CN113152083A - Silk macrobiological fiber containing tea polyphenol and preparation method thereof - Google Patents
Silk macrobiological fiber containing tea polyphenol and preparation method thereof Download PDFInfo
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- CN113152083A CN113152083A CN202110475636.1A CN202110475636A CN113152083A CN 113152083 A CN113152083 A CN 113152083A CN 202110475636 A CN202110475636 A CN 202110475636A CN 113152083 A CN113152083 A CN 113152083A
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- 239000000835 fiber Substances 0.000 title claims abstract description 159
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 152
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 150
- 241001122767 Theaceae Species 0.000 title claims abstract 31
- 238000002360 preparation method Methods 0.000 title abstract description 35
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 104
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 239000002608 ionic liquid Substances 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 33
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 30
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 30
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 239000012071 phase Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 22
- 230000004048 modification Effects 0.000 claims description 22
- 238000012986 modification Methods 0.000 claims description 22
- 238000002791 soaking Methods 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 13
- 239000003054 catalyst Substances 0.000 claims description 11
- 239000007822 coupling agent Substances 0.000 claims description 11
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 239000012266 salt solution Substances 0.000 claims description 9
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims description 7
- 239000008346 aqueous phase Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000001307 helium Substances 0.000 claims description 7
- 229910052734 helium Inorganic materials 0.000 claims description 7
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 7
- 239000004033 plastic Substances 0.000 claims description 7
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 4
- 238000000605 extraction Methods 0.000 abstract description 13
- 239000004753 textile Substances 0.000 abstract description 6
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 244000269722 Thea sinensis Species 0.000 description 135
- 235000013616 tea Nutrition 0.000 description 130
- 239000004744 fabric Substances 0.000 description 7
- 235000009569 green tea Nutrition 0.000 description 7
- 239000006228 supernatant Substances 0.000 description 5
- 229920003043 Cellulose fiber Polymers 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000003385 bacteriostatic effect Effects 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 241000255789 Bombyx mori Species 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 229920000297 Rayon Polymers 0.000 description 3
- 230000002421 anti-septic effect Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 108010022355 Fibroins Proteins 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 229930003949 flavanone Natural products 0.000 description 2
- 235000011981 flavanones Nutrition 0.000 description 2
- 150000002208 flavanones Chemical class 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 239000011135 tin Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- -1 vitamin Polyphenols Chemical class 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000222122 Candida albicans Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 108010013296 Sericins Proteins 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 235000021120 animal protein Nutrition 0.000 description 1
- 229930014669 anthocyanidin Natural products 0.000 description 1
- 235000008758 anthocyanidins Nutrition 0.000 description 1
- 229930002877 anthocyanin Natural products 0.000 description 1
- 235000010208 anthocyanin Nutrition 0.000 description 1
- 239000004410 anthocyanin Substances 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- YTJJRAWFHJBAMT-UHFFFAOYSA-N depside Natural products OC(=O)CC1=C(O)C=C(O)C=C1OC(=O)C1=CC=C(O)C(O)=C1 YTJJRAWFHJBAMT-UHFFFAOYSA-N 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 230000009982 effect on human Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- HVQAJTFOCKOKIN-UHFFFAOYSA-N flavonol Natural products O1C2=CC=CC=C2C(=O)C(O)=C1C1=CC=CC=C1 HVQAJTFOCKOKIN-UHFFFAOYSA-N 0.000 description 1
- 150000002216 flavonol derivatives Chemical class 0.000 description 1
- 235000011957 flavonols Nutrition 0.000 description 1
- NWKFECICNXDNOQ-UHFFFAOYSA-N flavylium Chemical compound C1=CC=CC=C1C1=CC=C(C=CC=C2)C2=[O+]1 NWKFECICNXDNOQ-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 235000009048 phenolic acids Nutrition 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/11—Compounds containing epoxy groups or precursors thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/10—Animal fibres
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the technical field of textile, in particular to a tea polyphenol-containing silk macrobio-fiber and a preparation method thereof, wherein the tea polyphenol-containing silk macrobio-fiber comprises the following fibers in percentage by weight: the mass content of the tea polyphenol in the silk macrobiological fiber containing the tea polyphenol is 4-10%. The preparation method of the silk macrobiological fiber containing tea polyphenol comprises the following steps: (1) extracting tea polyphenol; (2) preparing a tea polyphenol solution; (3) removing impurities from the silk fiber; (4) pretreating silk fiber; (5) the preparation method of the silk macrobiological fiber containing tea polyphenol has the advantages of high tea polyphenol extraction, firm attachment of the tea polyphenol and the fiber, strong washing resistance and extremely high antibacterial rate.
Description
Technical Field
The invention relates to the technical field of spinning, in particular to a large silk biological fiber containing tea polyphenol and a preparation method thereof.
Background
Silk is a continuous long fiber, also called natural silk, which is a natural fiber and is formed by coagulation of a silk liquid secreted by a mature silkworm during cocooning. Humans use one of the earliest animal fibers. The silk is one of ancient Chinese civilization products, and the Chinese workers invented the production as a very early thing, and the popular Huangdi's Fei rayon ancestor began to teach silkworms; there are many silks and many side-of-silk characters in the oracle bone inscription. According to archaeology, china has made silk threads, woven ribbons and simple silk fabrics from silk approximately 4700 years ago. Silk is used for weaving silk fabrics such as silk, fine silk fabrics, yarn, crape, silk, brocade, embroidery and the like in the period of business weeks.
The silk mainly comprises fibroin of an inner layer and sericin on the surface of the fibroin, and is derived from silkworm, is a pure natural material, has good biocompatibility, degradability, air permeability and moisture permeability, and has wide application in biomedicine, cosmetics and textile industries;
since the silk is pure natural animal protein, the processed silk has a poor bacteriostatic effect, and the textile using the silk as a raw material or a main material is easy to rapidly decay and generate peculiar smell under the condition of high humidity and high temperature, so that the use experience of the silk textile is poor, the use range of the silk textile is limited, and the maintenance difficulty of the silk textile is improved; in prior art, need through handling the silk fibre, promote the antibiotic effect of silk fibre, performance such as intensity, make the silk fibre can be effectual for a long time use, wherein the improvement of silk fibre antibacterial property mainly has fixes the antiseptic on the surface of silk fibre through reactive resin, fixes on the surface of silk fibre and fixes methods such as antiseptic through two components of the mutual reaction through antiseptic itself absorption.
Tea Polyphenols (Green Tea Polyphenols, abbreviated as GTP) is also called antioxidant, vitamin Polyphenols and Fanghailing, and is a general name of Polyphenols in Tea, and is white amorphous powder, easily soluble in water, soluble in ethanol, methanol, acetone and ethyl acetate, and insoluble in chloroform. The green tea has high tea polyphenol content accounting for 15-30% of the weight, and the tea polyphenol comprises the following main components: flavanones, anthocyanidins, flavonols, anthocyanins, phenolic acids and depside 6 compounds. Wherein, flavanones (mainly catechin compounds) are the most important and account for 60 to 80 percent of the total amount of tea polyphenol, and flavonoids and other phenolic substances are less. The tea polyphenols have various physiological activities of resisting oxidation, preventing radiation, resisting aging, reducing blood lipid, reducing blood sugar, inhibiting bacteria and inhibiting enzyme, etc.
Patent document (CN104146419A) discloses a green tea cellulose fiber fabric, which is prepared by extracting pure fiber pulp from green tea leaf raw material, producing viscose, processing into green tea cellulose viscose fiber through water washing, desulfurization, acid washing, oiling and drying, and spinning into green tea cellulose fiber fabric.
The green tea cellulose fiber fabric has certain health care effect on human skin, but the green tea cellulose fiber fabric has poor oxidation resistance and antibacterial performance, poor adhesion, washing resistance, complex processing steps and low preparation efficiency.
Disclosure of Invention
Aiming at the defects in the prior art, the silk macrobiological fiber containing tea polyphenol and the preparation method thereof are provided, the tea polyphenol extraction is high, the tea polyphenol and the fiber are firmly attached, the washing resistance is strong, and the antibacterial rate is extremely high.
In order to solve the technical problems, the technical scheme adopted by the invention is that the tea polyphenol-containing silk macrobiological fiber is composed of the following fibers in percentage by weight: the mass content of the tea polyphenol in the silk macrobiological fiber containing the tea polyphenol is 4-10%.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps:
(1) extracting tea polyphenol;
(2) preparing a tea polyphenol solution;
(3) removing impurities from the silk fiber;
(4) pretreating silk fiber;
(5) and preparing the silk macrobiological fiber containing tea polyphenol.
The preparation method of the silk macrobio-fiber containing tea polyphenol,
the process of the step (1) comprises the following steps:
s1, sucking a certain amount of ethanol solution, adding ammonium sulfate and ionic liquid with preset mass, dissolving for 13-16min with the assistance of ultrasonic wave, taking out, standing, phase splitting for 8-12min, reading and recording the volume of the upper phase and the lower phase to obtain an ionic liquid-assisted ethanol/ammonium sulfate double-aqueous phase system;
s2, adding tea powder with a predetermined mass into another clean and dry plastic centrifuge tube, adding the prepared ionic liquid auxiliary ethanol/ammonium sulfate, extracting in an ultrasonic water bath for a predetermined time, transferring into a centrifuge, centrifuging for 8-12min at 3800-.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (2):
s1, weighing a certain amount of tea polyphenol, placing the tea polyphenol into a container, and adding deionized water to prepare a solution with the mass concentration of 5-10%;
s2, adjusting the pH value to 4-8, and shaking to mix the components evenly.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (3):
s1, weighing a certain mass of sodium dodecyl benzene sulfonate to prepare an aqueous solution with the concentration of 0.04mol/L-0.06 mol/L;
s2, adding the prepared silk, soaking for 28-32min at a bath ratio of 1:5, and slowly stirring at a rotating speed of 80 r/min; removing oil stains and other impurities on the surface;
s3, drying at 58-62 ℃.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (4):
s1, preparing a metal salt solution with the concentration of 0.1-5%, adding a certain amount of silk fiber, heating to 50-80 ℃, and stirring for 30-120 min;
and S2, taking out the silk fiber, washing with water, and drying for later use.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (5):
s1, completely soaking the silk fibers in the tea polyphenol solution, transferring the solution into a stainless steel vacuum tank, adding a coupling agent and a catalyst, vacuumizing the tank by using a vacuum pump until the pressure reaches-0.033 to-0.036 MPa, keeping the pressure for 18 to 22 seconds, recovering the pressure to normal pressure, and soaking the tank for 8 to 12 minutes at the normal pressure;
s2, introducing inert gas into the modification liquid, wherein the modification time is 3.5-4.2 h; ultrasonic treatment is carried out in the modification process, the power density of ultrasonic wave is 120W/L, and the ultrasonic frequency is 30 KHz;
s3, taking out the modified silk fiber, washing with clear water, absolute methanol and clear water, and drying at 58-62 ℃ to obtain the silk macrobiological fiber containing tea polyphenol.
In the preparation method of the silk macrobio-fiber containing tea polyphenol, in the step (1), the ionic liquid is
[ C4mim ] Cl, the mass fraction of which is 8% -12%; 28-32% of ammonium sulfate by mass; ethanol volume fraction of 58-62%; the feed-liquid ratio is 1: 40g/m L; ultrasonic power 540W.
According to the preparation method of the silk macrobio-fiber containing tea polyphenol, the coupling agent is a silane coupling agent; the catalyst is zirconic acid n-propyl ester and toluenesulfonic acid, and the mass ratio is 2: 1.
In the preparation method of the silk macrobio-fiber containing tea polyphenol, the inert gas is one or more of helium and argon, and the gas flow is 1.5-10L/min.
The silk macrobio-fiber containing tea polyphenol and the preparation method thereof have the beneficial effects that the extraction rate of tea polyphenol is effectively improved by preparing an ionic liquid assisted ethanol/ammonium sulfate aqueous two-phase system and matching with the action of ultrasonic water bath extraction and a centrifugal machine. The extraction rate can reach more than 83 percent, and the purity of the obtained finished tea polyphenol reaches more than 90 percent.
The silk fiber removes impurities to remove oil stains and other impurities on the surface, prevents the oil stains and other impurities from influencing the adhesive force of the tea polyphenol and the silk fiber surface, and lays a foundation for generating polymerization active points for the silk fiber surface treatment.
The metal salt solution can make the surface of the silk fiber generate polymerization active points by surface treatment, which is beneficial to the combination of tea polyphenol and the surface of the silk fiber, so that the tea polyphenol and the silk fiber are firmly attached and have strong washing resistance.
The strength of the silk macrobiological fiber containing tea polyphenol prepared by the method can reach 5-8cN/dtex, the elongation at break is 10-16%, and the silk macrobiological fiber has excellent elasticity.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1
The silk macrobiological fiber containing tea polyphenol consists of the following fibers in percentage by weight: the mass content of the tea polyphenol in the silk macrobiological fiber containing the tea polyphenol is 3 percent.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps:
(1) extracting tea polyphenol;
(2) preparing a tea polyphenol solution;
(3) removing impurities from the silk fiber;
(4) pretreating silk fiber;
(5) and preparing the silk macrobiological fiber containing tea polyphenol.
The preparation method of the silk macrobio-fiber containing tea polyphenol,
the process of the step (1) comprises the following steps:
s1, absorbing a certain amount of ethanol solution, adding ammonium sulfate and ionic liquid with preset mass, dissolving for 13min with the assistance of ultrasonic wave, taking out, standing, phase splitting for 8min, reading and recording the volumes of the upper phase and the lower phase to obtain an ionic liquid-assisted ethanol/ammonium sulfate double-aqueous-phase system;
s2, adding tea powder with a predetermined mass into another clean and dry plastic centrifuge tube, adding the prepared ionic liquid auxiliary ethanol/ammonium sulfate, extracting in an ultrasonic water bath for a predetermined time, transferring into a centrifuge, centrifuging at 3800r/min for 8min, and enriching tea polyphenol into the supernatant ethanol clear liquid to be measured for concentration.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (2):
s1, weighing a certain amount of tea polyphenol, placing the tea polyphenol into a container, and adding deionized water to prepare a solution with the mass concentration of 5%;
s2, adjusting the pH value to 4, and shaking to mix the components evenly.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (3):
s1, weighing a certain mass of sodium dodecyl benzene sulfonate to prepare an aqueous solution with the concentration of 0.04 mol/L;
s2, adding the prepared silk, soaking for 28min at a bath ratio of 1:5, and slowly stirring at a rotating speed of 80 r/min; removing oil stains and other impurities on the surface;
s3, drying at 58 ℃.
The step (4) flow comprises the following steps:
s1, preparing a metal salt solution with the concentration of 0.1%, adding silk fibers, heating to 50 ℃, and stirring for 30 min;
and S2, taking out the silk fiber, washing with water, and drying for later use.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (5):
s1, completely soaking the silk fibers in the tea polyphenol solution, transferring the solution into a stainless steel vacuum tank, adding a coupling agent and a catalyst, vacuumizing the tank by using a vacuum pump until the pressure reaches-0.033, keeping the pressure for 18S, recovering the pressure to the normal pressure, and soaking the tank for 8min at the normal pressure;
s2, introducing inert gas into the modification liquid, wherein the modification time is 3.5 h; ultrasonic treatment is carried out in the modification process, the power density of ultrasonic wave is 120W/L, and the ultrasonic frequency is 30 KHz;
s3, taking out the modified silk fiber, washing with clear water, absolute methanol and clear water, and drying at 58 ℃ to obtain the silk macrobio-fiber containing tea polyphenol.
In the step (1), the ionic liquid is [ C4mim ] Cl, and the mass fraction of the ionic liquid is 8%; 28 percent of ammonium sulfate by mass; ethanol volume fraction 58%; the feed-liquid ratio is 1: 40g/m L; ultrasonic power 540W.
The coupling agent is a silane coupling agent; the catalyst is zirconic acid n-propyl ester and toluenesulfonic acid, and the mass ratio is 2: 1.
The inert gas is one or more of helium and argon, and the gas flow is 1.5L/min.
In the step (1) and the step (S2), the tea powder is 15g, and the preset time of ultrasonic water bath extraction is 20 min.
The metal salt is water-soluble salt, and the metal ions are aluminum, zinc, tin, silver, copper, iron and the like.
Example 2
The silk macrobiological fiber containing tea polyphenol consists of the following fibers in percentage by weight: the mass content of the tea polyphenol in the silk macrobiological fiber containing the tea polyphenol is 4 percent.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps:
(1) extracting tea polyphenol;
(2) preparing a tea polyphenol solution;
(3) removing impurities from the silk fiber;
(4) pretreating silk fiber;
(5) and preparing the silk macrobiological fiber containing tea polyphenol.
The preparation method of the silk macrobio-fiber containing tea polyphenol,
the process of the step (1) comprises the following steps:
s1, absorbing a certain amount of ethanol solution, adding ammonium sulfate and ionic liquid with preset mass, dissolving for 13min with the assistance of ultrasonic wave, taking out, standing, phase splitting for 8min, reading and recording the volumes of the upper phase and the lower phase to obtain an ionic liquid-assisted ethanol/ammonium sulfate double-aqueous-phase system;
s2, adding tea powder with a predetermined mass into another clean and dry plastic centrifuge tube, adding the prepared ionic liquid auxiliary ethanol/ammonium sulfate, extracting in an ultrasonic water bath for a predetermined time, transferring into a centrifuge, centrifuging at 3800r/min for 8min, and enriching tea polyphenol into the supernatant ethanol clear liquid to be measured for concentration.
The step (2) flow comprises the following steps:
s1, weighing a certain amount of tea polyphenol, placing the tea polyphenol into a container, and adding deionized water to prepare a solution with the mass concentration of 5%;
s2, adjusting the pH value to 4, and shaking to mix the components evenly.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (3):
s1, weighing a certain mass of sodium dodecyl benzene sulfonate to prepare an aqueous solution with the concentration of 0.04 mol/L;
s2, adding the prepared silk, soaking for 28min at a bath ratio of 1:5, and slowly stirring at a rotating speed of 80 r/min; removing oil stains and other impurities on the surface;
s3, drying at 58 ℃.
The step (4) flow comprises the following steps:
s1, preparing a metal salt solution with the concentration of 0.1%, adding silk fibers, heating to 50 ℃, and stirring for 30 min;
and S2, taking out the silk fiber, washing with water, and drying for later use.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (5):
s1, completely soaking the silk fibers in the tea polyphenol solution, transferring the solution into a stainless steel vacuum tank, adding a coupling agent and a catalyst, vacuumizing the tank by using a vacuum pump until the pressure reaches-0.033, keeping the pressure for 18S, recovering the pressure to the normal pressure, and soaking the tank for 8min at the normal pressure;
s2, introducing inert gas into the modification liquid, wherein the modification time is 3.5 h; ultrasonic treatment is carried out in the modification process, the power density of ultrasonic wave is 120W/L, and the ultrasonic frequency is 30 KHz;
s3, taking out the modified silk fiber, washing with clear water, absolute methanol and clear water, and drying at 58 ℃ to obtain the silk macrobio-fiber containing tea polyphenol.
In the step (1), the ionic liquid is [ C4mim ] Cl, and the mass fraction of the ionic liquid is 8%; 28 percent of ammonium sulfate by mass; ethanol volume fraction 58%; the feed-liquid ratio is 1: 40g/m L; ultrasonic power 540W.
The coupling agent is a silane coupling agent; the catalyst is zirconic acid n-propyl ester and toluenesulfonic acid, and the mass ratio is 2: 1.
The inert gas is one or more of helium and argon, and the gas flow is 1.5L/min.
In the step (1) and the step (S2), the tea powder is 15g, and the preset time of ultrasonic water bath extraction is 20 min.
The metal salt is water-soluble salt, and the metal ions are aluminum, zinc, tin, silver, copper, iron and the like.
Example 3
The same parts of this example as example 1 are not repeated, but the difference is that the silk macrobio fiber containing tea polyphenol is composed of the following fibers by weight percent: the mass content of the tea polyphenol in the silk macrobiological fiber containing the tea polyphenol is 7 percent.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps:
(1) extracting tea polyphenol;
(2) preparing a tea polyphenol solution;
(3) removing impurities from the silk fiber;
(4) pretreating silk fiber;
(5) and preparing the silk macrobiological fiber containing tea polyphenol.
The preparation method of the silk macrobio-fiber containing tea polyphenol,
the process of the step (1) comprises the following steps:
s1, absorbing a certain amount of ethanol solution, adding ammonium sulfate and ionic liquid with preset mass, dissolving for 15min with the assistance of ultrasonic wave, taking out, standing, phase splitting for 10min, reading and recording the volume of the upper phase and the lower phase to obtain an ionic liquid-assisted ethanol/ammonium sulfate double-aqueous-phase system;
s2, adding tea powder with a predetermined mass into another clean and dry plastic centrifuge tube, adding the prepared ionic liquid auxiliary ethanol/ammonium sulfate, extracting in an ultrasonic water bath for a predetermined time, transferring into a centrifuge, centrifuging at 4000r/min for 10min, and enriching tea polyphenol into the supernatant ethanol phase clear liquid to be measured for concentration.
The step (2) flow comprises the following steps:
s1, weighing a certain amount of tea polyphenol, placing the tea polyphenol into a container, and adding deionized water to prepare a solution with the mass concentration of 8%;
s2, adjusting the pH value to 6, and shaking to mix the components evenly.
The step (3) flow comprises the following steps:
s1, weighing a certain mass of sodium dodecyl benzene sulfonate to prepare an aqueous solution with the concentration of 0.05 mol/L;
s2, adding the prepared silk, soaking for 30min at a bath ratio of 1:5, and slowly stirring at a rotating speed of 80 r/min; removing oil stains and other impurities on the surface;
s3, drying at 60 ℃.
The step (4) flow comprises the following steps:
s1, preparing a metal salt solution with the concentration of 3%, adding silk fibers, heating to 60 ℃, and stirring for 50 min;
and S2, taking out the silk fiber, washing with water, and drying for later use.
The step (5) process comprises the following steps:
s1, completely soaking the silk fibers in the tea polyphenol solution, transferring the solution into a stainless steel vacuum tank, adding a coupling agent and a catalyst, vacuumizing the tank by using a vacuum pump until the pressure reaches-0.035 MPa, keeping the pressure for 20S, recovering the pressure to normal pressure, and soaking the tank for 10min at the normal pressure;
s2, introducing inert gas into the modification liquid, wherein the modification time is 4 h; ultrasonic treatment is carried out in the modification process, the power density of ultrasonic wave is 120W/L, and the ultrasonic frequency is 30 KHz;
s3, taking out the modified silk fiber, washing with clear water, absolute methanol and clear water, and drying at 60 ℃ to obtain the silk macrobiological fiber containing tea polyphenol.
In the step (1), the ionic liquid is [ C4mim ] Cl, and the mass fraction of the ionic liquid is 10%; ammonium sulfate mass fraction is 30%; ethanol volume fraction 60%; the feed-liquid ratio is 1: 40g/m L; ultrasonic power 540W.
The inert gas is one or more of helium and argon, and the gas flow is 5L/min.
In the step (1) and the step (S2), the tea powder is 20g, and the preset time for ultrasonic water bath extraction is 30 min.
Example 4
The same parts of this embodiment as those of embodiment 1 are not described again, but the differences are as follows: the silk macrobiological fiber containing tea polyphenol consists of the following fibers in percentage by weight: the mass content of the tea polyphenol in the silk macrobiological fiber containing the tea polyphenol is 10 percent.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps:
(1) extracting tea polyphenol;
(2) preparing a tea polyphenol solution;
(3) removing impurities from the silk fiber;
(4) pretreating silk fiber;
(5) and preparing the silk macrobiological fiber containing tea polyphenol.
The process of the step (1) comprises the following steps:
s1, absorbing a certain amount of ethanol solution, adding ammonium sulfate and ionic liquid with preset mass, dissolving for 16min with the assistance of ultrasound, taking out, standing, phase splitting for 12min, reading and recording the volumes of the upper phase and the lower phase to obtain an ionic liquid-assisted ethanol/ammonium sulfate double-aqueous-phase system;
s2, adding tea powder with a predetermined mass into another clean and dry plastic centrifuge tube, adding the prepared ionic liquid auxiliary ethanol/ammonium sulfate, extracting in an ultrasonic water bath for a predetermined time, transferring into a centrifuge, centrifuging at 4200r/min for 10min, and enriching tea polyphenol into the supernatant ethanol clear liquid to be measured for concentration.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (2):
s1, weighing a certain amount of tea polyphenol, placing the tea polyphenol into a container, and adding deionized water to prepare a solution with the mass concentration of 10%;
s2, adjusting the pH value to 8, and shaking to mix the components evenly.
The step (3) flow comprises the following steps:
s1, weighing a certain mass of sodium dodecyl benzene sulfonate to prepare an aqueous solution with the concentration of 0.06 mol/L;
s2, adding the prepared silk, soaking for 32min at a bath ratio of 1:5, and slowly stirring at a rotating speed of 80 r/min; removing oil stains and other impurities on the surface;
s3, drying at 62 ℃.
The step (4) flow comprises the following steps:
s1, preparing a metal salt solution with the concentration of 5%, adding silk fibers, heating to 80 ℃, and stirring for 120 min;
and S2, taking out the silk fiber, washing with water, and drying for later use.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (5):
s1, completely soaking the silk fiber in the tea polyphenol solution, transferring into a stainless steel vacuum tank, adding a coupling agent and a catalyst, vacuumizing by using a vacuum pump, keeping for 22S after reaching the pressure of 0.036MPa, recovering to normal pressure, and soaking for 12min at normal pressure
S2, introducing inert gas into the modification liquid, wherein the modification time is 4.2 h; ultrasonic treatment is carried out in the modification process, the power density of ultrasonic wave is 120W/L, and the ultrasonic frequency is 30 KHz;
s3, taking out the modified silk fiber, washing with clear water, absolute methanol and clear water, and drying at 60 ℃ to obtain the silk macrobiological fiber containing tea polyphenol.
In the step (1), the ionic liquid is [ C4mim ] Cl, and the mass fraction of the ionic liquid is 12%; 32% of ammonium sulfate by mass; ethanol volume fraction 62%; the feed-liquid ratio is 1: 40g/m L; ultrasonic power 540W.
The inert gas is one or more of helium and argon, and the gas flow is 10L/min.
In the step (1) and the step (S2), the tea powder is 25g, and the preset time for ultrasonic water bath extraction is 40 min.
Example 5
The same parts of this embodiment as those of embodiment 4 are not described again, but the differences are as follows: the silk macrobiological fiber containing tea polyphenol consists of the following fibers in percentage by weight: the mass content of the tea polyphenol in the silk macrobiological fiber containing the tea polyphenol is 11 percent.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps:
(1) extracting tea polyphenol;
(2) preparing a tea polyphenol solution;
(3) removing impurities from the silk fiber;
(4) pretreating silk fiber;
(5) and preparing the silk macrobiological fiber containing tea polyphenol.
The process of the step (1) comprises the following steps:
s1, absorbing a certain amount of ethanol solution, adding ammonium sulfate and ionic liquid with preset mass, dissolving for 16min with the assistance of ultrasound, taking out, standing, phase splitting for 12min, reading and recording the volumes of the upper phase and the lower phase to obtain an ionic liquid-assisted ethanol/ammonium sulfate double-aqueous-phase system;
s2, adding tea powder with a predetermined mass into another clean and dry plastic centrifuge tube, adding the prepared ionic liquid auxiliary ethanol/ammonium sulfate, extracting in an ultrasonic water bath for a predetermined time, transferring into a centrifuge, centrifuging at 4200r/min for 10min, and enriching tea polyphenol into the supernatant ethanol clear liquid to be measured for concentration.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (2):
s1, weighing a certain amount of tea polyphenol, placing the tea polyphenol into a container, and adding deionized water to prepare a solution with the mass concentration of 10%;
s2, adjusting the pH value to 8, and shaking to mix the components evenly.
The step (3) flow comprises the following steps:
s1, weighing a certain mass of sodium dodecyl benzene sulfonate to prepare an aqueous solution with the concentration of 0.06 mol/L;
s2, adding the prepared silk, soaking for 32min at a bath ratio of 1:5, and slowly stirring at a rotating speed of 80 r/min; removing oil stains and other impurities on the surface;
s3, drying at 62 ℃.
The step (4) flow comprises the following steps:
s1, preparing a metal salt solution with the concentration of 5%, adding silk fibers, heating to 80 ℃, and stirring for 120 min;
and S2, taking out the silk fiber, washing with water, and drying for later use.
The preparation method of the silk macrobio-fiber containing tea polyphenol comprises the following steps of (5):
s1, completely soaking the silk fiber in the tea polyphenol solution, transferring into a stainless steel vacuum tank, adding a coupling agent and a catalyst, vacuumizing by using a vacuum pump, keeping for 22S after reaching the pressure of 0.036MPa, recovering to normal pressure, and soaking for 12min at normal pressure
S2, introducing inert gas into the modification liquid, wherein the modification time is 4.2 h; ultrasonic treatment is carried out in the modification process, the power density of ultrasonic wave is 120W/L, and the ultrasonic frequency is 30 KHz;
s3, taking out the modified silk fiber, washing with clear water, absolute methanol and clear water, and drying at 60 ℃ to obtain the silk macrobiological fiber containing tea polyphenol.
In the step (1), the ionic liquid is [ C4mim ] Cl, and the mass fraction of the ionic liquid is 12%; 32% of ammonium sulfate by mass; ethanol volume fraction 62%; the feed-liquid ratio is 1: 40g/m L; ultrasonic power 540W.
The inert gas is one or more of helium and argon, and the gas flow is 10L/min.
In the step (1) and the step (S2), the tea powder is 25g, and the preset time for ultrasonic water bath extraction is 40 min.
By preparing an ionic liquid assisted ethanol/ammonium sulfate aqueous two-phase system, and combining with ultrasonic water bath extraction and centrifuge action, the extraction rate of tea polyphenol is effectively improved. The extraction rate can reach more than 83 percent, and the purity of the obtained finished tea polyphenol reaches more than 90 percent.
The silk fiber removes impurities to remove oil stains and other impurities on the surface, prevents the oil stains and other impurities from influencing the adhesive force of the tea polyphenol and the silk fiber surface, and lays a foundation for generating polymerization active points for the silk fiber surface treatment.
The metal salt solution can make the surface of the silk fiber generate polymerization active points by surface treatment, which is beneficial to the combination of tea polyphenol and the surface of the silk fiber, so that the tea polyphenol and the silk fiber are firmly attached and have strong washing resistance.
The strength of the silk macrobiological fiber containing tea polyphenol prepared by the method can reach 5-8cN/dtex, the elongation at break is 10-16%, and the silk macrobiological fiber has excellent elasticity.
TABLE 1
As shown in Table 1, the bacteriostasis rate is detected according to GB/T20944.3: the bacteriostatic rate of the tea polyphenol-containing silk macrobio fiber prepared in example 1 is low, and the bacteriostatic rate of the tea polyphenol-containing silk macrobio fiber prepared in example 5 is similar to that of the tea polyphenol-containing silk macrobio fiber prepared in example 4. The silk macrobio-fiber containing tea polyphenol prepared in example 2, 3 or 4 has high bacteriostatic rate on staphylococcus aureus, escherichia coli and candida albicans after being washed for 50 times.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and that various changes, modifications, additions and substitutions which are within the spirit and scope of the present invention and which can be made by those skilled in the art are also within the scope of the present invention.
Claims (10)
1. The big biological fiber of silk that contains tea polyphenol, its characterized in that: the fiber comprises the following fibers in percentage by weight: the mass content of the tea polyphenol in the silk macrobiological fiber containing the tea polyphenol is 4-10%.
2. The method for preparing the tea polyphenol-containing silk macrobio fiber according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1) extracting tea polyphenol;
(2) preparing a tea polyphenol solution;
(3) removing impurities from the silk fiber;
(4) pretreating silk fiber;
(5) and preparing the silk macrobiological fiber containing tea polyphenol.
3. The method of claim 2, wherein the step of preparing the tea polyphenol-containing silk macrobio fiber,
the process of the step (1) comprises the following steps:
s1, sucking a certain amount of ethanol solution, adding ammonium sulfate and ionic liquid with preset mass, dissolving for 13-16min with the assistance of ultrasonic wave, taking out, standing, phase splitting for 8-12min, reading and recording the volume of the upper phase and the lower phase to obtain an ionic liquid-assisted ethanol/ammonium sulfate double-aqueous phase system;
s2, adding tea powder with a predetermined mass into another clean and dry plastic centrifuge tube, adding the prepared ionic liquid auxiliary ethanol/ammonium sulfate, extracting in an ultrasonic water bath for a predetermined time, transferring into a centrifuge, centrifuging for 8-12min at 3800-.
4. The method for preparing the silk macrobio fiber containing tea polyphenol as claimed in claim 2, wherein the process of the step (2) comprises:
s1, weighing a certain amount of tea polyphenol, placing the tea polyphenol into a container, and adding deionized water to prepare a solution with the mass concentration of 5-10%;
s2, adjusting the pH value to 4-8, and shaking to mix the components evenly.
5. The method for preparing the silk macrobio fiber containing tea polyphenol as claimed in claim 1, wherein the process of the step (3) comprises:
s1, weighing a certain mass of sodium dodecyl benzene sulfonate to prepare an aqueous solution with the concentration of 0.04mol/L-0.06 mol/L;
s2, adding the prepared silk, soaking for 28-32min at a bath ratio of 1:5, and slowly stirring at a rotating speed of 80 r/min; removing oil stains and other impurities on the surface;
s3, drying at 58-62 ℃.
6. The method for preparing the silk macrobio fiber containing tea polyphenol as claimed in claim 2, wherein the process of the step (4) comprises:
s1, preparing a metal salt solution with the concentration of 0.1-5%, adding silk fibers, heating to 50-80 ℃, and stirring for 30-120 min;
and S2, taking out the silk fiber, washing with water, and drying for later use.
7. The method for preparing the silk macrobio fiber containing tea polyphenol as claimed in claim 2, wherein the process of the step (5) comprises:
s1, completely soaking the silk fibers in the tea polyphenol solution, transferring the solution into a stainless steel vacuum tank, adding a coupling agent and a catalyst, vacuumizing the tank by using a vacuum pump until the pressure reaches-0.033 to-0.036 MPa, keeping the pressure for 18 to 22 seconds, recovering the pressure to normal pressure, and soaking the tank for 8 to 12 minutes at the normal pressure;
s2, introducing inert gas into the modification liquid, wherein the modification time is 3.5-4.2 h; ultrasonic treatment is carried out in the modification process, the power density of ultrasonic wave is 120W/L, and the ultrasonic frequency is 30 KHz;
s3, taking out the modified silk fiber, washing with clear water, absolute methanol and clear water, and drying at 58-62 ℃ to obtain the silk macrobiological fiber containing tea polyphenol.
8. The method for preparing the silk macrobio fiber containing tea polyphenol as claimed in claim 2, wherein: in the step (1), the ionic liquid is [ C4mim ] Cl, and the mass fraction of the ionic liquid is 8-12%; 28-32% of ammonium sulfate by mass; ethanol volume fraction of 58-62%; the feed-liquid ratio is 1: 40g/m L; ultrasonic power 540W.
9. The method for preparing the silk macrobio fiber containing tea polyphenol as claimed in claim 7, wherein: the coupling agent is a silane coupling agent; the catalyst is zirconic acid n-propyl ester and toluenesulfonic acid, and the mass ratio is 2: 1.
10. The method for preparing the silk macrobio fiber containing tea polyphenol as claimed in claim 6, wherein: the inert gas is one or more of helium and argon, and the gas flow is 1.5-10L/min.
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