CN117822145B - Chlorogenic acid-containing slow-release multifunctional polylactic acid textile and preparation method thereof - Google Patents
Chlorogenic acid-containing slow-release multifunctional polylactic acid textile and preparation method thereof Download PDFInfo
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- CN117822145B CN117822145B CN202311827099.8A CN202311827099A CN117822145B CN 117822145 B CN117822145 B CN 117822145B CN 202311827099 A CN202311827099 A CN 202311827099A CN 117822145 B CN117822145 B CN 117822145B
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- 239000004626 polylactic acid Substances 0.000 title claims abstract description 164
- 229920000747 poly(lactic acid) Polymers 0.000 title claims abstract description 163
- CWVRJTMFETXNAD-FWCWNIRPSA-N 3-O-Caffeoylquinic acid Natural products O[C@H]1[C@@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-FWCWNIRPSA-N 0.000 title claims abstract description 145
- PZIRUHCJZBGLDY-UHFFFAOYSA-N Caffeoylquinic acid Natural products CC(CCC(=O)C(C)C1C(=O)CC2C3CC(O)C4CC(O)CCC4(C)C3CCC12C)C(=O)O PZIRUHCJZBGLDY-UHFFFAOYSA-N 0.000 title claims abstract description 145
- CWVRJTMFETXNAD-KLZCAUPSSA-N Neochlorogenin-saeure Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O CWVRJTMFETXNAD-KLZCAUPSSA-N 0.000 title claims abstract description 145
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 title claims abstract description 145
- 229940074393 chlorogenic acid Drugs 0.000 title claims abstract description 145
- FFQSDFBBSXGVKF-KHSQJDLVSA-N chlorogenic acid Natural products O[C@@H]1C[C@](O)(C[C@@H](CC(=O)C=Cc2ccc(O)c(O)c2)[C@@H]1O)C(=O)O FFQSDFBBSXGVKF-KHSQJDLVSA-N 0.000 title claims abstract description 145
- 235000001368 chlorogenic acid Nutrition 0.000 title claims abstract description 145
- BMRSEYFENKXDIS-KLZCAUPSSA-N cis-3-O-p-coumaroylquinic acid Natural products O[C@H]1C[C@@](O)(C[C@@H](OC(=O)C=Cc2ccc(O)cc2)[C@@H]1O)C(=O)O BMRSEYFENKXDIS-KLZCAUPSSA-N 0.000 title claims abstract description 145
- 239000004753 textile Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 claims abstract description 122
- 239000004715 ethylene vinyl alcohol Substances 0.000 claims abstract description 114
- 238000002156 mixing Methods 0.000 claims abstract description 83
- 239000000835 fiber Substances 0.000 claims abstract description 60
- 239000000463 material Substances 0.000 claims abstract description 36
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 238000002074 melt spinning Methods 0.000 claims abstract description 20
- 238000012545 processing Methods 0.000 claims abstract description 19
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 claims abstract description 17
- 229920001477 hydrophilic polymer Polymers 0.000 claims abstract description 12
- 238000005469 granulation Methods 0.000 claims description 50
- 230000003179 granulation Effects 0.000 claims description 50
- 238000009987 spinning Methods 0.000 claims description 40
- 238000000034 method Methods 0.000 claims description 25
- 238000009998 heat setting Methods 0.000 claims description 22
- 239000000155 melt Substances 0.000 claims description 12
- 238000005098 hot rolling Methods 0.000 claims description 11
- 230000003647 oxidation Effects 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 10
- 238000009941 weaving Methods 0.000 claims description 8
- 230000006750 UV protection Effects 0.000 claims description 7
- 230000002787 reinforcement Effects 0.000 claims description 4
- 238000002844 melting Methods 0.000 abstract description 14
- 230000008018 melting Effects 0.000 abstract description 14
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 238000001291 vacuum drying Methods 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 7
- 239000005977 Ethylene Substances 0.000 description 7
- 238000002835 absorbance Methods 0.000 description 7
- 238000009817 primary granulation Methods 0.000 description 7
- 238000009818 secondary granulation Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- RBMHUYBJIYNRLY-UHFFFAOYSA-N 2-[(1-carboxy-1-hydroxyethyl)-hydroxyphosphoryl]-2-hydroxypropanoic acid Chemical compound OC(=O)C(O)(C)P(O)(=O)C(C)(O)C(O)=O RBMHUYBJIYNRLY-UHFFFAOYSA-N 0.000 description 5
- OHDRQQURAXLVGJ-HLVWOLMTSA-N azane;(2e)-3-ethyl-2-[(e)-(3-ethyl-6-sulfo-1,3-benzothiazol-2-ylidene)hydrazinylidene]-1,3-benzothiazole-6-sulfonic acid Chemical compound [NH4+].[NH4+].S/1C2=CC(S([O-])(=O)=O)=CC=C2N(CC)C\1=N/N=C1/SC2=CC(S([O-])(=O)=O)=CC=C2N1CC OHDRQQURAXLVGJ-HLVWOLMTSA-N 0.000 description 5
- 229920001434 poly(D-lactide) Polymers 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 238000011056 performance test Methods 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 239000007853 buffer solution Substances 0.000 description 3
- 230000001186 cumulative effect Effects 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 241000205585 Aquilegia canadensis Species 0.000 description 2
- 230000002292 Radical scavenging effect Effects 0.000 description 2
- 244000269722 Thea sinensis Species 0.000 description 2
- 230000003064 anti-oxidating effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- 239000011165 3D composite Substances 0.000 description 1
- 229930182843 D-Lactic acid Natural products 0.000 description 1
- JVTAAEKCZFNVCJ-UWTATZPHSA-N D-lactic acid Chemical compound C[C@@H](O)C(O)=O JVTAAEKCZFNVCJ-UWTATZPHSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000208689 Eucommia ulmoides Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229920003232 aliphatic polyester Polymers 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 229940022769 d- lactic acid Drugs 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 229920001600 hydrophobic polymer Polymers 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006135 semi-crystalline thermoplastic polymer Polymers 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/08—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating
- D04H3/14—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length characterised by the method of strengthening or consolidating with bonds between thermoplastic yarns or filaments produced by welding
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H3/00—Non-woven fabrics formed wholly or mainly of yarns or like filamentary material of substantial length
- D04H3/005—Synthetic yarns or filaments
- D04H3/009—Condensation or reaction polymers
- D04H3/011—Polyesters
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a chlorogenic acid-containing slow-release multifunctional polylactic acid textile and a preparation method thereof, belonging to the field of preparation of functional fibers and non-woven materials. Firstly, melting and blending CGA and hydrophilic polymer ethylene-vinyl alcohol copolymer (EVOH) to pelletize to prepare EVOH/CGA blending slice; then, melting and blending PLA and EVOH/CGA blend slices for pelleting to prepare PLA/EVOH/CGA blend slices; and finally, taking PLA/EVOH/CGA blending slices as raw materials to perform melt spinning or spunbonding non-woven processing to prepare the slow-release multifunctional PLA fiber or non-woven material. According to the invention, the hydrophilic polymer EVOH is introduced, so that the release rate of the functional factor CGA is increased, and the release rate of the CGA in the PLA fiber or the nonwoven material can be regulated and controlled by controlling the content of the EVOH.
Description
Technical Field
The invention relates to a chlorogenic acid-containing slow-release multifunctional polylactic acid textile and a preparation method thereof, belonging to the field of preparation of functional fibers and non-woven materials.
Background
Polylactic acid (PLA) belongs to aliphatic polyester, is a biodegradable semi-crystalline thermoplastic polymer, and can be prepared into PLA fibers after spinning processing. The conventional preparation method of PLA fiber is melt spinning; the melt spinning method is economical and environment-friendly, has short process flow and high spinning efficiency, and is a main production mode of the current commercial PLA fiber, but the polymer can be thermally degraded in the hot processing process, so that the molecular weight of the polymer is reduced, and the mechanical property of the fiber is affected. Moreover, the traditional PLA fiber has the problems of single function, poor release performance and the like, and the wide application of the fiber is limited. Therefore, it is significant to develop PLA fiber materials with good functionality and release properties.
Chlorogenic acid (CGA) is one of the main antibacterial and antiviral effective pharmacological components of honeysuckle; has oxidation resistance, can absorb 280-400 nm ultraviolet light, and can protect skin from being damaged by the ultraviolet light; but it is inherently unstable and its content decreases over time at high temperatures or upon exposure to air.
Disclosure of Invention
[ Technical problem ]
PLA is a hydrophobic polymer, and CGA is embedded in PLA, so that release of the CGA is not facilitated, and oxidation resistance and ultraviolet resistance of the CGA are difficult to fully develop.
Technical scheme
In order to solve the problems, the invention firstly melt-blends and pellets CGA and hydrophilic polymer ethylene-vinyl alcohol copolymer (EVOH) to prepare EVOH/CGA blend slices; then, melting and blending PLA and EVOH/CGA blend slices for pelleting to prepare PLA/EVOH/CGA blend slices; and finally, taking PLA/EVOH/CGA blending slices as raw materials to perform melt spinning or spunbonding non-woven processing to prepare the slow-release multifunctional PLA fiber or non-woven material.
The invention takes natural extract CGA as a functional factor, has the functions of ultraviolet resistance and ultraviolet shielding, and has the melting point of about 210 ℃ which is close to the melting point of PLA; hydrophilic polymer EVOH is introduced to increase the hydrophilicity of the fiber or nonwoven material, which is favorable for releasing functional factors, and the melting point of the hydrophilic polymer EVOH is 160-195 ℃ which is close to the melting point of PLA; the melting points of EVOH and CGA are close to the melting point of PLA, and the modified-release type multifunctional PLA fiber and nonwoven material are suitable for melt blending processing with PLA, and simultaneously the physical and mechanical properties of the fiber and nonwoven material are maintained.
The first object of the present invention is to provide a method for preparing a CGA-containing slow-release multifunctional PLA textile, comprising the steps of:
(1) Carrying out melt blending granulation on hydrophilic polymer ethylene-vinyl alcohol copolymer (EVOH) and chlorogenic acid (CGA) to obtain EVOH/CGA blending slices;
(2) Carrying out melt blending granulation on polylactic acid PLA and EVOH/CGA blending slices to obtain PLA/EVOH/CGA blending slices;
(3) Carrying out melt spinning, drafting and heat setting on PLA/EVOH/CGA blending slices to obtain slow-release type multifunctional PLA fibers; or, performing spunbonding non-weaving processing on the PLA/EVOH/CGA blending slice to obtain a slow-release type multifunctional PLA non-woven material;
Wherein, the mass ratio of PLA, EVOH, CGA is 80-95: 5-20: 1 to 15.
In one embodiment of the invention PLA, EVOH, CGA is required to be dried prior to use so that the water content is not higher than 300ppm.
In one embodiment of the present invention, the melt blending granulation in step (1) is performed using a twin screw extruder at a granulation temperature of 170 to 230℃and a screw speed of 300 to 500rpm.
In one embodiment of the present invention, the EVOH/CGA blend pellets in step (1) are dried in vacuo at 70-80℃for 10-30 hours.
In one embodiment of the present invention, the melt blending granulation of step (1) may be preceded by premixing in a high speed mixer for 1-10min.
In one embodiment of the present invention, the melt blending granulation in step (2) is performed using a twin screw extruder at a granulation temperature of 170 to 230℃and a screw speed of 300 to 500rpm.
In one embodiment of the invention, the D-LA content of the D-lactic acid structural unit in the PLA of the step (2) is 0 to 10mol%; or a mixture of PLA and D-polylactic acid PDLA with the D-LA content of 0-10 mol percent, wherein the mass ratio of the PLA to the PDLA is 100: 5-50: 50.
In one embodiment of the invention, the PLA/EVOH/CGA blend pellets in step (2) are dried in vacuo at 70-80℃for 10-30 hours.
In one embodiment of the present invention, the melt blending granulation of step (2) may be preceded by premixing in a high speed mixer for 1-10min.
In one embodiment of the invention, the spinning temperature in the melt spinning of the step (3) is 180-240 ℃ and the spinning speed is 1500-5000 m/min; the drafting temperature is 85-130 ℃, and the drafting multiple is 4-10; the heat setting temperature is 120-170 ℃.
In one embodiment of the present invention, the spunbond nonwoven processing of step (3) is specifically: spinning into a net, hot rolling and reinforcing; wherein the spinning temperature in the spinning and net forming is 180-240 ℃, the spinning speed is 3000-6000 m/min, the net forming speed is 5-30 m/min, and the pump supply is 30-150 mL/min; the pressure of the hot rolling line is 65-75N/mm, and the temperature of the roller is 65-180 ℃.
The second purpose of the invention is to prepare the slow-release multifunctional PLA fiber or the slow-release multifunctional spun-bonded PLA non-woven material by the method.
The third object of the invention is to provide a slow-release multifunctional textile, which is a slow-release multifunctional PLA fiber or a slow-release multifunctional spun-bonded PLA non-woven material.
In one embodiment of the invention, the slow-release multifunctional textile is obtained by processing slow-release multifunctional PLA fibers or slow-release multifunctional spunbonded PLA non-woven materials, wherein the processing comprises one or more methods of spinning, weaving, cutting and bonding.
The fourth purpose of the invention is the application of the slow-release type multifunctional PLA fiber or the slow-release type multifunctional spun-bonded PLA non-woven material in the textile field.
A fifth object of the present invention is to provide a method for improving the uv and oxidation resistance of a polylactic acid textile, comprising the steps of:
(1) Carrying out melt blending granulation on hydrophilic polymer ethylene-vinyl alcohol copolymer (EVOH) and chlorogenic acid (CGA) to obtain EVOH/CGA blending slices;
(2) Carrying out melt blending granulation on polylactic acid PLA and EVOH/CGA blending slices to obtain PLA/EVOH/CGA blending slices;
(3) Carrying out melt spinning, drafting and heat setting on PLA/EVOH/CGA blend slices to obtain PLA fibers with ultraviolet resistance and oxidation resistance; or, performing spunbonding non-weaving processing on the PLA/EVOH/CGA blend slice to obtain a PLA non-woven material with ultraviolet resistance and oxidation resistance;
Wherein, the mass ratio of PLA, EVOH, CGA is 80-95: 5-20: 1 to 15.
The sixth object of the invention is to provide a method for improving the slow release performance of chlorogenic acid in polylactic acid textile, comprising the following steps:
(1) Carrying out melt blending granulation on hydrophilic polymer ethylene-vinyl alcohol copolymer (EVOH) and chlorogenic acid (CGA) to obtain EVOH/CGA blending slices;
(2) Carrying out melt blending granulation on polylactic acid PLA and EVOH/CGA blending slices to obtain PLA/EVOH/CGA blending slices;
(3) Carrying out melt spinning, drafting and heat setting on PLA/EVOH/CGA blending slices to obtain slow-release type multifunctional PLA fibers; or, performing spunbonding non-weaving processing on the PLA/EVOH/CGA blending slice to obtain a slow-release type multifunctional PLA non-woven material;
Wherein, the mass ratio of PLA, EVOH, CGA is 80-95: 5-20: 1 to 15.
[ Advantageous effects ]
(1) The PLA resource is renewable and biodegradable, and the problems of resource shortage, environmental pollution and the like existing in the development of synthetic fibers can be solved by taking the PLA resource as a raw material; the existing PLA fiber has low functionalization, the natural extract CGA is taken as a functional factor, and the PLA fiber and the non-woven material prepared by introducing the natural extract CGA into the PLA have the functions of antioxidation, ultraviolet shielding and the like, so that the requirements of people on the functional PLA fiber and the non-woven material can be met, and the CGA is derived from plants such as eucommia ulmoides, honeysuckle and the like, has the functions of antioxidation, ultraviolet shielding and the like, and is harmless to human bodies.
(2) According to the invention, the hydrophilic polymer EVOH is introduced, so that the release rate of the functional factor CGA is increased, and the release rate of the CGA in the PLA fiber or the nonwoven material can be regulated and controlled by controlling the content of the EVOH.
(3) The melting point of CGA is about 210 ℃, the melting point of EVOH is 160-195 ℃, and the melting point of EVOH is close to that of PLA, so that the CGA is suitable for melt blending processing with PLA to prepare slow-release type multifunctional PLA fiber and slow-release type multifunctional spun-bonded PLA non-woven material, and simultaneously, the physical and mechanical properties of the fiber and non-woven material are maintained, so that the slow-release type multifunctional PLA fiber and the slow-release type multifunctional spun-bonded PLA non-woven material have good spinnability; and the introduction of CGA and EVOH does not reduce the spinnability and mechanical properties of the PLA matrix.
(4) The ultraviolet transmittance of the slow-release type multifunctional PLA fiber prepared by the invention is below 6.5%, the free radical clearance is above 9.6%, the strength is above 2.0cN/dtex, and the accumulated release amount is above 2.5% in seven days; the ultraviolet transmittance of the slow-release type multifunctional PLA nonwoven material is below 3.8%, the free radical clearance is above 39.2%, and the accumulated release amount in seven days is above 3.36%.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for better illustration of the invention, and should not be construed as limiting the invention.
The testing method comprises the following steps:
1. The testing method of tensile mechanical properties comprises the following steps:
The tensile mechanical properties of the polylactic acid fibers are tested according to the national standard GB/T14344-2022 chemical fiber filament tensile property test method.
2. The oxidation resistance testing method comprises the following steps:
Respectively weighing 3mgABTS diammonium salt and 1mg K 2S2O8, respectively diluting with 0.735mL and 1.43mL of distilled water, and respectively taking diluted solutions according to the volume ratio of 1:1, mixing the materials in proportion; after standing for 12h in dark environment, the mixed solution is diluted by PBS buffer solution until the absorbance at 734nm is 0.70+/-0.02, and the solution is the ABTS solution.
Adding 1mL of prepared ABTS solution into 5mg of samples, standing for 2h at room temperature, measuring the absorbance of the solution by an enzyme-labeled instrument, setting three groups of experiments on each sample, recording the absorbance of the solution before and after the experiments, substituting the absorbance value into the following formula (1), calculating the clearance of the ABTS free radicals, and taking the average value of the calculation results.
Wherein: a spl is the initial absorbance of the ABTS solution; a ctrl represents the absorbance of the ABTS solution 2h after addition of the sample.
3. The release performance test method comprises the following steps:
20mg of fiber or nonwoven material is weighed and placed in a 15mL centrifuge tube with a cover, 10mLPBS buffer solution is added into the centrifuge tube, the centrifuge tube is placed in a constant temperature box at 37 ℃ to simulate an in-vitro release process, 200 mu L of solution is sucked at a set time point to test absorbance at 323nm, and then 200 mu L of PBS buffer solution is supplemented into the centrifuge tube to keep the volume of the solution constant.
And (3) calculating the CGA concentration of each time point through the standard absorption curve of the CGA, and substituting the CGA concentration value into the formula (2) to calculate the accumulated release rate of the CGA.
Wherein: q n is the cumulative release rate of the CGA at time n; c n is CGA concentration (mg/mL) of the nth sample; v i is the volume of solution (mL) removed at time i; m is CGA mass (mg) in the fiber or nonwoven.
4. The ultraviolet shielding performance test method comprises the following steps:
And (3) fibers: the fibers are closely arranged in parallel, two ends of the fibers are stuck on a rectangular die (the middle is hollowed, the length is 3cm, the width is 2.5 cm), a layer of the fibers is stuck on the front side and the back side respectively, the arranged fibers are placed in a light path of an ultraviolet-visible near-infrared spectrophotometer to test the transmittance, the wavelength of the ultraviolet-visible light is 200-600nm, and the interval is 2nm.
Nonwoven material: the nonwoven material is put into the light path of an ultraviolet-visible near-infrared spectrophotometer to test the transmittance, the wavelength of the ultraviolet-visible light is 200-600nm, and the interval is 2nm.
The starting materials used in the examples and comparative examples:
PLA, EVOH, CGA it was dried in a vacuum oven at 75 ℃ for 24 hours before use.
Example 1
A method for preparing chlorogenic acid-containing slow-release multifunctional PLA fiber, comprising the following steps:
(1) Primary granulation:
putting EVOH with 32% of ethylene structural unit content and CGA into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulation temperature is 195 ℃, and the screw rotation speed is 400rpm, so as to obtain EVOH/CGA blending slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(2) And (3) secondary granulation:
Putting PLA and EVOH/CGA blend slices with melt flow index of 8g/10min (210 ℃,2.16 kg) and D-LA content of 0.25mol% into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulating temperature is 195 ℃, and the screw rotating speed is 400rpm, so as to obtain PLA/EVOH/CGA blend slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(3) Preparing a slow-release type multifunctional polylactic acid fiber:
Melt spinning (spinning temperature is 195 ℃ and spinning speed is 2000 m/min) is carried out on PLA/EVOH/CGA blend slices to obtain a primary multifilament; drawing the as-spun multifilament at 90 deg.c and drawing multiple of 6; finally, performing heat setting, wherein the heat setting temperature is 120 ℃, and the slow-release type multifunctional PLA multifilament is obtained;
Wherein, PLA, EVOH, CGA mass ratio is 90:10:3.
Comparative example 1
The CGA in step (1) of example 1 was omitted, and the same as in example 1 was maintained to obtain a PLA multifilament yarn.
Comparative example 2
The EVOH in step (1) of example 1 was omitted, and the same procedure as in example 1 was repeated to obtain a PLA multifilament yarn.
Comparative example 3
The CGA in step (1) of example 1 was adjusted to tea polyphenol, and the other was kept the same as in example 1 to obtain PLA multifilament yarn.
Comparative example 4
EVOH in step (1) of example 1 was adjusted to BVOH (butene diol-vinyl alcohol copolymer, BVE-8049P, nippon Co., japan), and the same procedure as in example 1 was followed to obtain a PLA multifilament.
Performance test the PLA multifilament yarns obtained in example 1 and comparative examples 1 to 4 were subjected to the following test results:
Table 1 test results
As can be seen from table 1:
When the CGA in the PLA multifilament is 5%, introducing 10% of EVOH can obviously improve the free radical clearance rate of the PLA multifilament, namely the oxidation resistance, and the seven-day accumulated release rate of the CGA is obviously increased; the tensile mechanical properties of PLA fibers are not much different from those of PLA fibers when EVOH is not added;
When EVOH was omitted, the release rate of CGA was too slow, with a seven day cumulative release of CGA of only 0.61%, so that radical scavenging was only 6.1%;
When CGA is tea polyphenol, chemical reaction is easy to occur at high temperature, and PLA becomes black and crisp when melt blending is performed, so that spinning is difficult;
When EVOH is BVOH, BVOH is a water-soluble polymer, so that the accumulated release rate of CGA is increased to 55.2% in seven days, and the problem of burst release exists, so that the functional attenuation of the functional PLA fiber is fast; in addition, functional PLA fibers containing water-solubility BVOH can have problems with dissolution of the polymer BVOH during use.
Example 2
A method for preparing chlorogenic acid-containing slow-release multifunctional PLA fiber, comprising the following steps:
(1) Primary granulation:
putting EVOH with 32% of ethylene structural unit content and CGA into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulation temperature is 195 ℃, and the screw rotation speed is 400rpm, so as to obtain EVOH/CGA blending slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(2) And (3) secondary granulation:
Putting PLA and EVOH/CGA blend slices with melt flow index of 8g/10min (210 ℃,2.16 kg) and D-LA content of 0.25mol% into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulating temperature is 195 ℃, and the screw rotating speed is 400rpm, so as to obtain PLA/EVOH/CGA blend slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(3) Preparing a slow-release type multifunctional polylactic acid fiber:
Melt spinning (spinning temperature is 195 ℃ and spinning speed is 2000 m/min) is carried out on PLA/EVOH/CGA blend slices to obtain a primary multifilament; drawing the as-spun multifilament at 90 deg.c and drawing multiple of 6; finally, performing heat setting, wherein the heat setting temperature is 120 ℃, and the slow-release type multifunctional PLA multifilament is obtained;
Wherein, the mass ratio of PLA, EVOH and chlorogenic acid is 95:5:3.
Example 3
A method for preparing chlorogenic acid-containing slow-release multifunctional PLA fiber, comprising the following steps:
(1) Primary granulation:
putting EVOH with 32% of ethylene structural unit content and CGA into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulation temperature is 195 ℃, and the screw rotation speed is 400rpm, so as to obtain EVOH/CGA blending slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(2) And (3) secondary granulation:
Putting PLA and EVOH/CGA blend slices with melt flow index of 8g/10min (210 ℃,2.16 kg) and D-LA content of 0.25mol% into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulating temperature is 195 ℃, and the screw rotating speed is 400rpm, so as to obtain PLA/EVOH/CGA blend slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(3) Preparing a slow-release type multifunctional polylactic acid fiber:
Melt spinning (spinning temperature is 195 ℃ and spinning speed is 2000 m/min) is carried out on PLA/EVOH/CGA blend slices to obtain a primary multifilament; drawing the as-spun multifilament at 90 deg.c and drawing multiple of 6; finally, performing heat setting, wherein the heat setting temperature is 120 ℃, and the slow-release type multifunctional PLA multifilament is obtained;
wherein, PLA, EVOH, CGA mass ratio is 80:20:3.
Example 4
A method for preparing chlorogenic acid-containing slow-release multifunctional PLA fiber, comprising the following steps:
(1) Primary granulation:
putting EVOH with 32% of ethylene structural unit content and CGA into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulation temperature is 195 ℃, and the screw rotation speed is 400rpm, so as to obtain EVOH/CGA blending slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(2) And (3) secondary granulation:
Putting PLA and EVOH/CGA blend slices with melt flow index of 8g/10min (210 ℃,2.16 kg) and D-LA content of 0.25mol% into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulating temperature is 195 ℃, and the screw rotating speed is 400rpm, so as to obtain PLA/EVOH/CGA blend slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(3) Preparing a slow-release type multifunctional polylactic acid fiber:
Melt spinning (spinning temperature is 195 ℃ and spinning speed is 2000 m/min) is carried out on PLA/EVOH/CGA blend slices to obtain a primary multifilament; drawing the as-spun multifilament at 90 deg.c and drawing multiple of 6; finally, performing heat setting, wherein the heat setting temperature is 120 ℃, and the slow-release type multifunctional PLA multifilament is obtained;
wherein, PLA, EVOH, CGA mass ratio is 90:10:1.
Example 5
A method for preparing chlorogenic acid-containing slow-release multifunctional PLA fiber, comprising the following steps:
(1) Primary granulation:
putting EVOH with 32% of ethylene structural unit content and CGA into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulation temperature is 195 ℃, and the screw rotation speed is 400rpm, so as to obtain EVOH/CGA blending slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(2) And (3) secondary granulation:
Putting PLA and EVOH/CGA blend slices with melt flow index of 8g/10min (210 ℃,2.16 kg) and D-LA content of 0.25mol% into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulating temperature is 195 ℃, and the screw rotating speed is 400rpm, so as to obtain PLA/EVOH/CGA blend slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(3) Preparing a slow-release type multifunctional polylactic acid fiber:
Melt spinning (spinning temperature is 195 ℃ and spinning speed is 2000 m/min) is carried out on PLA/EVOH/CGA blend slices to obtain a primary multifilament; drawing the as-spun multifilament at 90 deg.c and drawing multiple of 6; finally, performing heat setting, wherein the heat setting temperature is 120 ℃, and the slow-release type multifunctional PLA multifilament is obtained;
wherein, PLA, EVOH, CGA mass ratio is 90:10:5.
Example 6
A method for preparing chlorogenic acid-containing slow-release multifunctional PLA fiber, comprising the following steps:
(1) Primary granulation:
putting EVOH with 32% of ethylene structural unit content and CGA into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulation temperature is 195 ℃, and the screw rotation speed is 400rpm, so as to obtain EVOH/CGA blending slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(2) And (3) secondary granulation:
Drying dextrorotatory polylactic acid (PDLA) with a melt flow index of 8g/10min (210 ℃,2.16 kg) and a D-LA content of 0.25mol percent in a vacuum oven with a melt flow index of 16g/10min (210 ℃,2.16 kg) for 24 hours at 75 ℃ for later use; then according to 50:50, weighing PLA and PDLA according to a mass ratio, putting the PLA and the PDLA into a high-speed mixer for premixing for 5min, and then melting, blending and granulating in a double-screw blender, wherein the granulating temperature is 230 ℃, and the screw rotating speed is 400rpm, so as to obtain a three-dimensional composite PLA (sc-PLA) slice; drying in a vacuum oven at 75 ℃ for 24 hours for standby;
putting the sc-PLA slice and the EVOH/CGA blending slice into a high-speed mixer for premixing for 5min, and then melting, blending and granulating in a double-screw blender at the granulating temperature of 230 ℃ and the screw rotating speed of 400rpm to obtain the sc-PLA/EVOH/CGA blending slice; the resulting slices were dried under vacuum at 75℃for 24h for use.
(3) Preparing a slow-release type multifunctional polylactic acid fiber:
Melt spinning (spinning temperature 235 ℃ C., spinning speed 2000 m/min) the sc-PLA/EVOH/CGA blend chips to obtain as-spun multifilament; drawing the as-spun multifilament at 120 deg.c and drawing multiple of 6; finally, performing heat setting, wherein the heat setting temperature is 160 ℃, and the slow-release type multifunctional PLA multifilament is obtained;
wherein, the mass ratio of sc-PLA, EVOH, CGA is 90:10:3.
Performance test the PLA multifilament yarns obtained in examples 2 to 6 were tested as follows:
Table 2 test results
Example 7
A method for preparing a chlorogenic acid-containing slow-release multifunctional PLA nonwoven material, comprising the following steps:
(1) Primary granulation:
Putting EVOH with 32% of ethylene structural unit content and CGA into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulation temperature is 195 ℃, and the screw rotation speed is 400rpm, so as to prepare EVOH/CGA blending slices; vacuum drying the prepared slice at 75deg.C for 24 h;
(2) And (3) secondary granulation:
putting PLA and EVOH/CGA blend slices with melt flow index of 8g/10min (210 ℃,2.16 kg) and D-LA content of 0.25mol% into a high-speed mixer for premixing for 5min, and then carrying out melt blending granulation in a double-screw blender, wherein the granulating temperature is 195 ℃, and the screw rotating speed is 400rpm, so as to obtain PLA/EVOH/CGA blend slices; the resulting slices were dried under vacuum at 75℃for 24h for use.
(3) Preparing a slow-release multifunctional polylactic acid non-woven material:
Taking PLA/EVOH/CGA blending slice as raw material, carrying out spunbonding non-weaving processing, and carrying out spinning net forming (the spinning temperature is 195 ℃, the spinning speed is 3500m/min, the net forming speed is 24m/min, the pump supply amount is 48 mL/min), hot rolling reinforcement (the hot rolling line pressure is 70N/mm, and the hot rolling mill temperature is 70 ℃), so as to prepare the slow-release type multifunctional polylactic acid non-woven material;
Wherein, PLA, EVOH, CGA mass ratio is 90:10:3.
The performance of the obtained slow-release multifunctional polylactic acid non-woven material is tested, and the test results are as follows:
The surface density was 35g/m 2, the ultraviolet transmittance was 3.8%, the radical scavenging rate was 39.2%, and the cumulative release rate of CGA for seven days was 3.36%.
While the invention has been described with reference to the preferred embodiments, it is not limited thereto, and various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A method for preparing a CGA-containing slow-release multifunctional PLA textile, comprising the steps of:
(1) Carrying out melt blending granulation on hydrophilic polymer ethylene-vinyl alcohol copolymer (EVOH) and chlorogenic acid (CGA) to obtain EVOH/CGA blending slices; wherein, the melt blending granulation is carried out by adopting a double-screw extruder, the granulation temperature is 170-230 ℃, and the screw rotating speed is 300-500 rpm;
(2) Carrying out melt blending granulation on polylactic acid PLA and EVOH/CGA blending slices to obtain PLA/EVOH/CGA blending slices; wherein, the melt blending granulation is carried out by adopting a double-screw extruder, the granulation temperature is 170-230 ℃, and the screw rotating speed is 300-500 rpm;
(3) Carrying out melt spinning, drafting and heat setting on PLA/EVOH/CGA blending slices to obtain slow-release type multifunctional PLA fibers; or, performing spunbonding non-weaving processing on the PLA/EVOH/CGA blending slice to obtain a slow-release type multifunctional PLA non-woven material;
Wherein, the mass ratio of PLA, EVOH, CGA is 80-95: 5-20: 1 to 15;
The spinning temperature in the melt spinning is 180-240 ℃ and the spinning speed is 1500-5000 m/min; the drafting temperature is 85-130 ℃, and the drafting multiple is 4-10; the heat setting temperature is 120-170 ℃;
the spunbonding non-woven processing is spunlaying and hot rolling reinforcement; wherein the spinning temperature in the spinning and net forming is 180-240 ℃, the spinning speed is 3000-6000 m/min, the net forming speed is 5-30 m/min, and the pump supply is 30-150 mL/min; the pressure of the hot rolling line is 65-75N/mm, and the temperature of the roller is 65-180 ℃.
2. The slow-release multifunctional PLA fiber prepared by the method of claim 1.
3. The slow-release multifunctional spunbond PLA nonwoven material prepared by the method of claim 1.
4. A slow-release multifunctional textile, characterized in that the slow-release multifunctional PLA fiber of claim 2 or the slow-release multifunctional spunbond PLA nonwoven material of claim 3 is used.
5. Use of the slow-release multifunctional PLA fiber of claim 2 in the textile field.
6. Use of the slow release multifunctional spunbond PLA nonwoven material of claim 3 in the textile field.
7. A method for improving the ultraviolet resistance and oxidation resistance of a polylactic acid textile, which is characterized by comprising the following steps:
(1) Carrying out melt blending granulation on hydrophilic polymer ethylene-vinyl alcohol copolymer (EVOH) and chlorogenic acid (CGA) to obtain EVOH/CGA blending slices; wherein, the melt blending granulation is carried out by adopting a double-screw extruder, the granulation temperature is 170-230 ℃, and the screw rotating speed is 300-500 rpm;
(2) Carrying out melt blending granulation on polylactic acid PLA and EVOH/CGA blending slices to obtain PLA/EVOH/CGA blending slices; wherein, the melt blending granulation is carried out by adopting a double-screw extruder, the granulation temperature is 170-230 ℃, and the screw rotating speed is 300-500 rpm;
(3) Carrying out melt spinning, drafting and heat setting on PLA/EVOH/CGA blend slices to obtain PLA fibers with ultraviolet resistance and oxidation resistance; or, performing spunbonding non-weaving processing on the PLA/EVOH/CGA blend slice to obtain a PLA non-woven material with ultraviolet resistance and oxidation resistance;
Wherein, the mass ratio of PLA, EVOH, CGA is 80-95: 5-20: 1 to 15;
The spinning temperature in the melt spinning is 180-240 ℃ and the spinning speed is 1500-5000 m/min; the drafting temperature is 85-130 ℃, and the drafting multiple is 4-10; the heat setting temperature is 120-170 ℃;
the spunbonding non-woven processing is spunlaying and hot rolling reinforcement; wherein the spinning temperature in the spinning and net forming is 180-240 ℃, the spinning speed is 3000-6000 m/min, the net forming speed is 5-30 m/min, and the pump supply is 30-150 mL/min; the pressure of the hot rolling line is 65-75N/mm, and the temperature of the roller is 65-180 ℃.
8. A method for improving the slow release performance of chlorogenic acid in polylactic acid textiles, which is characterized by comprising the following steps:
(1) Carrying out melt blending granulation on hydrophilic polymer ethylene-vinyl alcohol copolymer (EVOH) and chlorogenic acid (CGA) to obtain EVOH/CGA blending slices; wherein, the melt blending granulation is carried out by adopting a double-screw extruder, the granulation temperature is 170-230 ℃, and the screw rotating speed is 300-500 rpm;
(2) Carrying out melt blending granulation on polylactic acid PLA and EVOH/CGA blending slices to obtain PLA/EVOH/CGA blending slices; wherein, the melt blending granulation is carried out by adopting a double-screw extruder, the granulation temperature is 170-230 ℃, and the screw rotating speed is 300-500 rpm;
(3) Carrying out melt spinning, drafting and heat setting on PLA/EVOH/CGA blending slices to obtain slow-release type multifunctional PLA fibers; or, performing spunbonding non-weaving processing on the PLA/EVOH/CGA blending slice to obtain a slow-release type multifunctional PLA non-woven material;
Wherein, the mass ratio of PLA, EVOH, CGA is 80-95: 5-20: 1 to 15;
The spinning temperature in the melt spinning is 180-240 ℃ and the spinning speed is 1500-5000 m/min; the drafting temperature is 85-130 ℃, and the drafting multiple is 4-10; the heat setting temperature is 120-170 ℃;
the spunbonding non-woven processing is spunlaying and hot rolling reinforcement; wherein the spinning temperature in the spinning and net forming is 180-240 ℃, the spinning speed is 3000-6000 m/min, the net forming speed is 5-30 m/min, and the pump supply is 30-150 mL/min; the pressure of the hot rolling line is 65-75N/mm, and the temperature of the roller is 65-180 ℃.
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| CN115772713A (en) * | 2022-11-30 | 2023-03-10 | 安徽皖维高新材料股份有限公司 | Method for preparing PVA (polyvinyl alcohol) coarse denier fiber through melt plasticization-wet spinning |
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| CN115772713A (en) * | 2022-11-30 | 2023-03-10 | 安徽皖维高新材料股份有限公司 | Method for preparing PVA (polyvinyl alcohol) coarse denier fiber through melt plasticization-wet spinning |
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