CN116516517B - ES large biological fiber containing saussurea involucrata active ingredient and preparation method thereof - Google Patents
ES large biological fiber containing saussurea involucrata active ingredient and preparation method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 241001145025 Saussurea involucrata Species 0.000 title claims abstract description 22
- 239000004480 active ingredient Substances 0.000 title claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 50
- 239000012792 core layer Substances 0.000 claims abstract description 36
- 238000005507 spraying Methods 0.000 claims abstract description 24
- 239000002131 composite material Substances 0.000 claims abstract description 19
- 238000009987 spinning Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000001694 spray drying Methods 0.000 claims abstract description 16
- 239000010410 layer Substances 0.000 claims abstract description 13
- 108010059892 Cellulase Proteins 0.000 claims abstract description 6
- 108091005804 Peptidases Proteins 0.000 claims abstract description 6
- 239000004365 Protease Substances 0.000 claims abstract description 6
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims abstract description 6
- 229940106157 cellulase Drugs 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000001125 extrusion Methods 0.000 claims description 80
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 20
- 229920002401 polyacrylamide Polymers 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 230000005855 radiation Effects 0.000 claims description 14
- 238000005469 granulation Methods 0.000 claims description 13
- 230000003179 granulation Effects 0.000 claims description 13
- 230000004048 modification Effects 0.000 claims description 12
- 238000012986 modification Methods 0.000 claims description 12
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 10
- 239000004698 Polyethylene Substances 0.000 claims description 10
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 10
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 10
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 10
- 235000011152 sodium sulphate Nutrition 0.000 claims description 10
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000010411 cooking Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 5
- 150000001412 amines Chemical class 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229920002554 vinyl polymer Polymers 0.000 claims description 5
- 239000004246 zinc acetate Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 238000013329 compounding Methods 0.000 claims 1
- 238000010025 steaming Methods 0.000 abstract description 12
- 230000035699 permeability Effects 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000011162 core material Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 239000004744 fabric Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000008187 granular material Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000006057 Non-nutritive feed additive Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
-
- 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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- 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
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of ES large biological fiber containing saussurea involucrata active ingredient, which comprises the steps of preparing active particles, preparing skin layer materials, preparing core layer materials, carrying out composite spinning and post-treatment; cleaning herba Saussureae Involueratae, placing in deionized water, steaming at high temperature, adding protease and cellulase, vacuum spray drying to obtain primary active particles, and spraying active liquid to the surface of the primary active particles to obtain active particles; the invention can improve the softness, air permeability, strength and thermal stability of the ES fiber while improving the strength and deformation resistance of the ES fiber.
Description
Technical Field
The invention relates to an ES large biological fiber containing saussurea involucrata active ingredient and a preparation method thereof, belonging to the technical field of ES fibers.
Background
The ES fiber is a double-component sheath-core structure composite fiber, the sheath tissue has low melting point and good softness, and the core tissue has high melting point and high strength. After heat treatment, part of the cortex is melted to play a role in bonding, and the rest of the cortex still keeps the fiber state, meanwhile, the fiber has the characteristic of small heat shrinkage rate, and is particularly suitable for producing products such as sanitary materials, thermal insulation filling materials, filter materials and the like by a hot air penetrating process.
The ES fiber has the advantages of fluffiness, soft hand feeling, good elasticity, strong heat retention and good moisture absorption and air permeability; the product has stable acid resistance, alkali resistance, no toxicity, no chemical action and natural degradation; however, the ES fiber has low strength and is easy to deform, which seriously affects the popularization of the ES fiber.
Although the strength and the deformation resistance of the ES fiber are improved by modifying the ES fiber, the shaping component is generally added into the ES fiber, but the softness and the air permeability of the ES fiber are affected, so that the softness, the air permeability, the melting point, the strength and the thermal stability of the ES fiber are improved while the strength and the deformation resistance of the ES fiber are improved, and are key in the research, the development and the production of the ES fiber at present.
Patent CN102851788B discloses an ES fiber and its application, the raw materials of the ES fiber and its weight parts composition are: 5-50 parts of superfine diatomite; 20-70 parts of cortex resin; 20-70 parts of core resin; 0.2 to 1.0 of antioxidant; 0.1 to 1.0 percent of processing aid; 0.1 to 5.0 portions of coupling agent; the deficiency of this patent: the ES fibers have poor resistance to deformation.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides an ES large biological fiber containing a saussurea involucrata active ingredient and a preparation method thereof, which realize the following aims: the softness, air permeability, strength and thermal stability of the ES fibers can be improved while the strength and deformation resistance of the ES fibers are improved.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
The preparation method of the ES large biological fiber containing the active component of the saussurea involucrata comprises the steps of preparing active particles, preparing a skin layer material, preparing a core layer material, carrying out composite spinning and carrying out aftertreatment.
The preparation method comprises the steps of preparing active particles, cleaning herba Saussureae Involueratae, placing the herba Saussureae Involueratae in deionized water, controlling the mass ratio of herba Saussureae Involueratae to the deionized water to be 1:15-20, then performing high-temperature cooking, controlling the temperature of the high-temperature cooking to be 85-90 ℃, the time of the high-temperature cooking to be 30-40min, cooling to 25-30 ℃, adding protease and cellulase, standing at 25-30 ℃ for 40-50min, adjusting the pH to 10-11 by using 15-20% sodium hydroxide solution, then performing vacuum spray drying, controlling the vacuum degree of the vacuum spray drying to be 0.09-0.092MPa, the air inlet temperature to be 120-130 ℃, and performing vacuum spray drying to obtain primary active particles, spraying active liquid on the surfaces of the primary active particles, controlling the mass ratio of the primary active particles to be 1:2-3, the spraying pressure during spraying to be 0.35-0.45MPa, the spraying time to be 10-12s, and drying at 80-90 ℃ for 1.5-2h after the spraying to obtain the active particles;
The active liquid comprises the following raw materials in parts by weight: 30-40 parts of deionized water, 0.1-0.2 part of polyvinyl amine, 1-2 parts of zinc acetate, 2-3 parts of nano titanium dioxide and 1.5-2.5 parts of polyethylene glycol;
The particle size of the nano titanium dioxide is 300-400nm.
The preparation method comprises the steps of uniformly mixing PE slices, active particles, sodium stearate, light calcium carbonate, maleated rosin and sodium chloride, adding into a double-screw extruder, extruding and granulating, and extruding from the double-screw extruder to obtain the cortex material;
The length-diameter ratio of the twin-screw extruder is 40-45:1, the grain cutting is water-cooling grain cutting, the extrusion temperature of the first section is 250-255 ℃, the extrusion temperature of the second section is 255-260 ℃, the extrusion temperature of the third section is 260-265 ℃, the extrusion temperature of the fourth section is 265-270 ℃, the extrusion temperature of the fifth section is 275-280 ℃, the extrusion temperature of the sixth section is 270-275 ℃, and the extrusion temperature of the seventh section is 265-270 ℃.
The raw materials in the preparation of the skin layer material comprise the following components in parts by weight: 70-80 parts of PE slices, 5-7 parts of active particles, 2-3 parts of sodium stearate, 3-4 parts of light calcium carbonate, 1-2 parts of maleated rosin and 0.5-1 part of sodium chloride.
The preparation method comprises the steps of uniformly mixing PP slices, active particles, zwitterionic polyacrylamide, PET slices and sodium sulfate, adding into a double-screw extruder for extrusion granulation, controlling the length-diameter ratio of the double-screw extruder to be 35-40:1, performing water-cooling granulation, performing extrusion at the first section at 240-245 ℃, performing extrusion at 250-255 ℃, performing extrusion at the third section at 260-265 ℃, performing extrusion at 270-275 ℃, performing extrusion at the fifth section at 260-265 ℃, performing extrusion at the sixth section at 250-255 ℃, performing extrusion at the seventh section at 240-245 ℃, and performing extrusion from the double-screw extruder to obtain the core layer material;
The raw materials in the preparation of the core layer material comprise the following components in parts by weight: 70-80 parts of PP slice, 2-3 parts of active particles, 4-5 parts of zwitterionic polyacrylamide, 4-5 parts of PET slice and 1-2 parts of sodium sulfate.
The composite spinning is carried out, a core layer material is added into a screw extruder, the temperature of the screw extruder is controlled to be 220-225 ℃, and the pressure is controlled to be 0.3-0.35MPa, so that a core layer melt is obtained; simultaneously adding the cortex material into another screw extruder, controlling the temperature of the screw extruder to be 230-235 ℃ and the pressure to be 0.35-0.4MPa, and obtaining cortex melt; then the core layer melt and the skin layer melt enter a composite spinning machine component through a metering pump, and primary ES fibers are sprayed out through a spinneret plate after being compounded in the composite spinning component;
the mass ratio of the sheath melt to the core melt is 1:1.5-2;
the spinneret plate is characterized in that the spinneret plate is cross-shaped, the pressure of a nozzle is 2.0-2.5kg/cm 2, and the temperature of a die head is controlled at 210-220 ℃.
And (3) carrying out the post-treatment, namely carrying out radiation modification on the primary ES fibers through a high-speed electron field, controlling the radiation dose to be 90-100KGy, and obtaining the ES large biological fibers after the radiation modification is finished.
Compared with the prior art, the invention has the beneficial effects that:
(1) The ES large biological fiber containing the saussurea involucrata active ingredient prepared by the invention can improve the strength of the ES large biological fiber by adding the amphoteric ion polyacrylamide in the step of preparing the core layer material, and the dry breaking strength of the ES large biological fiber prepared by the invention is 3.5-4.5cN/dtex, and the wet breaking strength is 2.2-2.9cN/dtex.
(2) The ES large biological fiber containing the active ingredient of the saussurea involucrata prepared by the invention can improve the deformation resistance by adding the zwitterionic polyacrylamide and carrying out post-treatment on the fiber in the step of preparing the core layer material, and the lateral dimension change rate is 0.2-0.5% and the longitudinal dimension change rate is 0.2-0.4% after 100 times of standard water washing;
(3) The ES large biological fiber containing the active ingredient of the saussurea involucrata prepared by the invention can improve the softness by spraying the active liquid in the step of preparing active particles and adding the amphoteric ion polyacrylamide in the step of preparing core layer materials, the transverse softness can reach 40-45mN, and the longitudinal softness can reach 43-48mN;
(4) The ES large biological fiber containing the active ingredient of the saussurea involucrata prepared by the invention can improve the air permeability by adding the zwitterionic polyacrylamide and carrying out post-treatment on the fiber in the step of preparing the core layer material, and the air permeability of the fabric prepared by the ES large biological fiber containing the active ingredient of the saussurea involucrata prepared by the invention is improved to 1950-2050L/m < 2 >. S;
(5) The ES large biological fiber containing the saussurea involucrata active ingredient prepared by the invention can improve the thermal stability by spraying active liquid in the step of preparing active particles and adding amphoteric ion polyacrylamide in the step of preparing core layer materials, and can be stood for 3 months in an environment with the temperature of 120 ℃ and the humidity of 80%, wherein the dry breaking strength is 3.4-4.5cN/dtex, and the wet breaking strength is 2.1-2.7cN/dtex.
Detailed Description
Specific embodiments of the present invention will now be described in order to provide a clearer understanding of the technical features, objects and effects of the present invention.
Example 1
The preparation method of the ES large biological fiber containing the active component of the saussurea involucrata comprises the following specific steps:
1. Preparation of active particles: cleaning herba Saussureae Involueratae, placing in deionized water, controlling the mass ratio of herba Saussureae Involueratae to deionized water to be 1:15, then performing high-temperature steaming, controlling the temperature of the high-temperature steaming to be 85 ℃, the time of the high-temperature steaming to be 30min, cooling to 25 ℃, adding protease and cellulase, standing at 25 ℃ for 40min, adjusting the pH to 10 by using 15% sodium hydroxide solution, then performing vacuum spray drying, controlling the vacuum degree of the vacuum spray drying to be 0.09MPa, the air inlet temperature to be 120 ℃, and the vacuum spray drying to be finished to obtain primary active particles, spraying active liquid on the surfaces of the primary active particles, controlling the mass ratio of the primary active particles to the active liquid to be 1:2, and the spraying pressure during spraying to be 0.35MPa, wherein the spraying time is 10s, and drying is performed at 80 ℃ for 1.5h after the spraying to obtain active particles;
The active liquid comprises the following raw materials in parts by weight: 30 parts of deionized water, 0.1 part of polyvinyl amine, 1 part of zinc acetate, 2 parts of nano titanium dioxide and 1.5 parts of polyethylene glycol;
the particle size of the nano titanium dioxide is 300nm.
2. Preparing a cortex material: uniformly mixing PE slices, active particles, sodium stearate, light calcium carbonate, maleated rosin and sodium chloride, adding the mixture into a double-screw extruder for extrusion granulation, controlling the length-diameter ratio of the double-screw extruder to be 40:1, performing water-cooling granulation, wherein the extrusion temperature of the first section is 250 ℃, the extrusion temperature of the second section is 255 ℃, the extrusion temperature of the third section is 260 ℃, the extrusion temperature of the fourth section is 265 ℃, the extrusion temperature of the fifth section is 275 ℃, the extrusion temperature of the sixth section is 270 ℃, the extrusion temperature of the seventh section is 265 ℃, and extruding the mixture from the double-screw extruder to obtain a skin material;
The raw materials in the preparation of the skin layer material comprise the following components in parts by weight: 70 parts of PE slices, 5 parts of active particles, 2 parts of sodium stearate, 3 parts of light calcium carbonate, 1 part of maleated rosin and 0.5 part of sodium chloride.
3. Preparing a core layer material: uniformly mixing PP slices, active particles, zwitterionic polyacrylamide, PET slices and sodium sulfate, adding into a double-screw extruder for extrusion granulation, controlling the length-diameter ratio of the double-screw extruder to be 35:1, cutting into water-cooling granules, wherein the extrusion temperature of the first section is 240 ℃, the extrusion temperature of the second section is 250 ℃, the extrusion temperature of the third section is 260 ℃, the extrusion temperature of the fourth section is 270 ℃, the extrusion temperature of the fifth section is 260 ℃, the extrusion temperature of the sixth section is 250 ℃, and the extrusion temperature of the seventh section is 240 ℃, and extruding from the double-screw extruder to obtain a core layer material;
The raw materials in the preparation of the core layer material comprise the following components in parts by weight: 70 parts of PP slice, 2 parts of active particles, 4 parts of zwitterionic polyacrylamide, 4 parts of PET slice and 1 part of sodium sulfate.
4. And (3) composite spinning: adding a core layer material into a screw extruder, controlling the temperature of the screw extruder to 220 ℃ and the pressure to 0.3MPa, and obtaining a core layer melt; simultaneously adding the cortex material into another screw extruder, controlling the temperature of the screw extruder to be 230 ℃ and the pressure to be 0.35MPa, and obtaining cortex melt; then the core layer melt and the skin layer melt enter a composite spinning machine component through a metering pump, and primary ES fibers are sprayed out through a spinneret plate after being compounded in the composite spinning component;
the mass ratio of the sheath melt to the core melt is 1:1.5;
The spinneret plate is characterized in that the shape of a spinneret hole is cross-shaped, the pressure of a nozzle is 2.0kg/cm 2, and the temperature of a die head is controlled at 210 ℃.
5. Post-treatment: and carrying out radiation modification on the primary ES fiber by a high-speed electron field, controlling the radiation dose to be 90KGy, and obtaining the ES large biological fiber after the radiation modification is finished.
Example 2
The preparation method of the ES large biological fiber containing the active component of the saussurea involucrata comprises the following specific steps:
1. Preparation of active particles: cleaning herba Saussureae Involueratae, placing in deionized water, controlling the mass ratio of herba Saussureae Involueratae to deionized water to be 1:17, then performing high-temperature steaming, controlling the temperature of the high-temperature steaming to be 87 ℃ and the time of the high-temperature steaming to be 35min, cooling to 27 ℃ after the high-temperature steaming is finished, adding protease and cellulase, standing at 27 ℃ for 45min, adjusting the pH to 10 by using 17% sodium hydroxide solution, then performing vacuum spray drying, controlling the vacuum degree of the vacuum spray drying to be 0.091MPa, the air inlet temperature to be 125 ℃, and performing vacuum spray drying to obtain primary active particles, spraying active liquid on the surfaces of the primary active particles, controlling the mass ratio of the primary active particles to the active liquid to be 1:2.5, and drying at 85 ℃ for 1.7h after the spraying is finished, wherein the spraying pressure is 0.4MPa, and the spraying time is 11s, so as to obtain active particles;
The active liquid comprises the following raw materials in parts by weight: 35 parts of deionized water, 0.15 part of polyvinyl amine, 1.5 parts of zinc acetate, 2.5 parts of nano titanium dioxide and 2 parts of polyethylene glycol;
the particle size of the nano titanium dioxide is 350nm.
2. Preparing a cortex material: uniformly mixing PE slices, active particles, sodium stearate, light calcium carbonate, maleated rosin and sodium chloride, adding the mixture into a double-screw extruder for extrusion granulation, controlling the length-diameter ratio of the double-screw extruder to be 42:1, performing water-cooling granulation, wherein the extrusion temperature of the first section is 252 ℃, the extrusion temperature of the second section is 257 ℃, the extrusion temperature of the third section is 262 ℃, the extrusion temperature of the fourth section is 267 ℃, the extrusion temperature of the fifth section is 277 ℃, the extrusion temperature of the sixth section is 272 ℃, the extrusion temperature of the seventh section is 267 ℃, and extruding the mixture from the double-screw extruder to obtain a skin material;
The raw materials in the preparation of the skin layer material comprise the following components in parts by weight: 75 parts of PE slices, 6 parts of active particles, 2.5 parts of sodium stearate, 3.5 parts of light calcium carbonate, 1.5 parts of maleated rosin and 0.7 part of sodium chloride.
3. Preparing a core layer material: uniformly mixing PP slices, active particles, zwitterionic polyacrylamide, PET slices and sodium sulfate, adding into a double-screw extruder for extrusion granulation, controlling the length-diameter ratio of the double-screw extruder to be 37:1, cutting into water-cooling granules, wherein the extrusion temperature of the first section is 242 ℃, the extrusion temperature of the second section is 252 ℃, the extrusion temperature of the third section is 262 ℃, the extrusion temperature of the fourth section is 272 ℃, the extrusion temperature of the fifth section is 262 ℃, the extrusion temperature of the sixth section is 252 ℃, the extrusion temperature of the seventh section is 242 ℃, and extruding from the double-screw extruder to obtain a core layer material;
The raw materials in the preparation of the core layer material comprise the following components in parts by weight: 75 parts of PP slice, 2.5 parts of active particles, 4.5 parts of zwitterionic polyacrylamide, 4.5 parts of PET slice and 1.5 parts of sodium sulfate.
4. And (3) composite spinning: adding a core layer material into a screw extruder, controlling the temperature of the screw extruder to be 222 ℃ and the pressure to be 0.32MPa, and obtaining a core layer melt; simultaneously adding the cortex material into another screw extruder, controlling the temperature of the screw extruder to be 232 ℃ and the pressure to be 0.37MPa, and obtaining cortex melt; then the core layer melt and the skin layer melt enter a composite spinning machine component through a metering pump, and primary ES fibers are sprayed out through a spinneret plate after being compounded in the composite spinning component;
The mass ratio of the sheath melt to the core melt is 1:1.7;
the spinneret plate is characterized in that the spinneret plate is cross-shaped, the pressure of a nozzle is 2.2kg/cm 2, and the temperature of a die head is controlled at 215 ℃.
5. Post-treatment: and carrying out radiation modification on the primary ES fiber by a high-speed electron field, controlling the irradiation dose to be 95KGy, and obtaining the ES large biological fiber after the radiation modification is finished.
Example 3
The preparation method of the ES large biological fiber containing the active component of the saussurea involucrata comprises the following specific steps:
1. Preparation of active particles: cleaning herba Saussureae Involueratae, placing in deionized water, controlling the mass ratio of herba Saussureae Involueratae to deionized water to be 1:20, then performing high-temperature steaming, controlling the temperature of the high-temperature steaming to be 90 ℃, the time of the high-temperature steaming to be 40min, cooling to 30 ℃ after the high-temperature steaming is finished, adding protease and cellulase, standing for 50min at 30 ℃, adjusting the pH to 11 by using 20% sodium hydroxide solution, then performing vacuum spray drying, controlling the vacuum degree of the vacuum spray drying to be 0.092MPa, the air inlet temperature to be 130 ℃, and the vacuum spray drying to be finished to obtain primary active particles, spraying active liquid to the surfaces of the primary active particles, controlling the mass ratio of the primary active particles to the active liquid to be 1:3, and drying at 90 ℃ for 2h after the spraying is finished to obtain the active particles, wherein the spray pressure is 0.45 MPa;
The active liquid comprises the following raw materials in parts by weight: 40 parts of deionized water, 0.2 part of polyvinyl amine, 2 parts of zinc acetate, 3 parts of nano titanium dioxide and 2.5 parts of polyethylene glycol;
The particle size of the nano titanium dioxide is 400nm.
2. Preparing a cortex material: uniformly mixing PE slices, active particles, sodium stearate, light calcium carbonate, maleated rosin and sodium chloride, adding the mixture into a double-screw extruder for extrusion granulation, controlling the length-diameter ratio of the double-screw extruder to be 45:1, performing water-cooling granulation, wherein the extrusion temperature of the first section is 255 ℃, the extrusion temperature of the second section is 260 ℃, the extrusion temperature of the third section is 265 ℃, the extrusion temperature of the fourth section is 270 ℃, the extrusion temperature of the fifth section is 280 ℃, the extrusion temperature of the sixth section is 275 ℃, the extrusion temperature of the seventh section is 270 ℃, and extruding the mixture from the double-screw extruder to obtain a skin material;
the raw materials in the preparation of the skin layer material comprise the following components in parts by weight: 80 parts of PE slices, 7 parts of active particles, 3 parts of sodium stearate, 4 parts of light calcium carbonate, 2 parts of maleated rosin and 1 part of sodium chloride.
3. Preparing a core layer material: uniformly mixing PP slices, active particles, zwitterionic polyacrylamide, PET slices and sodium sulfate, adding into a double-screw extruder for extrusion granulation, controlling the length-diameter ratio of the double-screw extruder to be 40:1, cutting into water-cooling granules, wherein the extrusion temperature of the first section is 245 ℃, the extrusion temperature of the second section is 255 ℃, the extrusion temperature of the third section is 265 ℃, the extrusion temperature of the fourth section is 275 ℃, the extrusion temperature of the fifth section is 265 ℃, the extrusion temperature of the sixth section is 255 ℃, and the extrusion temperature of the seventh section is 240 ℃, and extruding from the double-screw extruder to obtain a core layer material;
the raw materials in the preparation of the core layer material comprise the following components in parts by weight: 80 parts of PP slice, 3 parts of active particles, 5 parts of zwitterionic polyacrylamide, 5 parts of PET slice and 2 parts of sodium sulfate.
4. And (3) composite spinning: adding the core layer material into a screw extruder, controlling the temperature of the screw extruder to 225 ℃ and the pressure to 0.35MPa, and obtaining a core layer melt; simultaneously adding the cortex material into another screw extruder, controlling the temperature of the screw extruder to be 235 ℃ and the pressure to be 0.4MPa, and obtaining cortex melt; then the core layer melt and the skin layer melt enter a composite spinning machine component through a metering pump, and primary ES fibers are sprayed out through a spinneret plate after being compounded in the composite spinning component;
the mass ratio of the sheath melt to the core melt is 1:2;
The spinneret plate is characterized in that the spinneret plate is cross-shaped, the pressure of a nozzle is 2.5kg/cm 2, and the temperature of a die head is controlled at 220 ℃.
5. Post-treatment: and carrying out radiation modification on the primary ES fiber by a high-speed electron field, controlling the radiation dose to be 100KGy, and obtaining the ES large biological fiber after the radiation modification is finished.
Comparative example 1
The preparation method of the ES macrobiological fiber containing the active ingredient of the saussurea involucrata described in the embodiment 1 is adopted, and the difference is that: the active liquid is not sprayed in the step of preparing the active particles.
Comparative example 2
The preparation method of the ES macrobiological fiber containing the active ingredient of the saussurea involucrata described in the embodiment 1 is adopted, and the difference is that: no zwitterionic polyacrylamide is added in the step of preparing the core material.
Comparative example 3
The preparation method of the ES macrobiological fiber containing the active ingredient of the saussurea involucrata described in the embodiment 1 is adopted, and the difference is that: the post-processing step is omitted.
The ES macrofibers prepared in examples 1 to 3 and comparative examples 1 to 3 were tested for dry break strength and wet break strength with reference to GB/T14337-2008 standard, and the test results are as follows:
The ES macrofibers prepared in examples 1 to 3 and comparative examples 1 to 3 were respectively woven into ES fabric, and then the ES fabric was subjected to 100 standard water washes, respectively, to test the transverse dimensional change rate and the longitudinal dimensional change rate, with the following test results:
The ES macrofibers prepared in examples 1 to 3 and comparative examples 1 to 3 were respectively woven into ES fabric, and then tested for transverse softness and longitudinal softness with reference to GB/T8942-2016 standard, with the following test results:
the ES macrofibers prepared in examples 1 to 3 and comparative examples 1 to 3 were respectively woven into ES fabric, and then tested for air permeability with reference to GB/T5453-1997 standard, with the following test results:
The ES macrofibers prepared in examples 1 to 3 and comparative examples 1 to 3 were respectively placed in an environment having a temperature of 120 ℃ and a humidity of 80% for 3 months, and then tested for dry breaking strength and wet breaking strength with reference to GB/T14337-2008 standard, and the test results were as follows:
the percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The preparation method of the ES large biological fiber containing the active component of the saussurea involucrata is characterized by comprising the steps of preparing active particles, preparing a skin layer material, preparing a core layer material, carrying out composite spinning and carrying out aftertreatment;
The preparation method comprises the steps of preparing active particles, cleaning herba Saussureae Involueratae, placing the herba Saussureae Involueratae in deionized water, controlling the mass ratio of herba Saussureae Involueratae to the deionized water to be 1:15-20, then performing high-temperature cooking, controlling the temperature of the high-temperature cooking to be 85-90 ℃, the time of the high-temperature cooking to be 30-40min, cooling to 25-30 ℃, adding protease and cellulase, standing at 25-30 ℃ for 40-50min, adjusting the pH to 10-11 by using 15-20% sodium hydroxide solution, then performing vacuum spray drying, controlling the vacuum degree of the vacuum spray drying to be 0.09-0.092MPa, the air inlet temperature to be 120-130 ℃, and performing vacuum spray drying to obtain primary active particles, spraying active liquid on the surfaces of the primary active particles, controlling the mass ratio of the primary active particles to be 1:2-3, the spraying pressure during spraying to be 0.35-0.45MPa, the spraying time to be 10-12s, and drying at 80-90 ℃ for 1.5-2h after the spraying to obtain the active particles;
The active liquid comprises the following raw materials in parts by weight: 30-40 parts of deionized water, 0.1-0.2 part of polyvinyl amine, 1-2 parts of zinc acetate, 2-3 parts of nano titanium dioxide and 1.5-2.5 parts of polyethylene glycol;
the particle size of the nano titanium dioxide is 300-400nm;
The preparation method comprises the steps of uniformly mixing PE slices, active particles, sodium stearate, light calcium carbonate, maleated rosin and sodium chloride, adding into a double-screw extruder, extruding and granulating, and extruding from the double-screw extruder to obtain the cortex material;
The length-diameter ratio of the twin-screw extruder is 40-45:1, the grain cutting is water-cooling grain cutting, the extrusion temperature of the first section is 250-255 ℃, the extrusion temperature of the second section is 255-260 ℃, the extrusion temperature of the third section is 260-265 ℃, the extrusion temperature of the fourth section is 265-270 ℃, the extrusion temperature of the fifth section is 275-280 ℃, the extrusion temperature of the sixth section is 270-275 ℃, and the extrusion temperature of the seventh section is 265-270 ℃;
the raw materials in the preparation of the skin layer material comprise the following components in parts by weight: 70-80 parts of PE slices, 5-7 parts of active particles, 2-3 parts of sodium stearate, 3-4 parts of light calcium carbonate, 1-2 parts of maleated rosin and 0.5-1 part of sodium chloride;
The preparation method comprises the steps of uniformly mixing PP slices, active particles, zwitterionic polyacrylamide, PET slices and sodium sulfate, adding into a double-screw extruder for extrusion granulation, controlling the length-diameter ratio of the double-screw extruder to be 35-40:1, performing water-cooling granulation, performing extrusion at the first section at 240-245 ℃, performing extrusion at 250-255 ℃, performing extrusion at the third section at 260-265 ℃, performing extrusion at 270-275 ℃, performing extrusion at the fifth section at 260-265 ℃, performing extrusion at the sixth section at 250-255 ℃, performing extrusion at the seventh section at 240-245 ℃, and performing extrusion from the double-screw extruder to obtain the core layer material;
The raw materials in the preparation of the core layer material comprise the following components in parts by weight: 70-80 parts of PP slice, 2-3 parts of active particles, 4-5 parts of zwitterionic polyacrylamide, 4-5 parts of PET slice and 1-2 parts of sodium sulfate.
2. The method for preparing the ES macrobiological fiber containing the active ingredient of the saussurea involucrata according to claim 1, wherein the composite spinning is characterized in that a core layer material is added into a screw extruder, the temperature of the screw extruder is controlled to be 220-225 ℃, and the pressure is controlled to be 0.3-0.35MPa, so as to obtain a core layer melt; simultaneously adding the cortex material into another screw extruder, controlling the temperature of the screw extruder to be 230-235 ℃ and the pressure to be 0.35-0.4MPa, and obtaining cortex melt; and then the core layer melt and the sheath layer melt enter a composite spinning machine component through a metering pump, and are subjected to compounding in the composite spinning component and then are sprayed out of the primary ES fiber through a spinneret plate.
3. The method for preparing the ES macrobiological fiber containing the saussurea involucrata active ingredient according to claim 2, wherein the mass ratio of the sheath melt to the core melt is 1:1.5-2.
4. The method for preparing the ES macrobiological fiber containing the active ingredient of the saussurea involucrata according to claim 1, wherein the post-treatment is characterized in that the primary ES fiber is subjected to radiation modification by a high-speed electron field, the radiation dosage is controlled to be 90-100KGy, and the ES macrobiological fiber is obtained after the radiation modification.
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| CN109487360A (en) * | 2018-08-22 | 2019-03-19 | 中科纺织研究院（青岛）有限公司 | A kind of polyester fiber containing plant extracts |
| CN112553709A (en) * | 2020-12-15 | 2021-03-26 | 百事基材料（青岛）股份有限公司 | ES macrobio fiber containing wormwood active ingredient |
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| CN111118656B (en) * | 2020-03-18 | 2021-05-18 | 百事基材料（青岛）股份有限公司 | ES fiber containing wormwood extract and preparation method thereof |
| CN113638074A (en) * | 2021-08-19 | 2021-11-12 | 百事基材料（青岛）股份有限公司 | Dacron macrobiological fiber containing active ingredients of ginger and preparation method thereof |
| CN115976686A (en) * | 2022-08-01 | 2023-04-18 | 南通长江石墨烯科技有限公司 | Tianshan saussurea involucrate composite fiber and preparation process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109487360A (en) * | 2018-08-22 | 2019-03-19 | 中科纺织研究院（青岛）有限公司 | A kind of polyester fiber containing plant extracts |
| CN112553709A (en) * | 2020-12-15 | 2021-03-26 | 百事基材料（青岛）股份有限公司 | ES macrobio fiber containing wormwood active ingredient |
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