Antibacterial durable silk quilt and preparation method thereof

Abstract

The application belongs to the technical field of silk products, and particularly relates to an antibacterial durable silk quilt and a preparation method thereof; wherein the antibacterial durable silk quilt comprises the following raw materials in parts by weight: mulberry silk 60-70 parts, filling 25-35 parts, chitosan 3-5 parts, and lavender essential oil 0.5-1 part; the filling is prepared through the steps of pretreatment, composite molding and the like of HAP, poplar powder and AgNO3 solution; silver ions released by Ag-HAP can directly destroy the structure of bacteria, and the porous structure of carbonized pine powder can adsorb bacteria and their metabolites; after the silver ions kill the bacteria, the carbonized pine powder rapidly adsorbs the residues to avoid secondary pollution caused by decomposition of dead bacteria; the silane coupling agent stably combines Ag-HAP and carbonized pine powder through a chemical bond, which not only avoids rapid loss of silver ions, but also ensures that the adsorption channels of the carbonized pine powder are not blocked, so that the antibacterial performance remains stable in long-term use.

Description

TECHNICAL FIELD

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

[0002] As a high-end home textile product, the silk quilt is favored by consumers in the market due to the natural lightness, softness, air permeability and skin-friendly properties of silk fibers. The natural sericin protein and amino acids contained in silk can not only provide a comfortable sleep experience for the human body, but also have certain moisturizing and skin care effects, and are therefore widely used in various scenes such as homes and hotels. However, there are still some problems to be solved in the long-term use of traditional silk quilts. On the one hand, although silk fibers have certain natural antibacterial properties, their antibacterial effect will gradually weaken in a humid environment or after long-term use, and bacteria, mold and other microorganisms are easy to breed, resulting in peculiar smell, mold of the silk quilt, and even possible health problems such as skin allergy, especially in humid areas or plum rain season in the south.

[0003] In the prior art, although some attempts have been made to add antibacterial agents or improve the weaving process to improve the performance of the silk quilt, most of them have problems such as easy loss of antibacterial agents, affecting the natural properties of silk, or complex process, high cost, etc. Therefore, developing a silk quilt and a preparation method thereof which can simultaneously consider efficient and durable antibacterial performance and excellent durability without damaging the natural advantages of silk has become an important research direction in the current home textile field, and has significant practical application value. SUMMARY

[0004] In view of the deficiencies of the prior art, the present application provides an antibacterial and durable silk quilt and a preparation method thereof. The preparation raw material filler of the antibacterial and durable silk quilt is prepared from HAP, poplar powder and AgNO3 through pretreatment, composite molding and other steps. The silver ions released by Ag-HAP can directly destroy the structure of bacteria, and the porous structure of carbonized pine powder can adsorb bacteria and their metabolites. After the silver ions kill the bacteria, the carbonized pine powder rapidly 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 powder through chemical bonds, which not only avoids the rapid loss of silver ions, but also ensures that the adsorption channels of carbonized pine powder are not blocked, so that the antibacterial performance remains stable in long-term use. Not only does it achieve efficient inhibition of common bacteria, improve 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 weak antibacterial property, easy breakage, single function and insufficient skin-friendliness of traditional silk quilts, and has significant technical advantages and practical value.

[0005] The application provides an antibacterial durable silk quilt, which comprises the following raw materials in parts by weight: 60-70 parts of mulberry silk, 25-35 parts of filling, 3-5 parts of chitosan, 1-2 parts of hyaluronic acid and 0.5-1 part of lavender essential oil.

[0006] The filling comprises the following raw materials: HAP (hydroxyapatite), poplar powder, pine powder and AgNO3 solution.

[0007] The preparation method of the filling comprises the following preparation steps:

[0008] (1) poplar powder is taken, impurities are removed by washing with deionized water, vacuum drying is carried out at 60 DEG C, pretreated poplar powder is added into a sulfuric acid solution with a mass concentration of 4%, constant temperature water bath stirring is carried out at 45 DEG C for 2 hours, centrifugal washing is carried out until neutral, and high-pressure homogenization circulation treatment is carried out, so that nanocellulose suspension is obtained;

[0009] (2) HAP is taken and dispersed in 0.1 mol / L AgNO3 solution, the dosage ratio of HAP and AgNO3 solution is 1 g:100 mL, stirring is carried out in the dark for 24 hours, the precipitate is collected by centrifugation, vacuum drying is carried out, and Ag-HAP powder is obtained;

[0010] (3) pine powder is taken, nitrogen is introduced into a tube furnace to remove air, the temperature is raised to 300 DEG C at a temperature rising rate of 5 DEG C / min under room temperature, pyrolysis is carried out for 2 hours, natural cooling is carried out to room temperature, the pine powder is sieved through a 200-mesh screen, 10% hydrochloric acid is used for soaking for 2 hours to remove ash, deionized water is used for washing until neutral, and drying is carried out at 60 DEG C, so that carbonized pine powder is obtained;

[0011] (4) the nanocellulose suspension, the Ag-HAP powder and the carbonized pine powder are mixed according to a mass ratio of 5:3:2, 1% of silane coupling agent KH-570 is added to the total mass of the mixture, ultrasonic dispersion is carried out for 30 minutes, then freeze-drying is carried out, hot-pressing is carried out at 80 DEG C, the pressure is 0.1 MPa, and the time is 10 minutes, so that the filling is obtained.

[0012] The application further provides a preparation method of the antibacterial durable silk quilt, and specifically comprises the following preparation steps:

[0013] S1, degumming of mulberry silk: the mulberry silk is immersed into an aqueous solution containing 0.5% of Na2CO3 and 0.1% of neutral protease, the bath ratio of the mulberry silk and the aqueous solution is 1:30, stirring is carried out, constant temperature treatment is carried out at 85 DEG C for 1 hour, deionized water is used for washing until neutral, vacuum drying is carried out at 60 DEG C for 4 hours, and mechanical opening treatment is carried out, so that degummed mulberry silk is obtained;

[0014] S2, crosslinking of silk fibers: a PEGDA (polyethylene glycol diacrylate) aqueous solution with a mass concentration of 5% is prepared, 0.5% of a photoinitiator Irgacure 2959 is added to form a photocrosslinking treatment solution, the degummed silk is immersed in the photocrosslinking treatment solution, 10 min of immersion, 10 min of 365 nm ultraviolet light irradiation, and 60 DEG C drying and curing to obtain pretreated silk;

[0015] S3, essential oil composite spinning: beta-cyclodextrin and lavender essential oil are mixed according to a molar ratio of 1:1, deionized water is added, stirring is carried out at 40 DEG C for 2 h, and freeze-drying is carried out to obtain an essential oil composite, the essential oil composite is mixed with a filler according to a mass ratio of 1:10 to form a mixed system, 0.1% of a polyoxyethylene sorbitan monolaurate dispersant is added to the mixed system, and an electrospinning process is used to prepare a composite fiber web;

[0016] S4, finishing silk cotton: chitosan and the composite fiber web are mixed according to a mass ratio of 1:10, and then added to an acetic acid solution with a mass concentration of 1%, stirring is carried out at 50 DEG C for 30 min to form a finishing liquid, the pretreated silk is immersed in the finishing liquid, a bath ratio of 1:20 is used, constant temperature water bath oscillation is carried out at 45 DEG C for 30 min, liquid squeezing is carried out, 100 DEG C drying is carried out, webbing is carried out, cross-laying is carried out, a thickness of 5-10 cm is obtained, and hot air setting is carried out at 80 DEG C to obtain silk cotton;

[0017] S5, assembling an antibacterial and durable silk quilt: hyaluronic acid is added to deionized water to prepare a hyaluronic acid solution with a mass concentration of 3%, silk fabric is obtained, the silk fabric is immersed and padded in the hyaluronic acid solution, vacuum drying is carried out to form a shell fabric, silk and carbonized pine powder are blended according to a mass ratio of 9:1 to prepare a non-woven fabric, a TiO2 film with a thickness of 20 nm is formed on the surface of the non-woven fabric by magnetron sputtering to form a lining, the silk cotton is sandwiched between the shell fabric and the lining, the filling is sealed after sealing, and light pressure setting is carried out at 80 DEG C to prepare an antibacterial and durable silk quilt.

[0018] Compared with the prior art, the application has the following beneficial effects:

[0019] The application adopts mulberry silk, fillers and lavender essential oil as raw materials to prepare the antibacterial durable mulberry silk, wherein the silver ions released by the Ag-HAP powder in the fillers can directly destroy the structure of bacteria, and the porous structure of the carbonized pine powder can adsorb bacteria and their metabolites; after the silver ions kill the bacteria, the carbonized pine powder quickly adsorbs the residues to avoid secondary pollution caused by the decomposition of dead bacteria, and can effectively inhibit drug-resistant bacteria, and the antibacterial effect of the single component is more comprehensive and more durable; the silane coupling agent added can stably combine the Ag-HAP powder and the carbonized pine powder through chemical bonds, which not only avoids the rapid loss of silver ions, but also ensures that the adsorption channels of the carbonized pine powder are not blocked, so that the antibacterial performance remains stable in long-term use; the long-chain structure of the nanocellulose can wrap the silk fibers, providing flexible support, while the rigid particles of the Ag-HAP powder and the fibrous structure of the carbonized pine powder act as rigid nodes to disperse external force impact, so that the silk quilt not only maintains proper elasticity, but also has anti-stretching and anti-tearing ability, solving the contradiction between traditional silk quilt that is "soft and easy to damage, tough and rigid". + The porous structure of the carbonized pine powder can adsorb bacteria and their metabolites; after the silver ions kill the bacteria, the carbonized pine powder quickly adsorbs the residues to avoid secondary pollution caused by the decomposition of dead bacteria, and can effectively inhibit drug-resistant bacteria, and the antibacterial effect of the single component is more comprehensive and more durable; the silane coupling agent added can stably combine the Ag-HAP powder and the carbonized pine powder through chemical bonds, which not only avoids the rapid loss of silver ions, but also ensures that the adsorption channels of the carbonized pine powder are not blocked, so that the antibacterial performance remains stable in long-term use; the long-chain structure of the nanocellulose can wrap the silk fibers, providing flexible support, while the rigid particles of the Ag-HAP powder and the fibrous structure of the carbonized pine powder act as rigid nodes to disperse external force impact, so that the silk quilt not only maintains proper elasticity, but also has anti-stretching and anti-tearing ability, solving the contradiction between traditional silk quilt that is "soft and easy to damage, tough and rigid". BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 The preparation process of the antibacterial durable mulberry silk quilt is shown in the figure;

[0021] Figure 2 SEM image of the filling prepared in the present application. DETAILED DESCRIPTION

[0022] In order to make the technical personnel in the art better understand the technical solutions of the present application, and make the above-mentioned features, objectives and advantages of the present application more clear and easy to understand, the present application will be further described below in conjunction with examples. The examples are only used to illustrate the present application and not to limit the scope of the present application.

[0023] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as is commonly understood by one of ordinary skill in the art. In addition, any method and material similar or equivalent to those described herein can be used in the present application. The preferred methods and materials described herein are only for demonstration, but cannot limit the content of the present application.

[0024] In the following examples, unless otherwise specified, all are conventional methods; The materials used in the following examples, unless otherwise specified, the raw materials are new materials purchased on the market.

[0025] According to Figure 1 The antibacterial durable silk quilt prepared according to the flow chart of the present application is prepared by the following examples:

[0026] Example 1: The present example provides an antibacterial durable silk quilt, which comprises the following raw materials by weight: mulberry silk 60 parts, filling 25 parts, chitosan 3 parts, hyaluronic acid 1 part, lavender essential oil 0.5 part;

[0027] The filling comprises the following raw materials: HAP, poplar powder, pine powder and AgNO3 solution;

[0028] The preparation method of the filling comprises the following preparation steps:

[0029] (1) Take 25 parts of poplar powder, wash with deionized water to remove impurities, and dry at 60°C under vacuum to form pretreated poplar powder. The pretreated poplar powder is added to a 4% sulfuric acid solution, and the ratio of pretreated poplar powder to sulfuric acid solution is 1 g:10 mL. Stir in a constant temperature water bath at 45°C for 2 h, centrifuge, wash to neutral, and then high-pressure homogenization cycle treatment 5 times to obtain a nanocellulose suspension;

[0030] (2) Take 3 parts of HAP and disperse in 0.1 mol / L AgNO3 solution, and the ratio of HAP to AgNO3 solution is 1 g:100 mL. Stir in the dark for 24 h, centrifuge to collect the precipitate, and vacuum dry to obtain Ag-HAP powder;

[0031] (3) Take 18 parts of pine powder, place it in a tube furnace, introduce nitrogen gas, set the flow rate to 50 mL / min, exclude air, heat to 300℃ at a rate of 5℃ / min, and keep the temperature for 2 hours. After natural cooling to room temperature, sieve through a 200-mesh sieve, soak in 10% hydrochloric acid for 2 hours to remove ash, wash with deionized water until neutral, and dry at 60℃ under vacuum to obtain carbonized pine powder;

[0032] (4) Mix the nanocellulose suspension, Ag-HAP powder, and carbonized pine powder according to a mass ratio of 5:3:2 to form a mixture, add 1% silane coupling agent KH-570 based on the total mass of the mixture, ultrasonic dispersion for 30 minutes, then freeze-drying, hot-pressing at 80℃, pressure 0.1 MPa, time 10 minutes, to obtain the filler.

[0033] The present embodiment also provides a preparation method of an antibacterial and durable silk quilt, which specifically comprises the following preparation steps:

[0034] S1, degumming of mulberry silk: immerse the mulberry silk in an aqueous solution containing 0.5% Na2CO3 and 0.1% neutral protease, with a bath ratio of 1:30 between the mulberry silk and the aqueous solution, stirring, constant temperature treatment at 85℃ for 1 hour, washing with deionized water until neutral, vacuum drying at 60℃ for 4 hours, and mechanical opening treatment to obtain degummed mulberry silk;

[0035] S2, cross-linking of mulberry silk fibers: prepare a 5% PEGDA aqueous solution with 0.5% photoinitiator Irgacure 2959, immerse the degummed mulberry silk in it, immerse for 10 minutes, irradiate with 365 nm ultraviolet light for 10 minutes, and dry and cure at 60℃ to obtain pretreated mulberry silk;

[0036] S3, essential oil composite spinning: mix β-cyclodextrin and 0.5 parts of lavender essential oil according to a molar ratio of 1:1, add deionized water, stir at 40℃ for 2 hours, freeze-dry to obtain an essential oil composite, mix the essential oil composite with 25 parts of filler according to a mass ratio of 1:10, add 0.1% polyoxyethylene sorbitan monolaurate dispersant, and use electrospinning process to prepare a composite fiber web, with a voltage setting of 18kV, a receiving distance of 20 cm, and a flow rate of 0.8 mL / h;

[0037] S4, finishing silk cotton: 3 parts of chitosan and composite fiber web are mixed according to a mass ratio of 1:10, and then added into an acetic acid solution with a mass concentration of 1%, stirred at 50 DEG C for 30 min to form a finishing liquid, the pretreated mulberry silk is immersed in the finishing liquid, the bath ratio is 1:20, constant temperature water bath oscillation at 45 DEG C for 30 min, padding, the padding rate is 70%, 100 DEG C drying, carding, cross-laying, the thickness is 5 cm, hot air setting at 80 DEG C, and the silk cotton is obtained;

[0038] S5, assembling the antibacterial durable silk quilt: 1 part of hyaluronic acid is added into deionized water to prepare a hyaluronic acid solution with a mass concentration of 3%, the mulberry silk fabric is immersed and padded in the hyaluronic acid solution, vacuum dried to form a shell fabric, the mulberry silk and carbonized pine powder are blended according to a mass ratio of 9:1 to form a non-woven fabric, a TiO2 film with a thickness of 20 nm is formed on the surface of the non-woven fabric by magnetron sputtering, and the lining is formed, the silk cotton is sandwiched between the shell fabric and the lining, sealed after filling, and light pressure setting is performed at 80 DEG C under a pressure of 0.1 MPa for 2 min to prepare the antibacterial durable silk quilt.

[0039] Embodiment 2: The antibacterial durable silk quilt provided by the embodiment includes the following raw materials in parts by weight: mulberry silk 65 parts, filler 30 parts, chitosan 4 parts, hyaluronic acid 1.5 parts, and lavender essential oil 0.8 parts.

[0040] The filler includes the following raw materials: HAP, poplar powder, pine powder and AgNO3 solution.

[0041] The preparation method of the filler includes the following preparation steps:

[0042] (1) 30 parts of poplar powder are washed with deionized water to remove impurities, and vacuum dried at 60 DEG C to form pretreated poplar powder, the pretreated poplar powder is added into a sulfuric acid solution with a mass concentration of 4%, the use amount ratio of the pretreated poplar powder to the sulfuric acid solution is 1 g:15 mL, constant temperature water bath stirring is performed at 45 DEG C for 2 h, centrifugation is performed, washing is performed until neutral, and high-pressure homogenization is performed for 5 times to obtain a nanocellulose suspension;

[0043] (2) 5 parts of HAP are dispersed in a 0.1 mol / L AgNO3 solution, stirred in the dark for 24 h, the precipitate is collected by centrifugation, and vacuum dried to obtain Ag-HAP powder;

[0044] (3) Take 20 parts of pine wood powder, place it in a tube furnace, introduce nitrogen gas, set the flow rate to 50 mL / min, exclude air, heat from room temperature to 300°C at a rate of 5°C / min, and keep the temperature for 2 hours. Perform pyrolysis, naturally cool to room temperature, pass through a 200-mesh sieve, soak in 10% hydrochloric acid for 2 hours to remove ash, wash with deionized water until neutral, and dry at 60°C under vacuum to obtain carbonized pine wood powder;

[0045] (4) Mix the nanocellulose suspension, Ag-HAP powder, and carbonized pine wood powder according to a mass ratio of 5:3:2 to form a mixture, add 1% of silane coupling agent KH-570 based on the total mass of the mixture, ultrasonic dispersion for 30 minutes, then freeze-drying, hot-pressing at 80°C, pressure 0.1 MPa, time 10 minutes, to obtain the filler.

[0046] The present embodiment also provides a preparation method of an antibacterial and durable silk quilt, which specifically comprises the following preparation steps:

[0047] S1, degumming of mulberry silk: immerse the mulberry silk in an aqueous solution containing 0.5% Na2CO3 and 0.1% neutral protease, with a bath ratio of 1:30 between the mulberry silk and the aqueous solution, stir, and treat at a constant temperature of 85°C for 1 hour. Rinse with deionized water until neutral, dry at 60°C under vacuum for 4 hours, and mechanically open to obtain degummed mulberry silk;

[0048] S2, cross-linking of mulberry silk fibers: prepare a 5% PEGDA aqueous solution with 0.5% photoinitiator Irgacure 2959, immerse the degummed mulberry silk in it, immerse for 10 minutes, irradiate with 365 nm ultraviolet light for 10 minutes, and dry and cure at 60°C to obtain pretreated mulberry silk;

[0049] S3, essential oil composite spinning: mix β-cyclodextrin and 0.8 parts of lavender essential oil according to a molar ratio of 1:1, add deionized water, stir at 40°C for 2 hours, freeze-dry to obtain an essential oil composite, mix the essential oil composite with 30 parts of filler according to a mass ratio of 1:10, add 0.1% polyoxyethylene sorbitan monolaurate dispersant, and use an electrospinning process to set the voltage to 20 kV, the receiving distance to 22 cm, and the flow rate to 1 mL / h to prepare a composite fiber web;

[0050] S4, finishing silk cotton: 4 parts of chitosan and composite fiber web are mixed according to a mass ratio of 1:10, and then added into an acetic acid solution with a mass concentration of 1%, stirred at 50 DEG C for 30 min to form a finishing liquid, the pretreated mulberry silk is immersed in the finishing liquid, the bath ratio is 1:20, constant temperature water bath oscillation at 45 DEG C for 30 min, padding, the padding rate is 75%, 100 DEG C drying, carding, cross-laying, the thickness is 8 cm, 80 DEG C hot air setting, and the silk cotton is obtained;

[0051] S5, assembling the antibacterial durable silk quilt: 1.5 parts of hyaluronic acid are added into deionized water to prepare a hyaluronic acid solution with a mass concentration of 3%, the mulberry silk fabric is immersed and padded in the hyaluronic acid solution, vacuum dried to form a shell fabric, the mulberry silk and carbonized pine powder are blended according to a mass ratio of 9:1 to form a lining fabric, a TiO2 film with a thickness of 20 nm is formed on the surface of the lining fabric by magnetron sputtering, the silk cotton is sandwiched between the shell fabric and the lining fabric, sealed after filling, and light pressure setting is performed at 80 DEG C under a pressure of 0.1 MPa for 2 min to prepare the antibacterial durable silk quilt.

[0052] Example 3: The antibacterial durable silk quilt provided by the example comprises the following raw materials in parts by weight: mulberry silk 70 parts, filler 35 parts, chitosan 5 parts, hyaluronic acid 2 parts, and lavender essential oil 1 part.

[0053] The filler comprises the following raw materials: HAP, poplar powder, pine powder and AgNO3 solution.

[0054] The preparation method of the filler comprises the following preparation steps:

[0055] (1) 30 parts of poplar powder are washed with deionized water to remove impurities, and vacuum dried at 60 DEG C to form pretreated poplar powder, the pretreated poplar powder is added into a sulfuric acid solution with a mass concentration of 4%, the use amount ratio of the pretreated poplar powder to the sulfuric acid solution is 1 g:15 mL, constant temperature water bath stirring is performed at 45 DEG C for 2 h, centrifugation is performed, washing is performed until neutral, and high-pressure homogenization is performed for 5 times to obtain a nanocellulose suspension;

[0056] (2) 3 parts of HAP are dispersed in a 0.1 mol / L AgNO3 solution, stirred in the dark for 24 h, the precipitate is collected by centrifugation, and vacuum dried to obtain Ag-HAP powder;

[0057] (3) Take 18 parts of pine powder, place it in a tube furnace, introduce nitrogen gas, set the flow rate to 50 mL / min, exclude air, heat from room temperature to 300℃ at a rate of 5℃ / min, keep for 2 h, naturally cool 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, vacuum dry at 60℃, and obtain carbonized pine powder;

[0058] (4) Mix the nanocellulose suspension, Ag-HAP powder, and carbonized pine powder according to a mass ratio of 5:3:2 to form a mixture, add 1% silane coupling agent KH-570 based on the total mass of the mixture, ultrasonic dispersion for 30 min, then freeze-drying, hot-pressing at 80℃, pressure 0.1 MPa, time 10 min, to obtain the filler.

[0059] The embodiment also provides a preparation method of the antibacterial and durable silk quilt, which specifically comprises the following preparation steps:

[0060] S1, degumming of mulberry silk: immerse the mulberry silk in an aqueous solution containing 0.5% Na2CO3 and 0.1% neutral protease by mass concentration, the bath ratio of mulberry silk to aqueous solution is 1:30, stir, treat at 85℃ for 1 h, wash with deionized water until neutral, vacuum dry at 60℃ for 4 h, and mechanically open to obtain degummed mulberry silk;

[0061] S2, crosslinking of mulberry silk fibers: prepare a 5% PEGDA aqueous solution containing 0.5% photoinitiator Irgacure 2959 by mass concentration, immerse the degummed mulberry silk in the solution, immerse for 10 min, irradiate with 365 nm ultraviolet light for 10 min, and dry and cure at 60℃ to obtain pretreated mulberry silk;

[0062] S3, essential oil composite spinning: mix β-cyclodextrin and 1 part of lavender essential oil according to a molar ratio of 1:1, add deionized water, stir at 40℃ for 2 h, freeze-dry to obtain an essential oil composite, mix the essential oil composite with 35 parts of filler according to a mass ratio of 1:10, add 0.1% polyoxyethylene sorbitan monolaurate dispersant, and use the electrospinning process to prepare a composite fiber web, with a voltage setting of 20 kV, a receiving distance of 20 cm, and a flow rate of 0.8 mL / h;

[0063] S4, finishing silk cotton: 5 parts of chitosan and composite fiber web are mixed according to a mass ratio of 1:10, then added into an acetic acid solution with a mass concentration of 1%, stirred at 50 DEG C for 30 min to form a finishing liquid, the pretreated mulberry silk is immersed in the finishing liquid, the bath ratio is 1:20, constant temperature water bath oscillation at 45 DEG C for 30 min, padding, the padding rate is 80%, dried at 100 DEG C, carded into a web, cross-laid, the thickness is 5-10 cm, hot air setting at 80 DEG C, to obtain silk cotton;

[0064] S5, assembling to obtain the antibacterial durable silk quilt: 2 parts of hyaluronic acid are added into deionized water to prepare a hyaluronic acid solution with a mass concentration of 3%, the mulberry silk fabric is immersed and padded in the hyaluronic acid solution, vacuum dried to form a shell fabric, the mulberry silk and carbonized pine powder are blended according to a mass ratio of 9:1 to prepare a non-woven fabric, a TiO2 film with a thickness of 20 nm is formed on the surface of the non-woven fabric by magnetron sputtering to form a lining, the silk cotton is sandwiched between the shell fabric and the lining, sealed after filling, light pressure setting at 80 DEG C under a pressure of 0.1 MPa for 2 min, to prepare the antibacterial durable silk quilt.

[0065] The difference between Comparative Example 1 and Example 1 is that the filling is not added, and the rest is exactly the same as Example 1.

[0066] The difference between Comparative Example 2 and Example 1 is that the lavender essential oil is not added, and the rest is exactly the same as Example 1.

[0067] The difference between Comparative Example 3 and Example 1 is that the PEGDA is not added, and the rest is exactly the same as Example 1.

[0068] Experimental Example

[0069] 1, bacteriostatic rate test: according to GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: shaking method", the antibacterial durable silk quilt prepared by Examples 1-3 and Comparative Examples 1-3 of the application is used as a sample, and the bacteriostatic rate of Escherichia coli (ATCC25922), Staphylococcus aureus (ATCC6538) and Candida albicans (ATCC10231) is determined, and the results are recorded in Table 1.

[0070] 2. Breaking strength test: According to GB / T3916-2013 "Determination of breaking strength and elongation at break of individual yarn in textile package", the anti-durable silk quilt prepared by the examples 1-3 and the comparative examples 1-3 of the present application is used as a sample to test the breaking strength of the sample; the tensile testing machine is adjusted, the appropriate clamping distance and tensile speed are set, and the instrument is ensured to be in normal working condition. The two ends of the sample are clamped in the upper and lower clamps of the testing machine respectively, the sample axis is kept consistent with the clamping line, the instrument is started to stretch until the sample is broken, and the maximum breaking strength value is recorded. The test is carried out in the warp and weft directions respectively for several times, and the average value is taken as the final result, and the sample breaking position is observed, if the sample breaks in the clamping area, the data is invalid and needs to be retested, and the results are recorded in table 1.

[0071] Table 1

[0072]

[0073] The results in table 1 show that the antibacterial rates of examples 1-3 on three kinds of bacteria are all in the range of 97.9%-99.9%, especially on escherichia coli and staphylococcus aureus, the antibacterial rates are mostly in the range of 99.8%-99.9%, which indicates that the anti-bacterial durable silk quilt prepared by the present application can efficiently inhibit common pathogenic bacteria, and the antibacterial effect is excellent and stable; the mechanical properties of examples are excellent: the breaking strength of examples 1-3 is 4.3-4.5 cN / dtex, which indicates that the anti-bacterial durable silk quilt prepared by the present application has good mechanical support through the synergy of raw materials while ensuring antibacterial, and is not easy to break and deform, and has strong durability.

[0074] 3. Wear resistance test: According to GB / T21196.3-2007, the anti-durable silk quilt prepared by the examples 1-3 and the comparative examples 1-3 of the present application is used as a sample to test the wear resistance of the sample by Martin Dale wear test, and the Martin Dale wear tester is used for testing. After the sample is rubbed for 1200 times under the pressure of 5kPa, there is no obvious pilling (pilling grade ≥4 grade) and no fiber shedding (mass loss rate ≤2%), which is better than the 500 times standard of ordinary silk quilt.

[0075] 4、Washing resistance test solution preparation: according to the standard requirements of AATCC 61-2013 2A method, a specified amount of powder or liquid detergent is added to deionized water, stirred and dissolved, and then preheated to a specified temperature to form a washing solution. The sample preparation is to cut a sample of a specified size from the quilt shell or filling layer of the silk quilt, combine it with a multi-fiber lining fabric, and make the two closely contact by sewing or fixing to ensure that the fiber strips of the lining fabric are aligned parallel to the edges of the sample. Place the combined sample in a stainless steel container, add the preheated washing solution and a specified amount of stainless steel beads, tightly cover the container and fix it on the washing test machine, and run it according to the set temperature and time. After washing, rinse the sample with warm water several times to remove residual detergent, and then dry it at a specified temperature or air dry. After drying, the sample is adjusted to the standard environment, the discoloration grade is evaluated compared to the original sample, and the staining of the lining fabric is also evaluated. The antibacterial rate retention rate after 50 washes is recorded in Table 1.

[0076] 5、Loft test: according to the standard of GB / T 24218.3-2010, the antibacterial durable silk quilt prepared in examples 1-3 and comparative examples 1-3 of the present application is taken as the sample silk quilt, an appropriate amount of filling cotton sample is taken from the sample silk quilt, impurities and lumps are removed, and the sample is adjusted to the standard temperature and humidity environment for a period of time. Check whether the cylinder, pressure plate and other parts of the loft tester are clean, and calibrate the pressure and volume measurement system of the instrument. Place the adjusted sample into the test cylinder, gently comb it to distribute it naturally, and avoid artificial compaction. Lower the pressure plate, apply a specified pressure and maintain it for a certain period of time, and record the volume data at this time. According to the measured volume and sample mass, calculate the volume per unit mass value as the loft index, repeat the test several times to take the average value, and the results are recorded in Table 2.

[0077] Table 2

[0078]

[0079] Table 2 shows that the abrasion resistance of examples 1-3 reaches 4-5 levels, indicating that the antibacterial durable silk quilt prepared by the present application has less fiber shedding and good abrasion resistance after rubbing; the washing resistance of examples 1-3 reaches 96.2%, indicating that the antibacterial durable silk quilt prepared by the present application still has excellent antibacterial properties and strong resistance to water washing loss after multiple washes; the loft data of examples 1-3 reaches 405-420 cm 3 / g, indicating that the present application can maintain good loft and warmth comfort of the silk quilt after washing by filling support and process optimization.

[0080] Figure 2The SEM image of the filling prepared by the application shows a silk-like interwoven structure, which is intertwined with each other to form a network structure, and the preparation process of the application is combined to prepare the fluffy antibacterial durable silk quilt.

[0081] In summary, the application realizes the performance leap of the antibacterial durable silk quilt through scientific raw material ratio and process design. The core lies in the synergistic effect of the filling, beta-cyclodextrin and PEGDA, which not only forms an efficient antibacterial system through the cooperation of Ag-HAP and carbonized pine powder, but also enhances the mechanical properties with the support of nano-cellulose and carbonized pine powder, solving the problems of weak antibacterial property and easy breakage of traditional silk quilt; the lavender essential oil is stabilized by beta-cyclodextrin through the packaging effect, prolonging the soothing effect while assisting antibacterial, and giving consideration to function and use experience; the crosslinking modification of PEGDA builds a flexible connection for silk fibers, improves the breaking strength and washing resistance, balances the skin-friendliness and durability, makes the product break through in antibacterial performance, mechanical strength, function retention and other aspects, and shows significant technical advantages and creativity, providing an efficient and feasible scheme for the preparation of antibacterial durable silk quilt.

[0082] The above describes the application and its embodiments, which are not limited, and the drawings only show one of the embodiments of the application, and the actual application is not limited thereto. In summary, if a person skilled in the art is inspired by it, without departing from the purpose of the application, without creative design, similar ways and embodiments of the technical solution should belong to the protection scope of the application.

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 photo-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, filling and sealing, and lightly pressing to shape, thereby preparing an antibacterial and durable silk quilt; 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 to neutrality, 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.

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: 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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