CN118497919A - Viscose fiber containing jasmine active ingredient and preparation method thereof - Google Patents
Viscose fiber containing jasmine active ingredient and preparation method thereof Download PDFInfo
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- CN118497919A CN118497919A CN202410715327.0A CN202410715327A CN118497919A CN 118497919 A CN118497919 A CN 118497919A CN 202410715327 A CN202410715327 A CN 202410715327A CN 118497919 A CN118497919 A CN 118497919A
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- jasmine
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- 239000000835 fiber Substances 0.000 title claims abstract description 170
- 229920000297 Rayon Polymers 0.000 title claims abstract description 167
- 235000010254 Jasminum officinale Nutrition 0.000 title claims abstract description 151
- 239000004480 active ingredient Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 240000005385 Jasminum sambac Species 0.000 title 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 195
- 241000207840 Jasminum Species 0.000 claims abstract description 150
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 122
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000001263 FEMA 3042 Substances 0.000 claims abstract description 66
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims abstract description 66
- 229920002258 tannic acid Polymers 0.000 claims abstract description 66
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims abstract description 66
- 229940033123 tannic acid Drugs 0.000 claims abstract description 66
- 235000015523 tannic acid Nutrition 0.000 claims abstract description 66
- 239000000284 extract Substances 0.000 claims abstract description 63
- 238000009987 spinning Methods 0.000 claims abstract description 62
- 239000011787 zinc oxide Substances 0.000 claims abstract description 61
- 239000000805 composite resin Substances 0.000 claims abstract description 55
- 239000004005 microsphere Substances 0.000 claims abstract description 55
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052802 copper Inorganic materials 0.000 claims abstract description 19
- 239000010949 copper Substances 0.000 claims abstract description 19
- 238000011068 loading method Methods 0.000 claims abstract description 11
- 239000004753 textile Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 100
- 238000006243 chemical reaction Methods 0.000 claims description 44
- 238000005406 washing Methods 0.000 claims description 44
- 239000000047 product Substances 0.000 claims description 40
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 32
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 30
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 30
- 230000001112 coagulating effect Effects 0.000 claims description 30
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 24
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 23
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 22
- 238000007789 sealing Methods 0.000 claims description 17
- 235000005074 zinc chloride Nutrition 0.000 claims description 16
- 239000011592 zinc chloride Substances 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 230000000149 penetrating effect Effects 0.000 claims description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 14
- 238000005520 cutting process Methods 0.000 claims description 14
- 230000003009 desulfurizing effect Effects 0.000 claims description 14
- 238000007598 dipping method Methods 0.000 claims description 14
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- 238000005554 pickling Methods 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 238000007493 shaping process Methods 0.000 claims description 14
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 14
- 235000011152 sodium sulphate Nutrition 0.000 claims description 14
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 14
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 14
- 229960001763 zinc sulfate Drugs 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 12
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- 238000000034 method Methods 0.000 claims description 5
- 235000019256 formaldehyde Nutrition 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 238000009736 wetting Methods 0.000 claims description 2
- 230000036541 health Effects 0.000 abstract description 7
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- 238000009827 uniform distribution Methods 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 30
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- 238000002835 absorbance Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- GGUPMVXPXHZNKF-UHFFFAOYSA-N benzene-1,2-diol;formaldehyde Chemical compound O=C.OC1=CC=CC=C1O GGUPMVXPXHZNKF-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 239000002657 fibrous material Substances 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920003043 Cellulose fiber Polymers 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
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- 239000002699 waste material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 206010002198 Anaphylactic reaction Diseases 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 235000019750 Crude protein Nutrition 0.000 description 1
- IOEJYZSZYUROLN-UHFFFAOYSA-M Sodium diethyldithiocarbamate Chemical compound [Na+].CCN(CC)C([S-])=S IOEJYZSZYUROLN-UHFFFAOYSA-M 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 125000003172 aldehyde group Chemical group 0.000 description 1
- 208000003455 anaphylaxis Diseases 0.000 description 1
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- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- IWLXWEWGQZEKGZ-UHFFFAOYSA-N azane;zinc Chemical compound N.[Zn] IWLXWEWGQZEKGZ-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
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- -1 phenolic acid compounds Chemical class 0.000 description 1
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- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
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Landscapes
- Artificial Filaments (AREA)
Abstract
The invention provides a viscose fiber containing jasmine active ingredients and a preparation method thereof, wherein the raw materials comprise the following components in parts by weight: (0.15-0.55): (0.1-0.3) viscose spinning solution, jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres; the copper loading of the viscose fiber is 1.4-1.8mg/g. The viscose fiber containing the jasmine active ingredient is prepared by using the jasmine extract and the zinc oxide/tannic acid formaldehyde resin composite microsphere as raw materials and carrying copper, and the preparation method not only improves the preparation process of the fiber by optimizing the extraction and purification technology of the jasmine active ingredient, but also realizes the uniform distribution of the jasmine active ingredient in the fiber, prepares the viscose fiber with unique health function, and meets the double requirements of modern consumers on textile functionality and ecological environmental protection.
Description
Technical Field
The invention relates to the technical field of fiber manufacturing, in particular to a viscose fiber containing jasmine active ingredients and a preparation method thereof.
Background
Viscose is a regenerated cellulose fiber, and the raw material of the viscose is natural cellulose, such as wood, cotton linters and the like. The viscose fiber has excellent hygroscopicity, air permeability, softness and drapability, and is widely applied to the fields of clothing, home textiles, medical treatment and the like. However, conventional viscose fibers are relatively single in functionality, and it is difficult to meet the diversified demands of modern consumers.
The jasmine residue is waste generated after scenting jasmine tea. The seemingly useless residues contain rich nutritional values, including basic nutritional ingredients such as crude proteins, crude fats and the like, and various active substances such as polysaccharides, flavonoids, aromatic ingredients and the like. These actives impart a range of biological activities to jasmine slag, such as promoting growth, anti-inflammatory, antioxidant, and modulating the immune system. At present, only a small part of jasmine flower residues are used for extracting essential oil, and most of jasmine flower residues have low utilization rate, so that serious waste is caused.
With the improvement of the living standard of people and the pursuit of health, the application of natural plant extracts in the textile industry is becoming more and more widespread. Particularly, natural plant extracts with health care, antibacterial, deodorization and other functions, such as jasmine extracts, become popular directions for innovation and research of textile materials due to unique biological activity and good skin affinity. Although there have been studies on the application of jasmine extracts to textiles, most use the post-finishing approach, i.e. coating or impregnating the textile surface with jasmine extracts. On one hand, the extraction and purification technology of jasmine active ingredients is not mature enough, so that the purity and activity of the extract are difficult to ensure; on the other hand, the method of adding jasmine extract to fiber material is not scientific enough, resulting in uneven distribution of active ingredient in the fiber, affecting the functionality of the fiber.
The traditional fiber materials have certain limitations in terms of functionality and environmental protection, and cannot meet the dual requirements of modern consumers on the functionality and ecological environmental protection of textiles. Therefore, the viscose fiber containing the jasmine active ingredient and the preparation method thereof are developed, and the viscose fiber has important practical significance and wide market prospect.
Disclosure of Invention
The invention aims to provide a viscose fiber containing jasmine active ingredients and a preparation method thereof, which not only can ensure that the active ingredients are uniformly distributed in the fiber, but also can improve the stability of the active ingredients and enhance the functionality of the viscose fiber.
In one aspect, the invention provides a viscose fiber containing jasmine active ingredients, which comprises the following raw materials in parts by weight: (0.15-0.55): (0.1-0.3) viscose spinning solution, jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres; the copper loading of the viscose fiber is 1.4-1.8mg/g.
Further, the preparation method of the jasmine extract comprises the following steps: taking jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding ammonia water, and stirring until wetting; adding chloroform, sealing at 3-4deg.C, and cold soaking for 8-10 hr; then carrying out ice bath ultrasonic extraction at 0 ℃ for 50-70min, and filtering; washing the residue with chloroform, and mixing filtrates; recovering chloroform at 80-82 deg.C, and volatilizing chloroform to obtain flos Jasmini sambac extract.
Further, the usage ratio of the jasmine powder, the ammonia water and the chloroform is (26-30) g: (22-28) mL: (500-600) mL.
Further, the prepared jasmine extract is stored in a refrigerator at the temperature of-10 to 0 ℃.
Further, the preparation method of the zinc oxide/tannic acid formaldehyde resin composite microsphere comprises the following steps: adding tannic acid, zinc chloride, ammonia water, formaldehyde and polyethylene glycol into water, mixing and stirring at normal temperature, performing hydrothermal reaction for 4-5h at 180-200 ℃, cooling, centrifuging, washing and drying to obtain the zinc oxide/tannic acid formaldehyde resin composite microsphere.
Further, the dosage ratio of 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.
On the other hand, the invention also provides a preparation method of the viscose fiber containing the jasmine active ingredient, which comprises the following steps:
(1) Preparing jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres;
(2) Adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into viscose spinning solution to obtain spinning solution, and extruding and coagulating the spinning solution by a spray head to react with coagulating bath to obtain nascent fiber tows; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product;
(3) 1-2g of viscose fiber initial product is weighed and pretreated by 2-3g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.03-0.06mmol/L, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Further, the coagulating bath components in the step (2) are 90-100g/L sulfuric acid, 40-50g/L zinc sulfate and 220-260g/L sodium sulfate, the reaction temperature is 40-50 ℃, the spinning speed is 40-45m/min, and the dipping bath time is 0.5-1s.
Further, the reaction condition in the step (3) is that the reaction is carried out for 80-100min under the sealed condition and the temperature is 70-76 ℃.
Viscose fibres containing jasmine active ingredient are used in textiles.
The invention has the beneficial effects that:
(1) According to the preparation method, the extraction and purification technology of the jasmine active ingredients is optimized, the preparation process of the fiber is improved, the uniform distribution of the jasmine active ingredients in the fiber is realized, and the viscose fiber with unique health function is prepared.
(2) The antibacterial active ingredients (such as volatile oil, flavonoid and phenolic acid compounds) in the jasmine flower can improve the antibacterial performance of the viscose fiber, and the viscose fiber containing the jasmine active ingredients and having unique health functions is prepared by the invention, has various health functions such as softness, comfort and air permeability of the traditional viscose fiber, improves the compatibility of the viscose fiber and organisms (such as skin), and reduces irritation or anaphylactic reaction; can be widely applied to the fields of clothing, home textile, medical treatment and health, and the like, meets the requirements of people on healthy, environment-friendly and functional fiber materials, and can also effectively improve the utilization rate of jasmine flowers.
(3) The zinc oxide/tannic acid formaldehyde resin composite microsphere is synthesized by taking tannic acid, zinc chloride and formaldehyde as precursors through hydrothermal reaction. Wherein, tannic acid is catalyzed by ammonia water to perform a condensation reaction on formaldehyde in raining, and zinc chloride is changed into ZnO through a zinc-ammonia complex and a zinc hydroxide to zinc oxide process under the hydrothermal action; the ZnO is uniformly coated by the resin, so that the dispersibility of the ZnO in the viscose spinning solution is improved, and the antibacterial performance and the mechanical performance of the viscose fiber are effectively improved.
(4) The invention adds jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into viscose spinning solution to prepare a viscose fiber initial product, and uses penetrant JFC pretreatment and copper sulfate solution impregnation, the viscose fiber is used as a regenerated cellulose fiber, and a cellulose chain segment of the viscose fiber comprises a terminal group with reducibility and non-reducibility. Wherein the reducing end thereof is represented by a latent aldehyde group which is activated under specific conditions and undergoes oxidation-reduction reaction with the copper sulfate solution. By this reaction, tiny, nano-sized copper-based particles can be formed inside the fiber, giving the fiber a unique micro-nano structure. Finally, copper is loaded on the viscose fiber, so that the antibacterial capacity is improved, the mechanical property of the fiber can be improved, the stability of the jasmine active ingredient is effectively improved by the treated viscose fiber, and the antibacterial capacity can be kept to a certain degree even after the viscose fiber is washed with water.
(5) According to the invention, through the addition of the zinc oxide/tannic acid formaldehyde resin composite microsphere and the pre-treatment of the penetrating agent JFC in the copper loading process, the surface binding force between a load and viscose fiber is increased, and meanwhile, a network interpenetrating structure can be formed among components, so that the flame retardant component in the system can be fully reserved after washing, and the application range of the fiber is expanded.
Detailed Description
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Raw materials which are not illustrated in the following examples are all commercially available, wherein viscose spinning solution (the content of alpha-fiber is 9.3%) is purchased from Xingda chemical fiber company of Sanyou group of Tangshan; staphylococcus aureus was purchased from shanghai micro-tech limited and escherichia coli was purchased from shanghai micro-tech limited.
Example 1
The embodiment provides a viscose fiber containing jasmine active ingredients, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 28g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 25mL of ammonia water, and stirring until the jasmine flower powder is wet; 480mL of chloroform is added and sealed at 3 ℃ for cold soaking for 9 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 60min and filtering; the residue was washed 3 times with chloroform in a total amount of 60mL, and the filtrates were combined; recovering chloroform at 81 deg.C, volatilizing chloroform to obtain jasmine extract, and storing in refrigerator at-5 deg.C;
(2) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.3g of tannic acid, 0.07g of zinc chloride, 1.1g of ammonia water (26%), 0.9g of formaldehyde (containing methanol stabilizer, 37%) and 0.17g of polyethylene glycol into 110mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction at 190 ℃ for 4.5 hours, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1.5g of viscose fiber initial product is weighed and pretreated by 2.5g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.045mmol/L, carrying out heat preservation reaction for 90min at the temperature of 73 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
Test example 1 fiber copper-carrying test
Deionized water is used for preparing copper sulfate solution of 0.005, 0.010, 0.015, 0.020, 0.025 and 0.030mmol/L, diethyl sodium dithiocarbamate solution is used as a color developing agent, ammonia water is used for adjusting pH, and the absorbance is tested under the condition that the pH is 10. The absorbance was plotted against the concentration, and a standard curve equation of the absorbance Y versus the copper sulfate solution concentration X was calculated, with a linear fit of y=10.3309x+0.0002 (R 2 =0.999).
And testing the absorbance Y of the reacted copper sulfate solution, and calculating the concentration X of the reacted copper sulfate solution according to a standard curve equation. And calculating the copper carrying amount of the viscose fiber by using the formula (1), wherein the unit is mg/g.
Copper carrying amount= (C 0-C)VM×103/m type (1)
Wherein: c 0 is the initial concentration of the copper sulfate solution, mmol/L; c is the concentration of the copper sulfate solution after reaction and mol/L; v is the volume of the copper sulfate solution, L; m is the molar mass of copper, g/mmol; m is the mass of the viscose fiber and g.
The copper loading of the viscose fiber in this example was 1.6mg/g.
Example 2
The embodiment provides a viscose fiber containing jasmine active ingredients, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 27g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 26mL of ammonia water, and stirring until the mixture is wet; adding 490mL chloroform, sealing at 4 ℃ and cold soaking for 9 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 50min and filtering; the residue was washed 3 times with chloroform in a total amount of 60mL, and the filtrates were combined; recovering chloroform at 80deg.C, volatilizing chloroform to obtain flos Jasmini sambac extract, and storing in refrigerator at-10deg.C;
(2) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.2g of tannic acid, 0.08g of zinc chloride, 1.2g of ammonia water (26%), 1.0g of formaldehyde (containing methanol stabilizer, 37%) and 0.18g of polyethylene glycol into 115mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction for 4 hours at 195 ℃, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 3:0.15:0.1; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1g of viscose fiber initial product is weighed and pretreated by 2g/L penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.03mmol/L, carrying out heat preservation reaction for 80min at the temperature of 70 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 90g/L sulfuric acid, 40g/L zinc sulfate and 220g/L sodium sulfate, the reaction temperature is 40 ℃, the spinning speed is 40m/min, and the dipping bath time is 0.5s.
The copper loading of the viscose fiber in this example was 1.4mg/g.
Example 3
The embodiment provides a viscose fiber containing jasmine active ingredients, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 29g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 28mL of ammonia water, and stirring until the mixture is wet; adding 500mL chloroform, sealing at 4 ℃ and cold soaking for 10 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 70min and then filtering; the residue was washed 3 times with chloroform in a total amount of 100mL, and the filtrates were combined; recovering chloroform at 82 deg.C, volatilizing chloroform to obtain flos Jasmini sambac extract, and storing in refrigerator at-10deg.C;
(2) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.45g of tannic acid, 0.09g of zinc chloride, 1.2g of ammonia water (26%), 1.0g of formaldehyde (containing methanol stabilizer, 37%) and 0.2g of polyethylene glycol into 120mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction at 200 ℃ for 4 hours, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 5:0.55:0.3; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; weighing 2g of viscose fiber initial product, and pretreating with 3g/L penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.06mmol/L, carrying out heat preservation reaction for 80min at the temperature of 76 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 100g/L sulfuric acid, 50g/L zinc sulfate and 260g/L sodium sulfate, the reaction temperature is 50 ℃, the spinning speed is 45m/min, and the dipping bath time is 1s.
The copper loading of the viscose fiber in this example was 1.8mg/g.
Example 4
The embodiment provides a viscose fiber containing jasmine active ingredients, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 30g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 28mL of ammonia water, and stirring until the powder is wet; adding 450mL chloroform, sealing at 3 ℃ and cold soaking for 10 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 50min and filtering; the residue was washed 3 times with 90mL of chloroform, and the filtrates were combined; recovering chloroform at 82 deg.C, volatilizing chloroform to obtain flos Jasmini sambac extract, and storing in refrigerator at-5deg.C;
(2) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.45g of tannic acid, 0.08g of zinc chloride, 1.2g of ammonia water (26%), 1.0g of formaldehyde (containing methanol stabilizer, 37%) and 0.2g of polyethylene glycol into 120mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction at 180 ℃ for 5 hours, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 4:0.5:0.5; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; weighing 2g of viscose fiber initial product, and pretreating with 2g/L penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.05mmol/L, carrying out heat preservation reaction for 100min at the temperature of 70 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 250g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 40m/min, and the dipping bath time is 1s.
The copper loading of the viscose fiber in this example was 1.7mg/g.
Comparative example 1
The comparative example provides a viscose fiber containing jasmine active ingredient, which comprises the following preparation steps:
(1) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.3g of tannic acid, 0.07g of zinc chloride, 1.1g of ammonia water (26%), 0.9g of formaldehyde (containing methanol stabilizer, 37%) and 0.17g of polyethylene glycol into 110mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction at 190 ℃ for 4.5 hours, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(2) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1.5g of viscose fiber initial product is weighed and pretreated by 2.5g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.045mmol/L, carrying out heat preservation reaction for 90min at the temperature of 73 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
In this comparative example, the jasmine extract was commercially available (Jian Huaxin Natural plant Co., ltd.) and the final copper loading of the viscose fiber was 1.58mg/g.
Comparative example 2
The comparative example provides a viscose fiber, the preparation steps include:
(1) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.3g of tannic acid, 0.07g of zinc chloride, 1.1g of ammonia water (26%), 0.9g of formaldehyde (containing methanol stabilizer, 37%) and 0.17g of polyethylene glycol into 110mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction at 190 ℃ for 4.5 hours, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(2) Preparing viscose fiber: adding zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 4:0.2; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1.5g of viscose fiber initial product is weighed and pretreated by 2.5g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.045mmol/L, carrying out heat preservation reaction for 90min at the temperature of 73 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
Comparative example 3
The comparative example provides a viscose fiber containing jasmine active ingredient, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 28g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 25mL of ammonia water, and stirring until the jasmine flower powder is wet; 480mL of chloroform is added and sealed at 3 ℃ for cold soaking for 9 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 60min and filtering; the residue was washed 3 times with chloroform in a total amount of 60mL, and the filtrates were combined; recovering chloroform at 81 deg.C, volatilizing chloroform to obtain jasmine extract, and storing in refrigerator at-5 deg.C;
(2) Preparing zinc oxide/catechol formaldehyde resin composite microspheres: adding 1.3g catechol, 0.07g zinc chloride, 1.1g ammonia water (26%), 0.9g formaldehyde (containing methanol stabilizer, 37%) and 0.17g polyethylene glycol into 110mL water, mixing and stirring at normal temperature, performing hydrothermal reaction at 190 ℃ for 4.5h, cooling, centrifuging, washing and drying to obtain zinc oxide/catechol formaldehyde resin composite microspheres;
(3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/catechol formaldehyde resin composite microspheres into the viscose spinning solution to obtain a spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/catechol formaldehyde resin composite microspheres is 4:0.35:0.2; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1.5g of viscose fiber initial product is weighed and pretreated by 2.5g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.045mmol/L, carrying out heat preservation reaction for 90min at the temperature of 73 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
Comparative example 4
The comparative example provides a viscose fiber containing jasmine active ingredient, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 28g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 25mL of ammonia water, and stirring until the jasmine flower powder is wet; 480mL of chloroform is added and sealed at 3 ℃ for cold soaking for 9 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 60min and filtering; the residue was washed 3 times with chloroform in a total amount of 60mL, and the filtrates were combined; recovering chloroform at 81 deg.C, volatilizing chloroform to obtain jasmine extract, and storing in refrigerator at-5 deg.C;
(2) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide is 4:0.35:0.2; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1.5g of viscose fiber initial product is weighed and pretreated by 2.5g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.045mmol/L, carrying out heat preservation reaction for 90min at the temperature of 73 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
Comparative example 5
The comparative example provides a viscose fiber containing jasmine active ingredient, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 28g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 25mL of ammonia water, and stirring until the jasmine flower powder is wet; 480mL of chloroform is added and sealed at 3 ℃ for cold soaking for 9 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 60min and filtering; the residue was washed 3 times with chloroform in a total amount of 60mL, and the filtrates were combined; recovering chloroform at 81 deg.C, volatilizing chloroform to obtain jasmine extract, and storing in refrigerator at-5 deg.C;
(2) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract is 4:0.35; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1.5g of viscose fiber initial product is weighed and pretreated by 2.5g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.045mmol/L, carrying out heat preservation reaction for 90min at the temperature of 73 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
Comparative example 6
The comparative example provides a viscose fiber containing jasmine active ingredient, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 28g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 25mL of ammonia water, and stirring until the jasmine flower powder is wet; 480mL of chloroform is added and sealed at 3 ℃ for cold soaking for 9 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 60min and filtering; the residue was washed 3 times with chloroform in a total amount of 60mL, and the filtrates were combined; recovering chloroform at 81 deg.C, volatilizing chloroform to obtain jasmine extract, and storing in refrigerator at-5 deg.C;
(2) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.3g of tannic acid, 0.07g of zinc chloride, 1.1g of ammonia water (26%), 0.9g of formaldehyde (containing methanol stabilizer, 37%) and 0.17g of polyethylene glycol into 110mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction at 190 ℃ for 4.5 hours, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1.5g of viscose fiber initial product is weighed and pretreated by 2.5g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.10mmol/L, carrying out heat preservation reaction for 90min at the temperature of 73 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
The copper loading of the viscose fiber in this comparative example was 1.36mg/g.
Excessive copper-based particles in the comparative example are easy to agglomerate to form a barrier for preventing the copper sulfate solution from penetrating into the fiber, so that the copper loading amount on the viscose fiber is reduced, and the performance of the viscose fiber is reduced due to the agglomerated copper-based particles.
Comparative example 7
The comparative example provides a viscose fiber containing jasmine active ingredient, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 28g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 25mL of ammonia water, and stirring until the jasmine flower powder is wet; 480mL of chloroform is added and sealed at 3 ℃ for cold soaking for 9 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 60min and filtering; the residue was washed 3 times with chloroform in a total amount of 60mL, and the filtrates were combined; recovering chloroform at 81 deg.C, volatilizing chloroform to obtain jasmine extract, and storing in refrigerator at-5 deg.C;
(2) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.3g of tannic acid, 0.07g of zinc chloride, 1.1g of ammonia water (26%), 0.9g of formaldehyde (containing methanol stabilizer, 37%) and 0.17g of polyethylene glycol into 110mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction at 190 ℃ for 4.5 hours, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product; 1.5g of viscose fiber initial product is weighed and pretreated by 2.5g/L of penetrating agent AEP; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.45mmol/L, carrying out heat preservation reaction for 90min at the temperature of 73 ℃ in a sealing state, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
Comparative example 8
The comparative example provides a viscose fiber containing jasmine active ingredient, which comprises the following preparation steps:
(1) Preparing jasmine extract: taking 28g of jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding 25mL of ammonia water, and stirring until the jasmine flower powder is wet; 480mL of chloroform is added and sealed at 3 ℃ for cold soaking for 9 hours; then carrying out ice bath ultrasonic extraction at 0 ℃ for 60min and filtering; the residue was washed 3 times with chloroform in a total amount of 60mL, and the filtrates were combined; recovering chloroform at 81 deg.C, volatilizing chloroform to obtain jasmine extract, and storing in refrigerator at-5 deg.C;
(2) Preparing zinc oxide/tannic acid formaldehyde resin composite microspheres: adding 1.3g of tannic acid, 0.07g of zinc chloride, 1.1g of ammonia water (26%), 0.9g of formaldehyde (containing methanol stabilizer, 37%) and 0.17g of polyethylene glycol into 110mL of water, mixing and stirring at normal temperature, performing hydrothermal reaction at 190 ℃ for 4.5 hours, cooling, centrifuging, washing and drying to obtain zinc oxide/tannic acid formaldehyde resin composite microspheres;
(3) Preparing viscose fiber containing jasmine active ingredients: adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into the viscose spinning solution to obtain spinning solution, wherein the weight ratio of the viscose spinning solution to the jasmine extract to the zinc oxide/tannic acid formaldehyde resin composite microspheres is 4:0.35:0.2; extruding through a nozzle and reacting with a coagulating bath to obtain a nascent fiber tow; and (3) drawing, plasticizing and shaping the nascent fiber tows, and then cutting, pickling, desulfurizing and washing to obtain the viscose fiber containing the jasmine active ingredient.
Wherein the coagulating bath comprises 95g/L sulfuric acid, 45g/L zinc sulfate and 240g/L sodium sulfate, the reaction temperature is 45 ℃, the spinning speed is 42m/min, and the dipping bath time is 0.7s.
Test example 2: the performance of the viscose fibers containing jasmine active ingredient prepared in the foregoing examples 1 to 4 and comparative examples 1 to 8 was investigated, and the following tests were carried out:
flame retardant performance test: the limiting oxygen index of the fiber is measured according to FZ/T50016-2011 by adopting a limiting oxygen index instrument, and the higher the numerical value is, the better the flame retardant property is; and the limiting oxygen index after 200 washes was tested.
Mechanical property test: the tensile property is tested by adopting a fiber constant-speed elongation tensile testing machine according to GB/T14337-2022, a fiber is randomly clamped from a sample, the fiber is placed in a clamping device with specified tension, the fiber is ensured to extend along the axial direction, the fiber is stretched to break, and the breaking strength and breaking elongation of the fiber are measured; test samples were not less than 30, and the test average value was taken.
Antibacterial performance test: according to the method in GB/T209444.3-2008, the inhibition rate of each viscose fiber containing jasmine active ingredient to staphylococcus aureus and escherichia coli is tested, and the inhibition rate of each viscose fiber to staphylococcus aureus and escherichia coli is tested after 200 times of washing.
The test results are shown in table 1 below:
TABLE 1
The limiting oxygen index of the viscose fiber prepared in the embodiment is not lower than 37.7%, the dry breaking strength is 11.6-12.1cN/tex, the dry breaking elongation is 70-76%, the antibacterial rate is as high as 99.8%, the antibacterial rate is not lower than 84% after 200 times of washing, and the antibacterial performance and antibacterial retention performance are excellent.
Finally, it should be noted that: the above embodiments are only for illustrating the present invention and not for limiting the technical solution described in the present invention; it will be understood by those skilled in the art that the present invention may be modified or equivalents; all technical solutions and modifications thereof that do not depart from the spirit and scope of the present invention are intended to be included in the scope of the appended claims.
Claims (10)
1. The viscose fiber containing the jasmine active ingredient is characterized by comprising the following raw materials in parts by weight: (0.15-0.55): (0.1-0.3) viscose spinning solution, jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres; the copper loading of the viscose fiber is 1.4-1.8mg/g.
2. The viscose fiber containing jasmine active ingredient according to claim 1, wherein the preparation method of the jasmine extract comprises the following steps: taking jasmine flower powder which is dried to constant weight and passes through a 60-mesh sieve, adding ammonia water, and stirring until wetting; adding chloroform, sealing at 3-4deg.C, and cold soaking for 8-10 hr; then carrying out ice bath ultrasonic extraction at 0 ℃ for 50-70min, and filtering; washing the residue with chloroform, and mixing filtrates; recovering chloroform at 80-82 deg.C, and volatilizing chloroform to obtain flos Jasmini sambac extract.
3. The viscose fiber containing jasmine active ingredient according to claim 4, wherein the usage ratio of jasmine powder, ammonia water and chloroform is (26-30) g: (22-28) mL: (500-600) mL.
4. The viscose fiber containing jasmine active ingredient according to claim 2, wherein the prepared jasmine extract is stored in a refrigerator at-10-0 ℃.
5. The viscose fiber containing jasmine active ingredient of claim 1, wherein the preparation method of the zinc oxide/tannic acid formaldehyde resin composite microsphere comprises the following steps: adding tannic acid, zinc chloride, ammonia water, formaldehyde and polyethylene glycol into water, mixing and stirring at normal temperature, performing hydrothermal reaction for 4-5h at 180-200 ℃, cooling, centrifuging, washing and drying to obtain the zinc oxide/tannic acid formaldehyde resin composite microsphere.
6. The viscose fiber containing jasmine active ingredient according to claim 5, wherein the dosage ratio of 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.
7. A method for preparing a viscose fiber containing jasmine active ingredient according to any one of claims 1 to 6, characterized in that the steps comprise:
(1) Preparing jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres;
(2) Adding jasmine extract and zinc oxide/tannic acid formaldehyde resin composite microspheres into viscose spinning solution to obtain spinning solution, and extruding and coagulating the spinning solution by a spray head to react with coagulating bath to obtain nascent fiber tows; drawing, plasticizing and shaping the primary fiber tows, cutting off, pickling, desulfurizing and washing to obtain a viscose primary product;
(3) 1-2g of viscose fiber initial product is weighed and pretreated by 2-3g/L of penetrating agent JFC; immersing the pretreated viscose fiber initial product in a copper sulfate solution with the concentration of 0.03-0.06mmol/L, taking out and washing after the reaction is finished, and drying to obtain the viscose fiber containing the jasmine active ingredient.
8. The viscose fiber containing jasmine active ingredient according to claim 7, wherein the coagulating bath component in the step (2) is 90-100g/L sulfuric acid, 40-50g/L zinc sulfate, 220-260g/L sodium sulfate, the reaction temperature is 40-50 ℃, the spinning speed is 40-45m/min, and the dipping time is 0.5-1s.
9. The viscose fiber containing jasmine active ingredient according to claim 7, wherein the reaction condition in the step (3) is that the reaction is carried out for 80-100min under the condition of sealing and the temperature is 70-76 ℃.
10. Use of the viscose fiber containing jasmine active ingredient according to any one of claims 1 to 6 or the viscose fiber containing jasmine active ingredient prepared by the preparation method according to any one of claims 7 to 9 in textiles.
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| CN1952224A (en) * | 2006-10-25 | 2007-04-25 | 秦如涛 | Aromatic viscose fiber and its making method |
| CN103103801A (en) * | 2012-12-10 | 2013-05-15 | 苏州尊元纺织有限公司 | Production method of aromatic viscose fabric |
| JP2015224191A (en) * | 2014-05-26 | 2015-12-14 | 金星製紙株式会社 | Skin modifying sheet |
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