Viscose fiber containing jasmine active ingredient and preparation method thereof

Abstract

The present invention provides a viscose fiber containing jasmine active ingredients and a preparation method thereof, wherein the raw materials include a viscose spinning solution, a jasmine extract and a zinc oxide / tannic acid formaldehyde resin composite microsphere having a weight ratio of (3-5): (0.15-0.55): (0.1-0.3); the viscose fiber has a copper loading of 1.4-1.8 mg / g. The viscose fiber containing jasmine active ingredients prepared by the present invention uses jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres as raw materials and is loaded with copper. The preparation method of the present invention not only optimizes the extraction and purification technology of jasmine active ingredients, improves the preparation process of the fiber, realizes the uniform distribution of jasmine active ingredients in the fiber, and prepares a viscose fiber with unique health functions, which meets the dual needs of modern consumers for textile functionality and ecological environmental protection.

Description

Technical Field

[0001] The invention relates to the technical field of fiber manufacturing, and in particular to viscose fiber containing jasmine active ingredients and a preparation method thereof. Background Art

[0002] Viscose fiber is a regenerated cellulose fiber, and its raw material is natural cellulose, such as wood, cotton linters, etc. Viscose fiber has excellent moisture absorption, breathability, softness and drape, and is widely used in clothing, home textiles, medical and other fields. However, traditional viscose fiber is relatively single in functionality and it is difficult to meet the diversified needs of modern consumers.

[0003] Jasmine residue is the waste produced after making jasmine tea. These seemingly useless residues are actually rich in nutritional value, including basic nutrients such as crude protein and crude fat, as well as a variety of active substances such as polysaccharides, flavonoids, and aromatic components. These active substances give jasmine residue a series of biological activities, such as promoting growth, anti-inflammatory, antioxidant, and regulating the immune system. At present, only a small amount of jasmine residue is used to extract essential oils, and most of them have a low utilization rate, resulting in serious waste.

[0004] With the improvement of people's living standards and the pursuit of health, natural plant extracts are being used more and more widely in the textile industry. In particular, natural plant extracts with health care, antibacterial, deodorant and other functions, such as jasmine extracts, have become a hot direction for innovation and research and development of textile materials due to their unique biological activity and good skin affinity. Although some studies have tried to apply jasmine extracts to textiles, most of them use post-finishing methods, that is, coating or impregnating jasmine extracts on the surface of textiles. On the one hand, the extraction and purification technology of jasmine active ingredients is not mature enough, which makes it difficult to ensure the purity and activity of the extracts; on the other hand, the method of adding jasmine extracts to fiber materials is not scientific enough, resulting in uneven distribution of active ingredients in the fiber, affecting the functionality of the fiber.

[0005] Traditional fiber materials have certain limitations in functionality and environmental protection, and cannot meet the dual demands of modern consumers for textile functionality and ecological environmental protection. Therefore, the development of a viscose fiber containing jasmine active ingredients and a preparation method thereof has important practical significance and broad market prospects. Summary of the invention

[0006] The purpose of the present invention is to provide a viscose fiber containing jasmine active ingredients and a preparation method thereof. The present invention can not only make the active ingredients evenly distributed in the fiber, but also improve the stability of the active ingredients and enhance the functionality of the viscose fiber.

[0007] On the one hand, the present invention provides a viscose fiber containing jasmine active ingredients, the raw materials comprising viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres in a weight ratio of (3-5): (0.15-0.55): (0.1-0.3); the copper loading amount of the viscose fiber is 1.4-1.8 mg / g.

[0008] Furthermore, the preparation method of the jasmine extract comprises: taking jasmine powder dried to constant weight and passed through a 60-mesh sieve, adding ammonia water and stirring until moistened; adding chloroform and sealing at 3-4°C for cold soaking for 8-10 hours; then performing ice bath ultrasonic extraction at 0°C for 50-70 minutes and filtering; washing the residue with chloroform and combining the filtrate; recovering chloroform at 80-82°C, and evaporating the chloroform to obtain the jasmine extract.

[0009] Furthermore, the usage ratio of the jasmine powder, ammonia water and chloroform is (26-30) g: (22-28) mL: (500-600) mL.

[0010] Furthermore, the prepared jasmine extract is stored in a -10-0°C refrigerator.

[0011] Furthermore, the preparation method of the zinc oxide / tannic acid formaldehyde resin composite microspheres comprises: adding tannic acid, zinc chloride, ammonia water, formaldehyde and polyethylene glycol into water, mixing and stirring at room temperature, performing a hydrothermal reaction at 180-200° C. for 4-5 hours, centrifuging after cooling, washing and drying to obtain the zinc oxide / tannic acid formaldehyde resin composite microspheres.

[0012] Furthermore, the dosage ratio of the tannic acid, zinc chloride, ammonia water, formaldehyde, polyethylene glycol and water is (1.15-1.45) g: (0.05-0.09) g: (1.0-1.2) g: (0.8-1.0) g: (0.14-0.2) g: (100-120) mL.

[0013] On the other hand, the present invention also provides a method for preparing viscose fiber containing jasmine active ingredients, the steps comprising:

[0014] (1) preparing jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0015] (2) adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to a viscose spinning solution to obtain a spinning solution, extruding the solution through a nozzle and reacting it with a coagulation bath to obtain a primary fiber bundle; the primary fiber bundle is stretched, plasticized and shaped, and then cut, pickled, desulfurized and washed to obtain a primary viscose fiber product;

[0016] (3) Weighing 1-2 g of a viscose fiber product, pre-treating it with 2-3 g / L of a penetrant JFC; immersing the pre-treated viscose fiber product in a copper sulfate solution having a concentration of 0.03-0.06 mmol / L, taking it out after the reaction is completed, washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0017] Furthermore, in step (2), the coagulation bath components are 90-100 g / L sulfuric acid, 40-50 g / L zinc sulfate, and 220-260 g / L sodium sulfate, the reaction temperature is 40-50° C., the spinning rate is 40-45 m / min, and the immersion time is 0.5-1 s.

[0018] Furthermore, the reaction conditions in step (3) are to keep the reaction in a sealed state at a temperature of 70-76° C. for 80-100 minutes.

[0019] Viscose fibers containing jasmine active ingredients are used in textiles.

[0020] The beneficial effects of the present invention are:

[0021] (1) In the present invention, different raw materials and components are configured to prepare viscose fiber, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres are used as raw materials, and copper is loaded. The preparation method of the present invention not only improves the fiber preparation process by optimizing the extraction and purification technology of jasmine active ingredients, but also realizes the uniform distribution of jasmine active ingredients in the fiber, thereby preparing viscose fiber with unique health functions.

[0022] (2) The antibacterial active ingredients in jasmine (such as volatile oils, flavonoids, and phenolic acid compounds) improve the antibacterial properties of viscose fibers. The present invention prepares viscose fibers containing jasmine active ingredients with unique health functions. The fibers not only have multiple health functions of traditional viscose fibers such as softness, comfort, and breathability, but also improve the compatibility of viscose fibers with organisms (such as skin) and reduce irritation or allergic reactions. They can be widely used in clothing, home textiles, medical and health fields, meet people's needs for healthy, environmentally friendly and functional fiber materials, and effectively improve the utilization rate of jasmine.

[0023] (3) The present invention uses tannic acid, zinc chloride and formaldehyde as precursors to synthesize zinc oxide / tannic acid formaldehyde resin composite microspheres through hydrothermal reaction. Tannic acid reacts with formaldehyde under the catalysis of ammonia water, and zinc chloride is converted into ZnO through the process of zinc-ammine complex, zinc hydroxide and zinc oxide under the action of hydrothermal reaction. There is a strong interaction force between the two, so that ZnO is evenly coated by the resin, which improves its dispersibility in the viscose spinning solution, thereby effectively improving the antibacterial and mechanical properties of viscose fibers.

[0024] (4) The present invention adds jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to the viscose spinning solution to obtain the initial product of viscose fiber, and uses the penetrant JFC for pretreatment and copper sulfate solution impregnation. As a regenerated cellulose fiber, the cellulose segment of the viscose fiber contains both reducing and non-reducing terminal groups. Among them, its reducing end is in the form of a potential aldehyde group, which can be activated under specific conditions and undergo a redox reaction with the copper sulfate solution. Through this reaction, tiny, nano-scale copper-based particles can be formed inside the fiber, thereby giving the fiber a unique micro-nano structure. In the end, not only is copper loaded on the viscose fiber to improve the antibacterial ability, but the mechanical properties of the fiber can also be improved. The treated viscose fiber effectively improves the stability of the jasmine active ingredients and can maintain a certain antibacterial ability even after washing.

[0025] (5) The present invention increases the surface bonding force between the load and the viscose fiber by adding zinc oxide / tannic acid formaldehyde resin composite microspheres and pre-treating with the penetrant JFC during the copper loading process. At the same time, a network interpenetrating structure can be formed between the components, so that the flame retardant components in the system can be fully retained after washing, thereby expanding the scope of use of the fiber. DETAILED DESCRIPTION

[0026] The technical solution of the present invention is described clearly and completely below. Obviously, the described embodiments 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 creative work are within the scope of protection of the present invention.

[0027] All raw materials not specified in the following examples are commercially available, among which, viscose spinning solution (acetone content 9.3%) was purchased from Tangshan Sanyou Group Xingda Chemical Fiber Co., Ltd.; Staphylococcus aureus was purchased from Shanghai Luwei Technology Co., Ltd., and Escherichia coli was purchased from Shanghai Luwei Technology Co., Ltd.

[0028] Example 1

[0029] This embodiment provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0030] (1) Preparation of jasmine extract: 28 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 25 mL of aqueous ammonia and stirred until moistened; 480 mL of chloroform was added and sealed at 3° C. for 9 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 60 min and then filtered; the residue was rinsed with a total of 60 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 81° C. and evaporated to dryness to obtain jasmine extract, which was stored in a -5° C. refrigerator;

[0031] (2) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.3 g of tannic acid, 0.07 g of zinc chloride, 1.1 g of ammonia water (26%), 0.9 g of formaldehyde (containing methanol stabilizer, 37%) and 0.17 g of polyethylene glycol were added to 110 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 190° C. for 4.5 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0032] (3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, cutting, pickling, desulfurization and washing the primary fiber bundle to obtain a viscose fiber primary product; weighing 1.5g of the primary viscose fiber product, pre-treating it with 2.5g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.045mmol / L, and keeping it warm for reaction at 73°C for 90min in a sealed state; after the reaction is completed, taking it out and washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0033] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0034] Test Example 1 Fiber Copper Loading Test

[0035] Deionized water was used to prepare 0.005, 0.010, 0.015, 0.020, 0.025, and 0.030 mmol / L copper sulfate solutions, sodium diethyldithiocarbamate solution was used as a color developer, and the pH was adjusted with ammonia water. The absorbance was tested at a pH of 10. The absorbance was plotted against the concentration, and the standard curve equation of absorbance Y and copper sulfate solution concentration X was calculated. The linear fitting relationship was Y=10.3309X+0.0002(R 2 =0.999).

[0036] The absorbance Y of the copper sulfate solution after the reaction is tested, and the concentration X of the copper sulfate solution after the reaction is calculated according to the standard curve equation. The copper loading of the viscose fiber is then calculated using formula (1) in mg / g.

[0037] Copper loading = (C0-C)VM×10 3 / m formula (1)

[0038] In the formula: C0 is the initial concentration of copper sulfate solution, mmol / L; C is the concentration of copper sulfate solution after reaction, mol / L; V is the volume of copper sulfate solution, L; M is the molar mass of copper, g / mmol; m is the mass of viscose fiber, g.

[0039] In this embodiment, the copper loading of the viscose fiber is 1.6 mg / g.

[0040] Example 2

[0041] This embodiment provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0042] (1) Preparation of jasmine extract: 27 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 26 mL of aqueous ammonia and stirred until moistened; 490 mL of chloroform was added and sealed and refrigerated at 4° C. for 9 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 50 min and then filtered; the residue was rinsed with a total of 60 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 80° C. and evaporated to dryness to obtain jasmine extract, which was stored in a -10° C. refrigerator;

[0043] (2) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.2 g tannic acid, 0.08 g zinc chloride, 1.2 g ammonia water (26%), 1.0 g formaldehyde (containing methanol stabilizer, 37%) and 0.18 g polyethylene glycol were added to 115 mL water, mixed and stirred at room temperature, and hydrothermally reacted at 195° C. for 4 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0044] (3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres is 3:0.15:0.1; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, cutting, pickling, desulfurization and washing the primary fiber bundle to obtain a viscose fiber primary product; weighing 1 g of the viscose fiber primary product, pre-treating it with 2 g / L of penetrant JFC; immersing the pre-treated viscose fiber primary product in a copper sulfate solution with a concentration of 0.03 mmol / L, and keeping it warm for reaction for 80 minutes under a sealed state and a temperature of 70°C. After the reaction is completed, taking it out and washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0045] The coagulation bath components are 90 g / L sulfuric acid, 40 g / L zinc sulfate, and 220 g / L sodium sulfate, the reaction temperature is 40°C, the spinning rate is 40 m / min, and the immersion time is 0.5 s.

[0046] In this embodiment, the copper loading of the viscose fiber is 1.4 mg / g.

[0047] Example 3

[0048] This embodiment provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0049] (1) Preparation of jasmine extract: 29 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 28 mL of aqueous ammonia and stirred until moistened; 500 mL of chloroform was added, sealed and refrigerated at 4° C. for 10 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 70 min and then filtered; the residue was rinsed with a total of 100 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 82° C. and evaporated to dryness to obtain a jasmine extract, which was stored in a refrigerator at -10° C.;

[0050] (2) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.45 g of tannic acid, 0.09 g of zinc chloride, 1.2 g of ammonia water (26%), 1.0 g of formaldehyde (containing methanol stabilizer, 37%) and 0.2 g of polyethylene glycol were added to 120 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 200° C. for 4 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0051] (3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres is 5:0.55:0.3; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, cutting, pickling, desulfurization and washing the primary fiber bundle to obtain a viscose fiber primary product; weighing 2g of the primary viscose fiber product, pre-treating it with 3g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.06mmol / L, and keeping it warm for reaction at 76°C for 80min in a sealed state; after the reaction is completed, taking it out and washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0052] The coagulation bath components are 100 g / L sulfuric acid, 50 g / L zinc sulfate, and 260 g / L sodium sulfate, the reaction temperature is 50°C, the spinning rate is 45 m / min, and the immersion time is 1 s.

[0053] In this embodiment, the copper loading of the viscose fiber is 1.8 mg / g.

[0054] Example 4

[0055] This embodiment provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0056] (1) Preparation of jasmine extract: 30 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve is added with 28 mL of aqueous ammonia and stirred until moistened; 450 mL of chloroform is added and sealed at 3° C. for 10 h; then ultrasonic extraction is performed in an ice bath at 0° C. for 50 min and then filtered; the residue is rinsed with a total of 90 mL of chloroform three times and the filtrate is combined; chloroform is recovered at 82° C. and evaporated to dryness to obtain a jasmine extract, which is stored in a -5° C. refrigerator;

[0057] (2) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.45 g of tannic acid, 0.08 g of zinc chloride, 1.2 g of ammonia water (26%), 1.0 g of formaldehyde (containing methanol stabilizer, 37%) and 0.2 g of polyethylene glycol were added to 120 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 180° C. for 5 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0058] (3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres is 4:0.5:0.5; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, cutting, pickling, desulfurization and washing the primary fiber bundle to obtain a viscose fiber primary product; weighing 2g of the primary viscose fiber product, pre-treating it with 2g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.05mmol / L, and keeping it warm for reaction at 70°C for 100min in a sealed state, taking it out after the reaction is completed, washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0059] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 250 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 40 m / min, and the immersion time is 1 s.

[0060] In this embodiment, the copper loading of the viscose fiber is 1.7 mg / g.

[0061] Comparative Example 1

[0062] This comparative example provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0063] (1) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.3 g of tannic acid, 0.07 g of zinc chloride, 1.1 g of ammonia water (26%), 0.9 g of formaldehyde (containing methanol stabilizer, 37%) and 0.17 g of polyethylene glycol were added to 110 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 190° C. for 4.5 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0064] (2) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, cutting, pickling, desulfurization and washing the primary fiber bundle to obtain a viscose fiber primary product; weighing 1.5g of the primary viscose fiber product, pre-treating it with 2.5g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.045mmol / L, and keeping it warm for reaction at 73°C for 90min in a sealed state; after the reaction is completed, taking it out and washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0065] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0066] In this comparative example, the jasmine extract was commercially available (Ji'an Huaxin Natural Plant Co., Ltd.), and the final copper loading of the viscose fiber was 1.58 mg / g.

[0067] Comparative Example 2

[0068] This comparative example provides a viscose fiber, and the preparation steps include:

[0069] (1) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.3 g of tannic acid, 0.07 g of zinc chloride, 1.1 g of ammonia water (26%), 0.9 g of formaldehyde (containing methanol stabilizer, 37%) and 0.17 g of polyethylene glycol were added to 110 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 190° C. for 4.5 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0070] (2) Preparing viscose fiber: adding zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution to zinc oxide / tannic acid formaldehyde resin composite microspheres is 4:0.2; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; the primary fiber bundle is stretched, plasticized and shaped, and then cut and pickled, desulfurized and washed with water to obtain a primary viscose fiber product; weighing 1.5 g of the primary viscose fiber product, and pre-treating it with 2.5 g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.045 mmol / L, and reacting it at a temperature of 73°C for 90 minutes in a sealed state, taking it out after the reaction is completed, washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0071] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0072] Comparative Example 3

[0073] This comparative example provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0074] (1) Preparation of jasmine extract: 28 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 25 mL of aqueous ammonia and stirred until moistened; 480 mL of chloroform was added and sealed at 3° C. for 9 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 60 min and then filtered; the residue was rinsed with a total of 60 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 81° C. and evaporated to dryness to obtain jasmine extract, which was stored in a -5° C. refrigerator;

[0075] (2) Preparation of zinc oxide / catechol formaldehyde resin composite microspheres: 1.3 g of catechol, 0.07 g of zinc chloride, 1.1 g of ammonia water (26%), 0.9 g of formaldehyde (containing methanol stabilizer, 37%) and 0.17 g of polyethylene glycol were added to 110 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 190° C. for 4.5 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / catechol formaldehyde resin composite microspheres;

[0076] (3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / catechol formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / catechol formaldehyde resin composite microspheres is 4:0.35:0.2; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, cutting, pickling, desulfurization and washing the primary fiber bundle to obtain a viscose fiber primary product; weighing 1.5g of the primary viscose fiber product, pre-treating it with 2.5g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.045mmol / L, and keeping it warm for reaction at 73°C for 90min in a sealed state; after the reaction is completed, taking it out and washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0077] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0078] Comparative Example 4

[0079] This comparative example provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0080] (1) Preparation of jasmine extract: 28 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 25 mL of aqueous ammonia and stirred until moistened; 480 mL of chloroform was added and sealed at 3° C. for 9 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 60 min and then filtered; the residue was rinsed with a total of 60 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 81° C. and evaporated to dryness to obtain jasmine extract, which was stored in a -5° C. refrigerator;

[0081] (2) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide is 4:0.35:0.2; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping the primary fiber bundle, cutting, pickling, desulfurization and water washing are performed to obtain a primary viscose fiber product; weighing 1.5 g of the primary viscose fiber product, pre-treating it with 2.5 g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.045 mmol / L, and keeping it warm for reaction for 90 minutes under a sealed state and a temperature of 73°C. After the reaction is completed, taking it out and washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0082] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0083] Comparative Example 5

[0084] This comparative example provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0085] (1) Preparation of jasmine extract: 28 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 25 mL of aqueous ammonia and stirred until moistened; 480 mL of chloroform was added and sealed at 3° C. for 9 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 60 min and then filtered; the residue was rinsed with a total of 60 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 81° C. and evaporated to dryness to obtain jasmine extract, which was stored in a -5° C. refrigerator;

[0086] (2) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution to jasmine extract is 4:0.35; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; the primary fiber bundle is stretched, plasticized and shaped, and then cut and pickled, desulfurized and washed with water to obtain a primary viscose fiber product; weighing 1.5 g of the primary viscose fiber product, and pre-treating it with 2.5 g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.045 mmol / L, and reacting it at a temperature of 73°C for 90 minutes in a sealed state, taking it out after the reaction is completed, washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0087] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0088] Comparative Example 6

[0089] This comparative example provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0090] (1) Preparation of jasmine extract: 28 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 25 mL of aqueous ammonia and stirred until moistened; 480 mL of chloroform was added and sealed at 3° C. for 9 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 60 min and then filtered; the residue was rinsed with a total of 60 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 81° C. and evaporated to dryness to obtain jasmine extract, which was stored in a -5° C. refrigerator;

[0091] (2) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.3 g of tannic acid, 0.07 g of zinc chloride, 1.1 g of ammonia water (26%), 0.9 g of formaldehyde (containing methanol stabilizer, 37%) and 0.17 g of polyethylene glycol were added to 110 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 190° C. for 4.5 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0092] (3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, cutting, pickling, desulfurization and washing the primary fiber bundle to obtain a viscose fiber primary product; weighing 1.5 g of the primary viscose fiber product, pre-treating it with 2.5 g / L of penetrant JFC; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.10 mmol / L, and keeping it warm for reaction at 73°C for 90 minutes in a sealed state; after the reaction is completed, taking it out and washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0093] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0094] The copper loading of the viscose fiber in this comparative example is 1.36 mg / g.

[0095] In this comparative example, too many copper-based particles tend to agglomerate, forming a barrier that prevents the copper sulfate solution from penetrating into the interior of the fiber, ultimately resulting in a reduction in the copper loading on the viscose fiber. At the same time, the agglomerated copper-based particles also cause the performance of the viscose fiber to decline.

[0096] Comparative Example 7

[0097] This comparative example provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0098] (1) Preparation of jasmine extract: 28 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 25 mL of aqueous ammonia and stirred until moistened; 480 mL of chloroform was added and sealed at 3° C. for 9 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 60 min and then filtered; the residue was rinsed with a total of 60 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 81° C. and evaporated to dryness to obtain jasmine extract, which was stored in a -5° C. refrigerator;

[0099] (2) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.3 g of tannic acid, 0.07 g of zinc chloride, 1.1 g of ammonia water (26%), 0.9 g of formaldehyde (containing methanol stabilizer, 37%) and 0.17 g of polyethylene glycol were added to 110 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 190° C. for 4.5 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0100] (3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, cutting, pickling, desulfurization and washing the primary fiber bundle to obtain a viscose fiber primary product; weighing 1.5 g of the primary viscose fiber product, pre-treating it with 2.5 g / L of penetrant AEP; immersing the pre-treated primary viscose fiber product in a copper sulfate solution with a concentration of 0.45 mmol / L, and keeping it warm for reaction at 73°C for 90 minutes in a sealed state; after the reaction is completed, taking it out and washing it with water, and drying it to obtain the viscose fiber containing the jasmine active ingredient.

[0101] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0102] Comparative Example 8

[0103] This comparative example provides a viscose fiber containing jasmine active ingredients, and the preparation steps include:

[0104] (1) Preparation of jasmine extract: 28 g of jasmine powder dried to constant weight and passed through a 60-mesh sieve was added with 25 mL of aqueous ammonia and stirred until moistened; 480 mL of chloroform was added and sealed at 3° C. for 9 h; then ultrasonic extraction was performed in an ice bath at 0° C. for 60 min and then filtered; the residue was rinsed with a total of 60 mL of chloroform for 3 times and the filtrate was combined; chloroform was recovered at 81° C. and evaporated to dryness to obtain jasmine extract, which was stored in a -5° C. refrigerator;

[0105] (2) Preparation of zinc oxide / tannic acid formaldehyde resin composite microspheres: 1.3 g of tannic acid, 0.07 g of zinc chloride, 1.1 g of ammonia water (26%), 0.9 g of formaldehyde (containing methanol stabilizer, 37%) and 0.17 g of polyethylene glycol were added to 110 mL of water, mixed and stirred at room temperature, and hydrothermally reacted at 190° C. for 4.5 h. After cooling, centrifugation, washing and drying were performed to obtain zinc oxide / tannic acid formaldehyde resin composite microspheres;

[0106] (3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, wherein the weight ratio of viscose spinning solution, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding from a nozzle and reacting with a coagulation bath to obtain a primary fiber bundle; after drawing, plasticizing and shaping, the primary fiber bundle is cut and pickled, desulfurized and washed with water to obtain viscose fiber containing jasmine active ingredients.

[0107] The coagulation bath components are 95 g / L sulfuric acid, 45 g / L zinc sulfate, and 240 g / L sodium sulfate, the reaction temperature is 45°C, the spinning rate is 42 m / min, and the immersion time is 0.7 s.

[0108] Test Example 2: The properties of the viscose fibers containing jasmine active ingredients prepared in the above Examples 1-4 and Comparative Examples 1-8 were investigated, and the following tests were performed:

[0109] Flame retardant performance test: Use a limiting oxygen index instrument to measure the limiting oxygen index of the fiber according to FZ / T50016--2011. The higher the value, the better the flame retardant performance; and test the limiting oxygen index after washing 200 times.

[0110] Mechanical properties test: The tensile properties are tested using a fiber constant rate elongation tensile testing machine in accordance with GB / T 14337--2022. A fiber is randomly clamped from the sample and placed in a clamping device with a specified tension to ensure that the fiber extends axially. The fiber is stretched until it breaks, and its breaking strength and elongation at break are measured. No less than 30 specimens are tested, and the test average value is taken.

[0111] Antibacterial performance test: According to the method in GB / T20944.3-2008, the inhibition rate of each viscose fiber containing jasmine active ingredients on Staphylococcus aureus and Escherichia coli was tested, and the inhibition rate on Staphylococcus aureus and Escherichia coli was tested after washing 200 times.

[0112] The test results are shown in Table 1 below:

[0113] Table 1

[0114]

[0115] The viscose fiber prepared in the above embodiment has a limiting oxygen index of not less than 37.7%, a dry breaking strength of 11.6-12.1 cN / tex, a dry breaking elongation of 70-76%, and an antibacterial rate of up to 99.8%. After 200 washes, the antibacterial rate is not less than 84%, and the antibacterial performance and antibacterial retention performance are excellent.

[0116] Finally, it should be noted that the above embodiments are only used to illustrate the present invention and are not intended to limit the technical solutions described in the present invention. Those skilled in the art should understand that the present invention can still be modified or replaced by equivalents. All technical solutions and improvements that do not depart from the spirit and scope of the present invention should be included in the scope of the claims of the present invention.

Claims

1. A viscose fiber containing jasmine active ingredients, characterized in that: The raw materials include viscose spinning liquid, jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres in a weight ratio of (3-5): (0.15-0.55): (0.1-0.3); the copper loading of the viscose fiber is 1.4-1.8 mg / g; the preparation method of the jasmine extract includes: taking jasmine powder dried to constant weight and passed through a 60-mesh sieve, adding ammonia water and stirring until wet; adding chloroform and sealing at 3-4°C for cold soaking for 8-10 hours; then extracting by ultrasonic extraction in an ice bath at 0°C for 50-70 minutes and filtering; washing the residue with chloroform and combining the filtrate; recovering the chloroform at 80-82°C, and waiting for the chloroform to evaporate to dryness to obtain the jasmine extract; The preparation steps of the viscose fiber containing jasmine active ingredients include: (1) Preparation of jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres; (2) adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, extruding from a nozzle and reacting with a coagulation bath to obtain primary fiber bundles; the primary fiber bundles are drawn, plasticized and shaped, and then cut, pickled, desulfurized and washed to obtain the primary product of viscose fiber; (3) Weigh 1-2 g of viscose fiber product and pretreat it with 2-3 g / L of penetrant JFC; immerse the pretreated viscose fiber product in a copper sulfate solution with a concentration of 0.03-0.06 mmol / L, take it out after the reaction is completed, wash it with water, and dry it to obtain the viscose fiber containing jasmine active ingredients.

2. The viscose fiber containing jasmine active ingredients according to claim 1, characterized in that: The dosage ratio of the jasmine powder, ammonia water and chloroform is (26-30) g: (22-28) mL: (500-600) mL.

3. The viscose fiber containing jasmine active ingredients according to claim 1, characterized in that: The prepared jasmine extract is stored in a -10-0°C refrigerator.

4. The viscose fiber containing jasmine active ingredients according to claim 1, characterized in that: The preparation method of the zinc oxide / tannic acid formaldehyde resin composite microspheres comprises: adding tannic acid, zinc chloride, ammonia water, formaldehyde and polyethylene glycol into water, mixing and stirring at room temperature, performing hydrothermal reaction at 180-200° C. for 4-5 hours, centrifuging after cooling, washing and drying to obtain the zinc oxide / tannic acid formaldehyde resin composite microspheres.

5. The viscose fiber containing jasmine active ingredients according to claim 4, characterized in that: The dosage ratio of the tannic acid, zinc chloride, ammonia water, formaldehyde, polyethylene glycol and water is (1.15-1.45) g: (0.05-0.09) g: (1.0-1.2) g: (0.8-1.0) g: (0.14-0.2) g: (100-120) mL.

6. A method for preparing viscose fiber containing jasmine active ingredients as claimed in any one of claims 1 to 5, characterized in that the steps include: (1) Preparation of jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres; (2) adding jasmine extract and zinc oxide / tannic acid formaldehyde resin composite microspheres to viscose spinning solution to obtain spinning solution, extruding from a nozzle and reacting with a coagulation bath to obtain primary fiber bundles; the primary fiber bundles are drawn, plasticized and shaped, and then cut, pickled, desulfurized and washed to obtain the primary product of viscose fiber; (3) Weigh 1-2 g of viscose fiber product and pretreat it with 2-3 g / L of penetrant JFC; immerse the pretreated viscose fiber product in a copper sulfate solution with a concentration of 0.03-0.06 mmol / L, take it out after the reaction is completed, wash it with water, and dry it to obtain the viscose fiber containing jasmine active ingredients.

7. The method for preparing viscose fiber containing jasmine active ingredients according to claim 6, characterized in that: In step (2), the coagulation bath components are 90-100 g / L sulfuric acid, 40-50 g / L zinc sulfate, and 220-260 g / L sodium sulfate, the reaction temperature is 40-50° C., the spinning rate is 40-45 m / min, and the immersion time is 0.5-1 s.

8. The method for preparing viscose fiber containing jasmine active ingredients according to claim 6, characterized in that: The reaction conditions in step (3) are to carry out the reaction in a sealed state at a temperature of 70-76° C. for 80-100 minutes.

9. Use of the viscose fiber containing jasmine active ingredients according to any one of claims 1 to 5 or the viscose fiber containing jasmine active ingredients prepared by the preparation method according to any one of claims 7 to 8 in textiles.

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