阅读说明：本技术 一种蚕丝织物的抗菌整理方法 (Antibacterial finishing method of silk fabric ) 是由 谢维 于 2020-12-29 设计创作，主要内容包括：本发明采用天然来源的抗菌肽、壳聚糖和茶多酚为原料加工制备得到了抗菌性能优异的蚕丝织物整理剂,且在蚕丝织物抗菌整理过程中,采用超声处理手段,其更加有利于清除蚕丝织物表面的杂质,有利于其吸附基团的暴露,能够促进本发明抗菌整理剂中的活性成分吸附在蚕丝织物的表面,提高抗菌整理的牢度性,对于蚕丝织物的加工产品,减少其使用过程中的细菌滋生,能够延长其使用寿命。(The silk fabric finishing agent with excellent antibacterial performance is prepared by processing the raw materials of natural antibacterial peptide, chitosan and tea polyphenol, and in the process of antibacterial finishing of silk fabrics, an ultrasonic treatment means is adopted, so that impurities on the surface of the silk fabrics can be removed, exposure of adsorption groups of the silk fabrics is facilitated, active ingredients in the antibacterial finishing agent can be promoted to be adsorbed on the surface of the silk fabrics, the fastness of antibacterial finishing is improved, bacterial growth in the using process of processed products of the silk fabrics is reduced, and the service life of the processed products of the silk fabrics can be prolonged.)

1. An antibacterial finishing method of silk fabric comprises the following steps:

step one, taking silk fabric, immersing the silk fabric into clear water solution with the pH value of 8-8.5, soaking and swelling for 2 hours at 80 ℃ in a bath ratio of 1:50, taking out the silk fabric, washing the silk fabric with clear water, and naturally drying the silk fabric for later use;

step two, taking the antibacterial finishing agent, and diluting the antibacterial finishing agent by 50 times by using tap water to obtain antibacterial finishing liquid;

and step three, immersing the silk fabric dried in the step one into the antibacterial finishing liquid in the step two at a bath ratio of 1:50, performing ultrasonic treatment for 10-20 minutes, taking out, washing with clear water, and naturally drying.

2. The method for the antimicrobial finishing of silk fabric according to claim 1, characterized in that the intensity of the ultrasonic treatment is 50-100W/kg silk fabric.

3. The method for antibacterial finishing of silk fabric according to claim 1, wherein the antibacterial finishing agent of silk fabric is prepared from antibacterial peptide, low molecular weight chitosan, and tea polyphenol.

4. The method for antimicrobial finishing of silk fabric according to claim 3, wherein the method for preparing the antimicrobial finishing agent of silk fabric comprises the following steps:

weighing antibacterial peptide, low-molecular-weight chitosan and tea polyphenol according to parts by weight, dissolving the low-molecular-weight chitosan by adopting an acetic acid solution with the concentration of 5% (v/v) at 40 ℃, then cooling to room temperature, adding the antibacterial peptide and the tea polyphenol, and stirring for dissolving to obtain a solution A;

adding Tween 80 into the solution A, uniformly stirring, and adjusting the pH value to 3.0-4.0 to obtain a solution B;

and step three, gradually dropwise adding a sodium tripolyphosphate solution with the concentration of 5g/L into the solution B in the step two at room temperature, and stirring at a high speed while dropwise adding until the sodium tripolyphosphate solution is completely dripped, so as to obtain the antibacterial finishing liquid.

5. The method for antibacterial finishing of silk fabric as claimed in claim 4, wherein in the solution A of the first step, the concentration of the antibacterial peptide is 62.5-125 mg/L; the concentration of the low molecular weight chitosan is 6-8 g/L; the concentration of tea polyphenols is 10-12 g/L; the final concentration of the Tween 80 in the solution B in the second step is 8 g/L; in the third step, the volume ratio of the sodium tripolyphosphate solution to the solution B is 1: 49.

6. The method for antibacterial finishing of silk fabric according to claim 3, wherein the amino acid sequence of the antibacterial peptide is as shown in SEQ ID No: 1 is shown.

7. The antibacterial finishing method of silk fabric as claimed in claim 3, wherein the small molecular weight chitosan is small molecular chitosan with a relative molecular mass of 4000-8000.

8. The antibacterial finishing method of silk fabrics according to claim 7, characterized in that the low molecular weight chitosan is prepared by the following method:

step one, dissolving high molecular weight chitosan: the viscosity average molecular weight is 3.0X 10⁵100g of high molecular weight chitosan with the deacetylation degree of 90.5 percent is dissolved in acetic acid solution with the volume fraction of 22 percent to obtain chitosan solution with the mass volume concentration of 25 percent (w/v);

step two, degrading high molecular weight chitosan: performing ultrasonic treatment on the chitosan solution prepared in the first step twice, wherein the temperature of the first ultrasonic treatment is 45 ℃, the time of the ultrasonic treatment is 4 hours, and the ultrasonic power is 600W; the temperature of the second ultrasonic treatment is 20 ℃, the time of the ultrasonic treatment is 5 hours, the ultrasonic power is 200W, the micromolecular chitosan with the average relative molecular mass of 4000-;

step three, purifying the low molecular weight chitosan: and (3) dropwise adding a sodium bicarbonate solution into the micromolecular chitosan solution prepared in the step two, adjusting the pH value to 7.0-7.5, standing for 5h, centrifuging at 3000rpm for 10min, separating the precipitate, washing with water to be neutral, and drying to obtain the micromolecular chitosan powder.

9. A silk fabric with antibacterial activity is characterized in that: the fabric is obtained by performing antibacterial finishing on silk fabrics by adopting the method of claims 1-8.

The technical field is as follows:

the invention belongs to the field of textiles, relates to an antibacterial finishing method of textile materials, and particularly relates to an antibacterial finishing method of silk fabrics.

Background art:

the silk fabric is woven by taking silk fiber as a raw material, is a traditional culture industry in China, extends the culture for thousands of years, has good affinity effect on human skin, and can well delay skin aging and nourish the skin. The characteristics of the silk fiber endow the silk fabric with the characteristics of smooth hand feeling, moisture absorption, air permeability, softness, comfort, soft luster, lightness, thinness, elegance and the like. Is always praised as 'fibre queen' by people and is used as high-grade textile raw material. Although silk has multiple advantages, silk also has the defects of easy wrinkling, poor light stability, easy yellowing, poor ultraviolet resistance, poor antibacterial capability and the like, and the application of silk fiber is limited by the defects. For example, in the process of using and maintaining silk fabrics, various microorganisms such as bacteria and the like are bred, and some microorganisms are harmful to human bodies and can rapidly grow and reproduce under proper environment and conditions, so that the health of the human bodies is influenced.

At present, various means are used for antibacterial finishing of silk fabrics, for example, a method for directly grafting nano silver on silk is researched by the Dutai and the like, the result shows that the nano silver on the silk exists in a dispersed and clustered manner, and within 20min, the silk with the size of 2cm multiplied by 3cm is matched with the silk with the size of 10 cm⁴The sterilization rate of CFU/ml bacteria reaches 90 percent. Research shows that the antibacterial silk can be prepared by grafting the nano silver combined with protein molecules onto the fibroin by glutaraldehyde (silkworm communication, 2016, 36 (04): 1-4); the mulberry silk is subjected to ultralow temperature freezing treatment and antibacterial treatment by using an improved organosilicon quaternary ammonium salt antibacterial agent, the antibacterial rate of the mulberry silk after the antibacterial finishing reaches 98.6%, and the antibacterial rate of the mulberry silk after the ultralow temperature freezing antibacterial treatment reaches 99.2% (silk, 2013, 50 (09): 21-24+ 30); polyurethane spinning stock solution is taken as a matrix by Jiangsu Hengyuan silk group Limited company, and the polyurethane-graphene composite fiber is prepared by adding graphene dispersion solution and adopting dry spinning or wet spinning; twisting polyurethane-graphene composite fibers as warps, twisting silk as wefts to perform weaving processing to obtain an antibacterial silk fabric, and testing the bacteriostasis rate of the sample by an absorption method, wherein the bacteriostasis rate is more than 99.9% (patent application publication CN 107142593A); the anti-wrinkle antibacterial agent used by welder industry and trade company limited, Suzhou adopts modified polysiloxane, chitosan and polyethylene glycol-6 which are mixed and then react with hemiacetal to further modify the polysiloxane, so that the polysiloxane has good anti-wrinkle and antibacterial properties and does not cause the phenomenon that silk fabrics are easy to turn yellow in the using process (patent application publication CN 107287905A). Although there are many studies and reports on antibacterial silk, mainly grafting antibacterial substance on sericin or silk bundle, for silk which needs to be processed into fabric for antibacterial application, the later processing process will have different degrees of influence on the antibacterial substance combined with silk, or to maintain its antibacterial effect, at later stageSome sacrifice is made in the processing process, and the residue of chemical components used in the conventional process also brings certain safety hazard to users.

The invention content is as follows:

in order to solve the technical problem that the silk fabric is easy to breed bacteria and fungus pollution in the using process, the invention aims to provide the antibacterial finishing method of the silk fabric.

In order to solve the technical problems, the invention adopts the following technical scheme:

an antibacterial finishing method of silk fabric comprises the following steps:

step one, taking silk fabric, immersing the silk fabric into clear water solution with the pH value of 8-8.5, soaking and swelling for 2 hours at 80 ℃ in a bath ratio of 1:50, taking out the silk fabric, washing the silk fabric with clear water, and naturally drying the silk fabric for later use;

step two, taking the antibacterial finishing agent, and diluting the antibacterial finishing agent by 50 times by using tap water to obtain antibacterial finishing liquid;

and step three, immersing the silk fabric dried in the step one into the antibacterial finishing liquid in the step two at a bath ratio of 1:50, performing ultrasonic treatment for 10-20 minutes, taking out, washing with clear water, and naturally drying.

Preferably, the intensity of the ultrasonic treatment is 50-100W/kg silk fabric.

Preferably, the antibacterial finishing agent for the silk fabric is prepared from antibacterial peptide, low-molecular-weight chitosan and tea polyphenol.

Preferably, the preparation method of the antibacterial finishing agent for silk fabrics comprises the following steps:

weighing antibacterial peptide, low-molecular-weight chitosan and tea polyphenol according to parts by weight, dissolving the low-molecular-weight chitosan by adopting an acetic acid solution with the concentration of 5% (v/v) at 40 ℃, then cooling to room temperature, adding the antibacterial peptide and the tea polyphenol, and stirring for dissolving to obtain a solution A;

adding Tween 80 into the solution A, uniformly stirring, and adjusting the pH value to 3.0-4.0 to obtain a solution B;

and step three, gradually dripping a sodium tripolyphosphate solution with the concentration of 5g/L into the solution B in the step two at room temperature, and stirring at a high speed while dripping until the sodium tripolyphosphate solution is completely dripped, thus obtaining the antibacterial finishing liquid.

Preferably, in the solution A in the first step, the concentration of the antibacterial peptide is 62.5-125 mg/L; the concentration of the low molecular weight chitosan is 6-8 g/L; the concentration of tea polyphenols is 10-12 g/L.

Preferably, the final concentration of Tween 80 in the solution B in the second step is 8 g/L.

Preferably, in the third step, the volume ratio of the sodium tripolyphosphate solution to the solution B is 1: 49.

Preferably, the amino acid sequence of the antibacterial peptide is shown in SEQ ID No: 1 is shown.

Preferably, the small molecular weight chitosan is the small molecular chitosan with the relative molecular mass of 4000-8000.

Preferably, the low molecular weight chitosan is prepared by the following method:

step one, dissolving high molecular weight chitosan: the viscosity average molecular weight is 3.0X 10⁵100g of high molecular weight chitosan with the deacetylation degree of 90.5 percent is dissolved in acetic acid solution with the volume fraction of 22 percent to obtain chitosan solution with the mass volume concentration of 25 percent (w/v);

step two, degrading high molecular weight chitosan: performing ultrasonic treatment on the chitosan solution prepared in the first step twice, wherein the temperature of the first ultrasonic treatment is 45 ℃, the time of the ultrasonic treatment is 4 hours, and the ultrasonic power is 600W; the temperature of the second ultrasonic treatment is 20 ℃, the time of the ultrasonic treatment is 5 hours, the ultrasonic power is 200W, and the micromolecular chitosan (the deacetylation degree is more than 95 percent) with the average relative molecular mass of 4000-;

step three, purifying the low molecular weight chitosan: and (3) dropwise adding a sodium bicarbonate solution into the micromolecular chitosan solution prepared in the step two, adjusting the pH value to 7.0-7.5, standing for 5h, centrifuging at 3000rpm for 10min, separating the precipitate, washing with water to be neutral, and drying to obtain the micromolecular chitosan powder.

Based on the technical scheme, the invention has the following advantages and beneficial effects:

firstly, the silk antibacterial finishing agent with good antibacterial activity is prepared by combining a plurality of natural antibacterial raw materials, wherein the high molecular weight chitosan is degraded by adopting an ultrasonic treatment technology to prepare the low molecular weight chitosan, and compared with the traditional chitosan macromolecule, the silk antibacterial finishing agent is more suitable for being used as the antibacterial finishing agent of silk fabrics. The invention also redesigns the natural antibacterial peptide Cecropin P1, on the basis of keeping the original antibacterial peptide active structure domain, and adds arginine (R) and lysine (K) with positive charges on the peptide segment through redesigning, so that the Cecropin P1 can be better adsorbed on the surface of the silk material, and can also be better adsorbed on the surface of bacteria with negative charges, and meanwhile, the antibacterial activity of the Cecropin P1 is also improved. The wearability test shows that compared with the traditional method of adopting high molecular weight chitosan as the antibacterial finishing agent, the antibacterial finishing agent of the invention adopts low molecular weight chitosan as the active ingredient, thereby reducing the influence of chitosan molecules on the air permeability of the silk fabric, and simultaneously having better crease resistance compared with high molecular weight chitosan. The antibacterial property detection shows that after the silk fabric is finished by the antibacterial finishing agent, the inhibition rate of the antibacterial finishing agent on two kinds of bacteria is higher than 90%, which indicates that the antibacterial property is excellent, and after the silk fabric is subjected to fastness tests of washing for 20 times and washing for 30 times, the antibacterial finishing agent and the antibacterial finishing method respectively can reach the standard of qualified antibacterial property, and the results show that the antibacterial finishing agent and the antibacterial finishing method can effectively improve the antibacterial property of the silk fabric.

Secondly, in the process of the antibacterial finishing of the silk fabric, an ultrasonic treatment means is adopted, which is more favorable for removing impurities on the surface of the silk fabric and exposing adsorption groups of the silk fabric, can promote active ingredients in the antibacterial finishing agent to be adsorbed on the surface of the silk fabric, improves the fastness of the antibacterial finishing, reduces the bacterial growth in the using process of a processed product of the silk fabric, and can prolong the service life of the processed product.

In conclusion, the silk fabric finishing agent with excellent antibacterial performance is prepared by processing the raw materials of natural antibacterial peptide, chitosan and tea polyphenol, and in the process of antibacterial finishing of silk fabric, an ultrasonic treatment means is adopted, so that impurities on the surface of the silk fabric can be removed, exposure of adsorption groups of the silk fabric is facilitated, active ingredients in the antibacterial finishing agent can be promoted to be adsorbed on the surface of the silk fabric, the fastness of antibacterial finishing is improved, bacterial growth in the using process of a processed product of the silk fabric is reduced, and the service life of the processed product can be prolonged.

The specific implementation mode is as follows:

example 1: preparation and activity determination of antibacterial peptide

(1) Design and preparation of antibacterial peptide

According to the action mechanism and the bacteriostatic activity structural site of Cecropin P1, the Cecropin P has the sequence shown as SEQ ID No: 2, the original Cecropin P1 antibacterial peptide is structurally designed, in the design process, the antibacterial peptide structural domain of the Cecropin P1 is kept, and arginine (R) and lysine (K) with positive charges are added, so that the Cecropin P1 antibacterial peptide can be better adsorbed on the surface of a silk material and can also be better adsorbed on the surface of bacteria with negative charges, and meanwhile, the antibacterial activity of the Cecropin P1 antibacterial peptide is also improved. The sequence of the redesigned antibacterial peptide is SEQ ID No: 1. wherein SEQ ID No: 1 is as follows: SWLSKTAKKLEKRAKKRKSRGIAIAIQGGRR, respectively; the amino acid sequence of the original Cecropin P1 antibacterial peptide is SEQ ID No: 2 SWLSKTAKKLENSAKKRISEGIAIAIQGGPR, Bioreagent company was assigned to synthesize the designed antimicrobial peptide by the solid phase method to obtain the antimicrobial peptide with a purity of > 95%.

(2) Bacteriostatic activity of antibacterial peptide

According to the common pollution condition in the silk fabric, staphylococcus aureus and escherichia coli are selected as detection index bacteria, and staphylococcus aureus with the number of ATCC29213 and escherichia coli with the number of ATCC25922, which are purchased from a reagent company, are respectively selected as standard bacteria for antibacterial activity detection.

And (3) quickly pouring 20-30mL of sterilized LB semisolid culture medium into a sterile culture dish, cooling and solidifying, and then inverting for later use. From a bacterial suspension (10)⁸CFU/mL) was added to the surface of the medium by 100. mu.L each, and the medium was uniformly coated with a sterilized coating bar. A drug sensitive strip (d =5 mm) adsorbed with 20. mu.g of antimicrobial peptide was attached to a medium, and placed in a constant temperature incubator and incubated at 37 ℃ for 24 hours. The growth of the bacteria in each culture dish was observed, and the diameter of the zone of inhibition (including the diameter of the filter paper sheet) was measured by the cross method. Through detection, for staphylococcus aureus, the average diameter of the inhibition zone of the original Cecropin P1 antibacterial peptide is 20.2mm, and the average diameter of the antibacterial peptide is 24.4 mm; for Escherichia coli, the average diameter of the inhibition zone of the original Cecropin P1 antibacterial peptide is 19.5mm, and the average diameter of the antibacterial peptide of the invention is 23.8mm, so that the antibacterial peptide of the invention has higher antibacterial activity compared with the original Cecropin P1 antibacterial peptide through redesigning the antibacterial peptide.

(3) Determination of MIC of antimicrobial peptides

Detecting Minimum Inhibitory Concentration (MIC) by micro 2-fold dilution method to respectively determine MIC of antibacterial peptide and original Cecropin P1 antibacterial peptide, diluting the bacteria to be detected cultured to logarithmic growth phase with LB liquid culture medium to reach bacteria content of 10⁶CFU/mL, 50. mu.L of bacterial suspension was added to 96-well culture plates. The antimicrobial peptide was diluted with LB liquid medium to a range of concentrations (100. mu.g/mL, 50. mu.g/mL, 25. mu.g/mL, 12.5. mu.g/mL, 6.25. mu.g/mL, 3.12. mu.g/mL, 1.56. mu.g/mL, 0.78. mu.g/mL, 0.39. mu.g/mL, 0.20. mu.g/mL), 50. mu.L each was added to the medium, and LB liquid medium was used as a negative control. Shaking for 1min, mixing, incubating at 37 deg.C for 18-20 hr, and measuring OD with spectrophotometer₆₀₀The value is obtained. The test results were repeated several times to obtain more than 3 times of consistent data as a result to determine MIC values. Specific MIC results are shown in table 1 below.

TABLE 1 MIC assay results for antimicrobial peptides

	Staphylococcus aureus	Escherichia coli
			The antibacterial peptide of the invention	3.12μg/mL	6.25μg/mL
Original Cecropin P1 antibacterial peptide	12.5μg/mL	25μg/mL

Based on the results shown in table 1, the antibacterial peptide redesigned in the invention has good antibacterial activity on staphylococcus aureus and escherichia coli, and the MIC values of the antibacterial peptide are lower than those of the original Cecropin P1 antibacterial peptide, which indicates that the antibacterial peptide redesigned in the invention has relatively better antibacterial activity.

Example 2: preparation of small molecular weight chitosan and antibacterial activity detection

(1) Preparation of low molecular weight chitosan

Step one, dissolving high molecular weight chitosan: the viscosity average molecular weight is 3.0X 10⁵100g of high molecular weight chitosan with the deacetylation degree of 90.5 percent is dissolved in acetic acid solution with the volume fraction of 22 percent to obtain chitosan solution with the mass volume concentration of 25 percent (w/v);

step two, degrading high molecular weight chitosan: performing ultrasonic treatment on the chitosan solution prepared in the first step twice, wherein the temperature of the first ultrasonic treatment is 45 ℃, the time of the ultrasonic treatment is 4 hours, and the ultrasonic power is 600W; the temperature of the second ultrasonic treatment is 20 ℃, the time of the ultrasonic treatment is 5 hours, the ultrasonic power is 200W, and the micromolecular chitosan (the deacetylation degree is more than 95 percent) with the average relative molecular mass of 4000-;

step three, purifying the low molecular weight chitosan: and (3) dropwise adding a sodium bicarbonate solution into the micromolecular chitosan solution prepared in the step two, adjusting the pH value to 7.0-7.5, standing for 5h, centrifuging at 3000rpm for 10min, separating the precipitate, washing with water to be neutral, and drying to obtain the micromolecular chitosan powder.

In the research and development process, the influence of different first ultrasonic treatment temperatures on the degradation of chitosan is researched, and the following room temperature treatment process is taken as a control group 1, and the preparation process is as follows:

control group 1: step one, dissolving high molecular weight chitosan: the viscosity average molecular weight is 3.0X 10⁵100g of high molecular weight chitosan with the deacetylation degree of 90.5 percent is dissolved in acetic acid solution with the volume fraction of 22 percent to obtain chitosan solution with the mass volume concentration of 25 percent (w/v);

step two, degrading high molecular weight chitosan: performing ultrasonic treatment on the chitosan solution prepared in the first step twice, wherein the temperature of the first ultrasonic treatment is room temperature, the time of the ultrasonic treatment is 4 hours, and the ultrasonic power is 600W; the temperature of the second ultrasonic treatment is room temperature, the time of the ultrasonic treatment is 5 hours, the ultrasonic power is 200W, the chitosan of the contrast group 1 is prepared, the average relative molecular mass is 10000-12000 and the deacetylation degree is more than 92.2 percent through determination;

step three, purifying the low molecular weight chitosan: and (3) dropwise adding a sodium bicarbonate solution into the micromolecular chitosan solution prepared in the step two, adjusting the pH value to 7.0-7.5, standing for 5h, centrifuging at 3000rpm for 10min, separating the precipitate, washing with water to be neutral, and drying to obtain the chitosan powder of the control group 1.

(2) Detection of antibacterial activity of low molecular weight chitosan

Respectively dissolving the chitosan powder with the small molecular weight and the chitosan with the high molecular weight which are prepared by the method in sterile water to prepare a solution with the concentration of 1 mg/mL.

Staphylococcus aureus designated ATCC29213 and Escherichia coli designated ATCC25922 were used as standard bacteria for the antimicrobial activity test.

Respectively adding 0.1mL of bacteria solution to be detected (with the bacteria content of 10) cultured to logarithmic growth phase into test tubes of LB liquid culture medium⁸CFU/mL) and 0.1mL of chitosan solution, taking 0.1mL of physiological saline as a control group in a blank tube, incubating for 24 hours in a shaking table at 37 ℃, calculating the number of bacteria by adopting a flat plate counting method, and calculating the antibacterial rate according to an antibacterial formula. Wherein the antibacterial formula is as follows: antibacterial rate = (blank CFU-test CFU)/blank CFU 100%. The specific results are shown in Table 2 below.

TABLE 2 results of antimicrobial Activity detection of chitosans of different molecular masses

	Staphylococcus aureus	Escherichia coli
			Raw material high molecular weight chitosan	78.3%	72.5%
The invention relates to low molecular weight chitosan	99.3%	99.7%
			Chitosan for control group 1	85.5%	88.2%

Based on the results shown in the above table 2, the small molecular weight chitosan prepared by the invention has better antibacterial activity compared with the high molecular weight chitosan as the raw material, the antibacterial rate of the small molecular weight chitosan reaches 99.3% for staphylococcus aureus, and the antibacterial rate of the small molecular weight chitosan reaches 99.7% for escherichia coli, which indicates that the small molecular weight chitosan can effectively inhibit the growth of common pathogenic bacteria in silk fabric, and compared with the room temperature ultrasonic degradation of the control group 1, the ultrasonic temperature is properly increased in the ultrasonic preparation process of the small molecular weight chitosan, the chitosan with smaller average molecular weight is obtained under the same treatment condition, and the antibacterial activity is also greatly improved.

Example 3: preparation of antibacterial finishing agent

Weighing antibacterial peptide, low-molecular-weight chitosan and tea polyphenol according to parts by weight, dissolving the low-molecular-weight chitosan by adopting an acetic acid solution with the concentration of 5% (v/v) at 40 ℃, then cooling to room temperature, adding the antibacterial peptide and the tea polyphenol, and stirring for dissolving to obtain a solution A;

adding Tween 80 into the solution A, uniformly stirring, and adjusting the pH value to 3.0-4.0 to obtain a solution B;

and step three, gradually dripping a sodium tripolyphosphate solution with the concentration of 5g/L into the solution B in the step two at room temperature, and stirring at a high speed while dripping until the sodium tripolyphosphate solution is completely dripped, thus obtaining the antibacterial finishing liquid.

Wherein in the solution A in the first step, the concentration of the antibacterial peptide is 62.5 mg/L; the concentration of the low molecular weight chitosan is 6 g/L; the concentration of tea polyphenols is 10 g/L.

The final concentration of the Tween 80 in the solution B in the second step is 8 g/L;

in the third step, the volume ratio of the sodium tripolyphosphate solution to the solution B is 1: 49.

Example 4: preparation of antibacterial finishing agent

Weighing antibacterial peptide, low-molecular-weight chitosan and tea polyphenol according to parts by weight, dissolving the low-molecular-weight chitosan by adopting an acetic acid solution with the concentration of 5% (v/v) at 40 ℃, then cooling to room temperature, adding the antibacterial peptide and the tea polyphenol, and stirring for dissolving to obtain a solution A;

adding Tween 80 into the solution A, uniformly stirring, and adjusting the pH value to 3.0-4.0 to obtain a solution B;

and step three, gradually dripping a sodium tripolyphosphate solution with the concentration of 5g/L into the solution B in the step two at room temperature, and stirring at a high speed while dripping until the sodium tripolyphosphate solution is completely dripped, thus obtaining the antibacterial finishing liquid.

Wherein in the solution A in the first step, the concentration of the antibacterial peptide is 125 mg/L; the concentration of the low molecular weight chitosan is 8 g/L; the concentration of tea polyphenols is 12 g/L.

The final concentration of the Tween 80 in the solution B in the second step is 8 g/L;

in the third step, the volume ratio of the sodium tripolyphosphate solution to the solution B is 1: 49.

Example 5: antibacterial finishing method of silk fabric

Step one, taking silk fabric, immersing the silk fabric into clear water solution with the pH value of 8-8.5, soaking and swelling for 2 hours at 80 ℃ in a bath ratio of 1:50, taking out the silk fabric, washing the silk fabric with clear water, and naturally drying the silk fabric for later use;

step two, taking the antibacterial finishing agent, and diluting the antibacterial finishing agent by 50 times by using tap water to obtain antibacterial finishing liquid;

and step three, immersing the silk fabric dried in the step one into the antibacterial finishing liquid in the step two, carrying out ultrasonic treatment for 10 minutes at the bath ratio of 1:50 and the ultrasonic power of 100W/kg, then taking out, washing with clear water, and naturally drying to obtain the silk fabric.

Example 6: antibacterial finishing method of silk fabric

Step one, taking silk fabric, immersing the silk fabric into clear water solution with the pH value of 8-8.5, soaking and swelling for 2 hours at 80 ℃ in a bath ratio of 1:50, taking out the silk fabric, washing the silk fabric with clear water, and naturally drying the silk fabric for later use;

step two, taking the antibacterial finishing agent, and diluting the antibacterial finishing agent by 50 times by using tap water to obtain antibacterial finishing liquid;

and step three, immersing the silk fabric dried in the step one into the antibacterial finishing liquid in the step two, carrying out ultrasonic treatment for 20 minutes at the bath ratio of 1:50 and the ultrasonic power of 50W/kg, then taking out, washing with clear water, and naturally drying to obtain the silk fabric.

Example 6: measurement of wearability of Silk Fabric

In order to compare with the conventional finishing method of chitosan as an antibacterial finishing agent, the invention replaces the small molecular weight chitosan in the antibacterial finishing agent of the example 4 with the viscosity-average molecular weight of 3.0 multiplied by 10 in an equivalent manner⁵And the high molecular weight chitosan with the deacetylation degree of 90.5 percent, and other conditions were kept unchanged, and the antibacterial finishing agent of the control group 2 was prepared, and the influence of the antibacterial finishing agent of the present invention and the conventional finishing agent on the wearability of silk fabrics was compared in the following two aspects of air permeability and wrinkle resistance.

(1) Air permeability

The air permeability test is carried out by adopting an M021A digital fabric air permeability instrument, and the test area is 20cm²The pressure difference between two sides of the fabric is measured under the condition of 100Pa, each fabric is tested for 10 times, and the results are averaged. The specific test results are shown in Table 3 below.

(2) Resistance to wrinkle

With reference to GB/T3819-1997 determination of recovery angle of crease recovery of textile fabrics, the fabric compression load is (10 +/-0.5) N, the quick elastic recovery time is (15 +/-1) s, and the slow elastic recovery time is 5min +/-5 s. The warp and weft directions of each fabric were measured 3 times respectively and the average value was taken. The specific test results are shown in Table 3 below.

TABLE 3 measurement results of wearability of silk fabrics

	Air permeability (mm/s)	Acute elastic recovery angle	Slow elastic recovery angle
				Finishing agent of example 3	352 mm/s	248°	342°
Finishing agent of example 4	344 mm/s	231°	337°
				Control 2 (high molecular weight chitosan)	143 mm/s	183°	291°

Based on the results shown in table 3 above, it can be seen that the antibacterial finishing agent of the present invention uses low molecular weight chitosan as an active ingredient, compared to the conventional method using high molecular weight chitosan as an antibacterial finishing agent, so as to reduce the influence of chitosan molecules on the air permeability of the silk fabric, and simultaneously, has better wrinkle resistance compared to high molecular weight chitosan.

Example 7: determination of antibacterial Properties of Silk Fabric

In order to research the influence of ultrasonic treatment on the antibacterial activity of the silk fabric, the invention provides a finishing method without ultrasonic treatment for comparison, and the comparison method comprises the following steps:

control group 3: step one, taking silk fabric, immersing the silk fabric into clear water solution with the pH value of 8-8.5, soaking and swelling for 2 hours at 80 ℃ in a bath ratio of 1:50, taking out the silk fabric, washing the silk fabric with clear water, and naturally drying the silk fabric for later use; step two, taking the antibacterial finishing agent in embodiment 3 of the invention, and diluting the antibacterial finishing agent by 50 times by using tap water to obtain antibacterial finishing liquid; and step three, soaking the silk fabric dried in the step one in the antibacterial finishing liquid in the step two at a bath ratio of 1:50 for 2 hours, then taking out, washing with clear water, and naturally drying to obtain the silk fabric.

The antibacterial finishing methods of the embodiments 5 and 6 and the comparison group 3 are respectively adopted to carry out antibacterial finishing on the silk fabrics of the same batch, the selected finishing agents are the antibacterial finishing agents of the embodiment 3, and the silk fabrics after the antibacterial finishing are taken later, according to the evaluation part 3 of the antibacterial performance of the national standard GB/T20944.3-2008 textile fabrics: oscillation test "the antibacterial properties of the silk fabrics finished by the antibacterial finishing methods of examples 5 to 6 and control 3 were tested, using staphylococcus aureus No. ATCC29213 and escherichia coli No. ATCC25922 as standard bacteria for antibacterial activity detection, and fastness tests were performed simultaneously for 20 washes and 30 washes, and the test results are shown in table 4 below.

TABLE 4 antimicrobial Activity and fastness test results

Staphylococcus aureus	Example 5	Example 6	Control group 3
				After antibacterial finishing	99.3%	97.1%	85.3%
Washing with water for 20 times	85.7%	84.3%	62.4%
				Washing with water for 30 times	77.6%	77.3%	55.3%
Escherichia coli	Example 5	Example 6	Control group 3
				After antibacterial finishing	94.6%	93.5%	83.1%
Washing with water for 20 times	90.3%	86.4%	59.5%
				Washing with water for 30 times	83.3%	75.8%	35.4%

Based on the results shown in Table 4, the bacteriostatic rate of Staphylococcus aureus specified in the national standard is more than or equal to 70%, the standard that the antibacterial property is qualified is that the Escherichia coli is more than or equal to 60 percent, after the silk fabric is finished by the antibacterial finishing agent, the inhibition rate of the finishing agent on two kinds of bacteria is higher than 90%, which shows that the antibacterial finishing agent prepared by the invention has excellent antibacterial performance, however, compared with the method without ultrasonic treatment, the method adopting ultrasonic finishing in the antibacterial finishing method can better promote the adsorption of active ingredients in the antibacterial finishing agent and silk fibers, the fastness is better, after the silk fabrics which are treated by the antibacterial finishing methods of the embodiments 5 and 6 of the invention are subjected to fastness tests of 20 times of washing and 30 times of washing, the antibacterial finishing agent and the antibacterial finishing method can respectively reach the standard of qualified antibacterial property, and the results show that the antibacterial finishing agent and the antibacterial finishing method can effectively improve the antibacterial property of the silk fabric.

The above is only a preferred embodiment of the present invention, and a person skilled in the art can make several modifications and decorations without departing from the technical principle of the present invention, and these modifications and decorations should be regarded as the protection scope of the present invention.

Sequence listing

<110> Hunan-Ming-sleep family science and technology Limited

<120> antibacterial finishing method of silk fabric

<160> 2

<170> SIPOSequenceListing 1.0

<210> 1

<211> 31

<212> PRT

<213> Artificial Synthesis (Artificial Sequence)

<400> 1

Ser Trp Leu Ser Lys Thr Ala Lys Lys Leu Glu Lys Arg Ala Lys Lys

1 5 10 15

Arg Lys Ser Arg Gly Ile Ala Ile Ala Ile Gln Gly Gly Arg Arg

20 25 30

<210> 2

<211> 31

<212> PRT

<213> Artificial Synthesis (Artificial Sequence)

<400> 2

Ser Trp Leu Ser Lys Thr Ala Lys Lys Leu Glu Asn Ser Ala Lys Lys

1 5 10 15

Arg Ile Ser Glu Gly Ile Ala Ile Ala Ile Gln Gly Gly Pro Arg

20 25 30