CN115506042B - Preparation method of multifunctional plant source composite material for fiber spinning - Google Patents
Preparation method of multifunctional plant source composite material for fiber spinning Download PDFInfo
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- CN115506042B CN115506042B CN202211217105.3A CN202211217105A CN115506042B CN 115506042 B CN115506042 B CN 115506042B CN 202211217105 A CN202211217105 A CN 202211217105A CN 115506042 B CN115506042 B CN 115506042B
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- 239000000835 fiber Substances 0.000 title claims abstract description 80
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 238000009987 spinning Methods 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 52
- 239000011159 matrix material Substances 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 39
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 38
- 229920000642 polymer Polymers 0.000 claims abstract description 38
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 34
- -1 polybutylene succinate Polymers 0.000 claims abstract description 29
- 229920002961 polybutylene succinate Polymers 0.000 claims abstract description 15
- 239000004631 polybutylene succinate Substances 0.000 claims abstract description 15
- 239000003607 modifier Substances 0.000 claims description 38
- 239000012752 auxiliary agent Substances 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 229910052710 silicon Inorganic materials 0.000 claims description 21
- 239000010703 silicon Substances 0.000 claims description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 17
- 230000000087 stabilizing effect Effects 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000005406 washing Methods 0.000 claims description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 13
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 11
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 229920002472 Starch Polymers 0.000 claims description 10
- 125000002091 cationic group Chemical group 0.000 claims description 10
- 239000008107 starch Substances 0.000 claims description 10
- 235000019698 starch Nutrition 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 7
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 229920000331 Polyhydroxybutyrate Polymers 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 5
- 239000005015 poly(hydroxybutyrate) Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 4
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 4
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 claims description 4
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 3
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 3
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 3
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims 1
- 229920000297 Rayon Polymers 0.000 abstract description 10
- 229920002334 Spandex Polymers 0.000 abstract description 6
- 239000004759 spandex Substances 0.000 abstract description 6
- 229920006052 Chinlon® Polymers 0.000 abstract description 5
- 229920004933 Terylene® Polymers 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract description 5
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 5
- 239000013543 active substance Substances 0.000 abstract description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- 229920000433 Lyocell Polymers 0.000 abstract description 3
- 239000004743 Polypropylene Substances 0.000 abstract description 3
- 229920006221 acetate fiber Polymers 0.000 abstract description 3
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Natural products C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 229920001155 polypropylene Polymers 0.000 abstract description 3
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 84
- 230000000844 anti-bacterial effect Effects 0.000 description 10
- 239000002245 particle Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000000284 extract Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 229920000728 polyester Polymers 0.000 description 8
- 238000004043 dyeing Methods 0.000 description 7
- 239000004480 active ingredient Substances 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 239000000419 plant extract Substances 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 238000010025 steaming Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 241000205585 Aquilegia canadensis Species 0.000 description 3
- 241001474374 Blennius Species 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229940094952 green tea extract Drugs 0.000 description 3
- 235000020688 green tea extract Nutrition 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 235000020737 peppermint extract Nutrition 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 241000222122 Candida albicans Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940095731 candida albicans Drugs 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 241000334160 Isatis Species 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000001525 mentha piperita l. herb oil Substances 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 229940105902 mint extract Drugs 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 235000019477 peppermint oil Nutrition 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000009970 yarn dyeing 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
- 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
- D01F1/103—Agents inhibiting growth of microorganisms
-
- 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
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
-
- 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
- D01F6/90—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 polyamides
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a preparation method of a multifunctional plant source composite material for fiber spinning, which comprises the steps of preparing modified plant source powder, preparing modified nano silicon dioxide, preparing a modified polymer matrix and modifying blending. The modified macromolecule matrix and the modified plant source powder have stronger intermolecular force, so that on one hand, the adhesive force of active substances in the plant source powder on the polybutylene succinate is enhanced, and the loss in the preparation of the composite material and the spinning process is reduced; on the other hand, the heat stability and acid and alkali resistance of the composite material are improved to a certain extent, so that the prepared composite material is suitable for spinning processes of various fibers such as terylene, chinlon, acrylon, polypropylene, spandex, lyocell, modal, acetate fiber, viscose fiber, copper spandex fiber and the like.
Description
Technical Field
The invention relates to the technical field of polymer composite materials, in particular to a preparation method of a multifunctional plant source composite material for fiber spinning.
Background
The fiber is divided into two main types of natural fiber and artificial synthetic fiber, wherein the natural fiber has the advantages of good hygroscopicity, ventilation, comfort and the like, and the artificial synthetic fiber has the advantages of strong wear resistance, stiff and smooth fabric, difficult deformation and the like. Along with the improvement of the living standard and the change of the concept, the demands of people on the health care function of the fiber are more and more, the concept of green and environment protection is also focused, and the plant source material has low cost and is safe and environment-friendly, so that a large number of enterprises are initiated to add the plant extract into the fiber, and the fiber is endowed with natural functionality.
The patent No. CN201710846179.6 entitled "double-component melting point differential colored polyester fiber with plant-derived antibacterial function and preparation method" provides a plant-derived polyester fiber, wherein plant extracts are added into the polyester fiber, however, in the process of mixing and extruding polyester chips and plant extracts, a large amount of plant extracts are deactivated due to overhigh temperature, so that loss of plant active ingredients is caused, and the production cost is increased.
The patent number CN201310140966.0 is named as viscose fiber with plant source antibacterial function and aromatic smell and a preparation method thereof, and the plant source antibacterial agent and the aromatic agent are added into the viscose fiber, wherein the plant source antibacterial agent is mixed powder of mint extract and isatis root extract, and the aromatic agent is peppermint oil coated by microcapsules, but because the particle size of the extract is too small, aggregation and sedimentation are easy to generate in spinning stock solution, and the mechanical property of the fiber can be influenced to a certain extent by directly adding the extract into the fiber.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of a multifunctional plant source composite material for fiber spinning, which realizes the following aims:
1. solves the problem of large loss of plant active substances in the fiber spinning process, and avoids the phenomenon that plant active particles with small particle size are easy to agglomerate and disperse unevenly in a load matrix;
2. the multifunctional plant source composite material has good heat stability and acid and alkali resistance, is suitable for the spinning process of various fibers, has wide application range, and is suitable for industrial-grade large-scale production, marketing and popularization;
3. the multifunctional plant source composite material has excellent adhesion effect with different fiber matrixes, reduces loss of plant source active ingredients, and improves mechanical properties of the fiber to a certain extent on the basis of endowing the fiber with natural and durable biological activity.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a multifunctional plant source composite material for fiber spinning comprises the following steps:
s1, preparing modified plant source powder
S11: placing plant source powder with particle size of 50-100nm in absolute ethanol, stirring for 10-20min, filtering, and collecting filtrate to obtain plant source solution;
s12: adding an interface modifier into the plant source solution in the step S11, carrying out ultrasonic treatment at the temperature of between 20 and 40 ℃ for 5 to 15 minutes at the temperature of between 150 and 200W, adjusting the pH value to between 7.5 and 8.5, heating to the temperature of between 50 and 60 ℃ for reaction for 10 to 20 minutes, cooling to the room temperature, steaming out absolute ethyl alcohol, and fully drying at the temperature of between 55 and 75 ℃ to obtain modified plant source powder.
The plant source powder in S11 is a plant extract, and the specific types are not limited, and are all suitable for the system.
Preferably, the interface modifier in S12 is (1.5-2.5) in mass ratio: (0.2-0.8) gamma-aminopropyl triethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane; the addition amount of the interface modifier is 0.5-1% of the mass of the plant source powder.
S2: preparation of modified nanosilicon dioxide
S21: adding nano silicon dioxide into N-methyl pyrrolidone at 50-60 ℃ for ultrasonic dispersion for 20-30min, wherein the ultrasonic frequency is 80-100kHz, adding a silicon-containing unsaturated modifier and a stabilizing additive, reacting for 10-20h, and obtaining an intermediate through centrifugal separation, ethanol washing and vacuum drying;
s22: and (3) placing the intermediate in distilled water, performing ultrasonic treatment for 15-25min at 100-120kHz, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 80-100 ℃, adding tert-butyl peroxybenzoate for reaction for 2-6h, and obtaining the modified nano silicon dioxide through centrifugation, water washing and drying.
Preferably, the mass ratio of the nano silicon dioxide, the silicon-containing unsaturated modifier and the stabilizing auxiliary agent in the S21 is (90-120): (0.5-1.5): (0.01-0.05).
Further, the silicon-containing unsaturated modifier is prepared from the following components in percentage by mass (0.4-1.2): (1.5-2) a mixture of vinyltris (β -methoxyethoxy) silane and γ -methacryloxypropyl-trimethoxysilane.
Further, the stabilizing aid comprises one or more of 2, 6-di-tert-butyl-p-cresol, p-hydroxyanisole and 1, 1-diphenyl-2-trinitrophenylhydrazine.
Preferably, the mass ratio of the intermediate, ethylene glycol dimethacrylate and tert-butyl peroxybenzoate in the S22 is (60-80): (90-100): (1-2).
S3: preparation of modified Polymer matrix
Adding a mixture of polyethylene glycol, cationic starch and modified nano silicon dioxide into polybutylene succinate, fully mixing under the condition of 1500-2500r/min, and then placing into a mixing mill for melt blending to obtain the modified polymer matrix.
Preferably, the mass ratio of the polybutylene succinate to the polyethylene glycol to the cationic starch to the modified nano silicon dioxide in the S3 is (40-50): (10-20): (4-8): (1-5).
Preferably, the hydroxyl value of the polyethylene glycol is 170-208mgKOH/g, and the molecular weight is 540-660; the melt blending temperature is 180-200 ℃.
S4: modified blending:
blending the modified plant source powder of S12 and the modified polymer matrix of S3 in proportion under the rotating speed of 550-750r/min, slowly heating to 110-120 ℃ at the speed of 4-8 ℃/min for reaction for 6-10h, adding a dry modification auxiliary agent, continuously heating to 130-140 ℃ for melt blending for 10-20min, extruding and cooling to obtain the multifunctional plant source composite material for fiber spinning.
Preferably, the addition amount of the modified plant source powder in the S4 is 4-12% of the mass of the modified polymer matrix; the mass ratio of the modified polymer matrix to the modified auxiliary agent is (4-8): (2-6); the modifying auxiliary agent is prepared from the following components in percentage by mass (2-4): (0.5-1.5) a mixture of microcrystalline cellulose and polyhydroxybutyrate.
The multifunctional plant-derived composite material can be used in spinning processes of terylene, chinlon, acrylon, polypropylene, spandex, lyocell, modal, acetate fiber, viscose fiber, copper spandex fiber and the like.
By adopting the technical scheme, the invention has the following technical effects:
1. the invention adopts the mass ratio of (1.5-2.5): the gamma-aminopropyl triethoxysilane and 3- (2, 3-epoxypropyl) propyl trioxysilane (0.2-0.8) are used for modifying the modified plant source powder, so that the interface performance between the plant source powder with small particle size and a high polymer matrix can be improved, the dispersion uniformity of the plant source powder in the polybutylene succinate is improved, and the phenomena of easy agglomeration and uneven dispersion of the plant active particles with small particle size in a load matrix are relieved.
2. Adding the nano silicon dioxide into the silicon-containing unsaturated modifier, wherein the silicon-containing unsaturated modifier acts on silicon hydroxyl on the surface of the nano silicon dioxide to improve the interface performance of the nano silicon dioxide; the addition of the stabilizing auxiliary agent plays a role in promoting the modification to be carried out more stably, and avoids the cross-linking between the silicon-containing unsaturated modifiers from influencing the modification reaction to a certain extent; and adding ethylene glycol dimethacrylate and tert-butyl peroxybenzoate into the intermediate, wherein one end of the silicon-containing unsaturated modifier is connected with the nano silicon dioxide, and the other end of the silicon-containing unsaturated modifier is connected with the ethylene glycol dimethacrylate, so that the ethylene glycol dimethacrylate is coated on the surface of the nano silicon dioxide, and the modification of the nano silicon dioxide is completed.
3. The modified polymer matrix and the modified plant source powder have stronger intermolecular force, so that on one hand, the adhesive force of active substances in the plant source powder on the polybutylene succinate is enhanced, the loss in the preparation of composite materials and spinning process is reduced, and the loss rate of the plant source active ingredients is lower than 3% through detection; on the other hand, the heat stability and acid and alkali resistance of the composite material are improved to a certain extent, so that the prepared composite material is suitable for spinning processes of various fibers such as terylene, chinlon, acrylon, polypropylene, spandex, lyocell, modal, acetate fiber, viscose fiber, copper spandex fiber and the like. The composite material is added into the fiber, shows excellent antibacterial effect, and has antibacterial rate to staphylococcus aureus, candida albicans and escherichia coli higher than 95 percent (detected by GB/T20944.3-2008 oscillation method), and antibacterial loss after washing for 100 timesFailure rate below 1% (average); the anti-mite effect is excellent, the mite avoiding rate is up to more than 99 percent (the detection of GB/T24253-2009 textile anti-mite performance evaluation) and the mite avoiding loss rate is lower than 2 percent (average value) after the washing is carried out for 100 times; good antistatic effect, and surface resistivity lower than 1×10 9 Omega cm (measured in GB/T24249-2009 antistatic cleaning fabrics); the addition of the modifying auxiliary agent enables the modified plant source powder to be more uniformly attached to the modified polymer matrix, improves the plasticity of the composite material, has good compatibility with fibers when being added into the fiber matrix, and improves the mechanical properties of the fibers.
4. The multifunctional plant source composite material prepared by the invention can further enhance the acting force of various dyes on the surface of the fiber on the basis of enhancing the effects of the strength, degradability, antibacterial property, mite resistance, antistatic property and the like of the chemical fiber, and improves the dyeability of the chemical fiber; in addition, the dyeing temperature of the fiber can be reduced, and the fiber has excellent dyeing effect on terylene and chinlon at 20-40 ℃.
Detailed Description
The invention will be further illustrated with reference to specific examples.
Example 1 preparation method of multifunctional plant-derived composite Material for fiber spinning
A preparation method of a multifunctional plant source composite material for fiber spinning comprises the following steps:
s1, preparing modified plant source powder
S11: placing plant source powder with the particle size of 100nm into absolute ethyl alcohol, fully stirring for 20min, filtering, and collecting filtrate to obtain plant source solution;
s12: adding an interface modifier into the plant source solution in the step S11, carrying out ultrasonic treatment at 200W and 40 ℃ for 15min, regulating the pH value to 8.5, heating to 60 ℃ for reaction for 20min, cooling to room temperature, steaming out absolute ethyl alcohol, and fully drying at 75 ℃ to obtain modified plant source powder.
The plant source powder in S11 is a mixture of green tea extract, honeysuckle extract, peppermint extract and seaweed extract.
Wherein, the interface modifier in S12 is 2.5 in mass ratio: 0.8 gamma-aminopropyl triethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane; the addition amount of the interface modifier is 1% of the mass of the plant source powder.
S2: preparation of modified nanosilicon dioxide
S21: adding nano silicon dioxide into N-methyl pyrrolidone at 60 ℃ for ultrasonic dispersion for 30min, wherein the ultrasonic frequency is 100kHz, adding a silicon-containing unsaturated modifier and a stabilizing additive, reacting for 20h, and performing centrifugal separation, ethanol washing and vacuum drying to obtain an intermediate;
s22: and (3) placing the intermediate in S21 in distilled water, carrying out ultrasonic treatment for 25min at 120kHz, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 100 ℃, adding tert-butyl peroxybenzoate for reaction for 6h, and obtaining the modified nano silicon dioxide through centrifugation, water washing and drying.
S21, the mass ratio of the nano silicon dioxide to the silicon-containing unsaturated modifier to the stabilizing auxiliary agent is 120:1.5:0.05.
the silicon-containing unsaturated modifier is characterized by comprising the following components in percentage by mass of 1.2:2 and gamma-methacryloxypropyl-trimethoxysilane.
The stabilizing auxiliary agent comprises 2, 6-di-tert-butyl p-cresol and p-hydroxyanisole in a mass ratio of 1:1.
S22, the mass ratio of the intermediate to the ethylene glycol dimethacrylate to the tert-butyl peroxybenzoate is 80:100:2.
s3: preparation of modified Polymer matrix
Adding a mixture of polyethylene glycol, cationic starch and modified nano silicon dioxide into polybutylene succinate, fully mixing under the condition of 2500r/min, and then placing the mixture into a mixing mill for melt blending to obtain the modified polymer matrix.
S3, the mass ratio of the polybutylene succinate to the polyethylene glycol to the cationic starch to the modified nano silicon dioxide is 50:20:8:5.
s3, the hydroxyl value of the polyethylene glycol is 208mgKOH/g, and the molecular weight is 660; the temperature of the melt blending was 200 ℃.
S4: modified blending:
and (3) blending the modified plant source powder in the step (S12) and the modified polymer matrix in the step (S3) in proportion under the rotating speed condition of 750r/min, slowly heating to 120 ℃ at the speed of 8 ℃/min for reaction for 10 hours, adding a dry modification auxiliary agent, continuously heating to 140 ℃ for melt blending for 20 minutes, extruding and cooling to obtain the multifunctional plant source composite material for fiber spinning.
The addition amount of the modified plant source powder is 12% of the mass of the modified polymer matrix.
And S4, the mass ratio of the modified polymer matrix to the modified auxiliary agent is 8:6, preparing a base material; the modifying auxiliary agent is prepared from the following components in percentage by mass: 1.5 and polyhydroxybutyrate.
Example 2 preparation method of multifunctional plant-derived composite Material for fiber spinning
A preparation method of a multifunctional plant source composite material for fiber spinning comprises the following steps:
s1, preparing modified plant source powder
S11: placing plant source powder with the particle size of 70nm into absolute ethyl alcohol, fully stirring for 15min, filtering, and collecting filtrate to obtain plant source solution;
s12: adding an interface modifier into the plant source solution in the step S11, carrying out ultrasonic treatment at 180W and 30 ℃ for 10min, regulating the pH value to 8, heating to 55 ℃ for reaction for 15min, cooling to room temperature, steaming out absolute ethyl alcohol, and fully drying at 65 ℃ to obtain modified plant source powder.
The plant source powder in S11 is a mixture of green tea extract, honeysuckle extract, peppermint extract and seaweed extract.
Wherein, the interface modifier in S12 is that the mass ratio is 2:0.5 gamma-aminopropyl triethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane; the addition amount of the interface modifier is 0.8% of the mass of the plant source powder.
S2: preparation of modified nanosilicon dioxide
S21: adding nano silicon dioxide into N-methyl pyrrolidone at 55 ℃ for ultrasonic dispersion for 25min, wherein the ultrasonic frequency is 90kHz, adding a silicon-containing unsaturated modifier and a stabilizing additive, reacting for 15h, and performing centrifugal separation, ethanol washing and vacuum drying to obtain an intermediate;
s22: and (3) placing the intermediate in S21 in distilled water, performing ultrasonic treatment for 20min at 110kHz, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 90 ℃, adding tert-butyl peroxybenzoate for reaction for 4h, and obtaining the modified nano silicon dioxide through centrifugation, water washing and drying.
S21, the mass ratio of the nano silicon dioxide to the silicon-containing unsaturated modifier to the stabilizing auxiliary agent is 110:1:0.03.
the silicon-containing unsaturated modifier is characterized by comprising the following components in percentage by mass of 0.8:1.7 vinyl tris (β -methoxyethoxy) silane and γ -methacryloxypropyl-trimethoxysilane.
The stabilizing auxiliary agent comprises parahydroxyanisole and 1, 1-diphenyl-2-trinitrophenylhydrazine in a mass ratio of 1:1.
The mass ratio of the intermediate to the glycol dimethacrylate to the tert-butyl peroxybenzoate in the S22 is 70:95:1.5.
s3: preparation of modified Polymer matrix
Adding the mixture of polyethylene glycol, cationic starch and modified nano silicon dioxide into polybutylene succinate, fully mixing under the condition of 2000r/min, and then placing the mixture into a mixing mill for melt blending to obtain the modified polymer matrix.
S3, the mass ratio of the polybutylene succinate to the polyethylene glycol to the cationic starch to the modified nano silicon dioxide is 45:15:6:3.
s3, the hydroxyl value of the polyethylene glycol is 190mgKOH/g, and the molecular weight is 600; the melt blending temperature was 190 ℃.
S4: modified blending:
blending the modified plant source powder of S12 and the modified polymer matrix of S3 in proportion under the rotating speed condition of 650r/min, slowly heating to 115 ℃ at the speed of 6 ℃/min for reaction for 8 hours, adding a dry modification auxiliary agent, continuously heating to 135 ℃ for melt blending for 15 minutes, extruding and cooling to obtain the multifunctional plant source composite material for fiber spinning.
The addition amount of the modified plant source powder is 9% of the mass of the modified polymer matrix.
And S4, the mass ratio of the modified polymer matrix to the modified auxiliary agent is 6:4, a step of; the modifying auxiliary agent is prepared from the following components in percentage by mass: 1 and polyhydroxybutyrate.
Example 3 preparation method of multifunctional plant-derived composite Material for fiber spinning
A preparation method of a multifunctional plant source composite material for fiber spinning comprises the following steps:
s1, preparing modified plant source powder
S11: placing plant source powder with the particle size of 50nm into absolute ethyl alcohol, fully stirring for 10min, filtering, and collecting filtrate to obtain plant source solution;
s12: adding an interface modifier into the plant source solution in the step S11, carrying out ultrasonic treatment at 150W and 20 ℃ for 5min, regulating the pH value to 7.5, heating to 50 ℃ for reaction for 10min, cooling to room temperature, steaming out absolute ethyl alcohol, and fully drying at 55 ℃ to obtain modified plant source powder.
The plant source powder in S11 is a mixture of green tea extract, honeysuckle extract, peppermint extract and seaweed extract.
Wherein, the interface modifier in S12 is that the mass ratio is 1.5:0.2 gamma-aminopropyl triethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane; the addition amount of the interface modifier is 0.5% of the mass of the plant source powder.
S2: preparation of modified nanosilicon dioxide
S21: adding nano silicon dioxide into N-methyl pyrrolidone at 50 ℃ for ultrasonic dispersion for 20min and ultrasonic frequency of 80kHz, adding a silicon-containing unsaturated modifier and a stabilizing additive, reacting for 10h, and performing centrifugal separation, ethanol washing and vacuum drying to obtain an intermediate;
s22: and (3) placing the intermediate in S21 in distilled water, performing ultrasonic treatment for 15min at 100kHz, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 80 ℃, adding tert-butyl peroxybenzoate for reaction for 2h, and obtaining the modified nano silicon dioxide through centrifugation, water washing and drying.
S21, the mass ratio of the nano silicon dioxide to the silicon-containing unsaturated modifier to the stabilizing auxiliary agent is 90:0.5:0.01.
the silicon-containing unsaturated modifier is characterized by comprising the following components in percentage by mass: 1.5 mixtures of vinyltris (β -methoxyethoxy) silane and γ -methacryloxypropyl-trimethoxysilane.
The stabilizing auxiliary is 2, 6-di-tert-butyl-p-cresol.
S22, the mass ratio of the intermediate to the ethylene glycol dimethacrylate to the tert-butyl peroxybenzoate is 60:90:1.
s3: preparation of modified Polymer matrix
Adding a mixture of polyethylene glycol, cationic starch and modified nano silicon dioxide into polybutylene succinate, fully mixing under the condition of 1500r/min, and then placing the mixture into a mixing mill for melt blending to obtain the modified polymer matrix.
S3, the mass ratio of the polybutylene succinate to the polyethylene glycol to the cationic starch to the modified nano silicon dioxide is 40:10:4:1.
s3, the hydroxyl value of the polyethylene glycol is 170mgKOH/g, and the molecular weight is 540; the temperature of the melt blending was 180 ℃.
S4: modified blending:
and (3) blending the modified plant source powder in the step (S12) and the modified polymer matrix in the step (S3) in proportion under the rotating speed condition of 550r/min, slowly heating to 110 ℃ at the speed of 4 ℃/min for reaction for 6 hours, adding a dry modification auxiliary agent, continuously heating to 130 ℃ for melt blending for 10 minutes, extruding and cooling to obtain the multifunctional plant source composite material for fiber spinning.
The addition amount of the modified plant source powder is 4% of the mass of the modified polymer matrix.
And S4, the mass ratio of the modified polymer matrix to the modified auxiliary agent is 4:2; the mass ratio of the modifying auxiliary agent is 2:0.5 of microcrystalline cellulose and polyhydroxybutyrate.
The multifunctional plant source composite materials for fiber spinning prepared in examples 1-3 were added to viscose fiber, polyester fiber and nylon fiber respectively according to an addition amount of 3% and their properties were tested, specifically shown in tables 1, 2 and 3.
TABLE 1
TABLE 2
TABLE 3 Table 3
Test standard:
mechanical properties: test strip method for measuring tensile properties breaking strength and breaking elongation of GB/T3923.1-2013 textile fabrics.
Dyeing uniformity: the gray card scale was determined in the viscose filament yarn dyeing uniformity test and assessment (FZ/T50015-2009).
Fastness to washing: GB-T/3921-2008 fabrics color fastness test, soaping fastness.
Antibacterial rate: GB/T209444.3-2008 Oscillating method.
Mite repellent rate: evaluation of anti-mite Properties of GB/T24253-2009 textiles.
Surface resistivity: GB/T24249-2009 antistatic cleaning fabrics.
As can be seen from the table, the multifunctional implants for spinning fibers prepared in examples 1-3The material source composite material is added into viscose fiber, polyester fiber and nylon fiber, the mechanical property of the fiber is excellent, the loss rate of plant source active ingredients in the spinning process is low, the dyeing property and the washing fastness of the fiber are good, the antibacterial property is good, the antibacterial rate to staphylococcus aureus, candida albicans and escherichia coli is higher than 95%, and the antibacterial loss rate after washing for 100 times is lower than 1% (average value); the anti-mite effect is excellent, the mite avoiding rate is up to more than 99 percent, and the mite avoiding loss rate is lower than 2 percent (average value) after the anti-mite agent is washed for 100 times; good antistatic effect, and surface resistivity lower than 1×10 9 Ω·cm。
The multifunctional plant source composite material prepared by the method has good thermal stability and acid and alkali resistance, reduces the loss of plant source active ingredients in the preparation process and spinning process of the composite material, enhances the strength of chemical fibers to endow fibers with functionality to a certain extent, further enhances the acting force of various dyes on the surfaces of the fibers, and improves the dyeability of the chemical fibers; in addition, the dyeing temperature of the fiber can be reduced, and the fiber has excellent dyeing effect on terylene and chinlon at 20-40 ℃.
Comparative example 1
Representative example 2 was chosen with mass ratios of 3:0.1 and 0.1, respectively: 3 and 3- (2, 3-epoxypropyl) propyl trioxysilane, and the rest are the same as in example 2, and during the modification blending, the modified plant source powder obtained in comparative example 1 still has the phenomena of agglomeration and uneven dispersion in the modified polymer matrix.
Comparative example 2
The representative example 2 is selected, the amount of the added interfacial modifier is 0, the rest is the same as the example 2, as the comparative example 2, under the condition that other preparation processes are unchanged, the phenomena of agglomeration and uneven dispersion of the plant source powder occur in the process of blending with the polymer matrix, which indicates that the interfacial modifier improves the mixing performance of the plant source powder and the polymer matrix, so that the modified plant source powder and the polymer matrix are mixed more uniformly, and the quality of the final product is further more stable.
Comparative example 3
Representative example 2 was selected, the step of preparing a modified polymer matrix was removed, modified plant source powder was directly blended with polybutylene succinate in a modified manner, the rest was the same as in example 2, and as comparative example 3, the prepared composite material was added to viscose fiber, polyester fiber and nylon fiber respectively in an amount of 3% and tested for properties, specifically as shown in table 4.
TABLE 4 Table 4
The modified polymer matrix and the modified plant source powder have stronger intermolecular force, so that on one hand, the adhesive force of active substances in the plant source powder on the polybutylene succinate is enhanced, and the loss in the preparation of the composite material and the spinning process is reduced; on the other hand, the thermal stability and acid and alkali resistance of the composite material are improved to a certain extent, and the mechanical property and dyeing property of the fiber are also improved.
Comparative example 4
Representative example 2 was selected, the step of removing the modifying auxiliary agent was performed, and the rest was the same as in example 2, and as comparative example 4, the prepared composite material was added to viscose fiber, polyester fiber and nylon fiber respectively in an amount of 3% and tested for mechanical properties, as shown in table 5.
TABLE 5
The addition of the modifying auxiliary agent enables the modified plant source powder to be more uniformly attached to the modified polymer matrix, improves the plasticity of the composite material, has good compatibility with fibers when being added into the fiber matrix, and improves the mechanical properties of the fibers.
The proportions are mass proportions, and the percentages are mass percentages, unless otherwise specified; the raw materials are all commercially available.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof. 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 (6)
1. The preparation method of the multifunctional plant source composite material for fiber spinning is characterized by comprising the steps of preparing modified plant source powder, preparing modified nano silicon dioxide, preparing a modified polymer matrix and modifying and blending; the preparation of the modified plant source powder comprises the following steps:
placing plant source powder into absolute ethyl alcohol, stirring, filtering and collecting filtrate to obtain plant source solution;
adding an interface modifier into the plant source solution for modification to obtain modified plant source powder;
the interface modifier is gamma-aminopropyl triethoxysilane and 3- (2, 3-epoxypropyl) propyl trioxysilane;
the mass ratio of the gamma-aminopropyl triethoxysilane to the 3- (2, 3-epoxypropyl) propyl trioxysilane is 1.5-2.5:0.2-0.8;
the preparation of the modified nano silicon dioxide comprises the following steps:
adding nano silicon dioxide into N-methyl pyrrolidone at 50-60 ℃ for ultrasonic dispersion for 20-30min, wherein the ultrasonic frequency is 80-100kHz, adding a silicon-containing unsaturated modifier and a stabilizing additive, reacting for 10-20h, and obtaining an intermediate through centrifugal separation, ethanol washing and vacuum drying;
placing the intermediate in distilled water, performing ultrasonic treatment for 15-25min at 100-120kHz, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 80-100 ℃, adding tert-butyl peroxybenzoate for reaction for 2-6h, and obtaining modified nano silicon dioxide through centrifugation, water washing and drying;
the preparation method comprises the steps of preparing a modified polymer matrix, adding a mixture of polyethylene glycol, cationic starch and modified nano silicon dioxide into polybutylene succinate, fully mixing under the condition of 1500-2500r/min, and then placing the mixture into a mixing roll for melt blending to obtain the modified polymer matrix;
the mass ratio of the polybutylene succinate to the polyethylene glycol to the cationic starch to the modified nano silicon dioxide is 40-50:10-20:4-8:1-5;
the modified blending is carried out, the modified plant source powder and the modified polymer matrix are blended according to a proportion under the rotating speed of 550-750r/min, the temperature is slowly increased to 110-120 ℃ at the speed of 4-8 ℃/min for reaction for 6-10h, then the dried modified auxiliary agent is added, the temperature is continuously increased to 130-140 ℃ for melt blending for 10-20min, and the multifunctional plant source composite material for fiber spinning is obtained after extrusion and cooling;
the mass ratio of the modified polymer matrix to the modified auxiliary agent is 4-8:2-6; the mass ratio of the modifying auxiliary agent is 2-4:0.5 to 1.5 of a mixture of microcrystalline cellulose and polyhydroxybutyrate.
2. The method for preparing the multifunctional plant source composite material for fiber spinning according to claim 1, wherein the condition of adding the interface modifier for modification is that after ultrasonic treatment for 5-15min at the temperature of 150-200W and the temperature of 20-40 ℃, the pH is adjusted to 7.5-8.5, the temperature is raised to 50-60 ℃ for reaction for 10-20min, the mixture is cooled to room temperature, absolute ethyl alcohol is distilled off, and the mixture is sufficiently dried at the temperature of 55-75 ℃.
3. The method for preparing the multifunctional plant source composite material for fiber spinning according to claim 1, wherein the addition amount of the interface modifier is 0.5% -1% of the mass of the plant source powder.
4. The preparation method of the multifunctional plant source composite material for fiber spinning according to claim 1, wherein the mass ratio of the nano silicon dioxide to the silicon-containing unsaturated modifier to the stabilizing auxiliary agent is 90-120:0.5-1.5:0.01-0.05;
the mass ratio of the intermediate to the glycol dimethacrylate to the tert-butyl peroxybenzoate is 60-80:90-100:1-2.
5. The preparation method of the multifunctional plant source composite material for fiber spinning according to claim 1, wherein the silicon-containing unsaturated modifier is characterized by comprising the following components in percentage by mass of 0.4-1.2:1.5-2 of a mixture of vinyltris (β -methoxyethoxy) silane and γ -methacryloxypropyl-trimethoxysilane;
the stabilizing auxiliary comprises one or a combination of more of 2, 6-di-tert-butyl p-cresol, p-hydroxyanisole and 1, 1-diphenyl-2-trinitrophenylhydrazine.
6. The method for preparing a multifunctional plant source composite material for fiber spinning according to claim 1, wherein the addition amount of the modified plant source powder is 4-12% of the mass of the modified polymer matrix.
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