolaurate dispersant was added. The composite fiber web was prepared by electrospinning at a voltage of 20 kV, a receiving distance of 22 cm, and a flow rate of 1 mL / h. S4, finishing silk cotton: 4 parts of chitosan and composite fiber web were mixed in a mass ratio of 1:10, then added to a 1% acetic acid solution, stirred at 50°C for 30 minutes to form a finishing solution, and the pretreated mulberry silk was immersed in the finishing solution with a bath ratio of 1:20, shaken in a constant temperature water bath at 45°C for 30 minutes, squeezed out, and the squeeze rate was 75%. The silk was dried at 100°C, carded into a web, cross-laid, and 8 cm thick. The silk was hot-air-set at 80°C to obtain silk cotton; S5, assemble to obtain an antibacterial and durable silk quilt: take 1.5 parts of hyaluronic acid, add deionized water to prepare a hyaluronic acid solution with a mass concentration of 3%, take mulberry silk fabric, immerse and roll it in the hyaluronic acid solution, and vacuum dry it to form a fabric, take mulberry silk and carbonized pine wood powder in a mass ratio of 9:1 to blend into a non-woven fabric, magnetron sputter a 20 nm thick TiO2 film on the surface to form a lining, sandwich silk cotton between the fabric and the lining, fill and seal, and lightly press and shape for 2 minutes at 80°C and a pressure of 0.1 MPa to prepare an antibacterial and durable silk quilt.

[0016] Example 3: This example provides an antibacterial and durable silk quilt, which comprises the following raw materials in parts by weight: 70 parts of mulberry silk, 35 parts of filler, 5 parts of chitosan, 2 parts of hyaluronic acid, and 1 part of lavender essential oil; The filler includes the following raw materials: HAP, poplar wood powder, pine wood powder and AgNO3 solution; The preparation method of the filler comprises the following preparation steps: (1) Take 30 parts of poplar wood powder, pass it through a 100-mesh sieve, wash it with deionized water to remove impurities, and vacuum dry it at 60 °C to form pretreated poplar wood powder. The pretreated poplar wood powder is added to a 4% sulfuric acid solution in a ratio of 1 g:15 mL. Stir in a constant temperature water bath at 45 °C for 2 h, centrifuge, wash until neutral, and then high-pressure homogenize and cycle for 5 times to obtain a nanocellulose suspension. (2) Disperse 3 portions of HAP in 0.1 mol / L AgNO3 solution, stir in the dark for 24 h, collect the precipitate by centrifugation, and vacuum dry to obtain Ag-HAP powder; (3) Take 18 parts of pine wood powder, place them in a tube furnace, introduce nitrogen at a flow rate of 50 mL / min, exclude air, and heat from room temperature to 300 °C at a heating rate of 5 °C / min, keep warm for 2 h, perform pyrolysis, cool naturally to room temperature, pass through a 200-mesh sieve, soak in 10% hydrochloric acid for 2 h to remove ash, wash with deionized water until neutral, and vacuum dry at 60 °C to obtain carbonized pine wood powder; (4) Nanocellulose suspension, Ag-HAP powder and carbonized pine wood powder were mixed in a mass ratio of 5:3:2 to form a mixture. Silane coupling agent KH-570 was added at 1% of the total mass of the mixture. The mixture was ultrasonically dispersed for 30 min and then freeze-dried. The mixture was hot-pressed at 80 °C with a pressure of 0.1 MPa for 10 min to obtain a filler.

[0017] This embodiment also provides a method for preparing an antibacterial and durable silk quilt, which specifically includes the following preparation steps: S1, degumming of mulberry silk: immersing the mulberry silk in an aqueous solution containing 0.5% Na2CO3 and 0.1% neutral protease at a bath ratio of 1:30, stirring, and treating at a constant temperature of 85°C for 1 h, rinsing with deionized water until neutral, vacuum drying at 60°C for 4 h, and mechanically opening to obtain degummed mulberry silk; S2, cross-linking of mulberry silk fibers: a 5% PEGDA aqueous solution was prepared, and a 0.5% photoinitiator Irgacure 2959 was added. The degummed mulberry silk was immersed in the solution for 10 min, irradiated with 365 nm UV light for 10 min, and dried at 60°C for curing to obtain pretreated mulberry silk. S3, essential oil composite spinning: β-cyclodextrin and 1 part of lavender essential oil were mixed in a molar ratio of 1:1, deionized water was added, and the mixture was stirred at 40°C for 2 h. The mixture was freeze-dried to obtain an essential oil composite. The essential oil composite was then mixed with 35 parts of filler in a mass ratio of 1:10, and 0.1% polyoxyethylene sorbitan monolaurate dispersant was added. The composite fiber web was prepared by electrospinning at a voltage of 20 kV, a receiving distance of 20 cm, and a flow rate of 0.8 mL / h. S4, finishing silk cotton: take 5 parts of chitosan and composite fiber web in a mass ratio of 1:10, then add it to a 1% acetic acid solution, stir at 50 ° C for 30 minutes to form a finishing solution, immerse the pretreated mulberry silk in the finishing solution with a bath ratio of 1:20, shake in a constant temperature water bath at 45 ° C for 30 minutes, squeeze the solution to a squeeze rate of 80%, dry at 100 ° C, card it into a web, cross-ply it to a thickness of 5-10 cm, and set it with hot air at 80 ° C to obtain silk cotton; S5, assemble to obtain an antibacterial and durable silk quilt: take 2 parts of hyaluronic acid, add deionized water to prepare a hyaluronic acid solution with a mass concentration of 3%, take mulberry silk fabric, immerse and roll it in the hyaluronic acid solution, and vacuum dry it to form a fabric, take mulberry silk and carbonized pine wood powder in a mass ratio of 9:1 to blend into a non-woven fabric, magnetron sputter a 20 nm thick TiO2 film on the surface to form a lining, sandwich silk cotton between the fabric and the lining, fill and seal, and lightly press and shape for 2 minutes at 80°C and a pressure of 0.1 MPa to prepare an antibacterial and durable silk quilt.

[0018] The difference between Comparative Example 1 and Example 1 is that the addition of the filler is omitted, and the rest is exactly the same as Example 1.

[0019] The difference between Comparative Example 2 and Example 1 is that the addition of lavender essential oil is cancelled, and the rest is exactly the same as Example 1.

[0020] The difference between Comparative Example 3 and Example 1 is that the addition of PEGDA is omitted, and the rest is exactly the same as Example 1.

[0021] Experimental example 1. Antibacterial rate test: According to GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method", the antibacterial and durable silk quilts prepared in Examples 1-3 of the present invention and Comparative Examples 1-3 were used as samples to measure the antibacterial rates of Escherichia coli (ATCC25922), Staphylococcus aureus (ATCC6538), and Candida albicans (ATCC10231). The results are recorded in Table 1.

[0022] 2. Breaking strength test: According to GB / T3916-2013 "Determination of breaking strength and breaking elongation of single yarn in textile package yarn", the durable silk quilts prepared in Examples 1-3 and Comparative Examples 1-3 of the present invention are used as samples to test the breaking strength of the samples; debug the tensile testing machine, set the appropriate clamping distance and stretching speed, and ensure that the instrument is in normal working condition. Clamp the two ends of the sample in the upper and lower clamps of the testing machine respectively, so that the axis of the sample is consistent with the clamping line, start the instrument to stretch until the sample breaks, and record the maximum breaking strength value. Carry out multiple tests in the warp and weft directions respectively, take the average value as the final result, and observe the fracture position of the sample. If it breaks in the clamping area, the data is invalid and needs to be retested. The results are recorded in Table 1.

[0023] Table 1

[0024] The results in Table 1 show that the antibacterial rates of Examples 1-3 against the three bacteria are all between 97.9% and 99.9%, especially against Escherichia coli and Staphylococcus aureus, the antibacterial rates are mostly between 99.8% and 99.9%, indicating that the antibacterial and durable silk quilts prepared by the present invention can effectively inhibit common pathogens, and have excellent and stable antibacterial effects; the mechanical properties of the examples are excellent: the breaking strength of Examples 1-3 is 4.3-4.5 cN / dtex, indicating that the antibacterial and durable silk quilts prepared by the present invention, while ensuring antibacterial properties, have good mechanical support through the synergy of raw materials, are not easy to break or deform, and are highly durable.

[0025] 3. Abrasion resistance test: According to GB / T21196.3-2007, the durable silk quilts prepared in Examples 1-3 of the present invention and Comparative Examples 1-3 were used as samples to carry out a Martindale abrasion test to test the wear resistance of the samples. The test was carried out using a Martindale abrasion tester. After the samples were rubbed 1200 times under a pressure of 5 kPa, there was no obvious pilling on the surface (pilling level ≥ level 4) and no fiber shedding (mass loss rate ≤ 2%), which is better than the 500-times standard of ordinary silk quilts.

[0026] 4. Preparation of the test solution for washing resistance: According to the requirements of AATCC 61-2013 Method 2A, add the specified amount of powdered or liquid detergent to deionized water, stir to dissolve, and preheat to the specified temperature to form a washing solution. For specimen preparation, cut a specimen of specified size from the shell or filling layer of a silk quilt and combine it with a multi-fiber adjacent fabric. The two are sewn or fixed in close contact, ensuring that the adjacent fabric fibers are aligned parallel to the specimen edges. Place the combined specimen in a stainless steel container, add the preheated detergent solution and the specified number of stainless steel beads, tightly cap the container, and secure it to a washing machine, running at the set temperature and time. After washing, remove the specimen, rinse it with warm water several times to remove residual detergent, dehydrate it, and then dry it at the specified temperature or air dry it. The dried specimen is conditioned under standard conditions and the discoloration level is assessed compared to the original specimen. The staining of the adjacent fabric is also evaluated. The antimicrobial retention after 50 washes is recorded in Table 1.

[0027] 5. Fluffiness test: According to the standard of GB / T 24218.3-2010, the antibacterial and durable silk quilts prepared in Examples 1-3 of the present invention and Comparative Examples 1-3 are used as sample silk quilts. An appropriate amount of filling cotton sample is removed from the sample silk quilt, impurities and lumps are removed, and the quilt is placed in a standard temperature and humidity environment for a period of time to adjust the humidity. Check whether the cylinder, pressure plate and other components of the fluffiness tester are clean, and calibrate the pressure and volume measurement system of the instrument. Place the conditioned sample into the test cylinder and gently comb it to distribute it naturally to avoid artificial compaction. Lower the pressure plate, apply the specified pressure and maintain it for a certain period of time, and record the volume data at this time. Based on the measured volume and sample mass, calculate the volume value per unit mass as the fluffiness index. Repeat the test multiple times and take the average value. The results are recorded in Table 2.

[0028] Table 2

[0029] The results in Table 2 show that the wear resistance of Examples 1-3 reaches level 4-5, indicating that the antibacterial and durable silk quilts prepared by the present invention are not easy to pilling after friction, have less fiber shedding, and are wear-resistant and durable. However, due to the lack of fillers, the fibers of the comparative example are easily worn and shed; the washing resistance of Examples 1-3 reaches 96.2%, indicating that after multiple washings, the antibacterial and durable silk quilts prepared by the present invention still have excellent antibacterial properties and strong resistance to water washing loss; the bulkiness data of Examples 1-3 reaches 405-420 cm 3 / g, indicating that the present invention, through the support of filling materials and process optimization, allows the silk quilt to remain fluffy and warm and comfortable after washing.

[0030] Figure 2The SEM image of the filler prepared by the present invention shows a filamentous interwoven structure that is entangled with each other to form a network structure. Combined with the preparation process of the present invention, a fluffy, antibacterial and durable silk quilt is produced.

[0031] In summary, the present invention has achieved a performance leap in antibacterial and durable silk quilts through scientific raw material ratios and process design. The core of the invention lies in the synergistic effect of fillers, β-cyclodextrin and PEGDA. It not only forms a high-efficiency antibacterial system through the combination of Ag-HAP and carbonized pine wood powder, but also enhances the mechanical properties with the support of nanocellulose and carbonized pine wood powder, solving the problem of weak antibacterial and easy breakage of traditional silk quilts; β-cyclodextrin stabilizes lavender essential oil through inclusion complexation, prolonging the calming effect while assisting in antibacterial properties, taking into account both function and user experience; PEGDA cross-linking modification builds flexible connections for silk fibers, improves breaking strength and washability, and balances skin-friendliness and durability, making the product a comprehensive breakthrough in antibacterial performance, mechanical strength, functional retention, etc., showing significant technical advantages and creativity, and providing an efficient and feasible solution for the preparation of antibacterial and durable silk quilts.

[0032] The present invention and its embodiments are described above. Such description is not restrictive. The drawings show only one embodiment of the present invention, and actual applications are not limited thereto. In short, if a person skilled in the art is inspired by the above, and does not deviate from the purpose of the present invention, any method and embodiment similar to the technical solution without creative design shall fall within the scope of protection of the present invention.

Claims

1. A method for preparing an antibacterial and durable silk quilt, characterized in that: Specifically comprising the following preparation steps: S1, degumming mulberry silk: immersing the mulberry silk in an aqueous solution, stirring, constant temperature treatment, washing until neutral, drying, and mechanically opening to obtain degummed mulberry silk; S2, cross-linking of silk fibers: taking a light cross-linking treatment solution, immersing the degummed mulberry silk in the solution, performing an immersion treatment, irradiating the solution with ultraviolet light, and drying the solution to obtain pretreated mulberry silk; S3, essential oil composite spinning: β-cyclodextrin and lavender essential oil are mixed, deionized water is added, stirred, and freeze-dried to obtain an essential oil composite, a filler is mixed with the essential oil composite to form a mixed system, a dispersant is added, and a composite fiber web is produced by electrospinning; S4, finishing the silk cotton: chitosan and the composite fiber web are added to an acetic acid solution and stirred to form a finishing solution, the pretreated mulberry silk is immersed in the finishing solution, shaken in a constant temperature water bath, squeezed, dried, carded into a web, cross-laid, and hot-air-set to obtain the silk cotton; S5, assembling an antibacterial and durable silk quilt: sandwiching silk cotton between the outer fabric and the lining, sealing after filling, and lightly pressing to shape, thereby preparing an antibacterial and durable silk quilt.

2. The method for preparing an antibacterial and durable silk quilt according to claim 1, characterized in that: In step S1, the aqueous solution is an aqueous solution containing a mass concentration of 0.5% Na2CO3 and a mass concentration of 0.1% neutral protease; the bath ratio of the mulberry silk and the aqueous solution is 1:

30.

3. The method for preparing an antibacterial and durable silk quilt according to claim 1, characterized in that: In step S3, the molar ratio of the β-cyclodextrin and the lavender essential oil is 1:1; the mass ratio of the essential oil complex to the filler is 1:10; and the dispersant is polyoxyethylene sorbitan monolaurate.

4. The method for preparing an antibacterial and durable silk quilt according to claim 1, characterized in that: In step S4, the mass ratio of the chitosan to the composite fiber web is 1:10; and the bath ratio of the pretreated mulberry silk to the finishing liquid is 1:

20.

5. The method for preparing an antibacterial and durable silk quilt according to claim 1, characterized in that: The antibacterial and durable silk quilt comprises the following raw materials in parts by weight: 60-70 parts of mulberry silk, 25-35 parts of filler, 3-5 parts of chitosan, 1-2 parts of hyaluronic acid, 0.5-1 part of lavender essential oil, and 0.5-1 part of sodium alginate; The filler includes the following raw materials: HAP, poplar wood powder, pine wood powder and AgNO3 solution; The preparation method of the filler comprises the following preparation steps: (1) Taking poplar wood powder, sieving, washing, and drying to form pretreated poplar wood powder, adding the pretreated poplar wood powder to a sulfuric acid solution, stirring in a constant temperature water bath, centrifuging, washing until neutral, and then high-pressure homogenization to obtain a nanocellulose suspension; (2) Disperse HAP in AgNO3 solution, stir in the dark, centrifuge, and dry to obtain Ag-HAP powder; (3) Take pine wood powder, introduce nitrogen, perform pyrolysis, cool, sieve, soak with hydrochloric acid, wash until neutral, and dry to obtain carbonized pine wood powder; (4) Nanocellulose suspension, Ag-HAP powder and carbonized pine wood powder were mixed, silane coupling agent KH-570 was added, ultrasonic dispersion was performed, and then freeze-dried and hot-pressed to obtain a filler.

6. The method for preparing an antibacterial and durable silk quilt according to claim 5, characterized in that: In step (2), the usage ratio of HAP and AgNO3 solution is 1 g:100 mL; in step (4), the mass ratio of the nanocellulose suspension, Ag-HAP powder and carbonized pine wood powder is 5:3:2.

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