CN115506042A - 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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- CN115506042A CN115506042A CN202211217105.3A CN202211217105A CN115506042A CN 115506042 A CN115506042 A CN 115506042A CN 202211217105 A CN202211217105 A CN 202211217105A CN 115506042 A CN115506042 A CN 115506042A
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- 239000000835 fiber Substances 0.000 title claims abstract description 85
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000009987 spinning Methods 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000000843 powder Substances 0.000 claims abstract description 52
- 239000011159 matrix material Substances 0.000 claims abstract description 37
- 229920000642 polymer Polymers 0.000 claims abstract description 36
- -1 polypropylene Polymers 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 52
- 239000003607 modifier Substances 0.000 claims description 39
- 238000002156 mixing Methods 0.000 claims description 38
- 239000012752 auxiliary agent Substances 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 23
- 238000012986 modification Methods 0.000 claims description 21
- 230000004048 modification Effects 0.000 claims description 21
- 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
- 238000010438 heat treatment Methods 0.000 claims description 20
- 230000000087 stabilizing effect Effects 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 239000005543 nano-size silicon particle Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims description 14
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 13
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 13
- 229920002961 polybutylene succinate Polymers 0.000 claims description 12
- 239000004631 polybutylene succinate Substances 0.000 claims description 12
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-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
- 238000001816 cooling Methods 0.000 claims description 10
- 238000001035 drying Methods 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
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 8
- 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
- 239000012153 distilled water Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 claims description 5
- 238000001704 evaporation Methods 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
- 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
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 235000010354 butylated hydroxytoluene Nutrition 0.000 claims description 4
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 4
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 4
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 4
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 claims description 4
- 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 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 2
- 229920000297 Rayon Polymers 0.000 abstract description 10
- 229920006052 Chinlon® Polymers 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 239000013543 active substance Substances 0.000 abstract description 4
- ZMKVBUOZONDYBW-UHFFFAOYSA-N 1,6-dioxecane-2,5-dione Chemical compound O=C1CCC(=O)OCCCCO1 ZMKVBUOZONDYBW-UHFFFAOYSA-N 0.000 abstract description 3
- 229920002972 Acrylic fiber Polymers 0.000 abstract description 3
- 229920000433 Lyocell Polymers 0.000 abstract description 3
- 239000004743 Polypropylene Substances 0.000 abstract description 3
- 229920002334 Spandex Polymers 0.000 abstract description 3
- 229920004933 Terylene® Polymers 0.000 abstract description 3
- 229920006221 acetate fiber Polymers 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 239000005020 polyethylene terephthalate Substances 0.000 abstract description 3
- 229920001155 polypropylene Polymers 0.000 abstract description 3
- 239000004759 spandex Substances 0.000 abstract description 3
- 241000196324 Embryophyta Species 0.000 description 86
- 229920000728 polyester Polymers 0.000 description 10
- 239000000284 extract Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000004043 dyeing Methods 0.000 description 6
- 239000004480 active ingredient Substances 0.000 description 5
- 230000003385 bacteriostatic effect Effects 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
- 239000004744 fabric Substances 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 229940105902 mint extract Drugs 0.000 description 4
- 230000002265 prevention Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004753 textile Substances 0.000 description 4
- 241000205585 Aquilegia canadensis Species 0.000 description 3
- 241001474374 Blennius Species 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 229940094952 green tea extract Drugs 0.000 description 3
- 235000020688 green tea extract Nutrition 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 229920001778 nylon Polymers 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
- 238000005054 agglomeration Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 229940095731 candida albicans Drugs 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 239000012209 synthetic fiber Substances 0.000 description 2
- 235000006679 Mentha X verticillata Nutrition 0.000 description 1
- 235000002899 Mentha suaveolens Nutrition 0.000 description 1
- 235000001636 Mentha x rotundifolia Nutrition 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000010231 banlangen Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000009423 ventilation 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. Stronger intermolecular acting force exists between the modified polymer matrix and the modified plant source powder, so that on one hand, the adhesive force of active substances in the plant source powder on the poly (butylene succinate) is enhanced, and the loss in the process of preparing a composite material and spinning is reduced; on the other hand, the thermal stability and the acid and alkali resistance of the composite material are improved to a certain extent, so that the prepared composite material is suitable for the spinning process of various fibers such as terylene, chinlon, acrylic fiber, polypropylene fiber, spandex, lyocell, modal, acetate fiber, viscose fiber, cuprammonium 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 categories 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 living standard and the change of concept of people, people have more and more requirements on the health care function of fiber, and also pay more attention to the concept of green environmental protection, and the plant source material has low cost, is safe and environment-friendly, so that a large number of enterprises add plant extracts into the fiber to endow the fiber with natural functionality.
Patent No. CN201710846179.6 entitled "two-component melting point differential colored polyester fiber with plant-derived antibacterial function and preparation method" provides a plant-derived polyester fiber, plant extract is added into the polyester fiber, however, during the mixing and extrusion process of polyester chip and plant extract, due to too high temperature, a large amount of plant extract is inactivated, which causes loss of plant active ingredients, which means increase of production cost.
In patent No. CN201310140966.0 entitled "viscose fiber with plant-derived antibacterial function and aromatic smell and preparation method thereof", it is mentioned that plant-derived antibacterial agent and aromatic agent are added into viscose fiber, wherein the plant-derived antibacterial agent is mixed powder of mint extract and radix isatidis extract, and the aromatic agent is microcapsule-coated mint oil, but because the particle size of the extract is too small, aggregation and sedimentation phenomena are easily generated in spinning solution, and adding the extract directly into the fiber can have a certain influence on the mechanical properties of 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 purposes:
1. the problem of large loss of plant source active substances in the fiber spinning process is solved, and the phenomena of easy agglomeration and uneven dispersion of small-particle-size plant active particles in a load matrix are avoided;
2. the multifunctional plant source composite material is prepared, has good thermal stability and acid and alkali resistance, is suitable for spinning processes of various fibers, has wide application range, and is suitable for industrial large-scale production, sale and popularization;
3. the prepared multifunctional plant source composite material has excellent adhesion effect with different types of fiber matrixes, reduces the loss of plant source active ingredients, and improves the mechanical property of the fibers to a certain extent on the basis of endowing the fibers with natural and lasting 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 anhydrous 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 S11, carrying out ultrasonic treatment for 5-15min under the conditions of 150-200W and 20-40 ℃, adjusting the pH value to 7.5-8.5, heating to 50-60 ℃, reacting for 10-20min, cooling to room temperature, evaporating absolute ethyl alcohol, and fully drying at 55-75 ℃ to obtain modified plant source powder.
Wherein, the plant source powder of S11 is a plant extract, and the specific types are not limited and are all applicable to the system.
Preferably, the interface modifier S12 is prepared from the following components in a mass ratio of (1.5-2.5): gamma-aminopropyltriethoxysilane (0.2-0.8) 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 Nano-silica
S21: under the condition of 50-60 ℃, adding nano silicon dioxide into N-methyl pyrrolidone for ultrasonic dispersion for 20-30min, wherein the ultrasonic frequency is 80-100kHz, adding a silicon-containing unsaturated modifier and a stabilizing auxiliary agent, reacting for 10-20h, and then carrying out centrifugal separation, ethanol washing and vacuum drying to obtain an intermediate;
s22: and (2) placing the intermediate of S21 in distilled water, carrying out 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, reacting for 2-6h, centrifuging, washing with water, and drying to obtain the modified nano-silica.
Preferably, the mass ratio of the nano silicon dioxide, the silicon-containing unsaturated modifier and the stabilizing additive in S21 is (90-120): (0.5-1.5): (0.01-0.05).
Further, the unsaturated modifier containing silicon is prepared from the following components in a mass ratio of (0.4-1.2): (1.5-2) a mixture of vinyltris (. Beta. -methoxyethoxy) silane and gamma-methacryloxypropyl-trimethoxysilane.
Further, the stabilizing auxiliary agent 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 S22, ethylene glycol dimethacrylate and tert-butyl peroxybenzoate is (60-80): (90-100): (1-2).
S3: preparation of modified Polymer matrices
Adding a mixture of polyethylene glycol, cationic starch and modified nano-silica into polybutylene succinate, fully mixing under the condition of 1500-2500r/min, and placing the mixture into a mixing roll for melt blending to obtain the modified polymer matrix.
Preferably, the mass ratio of the polybutylene succinate, the polyethylene glycol, the cationic starch and the modified nano-silica in S3 is (40-50): (10-20): (4-8): (1-5).
Preferably, the hydroxyl value of the polyethylene glycol S3 is 170-208mgKOH/g, and the molecular weight is 540-660; the temperature of the melt blending is 180-200 ℃.
S4: modification and blending:
and proportionally mixing the modified plant source powder of S12 and the modified polymer matrix of S3 at a rotating speed of 550-750r/min, slowly heating to 110-120 ℃ at a speed of 4-8 ℃/min for reacting for 6-10h, adding a dried modification auxiliary agent, continuously heating to 130-140 ℃ for melt blending for 10-20min, and extruding and cooling to obtain the multifunctional plant source composite material for fiber spinning.
Preferably, the adding amount of the modified plant source powder of S4 is 4-12% of the mass of the modified polymer matrix; the mass ratio of the modified polymer matrix to the modifying auxiliary agent is (4-8): (2-6); the modifying auxiliary agent is prepared from (2-4) by mass: (0.5-1.5) a mixture of microcrystalline cellulose and polyhydroxybutyrate.
The multifunctional plant source composite material can be used for the spinning process of terylene, chinlon, acrylic fiber, polypropylene fiber, spandex, lyocell, modal, acetate fiber, viscose fiber, copper ammonia fiber and the like.
Due to the adoption of the technical scheme, the invention achieves the technical effects that:
1. the invention adopts the following components in percentage by mass (1.5-2.5): the gamma-aminopropyltriethoxysilane (0.2-0.8) and the 3- (2, 3-epoxypropyl) propyltrioxysilane modify the modified plant source powder, which can improve the interface performance between the small-particle-size plant source powder and the polymer matrix, improve the dispersion uniformity of the plant source powder in the polybutylene succinate, and alleviate the phenomena of easy agglomeration and non-uniform dispersion of the small-particle-size plant active particles in the load matrix.
2. Adding the silicon-containing unsaturated modifier into the nano silicon dioxide, wherein on one hand, the silicon-containing unsaturated modifier is reacted with 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 additive plays a role in promoting the modification to be more stably carried out, and certain influence on the modification reaction caused by the crosslinking between the silicon-containing unsaturated modifiers is avoided; adding ethylene glycol dimethacrylate and tert-butyl peroxybenzoate into the intermediate, connecting one end of the silicon-containing unsaturated modifier with the nano-silica and the other end with the ethylene glycol dimethacrylate, and coating the ethylene glycol dimethacrylate on the surface of the nano-silica, thereby completing the modification of the nano-silica.
3. According to the invention, stronger intermolecular acting force exists between the modified polymer matrix and the modified plant source powder, so that the adhesive force of active substances in the plant source powder on the poly (butylene succinate) is enhanced, and the processes of preparing a composite material and spinning are reducedThe loss of the plant source active ingredients is detected to be lower than 3 percent; on the other hand, the thermal stability and the acid and alkali resistance of the composite material are improved to a certain extent, so that the prepared composite material is suitable for the spinning process of various fibers such as terylene, chinlon, acrylic fiber, polypropylene fiber, spandex, lyocell, modal, acetate fiber, viscose fiber, cuprammonium fiber and the like. The composite material is added into the fibers, so that an excellent antibacterial effect is shown, the bacteriostatic rate of staphylococcus aureus, candida albicans and escherichia coli is higher than 95% (detected by GB/T20944.3-2008 oscillation method), and the bacteriostatic loss rate is lower than 1% (average value) after 100 times of water washing; the acarid prevention effect is excellent, the acarid avoidance rate is as high as more than 99% (detected by GB/T24253-2009 evaluation of acarid prevention performance of textiles), and after 100 times of washing, the acarid avoidance loss rate is lower than 2% (average value); good antistatic effect, surface resistivity is lower than 1 x 10 9 Omega cm (measured in GB/T24249-2009 antistatic clean fabric); the addition of the modified 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 added into the fiber matrix, and improves the mechanical property 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 fiber surface on the basis of enhancing the effects of chemical fiber strength, degradability, antibiosis, mite prevention, antistatic property and the like, and improves the dyeability of the chemical fiber; in addition, the dyeing temperature of the fiber can be reduced, and the polyester and the chinlon can be dyed at 20-40 ℃.
Detailed Description
The invention is further illustrated below 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 particle size of 100nm in anhydrous ethanol, stirring for 20min, filtering, and collecting filtrate to obtain plant source solution;
s12: adding an interface modifier into the plant source solution obtained in the step S11, carrying out ultrasonic treatment for 15min at the temperature of 40 ℃ under the condition of 200W, adjusting the pH value to 8.5, heating to 60 ℃, reacting for 20min, cooling to room temperature, evaporating absolute ethyl alcohol, and fully drying at 75 ℃ to obtain modified plant source powder.
S11, the plant source powder is a mixture of a green tea extract, a honeysuckle extract, a mint extract and a seaweed extract.
Wherein the S12 interfacial modifier is a mixture of the following components in a mass ratio of 2.5:0.8 of gamma-aminopropyltriethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane; the addition amount of the interface modifier is 1 percent of the mass of the plant source powder.
S2: preparation of modified Nano-silica
S21: adding nano silicon dioxide into N-methyl pyrrolidone for ultrasonic dispersion for 30min at the temperature of 60 ℃, adding a silicon-containing unsaturated modifier and a stabilizing auxiliary agent, reacting for 20h, and then performing centrifugal separation, ethanol washing and vacuum drying to obtain an intermediate;
s22: and (3) placing the intermediate of S21 in distilled water, carrying out ultrasonic treatment at 120kHz for 25min, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 100 ℃, adding tert-butyl peroxybenzoate to react for 6h, and carrying out centrifugation, water washing and drying to obtain the modified nano-silica.
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 prepared from the following components in a mass ratio of 1.2:2, a mixture of vinyltris (β -methoxyethoxy) silane and γ -methacryloxypropyl-trimethoxysilane.
The stabilizing auxiliary agent comprises 2, 6-di-tert-butyl-p-cresol and p-hydroxyanisole in a mass ratio of 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 matrices
And adding a mixture of polyethylene glycol, cationic starch and modified nano-silica into polybutylene succinate, fully mixing at 2500r/min, and putting the mixture into a mixing roll 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-silica is 50:20:8:5.
s3, the hydroxyl value of the polyethylene glycol is 208mgKOH/g, and the molecular weight is 660; the melt blending temperature was 200 ℃.
S4: modification and blending:
and (2) blending the modified plant source powder of S12 and the modified polymer matrix of S3 at a rotation speed of 750r/min in proportion, slowly heating to 120 ℃ at a speed of 8 ℃/min to react for 10 hours, adding a dried modification auxiliary agent, continuously heating to 140 ℃, melting and blending for 20min, and 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 high polymer matrix.
S4, the mass ratio of the modified polymer matrix to the modification auxiliary agent is 8:6; the modifying auxiliary agent is prepared from the following components in percentage by mass of 4:1.5 of a mixture of microcrystalline cellulose and polyhydroxybutyrate.
Embodiment 2 preparation method of multifunctional plant source 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 the plant source powder with the particle size of 70nm in 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 obtained in the step S11, carrying out ultrasonic treatment for 10min at 180W and 30 ℃, adjusting the pH to 8, heating to 55 ℃, reacting for 15min, cooling to room temperature, evaporating absolute ethyl alcohol, and fully drying at 65 ℃ to obtain modified plant source powder.
S11, the plant source powder is a mixture of a green tea extract, a honeysuckle extract, a mint extract and a seaweed extract.
Wherein the interface modifier S12 is prepared from the following components in a mass ratio of 2: gamma-aminopropyltriethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane at 0.5; the addition amount of the interface modifier is 0.8 percent of the mass of the plant source powder.
S2: preparation of modified Nano-silica
S21: adding nano silicon dioxide into N-methyl pyrrolidone for ultrasonic dispersion for 25min at 55 ℃, wherein the ultrasonic frequency is 90kHz, adding a silicon-containing unsaturated modifier and a stabilizing auxiliary agent, reacting for 15h, and then carrying out 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 at 110kHz for 20min, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 90 ℃, adding tert-butyl peroxybenzoate, reacting for 4h, and centrifuging, washing and drying to obtain the modified nano-silica.
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 prepared from the following components in a mass ratio of 0.8:1.7 mixtures of vinyltris (. Beta. -methoxyethoxy) silane and gamma. -methacryloxypropyl-trimethoxysilane.
The stabilizing auxiliary agent comprises p-hydroxyanisole and 1, 1-diphenyl-2-trinitrophenylhydrazine in a mass ratio of 1.
S22, the mass ratio of the intermediate to the ethylene glycol dimethacrylate to the tert-butyl peroxybenzoate is 70:95:1.5.
s3: preparation of modified Polymer matrices
Adding a mixture of polyethylene glycol, cationic starch and modified nano-silica into polybutylene succinate, fully mixing at 2000r/min, and placing in a mixing roll 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-silica 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: modification and blending:
and (2) blending the modified plant source powder of S12 and the modified polymer matrix of S3 at a rotation speed of 650r/min in proportion, slowly heating to 115 ℃ at a speed of 6 ℃/min to react for 8h, adding a dried modification auxiliary agent, continuously heating to 135 ℃ to melt and blend for 15min, and 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.
S4, the mass ratio of the modified polymer matrix to the modification auxiliary agent is 6:4; the modifying auxiliary agent is prepared from the following components in percentage by mass of 3:1 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 particle size of 50nm in anhydrous ethanol, stirring for 10min, filtering, and collecting filtrate to obtain plant source solution;
s12: adding an interface modifier into the plant source solution obtained in the step S11, carrying out ultrasonic treatment for 5min at the temperature of 20 ℃ and 150W, adjusting the pH value to 7.5, heating to 50 ℃ for reaction for 10min, cooling to room temperature, evaporating absolute ethyl alcohol, and fully drying at 55 ℃ to obtain modified plant source powder.
S11, the plant source powder is a mixture of a green tea extract, a honeysuckle extract, a mint extract and a seaweed extract.
Wherein the S12 interfacial modifier is a mixture of the following components in a mass ratio of 1.5:0.2 of gamma-aminopropyltriethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane; the addition amount of the interface modifier is 0.5 percent of the mass of the plant source powder.
S2: preparation of modified Nano-silica
S21: adding nano silicon dioxide into N-methyl pyrrolidone for ultrasonic dispersion for 20min at 50 ℃, adding a silicon-containing unsaturated modifier and a stabilizing auxiliary agent for reaction for 10h, and performing centrifugal separation, ethanol washing and vacuum drying to obtain an intermediate;
s22: and (3) placing the intermediate of S21 in distilled water, carrying out ultrasonic treatment at 100kHz for 15min, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 80 ℃, adding tert-butyl peroxybenzoate to react for 2h, and carrying out centrifugation, water washing and drying to obtain the modified nano-silica.
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 prepared from the following components in a mass ratio of 0.4:1.5 mixtures of vinyltris (. Beta. -methoxyethoxy) silane and gamma. -methacryloxypropyl-trimethoxysilane.
The stabilizing additive 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 matrices
Adding a mixture of polyethylene glycol, cationic starch and modified nano-silica into polybutylene succinate, fully mixing at 1500r/min, and placing in a mixing roll 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-silica is 40:10:4:1.
s3, the hydroxyl value of the polyethylene glycol is 170mgKOH/g, and the molecular weight is 540; the melt blending temperature was 180 ℃.
S4: modification and blending:
and (3) blending the modified plant source powder of S12 and the modified polymer matrix of S3 at a rotation speed of 550r/min in proportion, slowly heating to 110 ℃ at a speed of 4 ℃/min for reacting for 6h, adding a dried modification auxiliary agent, continuously heating to 130 ℃, melting and blending for 10min, 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.
S4, the mass ratio of the modified polymer matrix to the modification auxiliary agent is 4:2; the modifying auxiliary agent is prepared from the following components in percentage by mass: 0.5 of a mixture of microcrystalline cellulose and polyhydroxybutyrate.
The multifunctional plant-derived composite materials for fiber spinning prepared in examples 1 to 3 were added to viscose, polyester and nylon fibers in an amount of 3% and tested for their properties, as shown in tables 1, 2 and 3.
TABLE 1
TABLE 2
TABLE 3
And (4) testing standard:
mechanical properties: GB/T3923.1-2013 bar sample method for measuring tensile property, breaking strength and breaking elongation of textile fabrics.
Dyeing uniformity: test and evaluation of dyeing uniformity of viscose filaments (FZ/T50015-2009) determination of grey-card grade.
Color fastness to washing: GB-T/3921-2008 textile color fastness test and soaping resistance color fastness.
The bacteriostasis rate is as follows: GB/T20944.3-2008 oscillating method.
Mite avoidance rate: GB/T24253-2009 evaluation of anti-mite performance of textiles.
Surface resistivity: GB/T24249-2009 antistatic clean fabric.
It can be seen from the table that when the multifunctional plant-derived composite material for fiber spinning prepared in examples 1 to 3 is added into viscose fiber, polyester fiber and polyamide fiber, the mechanical properties of the fiber are excellent, the loss rate of the plant-derived active ingredients in the spinning process is low, the dyeing property and the color fastness to washing of the fiber are good, the fiber has good bacteriostatic activity, the bacteriostatic rate of staphylococcus aureus, candida albicans and escherichia coli are all higher than 95%, and the bacteriostatic loss rate after washing for 100 times is lower than 1% (average value); the acarid prevention effect is excellent, the acarid avoidance rate is up to more than 99%, and after 100 times of water washing, the acarid avoidance loss rate is lower than 2% (average value); good antistatic effect, surface resistivity lower than 1 × 10 9 Ω·cm。
The multifunctional plant source composite material prepared by the invention has good thermal stability and acid and alkali resistance, reduces the loss of plant source active ingredients in the preparation process and the spinning process of the composite material, enhances the strength of chemical fibers to a certain extent to endow the fibers with functionality, 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 polyester and the chinlon can be dyed at 20-40 ℃.
Comparative example 1
Representative example 2 was chosen, using a mass ratio of 3.1 and 0.1: the gamma-aminopropyltriethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane of 3 modified the plant source powder, the rest was the same as example 2, and the modified plant source powder obtained in comparative example 1 still showed aggregation and non-uniform dispersion in the modified polymer matrix during modification and blending.
Comparative example 2
The representative example 2 is selected, the amount of the added interface modifier is 0, and the balance is consistent with that of the example 2, as a comparative example 2, under the condition that other preparation processes are not changed, the plant source powder is agglomerated and dispersed unevenly in the process of blending with the polymer matrix, which shows that the interface 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 evenly, and the quality of a final product is further stable.
Comparative example 3
Selecting representative example 2, removing the step of preparing a modified high-molecular matrix, directly modifying and blending modified plant source powder and polybutylene succinate, wherein the rest is consistent with example 2 as comparative example 3, and adding the prepared composite material into viscose fibers, polyester fibers and nylon fibers according to the addition of 3% respectively and testing the performance of the composite material, which is specifically shown in table 4.
TABLE 4
It can be seen that stronger intermolecular acting force exists between the modified polymer matrix and the modified plant source powder, so that on one hand, the adhesive force of active substances in the plant source powder on the poly (butylene succinate) is enhanced, and the loss in the processes of preparing a composite material and spinning is reduced; on the other hand, the thermal stability and the acid and alkali resistance of the composite material are improved to a certain extent, and the mechanical property and the dyeing property of the fiber are also improved.
Comparative example 4
Selecting representative example 2, removing the step of modifying additives, and taking the rest as the comparative example 4, wherein the prepared composite material is respectively added into viscose fibers, polyester fibers and nylon fibers according to the addition of 3 percent and tested for mechanical properties, and the specific table is shown in table 5.
TABLE 5
The addition of the modified 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 added into the fiber matrix, and improves the mechanical property of the fibers.
Unless otherwise specified, the proportions are mass proportions, and the percentages are mass percentages; the raw materials are all purchased from the market.
Finally, it should be noted that: 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 embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a 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 high molecular matrix and modifying and blending; the preparation of the modified plant source powder comprises the following steps:
placing the plant source powder in absolute ethyl alcohol, stirring and 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-aminopropyltriethoxysilane and 3- (2, 3-epoxypropyl) propyltrioxysilane;
the mass ratio of the gamma-aminopropyltriethoxysilane to the 3- (2, 3-epoxypropyl) propyltrioxysilane is 1.5-2.5:0.2-0.8.
2. The preparation method of the multifunctional plant-derived composite material for fiber spinning according to claim 1, wherein the modification by adding the interfacial modifier is carried out by performing ultrasonic treatment at 20-40 ℃ for 5-15min under 150-200W, adjusting pH to 7.5-8.5, heating to 50-60 ℃ for reaction for 10-20min, cooling to room temperature, evaporating absolute ethyl alcohol, and fully drying at 55-75 ℃.
3. The preparation method of the multifunctional plant-derived composite material for fiber spinning according to claim 1, wherein the addition amount of the interfacial modifier is 0.5-1% of the mass of the plant-derived powder.
4. The preparation method of the multifunctional plant-derived composite material for fiber spinning according to claim 1, wherein the preparation of the modified nano silica comprises the following steps:
under the condition of 50-60 ℃, adding nano silicon dioxide into N-methyl pyrrolidone for ultrasonic dispersion for 20-30min, wherein the ultrasonic frequency is 80-100kHz, adding a silicon-containing unsaturated modifier and a stabilizing auxiliary agent, reacting for 10-20h, and then carrying out centrifugal separation, ethanol washing and vacuum drying to obtain an intermediate;
and (3) placing the intermediate in distilled water, carrying out ultrasonic treatment at 100-120kHz for 15-25min, adding ethylene glycol dimethacrylate under the protection of nitrogen, heating to 80-100 ℃, adding tert-butyl peroxybenzoate, reacting for 2-6h, centrifuging, washing with water, and drying to obtain the modified nano silicon dioxide.
5. The preparation method of the multifunctional plant-derived composite material for fiber spinning according to claim 4, wherein the mass ratio of the nano-silica, the silicon-containing unsaturated modifier and the stabilizing additive is 90-120:0.5-1.5:0.01-0.05;
the mass ratio of the intermediate to the ethylene glycol dimethacrylate to the tert-butyl peroxybenzoate is 60-80:90-100:1-2.
6. The preparation method of the multifunctional plant-derived composite material for fiber spinning according to claim 4, wherein the silicon-containing unsaturated modifier is a mixture of the silicon-containing unsaturated modifier and the unsaturated modifier in a mass ratio of 0.4-1.2:1.5-2 mixtures of vinyltris (β -methoxyethoxy) silane and γ -methacryloxypropyl-trimethoxysilane;
the stabilizing auxiliary agent comprises one or more of 2, 6-di-tert-butyl-p-cresol, p-hydroxyanisole and 1, 1-diphenyl-2-trinitrophenylhydrazine.
7. The preparation method of the multifunctional plant-derived composite material for fiber spinning according to claim 1, wherein the preparation of the modified polymer matrix comprises the steps of adding a mixture of polyethylene glycol, cationic starch and modified nano-silica into polybutylene succinate, fully mixing at 1500-2500r/min, and melt blending in a mixing roll 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-silica is (40-50): 10-20:4-8:1-5.
8. The preparation method of the multifunctional plant-derived composite material for fiber spinning according to claim 1, wherein the modification and blending are performed by blending the modified plant-derived powder and the modified polymer matrix at a rotation speed of 550-750r/min in proportion, slowly heating to 110-120 ℃ at a speed of 4-8 ℃/min to react for 6-10h, adding a dried modification auxiliary agent, continuously heating to 130-140 ℃ to melt and blend for 10-20min, and performing extrusion and cooling to obtain the multifunctional plant-derived composite material for fiber spinning.
9. The method for preparing the multifunctional plant-derived composite material for fiber spinning according to claim 8, wherein the addition amount of the modified plant-derived powder is 4-12% of the mass of the modified polymer matrix.
10. The preparation method of the multifunctional plant-derived composite material for fiber spinning according to claim 8, wherein the mass ratio of the modified polymer matrix to the modification auxiliary agent is 4-8:2-6; the modifying auxiliary agent is prepared from the following components in a mass ratio of 2-4:0.5-1.5 of a mixture of microcrystalline cellulose and polyhydroxybutyrate.
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