Cellulose fiber containing jasmine polyphenols, preparation method thereof, and fabric

Abstract

The present invention discloses a cellulose fiber containing jasmine polyphenols and its preparation method and fabric, and relates to the field of functional fiber technology. The method comprises the following steps: dissolving cotton pulp in a solvent, adding jasmine polyphenol-nanocellulose crystal complex, stirring evenly, and obtaining a spinning solution; passing the spinning solution through a deaeration process to remove bubbles in the spinning solution to obtain a deaerated spinning solution; extruding the deaerated spinning solution through the spinneret of a spinning machine to obtain a thin stream of spinning solution; sending the thin stream of spinning solution into a coagulation bath for solidification and molding to obtain nascent cellulose fiber; stretching, washing and drying the nascent cellulose fiber to obtain a cellulose fiber containing jasmine polyphenols. The present invention can stably bind jasmine polyphenols to the surface of cellulose fiber in large quantities and has good antibacterial persistence.

Description

Technical Field

[0001] The present invention relates to the technical field of high-performance fibers, in particular to cellulose fibers containing jasmine polyphenols and a preparation method thereof. Background Art

[0002] Jasmine polyphenol cellulose fiber is a functional fiber made by loading jasmine polyphenol onto cellulose fiber through a certain process with cellulose as the base material. The fabrics made from it have unique properties and application potential. Cellulose fiber is natural, environmentally friendly and has good hygroscopicity. Jasmine polyphenol is a natural polyphenol compound extracted from jasmine flowers. It has good biosafety and exhibits excellent antibacterial and bactericidal activity against common harmful bacteria such as Escherichia coli and Staphylococcus aureus. It can inhibit bacterial growth by destroying bacterial cell membranes and interfering with cell metabolism. The combination of the two gives the fiber natural antibacterial properties, so that the fabrics made from it not only retain the soft, breathable, skin-friendly and comfortable characteristics of cellulose fiber, but also have certain antibacterial functions. It has potential application value in the fields of medical care, daily clothing, home textiles, etc.

[0003] However, current cellulose fibers containing jasmine polyphenols and their fabrics have significant performance shortcomings. Due to limitations in the bonding method and process for jasmine polyphenols to cellulose fibers during fiber preparation, the amount of jasmine polyphenols loaded on the fibers is relatively low. On the one hand, in existing processes, jasmine polyphenols and cellulose fibers are mostly bonded through physical adsorption or simple hydrogen bonds and van der Waals forces. This weak interaction makes it difficult for jasmine polyphenols to adhere to the fiber surface and interior in large quantities and stably. On the other hand, the dense structure of cellulose fibers themselves and the complex internal pore structure hinder the full penetration and loading of jasmine polyphenols, resulting in insufficient content of effective antimicrobial ingredients. The low amount of jasmine polyphenol loaded directly leads to poor antimicrobial performance of the fabric. In actual use, the limited amount of jasmine polyphenols cannot consistently and effectively inhibit bacterial growth. Moreover, the small amount of jasmine polyphenols loaded is easily lost rapidly under the influence of the external environment (such as washing, friction, light, etc.), further weakening the antimicrobial ability of the fabric and failing to meet the market demand for high-performance, long-lasting antimicrobial textiles. Summary of the Invention

[0004] The present invention aims to provide a cellulose fiber containing jasmine polyphenols and a method for preparing the same, thereby resolving the technical issues raised in the prior art, such as the difficulty in attaching large amounts of jasmine polyphenols to the fiber surface and interior, and the poor antibacterial durability of the fabric. The present invention enables the stable attachment of large amounts of jasmine polyphenols to the cellulose fiber surface, while also providing excellent and durable antibacterial properties.

[0005] To achieve the above object, the present invention provides the following technical solutions:

[0006] A method for preparing cellulose fiber containing jasmine polyphenols comprises the following steps:

[0007] S1, dissolving cotton pulp in a solvent, adding jasmine polyphenol-nanocellulose crystal composite, and stirring evenly to obtain a spinning solution;

[0008] S2, degassing the spinning solution to remove bubbles in the spinning solution to obtain a degassing spinning solution;

[0009] S3, extruding the deaerated spinning solution through a spinneret of a spinning machine to obtain a thin stream of spinning solution;

[0010] S4, sending the spinning solution stream into a coagulation bath for solidification and forming to obtain nascent cellulose fibers;

[0011] S5. The nascent cellulose fibers are stretched, washed, and dried to obtain cellulose fibers containing jasmine polyphenols.

[0012] In the technical solution of the present invention, cotton pulp is dissolved as a raw material to form a spinning solution, and a jasmine polyphenol-nanocellulose crystal complex is added. The nanocellulose crystals have a high specific surface area and good dispersibility. The nanocellulose crystals are used as a carrier to form a complex with jasmine polyphenols, which is then added to the spinning base solution made by dissolving cotton pulp. This can significantly increase the loading of jasmine polyphenols on the fiber, giving the fiber excellent antioxidant and antibacterial properties. A degassing treatment eliminates bubbles to ensure uniformity and stability of the spinning solution. Fluid mechanics is used to extrude the degassing spinning solution into a thin stream. The cellulose phase is separated and solidified by the concentration difference in the coagulation bath. The fiber strength and toughness are then enhanced by stretching and orientation. The fiber is then washed to remove impurities and dried to stabilize its physical state, ultimately producing a jasmine polyphenol-containing cellulose fiber with excellent performance.

[0013] Preferably, in step S1, the amount of the jasmine polyphenol-nanocellulose crystal composite added is 2-5 wt% of the mass of the cotton pulp.

[0014] Preferably, in step S2, the vacuum degree is -0.08 to -0.1 MPa, and the degassing time is 30 to 60 minutes.

[0015] Preferably, in step S3, the extrusion pressure is 0.5-0.8 MPa.

[0016] Preferably, in step S4, the coagulation bath is a mixed solution of sulfuric acid and sodium sulfate, and the bath temperature is 40-50°C.

[0017] Preferably, in the step S5, the stretching ratio is 1.2 to 1.8 times.

[0018] Preferably, in step S1, the method for preparing the jasmine polyphenol-nanocellulose crystal composite comprises the following steps:

[0019] S11, treating the nanofiber crystals with an ammonium persulfate oxidation method to obtain carboxylated nanocellulose crystals;

[0020] S12, activating the carboxylated nanocellulose crystals with 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and N-hydroxysuccinimide, and then reacting with polyethyleneimine to obtain an amino-treated nanocellulose carrier;

[0021] S13, coupling the succinylated jasmine polyphenol to the amino-modified nanocellulose support via an amide bond to form a complex intermediate, thereby obtaining a complex intermediate;

[0022] S14. Forming a coating layer on the surface of the complex intermediate by a sodium alginate-calcium chloride cross-linking method to obtain a jasmine polyphenol-nanocellulose crystal complex.

[0023] In the technical solution of the present invention, the nanofiber crystals are first oxidized by ammonium persulfate to introduce carboxyl groups on their surface to provide active sites for subsequent reactions. The carboxyl groups are then activated by EDC / NHS and reacted with polyethyleneimine to obtain an amino carrier. Its "flexible amino arm" structure is conducive to capturing polyphenol molecules and the existence of hydrogen bonding forces between the two, thereby allowing a large amount of jasmine polyphenols to bind to the nanocellulose crystals. It is then incorporated into the spinning solution to impart antibacterial properties to the fiber. However, the problem encountered by the invention team during the research and development process is that after jasmine polyphenols are bound to the nanocellulose crystals, they are prone to agglomeration, which affects the improvement of the antibacterial properties of cellulose fibers by jasmine polyphenols. In order to solve this problem, the present invention forms a coating layer on the surface of the nanocellulose crystals after jasmine polyphenols are bound to the nanocellulose crystals by a sodium alginate-calcium chloride cross-linking method, so that its surface is negatively charged (the coating layer loads -COO - ), under the electrostatic repulsion force, the nanocellulose crystals repel each other, preventing jasmine polyphenols from binding to the nanocellulose crystals and agglomerating in the spinning solution, affecting its effect on improving the antibacterial properties of cellulose fibers. Figure 1 This is a scanning electron micrograph of a jasmine polyphenol-nanocellulose crystal complex. The nanocellulose crystals form a network structure interwoven with each other, and their surface is relatively rough, due to the presence of a calcium alginate coating.

[0024] Preferably, the preparation method of succinylated jasmine polyphenol comprises the following steps:

[0025] Jasmine flowers, jasmine leaves or jasmine branches are used as raw materials, which are crushed and then extracted with an ethanol aqueous solution, followed by vacuum distillation and freeze drying to obtain jasmine polyphenols.

[0026] The jasmine polyphenol and succinic anhydride are used as raw materials, the reaction is carried out under the protection of nitrogen with the catalysis of 4-dimethylaminopyridine, and the product is obtained after post-treatment.

[0027] In the technical solution of the present invention, as mentioned above, EDC / NHS is utilized to activate carboxyl groups, and reacted with polyethyleneimine to obtain an amino carrier. Its "flexible amino arm" structure is conducive to capturing polyphenol molecules and there is a hydrogen bond force between the two, thereby making a large amount of jasmine polyphenols be combined on the nanocellulose crystals. However, in use of fiber and fabric, jasmine polyphenols easily fall off from the fiber surface. The present invention is to further solve this problem, and succinylation is carried out to jasmine polyphenols. Succinylation is to introduce carboxyl functional groups on the jasmine polyphenol molecules by chemical modification, significantly improve its reactivity, and significantly increase its carboxyl content, thereby being able to efficiently condense with the amino group on the amino nanocellulose carrier surface to form a stable amide bond. Amide bond belongs to a covalent bond, has a higher bond energy, can resist the destruction of complex environmental factors such as acid and alkali, high temperature, mechanical external force, and effectively avoids the coming off and degradation of polyphenol molecules. At the same time, the formation of amide bonds allows jasmine polyphenols to be anchored on the nanocellulose carrier in the form of chemical bonds. Compared with physical adsorption or weak interactions, this significantly reduces the risk of polyphenol loss during processing such as spinning solution preparation, fiber forming, and subsequent use, giving it long-lasting antioxidant and antibacterial properties.

[0028] A cellulose fiber containing jasmine polyphenol is prepared by the above method.

[0029] A cellulose fiber fabric containing jasmine polyphenols is prepared from the cellulose fiber containing jasmine polyphenols.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] By using nanocellulose crystals as carriers, their high specific surface area and good dispersibility effectively increase the loading capacity of jasmine polyphenols on cellulose fibers. At the same time, the jasmine polyphenols are succinylated and activated with EDC / NHS and grafted with polyethyleneimine, allowing the polyphenols to bind to the nanocellulose crystals through stable amide bonds, forming a strong covalent bond. Compared to traditional physical adsorption methods, this chemically bonded structure can effectively resist the influence of complex environmental factors such as acidity and alkali, high temperature, and mechanical external forces. It greatly reduces the risk of jasmine polyphenols being lost during spinning solution preparation, fiber forming, and subsequent use, ensuring the long-term and stable performance of the fiber's antioxidant and antibacterial properties.

[0032] To address the problem of jasmine polyphenols easily agglomerating after binding to nanocellulose crystals, this patent uses a sodium alginate-calcium chloride crosslinking method to form a coating on the surface of the composite. This coating imparts a negative charge to the surface of the nanocellulose crystals. Based on the principle of electrostatic repulsion, it effectively prevents the agglomeration of nanoparticles in the spinning solution, ensuring the uniform dispersion of jasmine polyphenols in the fiber, thereby fully enhancing its antibacterial properties of cellulose fibers and avoiding functional failure caused by agglomeration. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is a scanning electron microscope image of the jasmine polyphenol-nanocellulose crystal complex. DETAILED DESCRIPTION

[0034] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the implementation regulations described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0035] Example 1

[0036] Preparation of succinylated jasmine polyphenols:

[0037] Step 1: Grind dried jasmine leaves through an 80-mesh sieve. Add 75% ethanol at a solid-liquid ratio of 1:20 (g / mL). Extract at 75±2°C with ultrasonic-reflux extraction for 60 minutes (ultrasound power 300W, 5s / 5s intermittent mode). Concentrate under reduced pressure to 1 / 10 of the original volume and freeze-dry at -40°C for 24 hours to obtain jasmine polyphenols.

[0038] Step 2: Dissolve 1.00 g of jasmine polyphenols in 50 mL of anhydrous pyridine, add 1.20 g of succinic anhydride and 0.10 g of DMAP catalyst, and react at 60 ± 1°C under nitrogen with magnetic stirring (500 rpm) for 8 hours. Slowly pour the reaction solution into 200 mL of glacial ether to precipitate. Centrifuge (6000 rpm, 10 min) and vacuum dry to obtain the product.

[0039] Preparation of jasmine polyphenol-nanocellulose crystal complex:

[0040] Step 1: Add 10.00 g of nanocellulose crystals (20-50 nm in diameter, 500-1000 nm in length) and 200 mL of ultrapure water to a three-necked flask. Ultrasonic dispersion was performed in an ice-water bath (power 200 W, frequency 40 kHz) for 30 minutes to form a uniform suspension. Slowly add 2.00 g of ammonium persulfate (purity ≥ 98%), heat to 65 ± 1°C in an oil bath, and stir at 300 rpm for 6 hours. After the reaction, cool to room temperature, transfer to a centrifuge tube, and centrifuge at 8000 rpm for 15 minutes. Discard the supernatant. Resuspend the precipitate in ultrapure water, transfer to a dialysis bag, and dialyze at 4°C for 48 hours. After dialysis, freeze-dry to obtain the carboxylated nanocellulose crystals.

[0041] Step 2: Dissolve 1.00 g of carboxylated nanocellulose crystals in 50 mL of PBS buffer (0.1 M, pH 6.0) in a conical flask. Add 0.15 g of EDC (purity ≥98%) and 0.10 g of NHS (purity ≥98%) and activate with stirring for 30 minutes in the dark. Then, slowly add a solution of 0.20 g of PEI (Mw = 2000 Da, purity ≥99%) in 10 mL of PBS dropwise. Purify the air with nitrogen. Seal the flask and shake at 25°C for 12 hours (150 rpm). Transfer the reaction mixture to a centrifuge tube and centrifuge at 8000 rpm for 20 minutes. Discard the filtrate, resuspend in ultrapure water, and repeat the centrifugation and washing process five times. Collect the retentate and lyophilize it to obtain the amino-modified nanocellulose carrier.

[0042] Step 3: Disperse 0.50 g of succinylated jasmine polyphenol and 0.30 g of amino-modified nanocellulose support in 100 mL of PBS buffer (0.01 M, pH 5.5). Add 0.45 g of an EDC / NHS mixture (molar ratio 1:1). Aerate with nitrogen and allow to react for 24 hours (25°C, 150 rpm) in the dark. After the reaction, load the solution onto a gel column and elute with ultrapure water at a flow rate of 1 mL / min. The collected solution is lyophilized to obtain the complex intermediate.

[0043] Step 4: Disperse 0.20 g of the complex intermediate in 20 mL of a 1 wt% sodium alginate solution and sonicate for 5 minutes (100 W, 40 kHz). Add 6.4 mL of a 5 wt% CaCl₂ solution dropwise at 0.5 mL / min while stirring mechanically at 100 rpm, and allow the cross-linking reaction to proceed for 20 minutes. After the reaction, centrifuge at 4000 rpm for 10 minutes, collect the precipitate, and wash three times with ultrapure water. The precipitate is dispersed in 10 mL of ultrapure water, aliquoted into lyophilized vials, pre-frozen at -50°C for 4 hours, and then freeze-dried under vacuum for 24 hours to obtain the jasmine polyphenol-nanocellulose composite.

[0044] A method for preparing cellulose fiber containing jasmine polyphenols comprises the following steps:

[0045] Step 1: Add 20.00g of cotton pulp and 400mL of an 87wt% NMMO aqueous solution to a three-necked flask. Purge with nitrogen. Raise the temperature to 85±1°C and stir at 200 rpm for 4 hours until the cotton pulp is completely dissolved. Cool to 45°C, add 0.80g of jasmine polyphenol-nanocellulose crystal complex, and continue stirring for 3 hours to form a uniform spinning solution.

[0046] Step 2: Transfer the spinning solution to a rotary evaporator, maintain a water bath temperature of 25°C, turn on the vacuum pump, adjust the vacuum degree to -0.09 MPa, and degas for 50 minutes.

[0047] Step 3: Inject the degassed spinning solution into the spinning machine barrel, connect it to a 100-hole spinneret (pore size 0.1 mm), and extrude it under a nitrogen pressure of 0.6 MPa to form a spinning stream.

[0048] Step 4: The spinning stream is fed into a coagulation bath (a mixed solution of 5wt% H2SO4 and 20wt% Na2SO4) at 45°C. The spinning speed is set at 10m / min. After the filaments remain in the coagulation bath for 90 seconds, they are drawn out through a godet to obtain nascent cellulose fibers.

[0049] Step 5: The spun fibers were heat-stretched at a draw ratio of 1.6 (stretching temperature 60°C). The fibers were then washed in a washing tank with 60°C deionized water (water to fiber mass ratio 50:1) for 15 minutes. The washed fibers were dried in a vacuum drying oven at 60°C to a moisture content of ≤5% and rolled to obtain cellulose fibers containing jasmine polyphenols.

[0050] Example 2

[0051] The preparation of succinylated jasmine polyphenol was the same as in Example 1.

[0052] The preparation of jasmine polyphenol-nanocellulose crystal composite was the same as in Example 1.

[0053] A method for preparing cellulose fiber containing jasmine polyphenols comprises the following steps:

[0054] Step 1: Add 20.00g of cotton pulp and 400mL of an 87wt% NMMO aqueous solution to a three-necked flask. Purge with nitrogen. Raise the temperature to 85±1°C and stir at 200 rpm for 4 hours until the cotton pulp is completely dissolved. Cool to 45°C, add 0.50g of the jasmine polyphenol-nanocellulose crystal complex, and continue stirring for 3 hours to form a uniform spinning solution.

[0055] Step 2: Transfer the spinning solution to a rotary evaporator, maintain a water bath temperature of 25°C, turn on the vacuum pump, adjust the vacuum degree to -0.09 MPa, and degas for 50 minutes.

[0056] Step 3: Inject the degassed spinning solution into the spinning machine barrel, connect it to a 100-hole spinneret (pore size 0.1 mm), and extrude it under a nitrogen pressure of 0.6 MPa to form a spinning stream.

[0057] Step 4: The spinning stream is fed into a coagulation bath (a mixed solution of 5wt% H2SO4 and 20wt% Na2SO4) at 45°C. The spinning speed is set at 10m / min. After the filaments remain in the coagulation bath for 90 seconds, they are drawn out through a godet to obtain nascent cellulose fibers.

[0058] Step 5: The spun fibers were heat-stretched at a draw ratio of 1.3 (stretching temperature 60°C). The fibers were then washed in a washing tank with 60°C deionized water (water to fiber mass ratio 50:1) for 15 minutes. The washed fibers were dried in a vacuum drying oven at 60°C to a moisture content of ≤5% and rolled to obtain cellulose fibers containing jasmine polyphenols.

[0059] Example 3

[0060] The preparation of succinylated jasmine polyphenol was the same as in Example 1.

[0061] The preparation of jasmine polyphenol-nanocellulose crystal composite was the same as in Example 1.

[0062] A method for preparing cellulose fiber containing jasmine polyphenols comprises the following steps:

[0063] Step 1: Add 20.00g of cotton pulp and 400mL of an 87wt% NMMO aqueous solution to a three-necked flask. Purge with nitrogen. Raise the temperature to 85±1°C and stir at 200 rpm for 4 hours until the cotton pulp is completely dissolved. Cool to 45°C, add 0.7g of jasmine polyphenol-nanocellulose crystal complex, and continue stirring for 3 hours to form a uniform spinning solution.

[0064] Step 2: Transfer the spinning solution to a rotary evaporator, maintain a water bath temperature of 25°C, turn on the vacuum pump, adjust the vacuum degree to -0.09 MPa, and degas for 50 minutes.

[0065] Step 3: Inject the degassed spinning solution into the spinning machine barrel, connect it to a 100-hole spinneret (pore size 0.1 mm), and extrude it under a nitrogen pressure of 0.6 MPa to form a spinning stream.

[0066] Step 4: The spinning stream is fed into a coagulation bath (a mixed solution of 5wt% H2SO4 and 20wt% Na2SO4) at 45°C. The spinning speed is set at 10m / min. After the filaments remain in the coagulation bath for 90 seconds, they are drawn out through a godet to obtain nascent cellulose fibers.

[0067] Step 5: The spun fibers were heat-stretched at a draw ratio of 1.5 (stretching temperature 60°C). The fibers were then washed in a washing tank with 60°C deionized water (water to fiber mass ratio 50:1) for 15 minutes. The washed fibers were dried in a vacuum drying oven at 60°C to a moisture content of ≤5% and rolled to obtain cellulose fibers containing jasmine polyphenols.

[0068] Example 4

[0069] The preparation of succinylated jasmine polyphenol was the same as in Example 1.

[0070] The preparation of jasmine polyphenol-nanocellulose crystal composite was the same as in Example 1.

[0071] A method for preparing cellulose fiber containing jasmine polyphenols comprises the following steps:

[0072] Step 1: Add 20.00g of cotton pulp and 400mL of an 87wt% NMMO aqueous solution to a three-necked flask. Purge with nitrogen. Raise the temperature to 85±1°C and stir at 200rpm for 4 hours until the cotton pulp is completely dissolved. Cool to 45°C, add 1.00g of jasmine polyphenol-nanocellulose crystal complex, and continue stirring for 3 hours to form a uniform spinning solution.

[0073] Step 2: Transfer the spinning solution to a rotary evaporator, maintain a water bath temperature of 25°C, turn on the vacuum pump, adjust the vacuum degree to 0.1 MPa, and degas for 60 minutes.

[0074] Step 3: Inject the degassed spinning solution into the spinning machine barrel, connect it to a 100-hole spinneret (pore size 0.1 mm), and extrude it under a nitrogen pressure of 0.8 MPa to form a spinning stream.

[0075] Step 4: The spinning stream is fed into a coagulation bath (a mixed solution of 5wt% H2SO4 and 20wt% Na2SO4) at 50°C. The spinning speed is set at 10m / min. After the filaments remain in the coagulation bath for 90 seconds, they are drawn out through a godet to obtain nascent cellulose fibers.

[0076] Step 5: The spun fibers were heat-stretched at a draw ratio of 1.8 (stretching temperature 60°C). The fibers were then washed in a washing tank with 60°C deionized water (water to fiber mass ratio 50:1) for 15 minutes. The washed fibers were dried in a vacuum drying oven at 60°C to a moisture content of ≤5% and rolled to obtain cellulose fibers containing jasmine polyphenols.

[0077] Example 5

[0078] The preparation of succinylated jasmine polyphenol was the same as in Example 1.

[0079] The preparation of jasmine polyphenol-nanocellulose crystal composite was the same as in Example 1.

[0080] A method for preparing cellulose fiber containing jasmine polyphenols comprises the following steps:

[0081] Step 1: Add 20.00g of cotton pulp and 400mL of an 87wt% NMMO aqueous solution to a three-necked flask. Purge with nitrogen. Raise the temperature to 85±1°C and stir at 200 rpm for 4 hours until the cotton pulp is completely dissolved. Cool to 45°C, add 0.40g of jasmine polyphenol-nanocellulose crystal complex, and continue stirring for 3 hours to form a uniform spinning solution.

[0082] Step 2: Transfer the spinning solution to a rotary evaporator, maintain a water bath temperature of 25°C, turn on the vacuum pump, adjust the vacuum degree to -0.08 MPa, and degas for 30 minutes.

[0083] Step 3: Inject the degassed spinning solution into the spinning machine barrel, connect it to a 100-hole spinneret (pore size 0.1 mm), and extrude it under a nitrogen pressure of 0.5 MPa to form a spinning stream.

[0084] Step 4: The spinning stream is fed into a coagulation bath (a mixed solution of 5wt% H2SO4 and 20wt% Na2SO4) at 40°C. The spinning speed is set at 10m / min. After the filaments remain in the coagulation bath for 90 seconds, they are drawn out through a godet to obtain nascent cellulose fibers.

[0085] Step 5: The spun fibers were heat-stretched at a draw ratio of 1.2 (stretching temperature 60°C). The fibers were then washed in a washing tank with 60°C deionized water (water to fiber mass ratio 50:1) for 15 minutes. The washed fibers were dried in a vacuum drying oven at 60°C to a moisture content of ≤5% and rolled to obtain cellulose fibers containing jasmine polyphenols.

[0086] Comparative Example 1

[0087] The difference between Comparative Example 1 and Example 1 is that the jasmine polyphenol-nanocellulose crystal composite is replaced with jasmine polyphenol during the preparation of the cellulose fiber.

[0088] Comparative Example 2

[0089] The difference between Comparative Example 2 and Example 1 is that step 4 is omitted during the preparation of the jasmine polyphenol-nanocellulose crystal composite, that is, the jasmine polyphenol-nanocellulose is not coated with calcium alginate.

[0090] Comparative Example 3

[0091] The difference between Comparative Example 3 and Example 1 is that succinylated jasmine polyphenol is replaced with ordinary jasmine polyphenol during the preparation of the jasmine polyphenol-nanocellulose crystal composite.

[0092] Performance testing:

[0093] The fibers prepared in each embodiment and comparative example were first equilibrated in an environment with a temperature of 20-25°C and a relative humidity of 65%±2% for 24 hours to remove short fibers and impurities. The pretreated fibers were then blended with cotton fibers in a ratio of 6:4 and spun into 32-count yarns through the following steps: opening and cleaning, carding, drawing, roving, and spinning. The yarns were then wound and warped, and the warp yarns were sized with a polyacrylic acid sizing agent. The fabric samples were then woven using a rapier loom with a plain weave to obtain the fabric samples.

[0094] 1. Antibacterial performance test: The test was conducted according to GB / T 20944.3-2008 Evaluation of antibacterial properties of textiles Part 3: Oscillation method. Five 2cm×2cm fabric samples were placed in a suspension containing Escherichia coli (ATCC 8739) and Staphylococcus aureus (ATCC 6538) (concentration of about 1×10 5 CFU / mL) in conical flasks and shake-culture at 37°C and 180 rpm for 18 hours. After incubation, the bacterial suspension was diluted appropriately and spread onto nutrient agar. After incubation at 37°C for 24 hours, colonies were counted. The antibacterial rate was calculated as follows: Antibacterial rate (%) = (AB) / A × 100%, where A is the colony count of the blank control sample and B is the colony count of the treated sample. The test results are shown in Table 1.

[0095] 2. Mechanical Properties: Referring to GB / T 3923.1-2013 Textiles—Tensile Properties of Fabrics—Part 1: Determination of Breaking Force and Elongation (Strip Method), fabrics were cut into 5 cm wide and 25 cm long specimens. Testing was performed on a Constant Rate of Elongation (CRE) electronic universal testing machine with a clamp distance of 20 cm and a tensile speed of 100 mm / min. Each specimen was tested five times, and the breaking strength was calculated using the average value. The test results are shown in Table 1.

[0096] 3. Durability Testing: Following GB / T 8629-2017 Textile Testing - Household Washing and Drying Procedures, use a standard detergent (concentration 2g / L) and perform 30 wash cycles at 40°C. After 30 wash cycles, repeat the E. coli antibacterial performance test described above, and record the performance retention rate to evaluate the stability of jasmine polyphenols on the fabric. The test results are shown in Table 1.

[0097] Table 1:

[0098]

[0099] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing cellulose fiber containing jasmine polyphenols, characterized in that: The following steps are involved: S1, dissolving cotton pulp in a solvent, adding jasmine polyphenol-nanocellulose crystal composite, and stirring evenly to obtain a spinning solution; S2, degassing the spinning solution to remove bubbles in the spinning solution to obtain a degassing spinning solution; S3, extruding the deaerated spinning solution through a spinneret of a spinning machine to obtain a thin stream of spinning solution; S4, sending the spinning solution stream into a coagulation bath for solidification and forming to obtain nascent cellulose fibers; S5, stretching, washing, and drying the nascent cellulose fibers to obtain cellulose fibers containing jasmine polyphenols; The preparation method of the jasmine polyphenol-nanocellulose crystal composite comprises the following steps: S11, treating the nanofiber crystals with an ammonium persulfate oxidation method to obtain carboxylated nanocellulose crystals; S12, activating the carboxylated nanocellulose crystals with 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride and N-hydroxysuccinimide, and then reacting with polyethyleneimine to obtain an amino-treated nanocellulose carrier; S13, coupling the succinylated jasmine polyphenol to the amino-modified nanocellulose support via an amide bond to form a complex intermediate, thereby obtaining a complex intermediate; S14. Forming a coating layer on the surface of the complex intermediate by a sodium alginate-calcium chloride cross-linking method to obtain a jasmine polyphenol-nanocellulose crystal complex.

2. The method for preparing cellulose fiber containing jasmine polyphenols according to claim 1, wherein: In the step S1, the amount of the jasmine polyphenol-nanocellulose crystal composite added is 2-5 wt% of the mass of the cotton pulp.

3. The method for preparing cellulose fiber containing jasmine polyphenols according to claim 1, wherein: In step S2, the vacuum degree is -0.08 to -0.1 MPa, and the degassing time is 30 to 60 minutes.

4. The method for preparing cellulose fiber containing jasmine polyphenols according to claim 1, wherein: In step S3, the extrusion pressure is 0.5-0.8 MPa.

5. The method for preparing cellulose fiber containing jasmine polyphenols according to claim 1, wherein: In step S4, the coagulation bath is a mixed solution of sulfuric acid and sodium sulfate, and the bath temperature is 40-50°C.

6. The method for preparing cellulose fiber containing jasmine polyphenols according to claim 1, characterized in that: In the step S5, the stretching ratio is 1.2 to 1.8 times.

7. The method for preparing cellulose fiber containing jasmine polyphenols according to claim 1, characterized in that: The preparation method of the succinylated jasmine polyphenol comprises the following steps: Jasmine flowers, jasmine leaves or jasmine branches are used as raw materials, which are crushed and then extracted with an ethanol aqueous solution, followed by vacuum distillation and freeze drying to obtain jasmine polyphenols. The jasmine polyphenol and succinic anhydride are used as raw materials, the reaction is carried out under the protection of nitrogen with the catalysis of 4-dimethylaminopyridine, and the product is obtained after post-treatment.

8. A cellulose fiber containing jasmine polyphenols, characterized in that: The method is prepared by any one of claims 1 to 7.

9. A cellulose fiber fabric containing jasmine polyphenols, characterized in that: The invention is prepared from the cellulose fiber containing jasmine polyphenols according to claim 8.

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