CN116397349B - Antistatic functional fiber material and preparation method and application thereof - Google Patents
Antistatic functional fiber material and preparation method and application thereof Download PDFInfo
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- CN116397349B CN116397349B CN202310298996.8A CN202310298996A CN116397349B CN 116397349 B CN116397349 B CN 116397349B CN 202310298996 A CN202310298996 A CN 202310298996A CN 116397349 B CN116397349 B CN 116397349B
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- isoxazole
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- dicarboxylic acid
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- 239000002657 fibrous material Substances 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- OSKMGGSWKBKSMF-UHFFFAOYSA-N 1,2-oxazole-3,5-dicarboxylic acid Chemical class OC(=O)C=1C=C(C(O)=O)ON=1 OSKMGGSWKBKSMF-UHFFFAOYSA-N 0.000 claims abstract description 61
- GVNHOISKXMSMPX-UHFFFAOYSA-N 2-[butyl(2-hydroxyethyl)amino]ethanol Chemical compound CCCCN(CCO)CCO GVNHOISKXMSMPX-UHFFFAOYSA-N 0.000 claims abstract description 61
- -1 glycerol triglycidyl ether modified aniline Chemical class 0.000 claims abstract description 33
- DGSDBJMBHCQYGN-UHFFFAOYSA-M sodium;2-ethylhexyl sulfate Chemical compound [Na+].CCCCC(CC)COS([O-])(=O)=O DGSDBJMBHCQYGN-UHFFFAOYSA-M 0.000 claims abstract description 33
- 238000005406 washing Methods 0.000 claims abstract description 28
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 27
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 27
- 239000011737 fluorine Substances 0.000 claims abstract description 27
- 239000000661 sodium alginate Substances 0.000 claims abstract description 27
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 27
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 27
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims abstract description 26
- 239000013638 trimer Substances 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 19
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 19
- 241001330002 Bambuseae Species 0.000 claims abstract description 19
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 19
- 239000011425 bamboo Substances 0.000 claims abstract description 19
- 239000003610 charcoal Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000007822 coupling agent Substances 0.000 claims abstract description 15
- 229920000728 polyester Polymers 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 38
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 28
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000002904 solvent Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000009835 boiling Methods 0.000 claims description 21
- 239000003960 organic solvent Substances 0.000 claims description 21
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- 238000009987 spinning Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 15
- SYEWHONLFGZGLK-UHFFFAOYSA-N 2-[1,3-bis(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COCC(OCC1OC1)COCC1CO1 SYEWHONLFGZGLK-UHFFFAOYSA-N 0.000 claims description 14
- JGFZNNIVVJXRND-UHFFFAOYSA-N N,N-diisopropylethylamine Substances CCN(C(C)C)C(C)C JGFZNNIVVJXRND-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 14
- 238000002074 melt spinning Methods 0.000 claims description 14
- 238000002390 rotary evaporation Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- XXFAKYKJDDMEGJ-UHFFFAOYSA-N 1-fluoro-3-(fluoromethyl)benzene Chemical compound FCC1=CC=CC(F)=C1 XXFAKYKJDDMEGJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 7
- 230000005494 condensation Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 238000001125 extrusion Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000006068 polycondensation reaction Methods 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical group O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 239000000835 fiber Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical group C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- MHGOKSLTIUHUBF-UHFFFAOYSA-N 2-ethylhexyl sulfate Chemical compound CCCCC(CC)COS(O)(=O)=O MHGOKSLTIUHUBF-UHFFFAOYSA-N 0.000 description 2
- 241001116389 Aloe Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 2
- 235000011201 Ginkgo Nutrition 0.000 description 2
- 235000008100 Ginkgo biloba Nutrition 0.000 description 2
- 244000194101 Ginkgo biloba Species 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 235000011399 aloe vera Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000004185 ester group Chemical group 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- ZXLOSLWIGFGPIU-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCN1CN(C)C=C1 ZXLOSLWIGFGPIU-UHFFFAOYSA-N 0.000 description 1
- FQERWQCDIIMLHB-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CC[NH+]1CN(C)C=C1 FQERWQCDIIMLHB-UHFFFAOYSA-N 0.000 description 1
- 244000198134 Agave sisalana Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 206010008479 Chest Pain Diseases 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 235000008694 Humulus lupulus Nutrition 0.000 description 1
- 241001349804 Juncus alpinoarticulatus Species 0.000 description 1
- 208000000418 Premature Cardiac Complexes Diseases 0.000 description 1
- 206010038743 Restlessness Diseases 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000004781 alginic acids Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 206010003119 arrhythmia Diseases 0.000 description 1
- 230000006793 arrhythmia Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- CTAPFRYPJLPFDF-UHFFFAOYSA-N isoxazole Chemical group C=1C=NOC=1 CTAPFRYPJLPFDF-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 235000011056 potassium acetate Nutrition 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000002861 ventricular Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/008—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting against electric shocks or static electricity
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D31/00—Materials specially adapted for outerwear
- A41D31/04—Materials specially adapted for outerwear characterised by special function or use
- A41D31/26—Electrically protective, e.g. preventing static electricity or electric shock
-
- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The invention provides an antistatic functional fiber material, a preparation method and application thereof, which are prepared from the following raw materials in parts by weight: 15-25 parts of fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, 35-45 parts of polyester chips, 5-8 parts of nano bamboo charcoal powder, 1-3 parts of coupling agent, 3-5 parts of glycerol triglycidyl ether modified aniline trimer, 1-3 parts of 2-ethylhexyl sulfate sodium salt and 2-4 parts of sodium alginate. The antistatic functional fiber material disclosed by the invention has the advantages of remarkable antistatic effect, good antistatic durability, good washing fastness, environmental friendliness and excellent mechanical properties.
Description
Technical Field
The invention relates to the technical field of functional fiber materials, in particular to an antistatic functional fiber material, and a preparation method and application thereof.
Background
Along with the development of science and technology, the improvement of society and the improvement of living standard, the requirements of people on living quality are higher and higher. The functional fiber material product has been extended from the basic function of the shade against cold to the functions of beautiful, comfortable, fashionable, protection and the like, and the consumption concept of people is gradually developed from practical use to health care, environmental protection and multifunction. Various functional fiber material products are widely focused and developed, so that the market demand of the functional fiber materials is increased and the performance requirements are also increased.
The fiber material product can generate static electricity with different degrees in daily use, and especially in dry areas and autumn and winter, the static electricity phenomenon is obvious. Static electricity can cause people to feel tingling and tingling, and is restless, headache is generated, and the feeling is very uncomfortable. In addition, excessive static electricity can promote the aggravation of cardiovascular diseases or induce arrhythmia such as ventricular premature beat, and produce symptoms such as chest distress, dyspnea, cough, etc. It is under this situation that the fibrous material with antistatic function has been developed, and its appearance has attracted a great deal of attention, and antistatic performance has become an important index for measuring the grade of fibrous material products.
The existing antistatic functional fiber material mostly adopts an antistatic auxiliary agent after-finishing or doping method to realize the antistatic function, but after-finishing antistatic functional fiber material is washed for many times, the antistatic effect is poorer and worse, and the performance stability and the service life are required to be further improved. The doped antistatic functional fiber material is easy to extravasate in the long-term use process due to poor compatibility between the antistatic auxiliary agent and the fiber material matrix, so that the performance stability is insufficient, and the common antistatic auxiliary agent has the defects of insufficient antistatic function and harm to human health. Other antistatic functional fiber materials on the market also commonly have the technical problems of insufficient wearing comfort and mechanical properties to be further improved.
In order to solve the problems, patent CN103966689B discloses an antistatic bamboo fiber fabric, which is prepared from the following raw materials in parts by weight: 3-4 parts of nano chitin, 40-50 parts of 1-ethyl-3-methylimidazole acetate, 3-5 parts of potassium acetate, 40-50 parts of 1-ethyl-3-methylimidazole chloride, 14-17 parts of plastic starch, 2-3 parts of aloe gel, 14-20 parts of Chinese alpine rush fiber, 7-10 parts of water, 60-70 parts of bamboo fiber, 5-8 parts of sisal fiber, 1-2 parts of graphite powder, 1-2 parts of hop, 1-2 parts of ginkgo leaf and 0.4-0.8 part of spinning auxiliary agent; the nano aloe gel and the graphite powder are added into the fabric, so that the fabric has good antistatic performance; by adding nano chitin and plastic starch, the strength of the fiber is increased, and the hand feeling and water resistance are improved; by adding hops and ginkgo leaves, skin microcirculation can be enhanced. However, the antistatic fiber material has insufficient antistatic durability, poor washing fastness and further prolonged service life.
Therefore, the field still needs an antistatic functional fiber material with remarkable antistatic effect, good antistatic durability, good washing fastness, environmental protection and excellent mechanical properties.
Disclosure of Invention
In view of the above problems, the invention aims to provide an antistatic functional fiber material with remarkable antistatic effect, good antistatic durability, good washing fastness, environmental protection and excellent mechanical properties, and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: an antistatic functional fiber material is prepared from the following raw materials in parts by weight: 15-25 parts of fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, 35-45 parts of polyester chips, 5-8 parts of nano bamboo charcoal powder, 1-3 parts of coupling agent, 3-5 parts of glycerol triglycidyl ether modified aniline trimer, 1-3 parts of 2-ethylhexyl sulfate sodium salt and 2-4 parts of sodium alginate.
Preferably, the preparation method of the glycerol triglycidyl ether modified aniline trimer comprises the following steps: adding the aniline tetramer and the glycerol triglycidyl ether into an organic solvent, stirring and reacting for 4-6 hours at 70-80 ℃, and then removing the solvent by rotary evaporation to obtain the glycerol triglycidyl ether modified aniline trimer.
Preferably, the molar ratio of the aniline tetramer to the glycerol triglycidyl ether to the organic solvent is 3:1 (15-20).
Preferably, the source of the aniline tetramer is not particularly limited, and in one embodiment of the present invention, the aniline tetramer is prepared according to the preparation method of the aniline tetramer in CN103866423B example 1.
Preferably, the organic solvent is at least one of N, N-dimethylformamide and N, N-dimethylacetamide.
Preferably, the coupling agent is at least one of a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH 570.
Preferably, the granularity of the nano bamboo charcoal powder is 300-500nm.
Preferably, the polyester chip is a polyester fine denier composite spinning special chip FC510A.
Preferably, the preparation method of the fluorine-containing phenyl ionization modified 3, 5-isoxazoledicarboxylic acid/N-butyl diethanolamine polycondensate comprises the following steps:
s1, uniformly mixing 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent, adding into a closed reaction kettle provided with a condensation reflux device, replacing air in the kettle with inert gas, reacting for 3-5 hours at the normal pressure of 110-120 ℃, heating to 240-250 ℃, performing polycondensation reaction for 12-18 hours at 300-500Pa, cooling to room temperature, adjusting to normal pressure, washing the precipitated product with ethanol for 3-6 times, and performing rotary evaporation to remove ethanol to obtain a 3, 5-isoxazole dicarboxylic acid/N-butyldiethanolamine polycondensate;
and S2, adding the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate and m-fluorobenzyl fluoride prepared in the step S1 into dimethyl sulfoxide, stirring at 60-80 ℃ for reaction for 4-6 hours, discharging and precipitating in water, washing the precipitated polymer with ethanol for 3-7 times, and drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate.
Preferably, the molar ratio of the 3, 5-isoxazoledicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and the high boiling point solvent in the step S1 is 1:1 (0.8-1.2): (0.4-0.6): (10-15).
Preferably, the high boiling point solvent is sulfolane; the inert gas is any one of nitrogen, helium, neon and argon.
Preferably, the mass ratio of the 3, 5-isoxazoledicarboxylic acid/N-butyldiethanolamine polycondensate, m-fluorochlorobenzyl and dimethyl sulfoxide in the step S2 is 1 (0.2-0.4): 4-6.
Another object of the present invention is to provide a method for preparing the antistatic functional fiber material, comprising the steps of: uniformly mixing the raw materials in parts by weight, adding into a double-screw extruder for extrusion, carrying out melt spinning to obtain a crude fiber material, soaking the crude fiber material into a mixed aqueous solution of 2-ethylhexyl sulfate sodium salt and sodium alginate at 50-60 ℃ for 10-20 hours, taking out, washing with water for 3-7 times, and finally drying in a vacuum drying oven at 90-100 ℃ to constant weight to obtain the antistatic functional fiber material.
Preferably, the mass ratio of the sodium 2-ethylhexyl sulfate to water in the mixed aqueous solution of the sodium 2-ethylhexyl sulfate and the sodium alginate is 1 (20-30).
Preferably, the spinning temperature of the melt spinning is 250-260 ℃ and the spinning speed is 1500-2000m/min.
The invention also aims to provide an application of the antistatic functional fiber material in manufacturing antistatic working clothes.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method of the antistatic functional fiber material disclosed by the invention has the advantages of simple process, convenience in operation, low equipment dependence and energy consumption, high preparation efficiency and high finished product qualification rate, and is suitable for continuous large-scale production.
(2) According to the antistatic functional fiber material disclosed by the invention, through reasonable selection of raw material components and proportions, the raw materials can better perform interaction, so that the final antistatic functional fiber material is endowed with obvious antistatic effect, better antistatic durability, better water-resistance fastness, excellent environmental protection and mechanical properties.
(3) The fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate molecular main chain contains ester groups, so that the antistatic functional fiber material disclosed by the invention has good compatibility with polyester chips and good performance stability after blending; the molecular chain of the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate contains fluorine-containing benzene, quaternary ammonium salt, isoxazole, butyl and ester group structures which are matched with each other, so that the prepared fiber material has the advantages of good mechanical properties, difficult broken wire, good performance stability, good water fastness, long service life and excellent antistatic effect and durability.
(4) The antistatic functional fiber material disclosed by the invention has the advantages that the glycerol triglycidyl ether modified aniline trimer, the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate and the nanometer bamboo charcoal powder are synergistic, so that the prepared antistatic functional fiber material has excellent antistatic performance and good antistatic durability; the nano bamboo charcoal powder can also play roles in enhancing, protecting health, deodorizing and improving the use environment protection. The treatment of the glycerol triglycidyl ether modified aniline trimer can improve the antistatic property, and can also improve the compatibility of all raw materials, thereby improving the antistatic durability and the washing resistance.
(5) The preparation process of the antistatic functional fiber material disclosed by the invention is provided with the step of soaking the fiber material into a mixed aqueous solution of 2-ethylhexyl sulfate sodium salt and sodium alginate at 50-60 ℃, wherein sodium ions on the 2-ethylhexyl sulfate sodium salt and sodium alginate can be subjected to ion exchange with quaternary ammonium salt cations on fluorine-containing phenyl ionization modified 3, 5-isoxazoledicarboxylic acid/N-butyl diethanolamine polycondensate, and a 2-ethylhexyl sulfate and alginic acid structure is introduced to the surface of the fiber material, so that the antistatic property is enhanced, and an interpenetrating network ion crosslinked structure can be formed on the surface of the fiber material, and the physical property and performance stability of the fiber material can be effectively improved.
Detailed Description
In order to better understand the technical solution of the present invention, the following describes the product of the present invention in further detail with reference to examples.
The aniline tetramer in each embodiment of the invention is prepared according to the preparation method of the aniline tetramer in the embodiment 1 of CN 103866423B; the polyester chip is a special chip FC510A for polyester fine denier composite spinning.
Example 1
An antistatic functional fiber material is prepared from the following raw materials in parts by weight: 15 parts of fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, 35 parts of polyester chip, 5 parts of nano bamboo charcoal powder, 1 part of coupling agent, 3 parts of glycerol triglycidyl ether modified aniline trimer, 1 part of 2-ethylhexyl sulfate sodium salt and 2 parts of sodium alginate.
The preparation method of the glycerol triglycidyl ether modified aniline trimer comprises the following steps: adding aniline tetramer and glycerol triglycidyl ether into an organic solvent, stirring and reacting for 4 hours at 70 ℃, and removing the solvent by rotary evaporation to obtain glycerol triglycidyl ether modified aniline trimer; the molar ratio of the aniline tetramer to the glycerol triglycidyl ether to the organic solvent is 3:1:15; the organic solvent is N, N-dimethylformamide.
The coupling agent is a silane coupling agent KH550; the granularity of the nano bamboo charcoal powder is 300nm.
The preparation method of the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate comprises the following steps:
s1, uniformly mixing 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent, adding the mixture into a closed reaction kettle provided with a condensation reflux device, replacing air in the kettle with inert gas, reacting at the normal pressure of 110 ℃ for 3 hours, heating to 240 ℃, carrying out polycondensation reaction at 300Pa for 12 hours, cooling to room temperature, adjusting to the normal pressure, washing a precipitated product with ethanol for 3 times, and carrying out rotary evaporation to remove ethanol to obtain a 3, 5-isoxazole dicarboxylic acid/N-butyldiethanolamine polycondensate; determination of M of the polycondensate by GPC test, U.S. Waters515-2410 n ＝18620g/mol，M W /M n ＝1.58；
And S2, adding the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate and m-fluorobenzyl fluoride prepared in the step S1 into dimethyl sulfoxide, stirring at 60 ℃ for reaction for 4 hours, discharging, precipitating in water, washing the precipitated polymer with ethanol for 3 times, and drying at 85 ℃ in a vacuum drying oven to constant weight to obtain the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate. The grafting ratio of this reaction was 15.5% by weight (ratio of the amount of change in weight of the polycondensate after the reaction to the mass of the polycondensate as calculated by weight change analysis).
The molar ratio of the 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and the high boiling point solvent in the step S1 is 1:1:0.8:0.4:10; the high boiling point solvent is sulfolane; the inert gas is nitrogen.
The mass ratio of the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, m-chlorofluorobenzyl and dimethyl sulfoxide in the step S2 is 1:0.2:4.
The preparation method of the antistatic functional fiber material comprises the following steps: uniformly mixing the raw materials in parts by weight, adding the mixture into a double-screw extruder for extrusion, carrying out melt spinning to obtain a crude fiber material, soaking the crude fiber material into a mixed aqueous solution of 2-ethylhexyl sulfate sodium salt and sodium alginate at 50 ℃ for 10 hours, taking out the crude fiber material, washing the crude fiber material with water for 3 times, and finally drying the crude fiber material in a vacuum drying oven at 90 ℃ to constant weight to obtain the antistatic functional fiber material; the mass ratio of the 2-ethylhexyl sulfate sodium salt to water in the mixed aqueous solution of the 2-ethylhexyl sulfate sodium salt and the sodium alginate is 1:20; the spinning temperature of the melt spinning is 250 ℃, and the spinning speed is 1500m/min.
Example 2
An antistatic functional fiber material is prepared from the following raw materials in parts by weight: 17 parts of fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, 38 parts of polyester chip, 6 parts of nano bamboo charcoal powder, 1.5 parts of coupling agent, 3.5 parts of glycerol triglycidyl ether modified aniline trimer, 1.5 parts of 2-ethylhexyl sulfate sodium salt and 2.5 parts of sodium alginate.
The preparation method of the glycerol triglycidyl ether modified aniline trimer comprises the following steps: adding aniline tetramer and glycerol triglycidyl ether into an organic solvent, stirring and reacting for 4.5 hours at 73 ℃, and then removing the solvent by rotary evaporation to obtain glycerol triglycidyl ether modified aniline trimer; the molar ratio of the aniline tetramer to the glycerol triglycidyl ether to the organic solvent is 3:1:17; the organic solvent is N, N-dimethylacetamide.
The coupling agent is silane coupling agent KH560; the granularity of the nano bamboo charcoal powder is 350nm.
The preparation method of the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate comprises the following steps:
s1, uniformly mixing 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent, adding the mixture into a closed reaction kettle provided with a condensation reflux device, replacing air in the kettle with inert gas, reacting at the normal pressure of 113 ℃ for 3.5 hours, heating to 243 ℃, carrying out polycondensation reaction at 350Pa for 13 hours, cooling to room temperature, adjusting to the normal pressure, washing the precipitated product with ethanol for 4 times, and removing the ethanol by rotary evaporation to obtain a 3, 5-isoxazole dicarboxylic acid/N-butyldiethanolamine polycondensate;
and S2, adding the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate and m-fluorobenzyl fluoride prepared in the step S1 into dimethyl sulfoxide, stirring at 65 ℃ for 4.5 hours, discharging, precipitating in water, washing the precipitated polymer with ethanol for 4 times, and drying in a vacuum drying oven at 87 ℃ until the weight is constant to obtain the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate.
The molar ratio of the 3, 5-isoxazole dicarboxylic acid, N-butyl diethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and the high boiling point solvent in the step S1 is 1:1:0.9:0.45:12; the high boiling point solvent is sulfolane; the inert gas is helium.
The mass ratio of the 3, 5-isoxazoledicarboxylic acid/N-butyldiethanolamine polycondensate, the metaflumetol and the dimethyl sulfoxide in the step S2 is 1:0.25:4.5.
The preparation method of the antistatic functional fiber material comprises the following steps: uniformly mixing the raw materials in parts by weight, adding the mixture into a double-screw extruder for extrusion, carrying out melt spinning to obtain a crude fiber material, soaking the crude fiber material into a mixed aqueous solution of sodium 2-ethylhexyl sulfate at 53 ℃ and sodium alginate for 12 hours, taking out the crude fiber material, washing the crude fiber material with water for 4 times, and finally drying the crude fiber material in a vacuum drying oven at 93 ℃ to constant weight to obtain the antistatic functional fiber material; the mass ratio of the 2-ethylhexyl sulfate sodium salt to water in the mixed aqueous solution of the 2-ethylhexyl sulfate sodium salt and the sodium alginate is 1:23; the spinning temperature of the melt spinning is 253 ℃, and the spinning speed is 1700m/min.
Example 3
An antistatic functional fiber material is prepared from the following raw materials in parts by weight: 20 parts of fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, 40 parts of polyester chip, 6.5 parts of nano bamboo charcoal powder, 2 parts of coupling agent, 4 parts of glycerol triglycidyl ether modified aniline trimer, 2 parts of 2-ethylhexyl sulfate sodium salt and 3 parts of sodium alginate.
The preparation method of the glycerol triglycidyl ether modified aniline trimer comprises the following steps: adding aniline tetramer and glycerol triglycidyl ether into an organic solvent, stirring and reacting for 5 hours at 75 ℃, and removing the solvent by rotary evaporation to obtain glycerol triglycidyl ether modified aniline trimer; the molar ratio of the aniline tetramer to the glycerol triglycidyl ether to the organic solvent is 3:1:18; the organic solvent is N, N-dimethylformamide.
The coupling agent is a silane coupling agent KH570; the granularity of the nano bamboo charcoal powder is 400nm.
The preparation method of the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate comprises the following steps:
s1, uniformly mixing 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent, adding the mixture into a closed reaction kettle provided with a condensation reflux device, replacing air in the kettle with inert gas, reacting at the normal pressure of 115 ℃ for 4 hours, heating to 245 ℃, performing polycondensation reaction at 400Pa for 15 hours, cooling to room temperature, adjusting to the normal pressure, washing a precipitated product with ethanol for 5 times, and performing rotary evaporation to remove ethanol to obtain a 3, 5-isoxazole dicarboxylic acid/N-butyldiethanolamine polycondensate;
and S2, adding the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate and m-fluorobenzyl fluoride prepared in the step S1 into dimethyl sulfoxide, stirring at 70 ℃ for reacting for 5 hours, discharging, precipitating in water, washing the precipitated polymer with ethanol for 5 times, and drying at 90 ℃ in a vacuum drying oven to constant weight to obtain the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate.
The molar ratio of the 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and the high boiling point solvent in the step S1 is 1:1:0.5:13; the high boiling point solvent is sulfolane; the inert gas is neon; the mass ratio of the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, m-chlorofluorobenzyl and dimethyl sulfoxide in the step S2 is 1:0.3:5.
The preparation method of the antistatic functional fiber material comprises the following steps: uniformly mixing the raw materials in parts by weight, adding the mixture into a double-screw extruder for extrusion, carrying out melt spinning to obtain a crude fiber material, soaking the crude fiber material into a mixed aqueous solution of sodium 2-ethylhexyl sulfate and sodium alginate at 55 ℃ for 15 hours, taking out the crude fiber material, washing the crude fiber material with water for 5 times, and finally drying the crude fiber material in a vacuum drying oven at 95 ℃ to constant weight to obtain the antistatic functional fiber material; the mass ratio of the 2-ethylhexyl sulfate sodium salt to water in the mixed aqueous solution of the 2-ethylhexyl sulfate sodium salt and the sodium alginate is 1:25; the spinning temperature of the melt spinning is 255 ℃, and the spinning speed is 1800m/min.
Example 4
An antistatic functional fiber material is prepared from the following raw materials in parts by weight: 23 parts of fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, 43 parts of polyester chip, 7.5 parts of nano bamboo charcoal powder, 2.5 parts of coupling agent, 4.5 parts of glycerol triglycidyl ether modified aniline trimer, 2.5 parts of 2-ethylhexyl sulfate sodium salt and 3.5 parts of sodium alginate.
The preparation method of the glycerol triglycidyl ether modified aniline trimer comprises the following steps: adding aniline tetramer and glycerol triglycidyl ether into an organic solvent, stirring at 78 ℃ for reaction for 5.5 hours, and removing the solvent by rotary evaporation to obtain glycerol triglycidyl ether modified aniline trimer; the molar ratio of the aniline tetramer to the glycerol triglycidyl ether to the organic solvent is 3:1:19; the organic solvent is N, N-dimethylformamide.
The coupling agent is a mixture formed by mixing a silane coupling agent KH550, a silane coupling agent KH560 and a silane coupling agent KH570 according to a mass ratio of 1:3:2; the granularity of the nano bamboo charcoal powder is 450nm.
The preparation method of the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate comprises the following steps:
s1, uniformly mixing 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent, adding the mixture into a closed reaction kettle provided with a condensation reflux device, replacing air in the kettle with inert gas, reacting for 4.5 hours at the normal pressure and 118 ℃, heating to 248 ℃, carrying out polycondensation reaction under 450Pa for 17 hours, cooling to room temperature, adjusting to normal pressure, washing a precipitated product with ethanol for 6 times, and removing ethanol by rotary evaporation to obtain a 3, 5-isoxazole dicarboxylic acid/N-butyldiethanolamine polycondensate;
and S2, adding the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate and m-fluorobenzyl fluoride prepared in the step S1 into dimethyl sulfoxide, stirring at 75 ℃ for reacting for 5.5 hours, discharging, precipitating in water, washing the precipitated polymer with ethanol for 6 times, and drying in a vacuum drying oven at 93 ℃ until the weight is constant to obtain the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate.
The molar ratio of the 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and the high boiling point solvent in the step S1 is 1:1.1:0.55:14; the high boiling point solvent is sulfolane; the inert gas is argon.
The mass ratio of the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, m-chlorofluorobenzyl and dimethyl sulfoxide in the step S2 is 1:0.35:5.5.
The preparation method of the antistatic functional fiber material comprises the following steps: uniformly mixing the raw materials in parts by weight, adding the mixture into a double-screw extruder for extrusion, carrying out melt spinning to obtain a crude fiber material, soaking the crude fiber material into a mixed aqueous solution of 2-ethylhexyl sulfate sodium salt and sodium alginate at 58 ℃ for 19 hours, taking out the crude fiber material, washing the crude fiber material with water for 6 times, and finally drying the crude fiber material in a vacuum drying oven at 98 ℃ to constant weight to obtain the antistatic functional fiber material; the mass ratio of the 2-ethylhexyl sulfate sodium salt to water in the mixed aqueous solution of the 2-ethylhexyl sulfate sodium salt and the sodium alginate is 1:28; the spinning temperature of the melt spinning is 258 ℃, and the spinning speed is 1900m/min.
Example 5
An antistatic functional fiber material is prepared from the following raw materials in parts by weight: 25 parts of fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, 45 parts of polyester chip, 8 parts of nano bamboo charcoal powder, 3 parts of coupling agent, 5 parts of glycerol triglycidyl ether modified aniline trimer, 3 parts of 2-ethylhexyl sulfate sodium salt and 4 parts of sodium alginate.
The preparation method of the glycerol triglycidyl ether modified aniline trimer comprises the following steps: adding aniline tetramer and glycerol triglycidyl ether into an organic solvent, stirring and reacting for 6 hours at 80 ℃, and removing the solvent by rotary evaporation to obtain glycerol triglycidyl ether modified aniline trimer; the molar ratio of the aniline tetramer to the glycerol triglycidyl ether to the organic solvent is 3:1:20; the organic solvent is N, N-dimethylformamide.
The coupling agent is a silane coupling agent KH550; the granularity of the nano bamboo charcoal powder is 500nm.
The preparation method of the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate comprises the following steps:
s1, uniformly mixing 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent, adding the mixture into a closed reaction kettle provided with a condensation reflux device, replacing air in the kettle with inert gas, reacting at 120 ℃ for 5 hours under normal pressure, heating to 250 ℃, performing polycondensation reaction at 500Pa for 18 hours, cooling to room temperature, adjusting to normal pressure, washing a precipitated product with ethanol for 6 times, and performing rotary evaporation to remove ethanol to obtain a 3, 5-isoxazole dicarboxylic acid/N-butyldiethanolamine polycondensate;
and S2, adding the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate and m-fluorobenzyl fluoride prepared in the step S1 into dimethyl sulfoxide, stirring at 80 ℃ for reaction for 6 hours, discharging, precipitating in water, washing the precipitated polymer with ethanol for 7 times, and drying in a vacuum drying oven at 95 ℃ to constant weight to obtain the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate.
The molar ratio of the 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and the high boiling point solvent in the step S1 is 1:1.2:0.6:15; the high boiling point solvent is sulfolane; the inert gas is nitrogen; the mass ratio of the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, m-chlorofluorobenzyl and dimethyl sulfoxide in the step S2 is 1:0.4:6.
The preparation method of the antistatic functional fiber material comprises the following steps: uniformly mixing the raw materials in parts by weight, adding the mixture into a double-screw extruder for extrusion, carrying out melt spinning to obtain a crude fiber material, soaking the crude fiber material into a mixed aqueous solution of sodium 2-ethylhexyl sulfate at 60 ℃ and sodium alginate for 20 hours, taking out the crude fiber material, washing the crude fiber material with water for 7 times, and finally drying the crude fiber material in a vacuum drying oven at 100 ℃ to constant weight to obtain the antistatic functional fiber material; the mass ratio of the 2-ethylhexyl sulfate sodium salt to water in the mixed aqueous solution of the 2-ethylhexyl sulfate sodium salt and the sodium alginate is 1:30; the spinning temperature of the melt spinning is 260 ℃ and the spinning speed is 2000m/min.
Comparative example 1
An antistatic functional fiber material was substantially the same as in example 1 except that no glycerol triglycidyl ether modified aniline trimer was added.
Comparative example 2
An antistatic functional fiber material was substantially the same as in example 1 except that the raw materials did not include 2-ethylhexyl sulfate sodium salt and sodium alginate.
In order to further illustrate the unexpected positive technical effects obtained by the products of the embodiments of the present invention, the antistatic functional fiber materials prepared by the embodiments are subjected to the related performance test, the test results are shown in table 1, and the test method is as follows: the antistatic functional fiber materials prepared in each example are woven into fabrics, and then tested by referring to the standard method of GB/T12014-89 antistatic working clothes, GB/T12703-1991 brief introduction of Fabric static testing method.
TABLE 1
| Project | Resistivity (. Times.10) 5 Ω·cm) | Resistivity after 30 times of water washing (×10) 5 Ω·cm) |
| Example 1 | 6.5 | 6.7 |
| Example 2 | 6.1 | 6.2 |
| Example 3 | 5.9 | 6.0 |
| Example 4 | 5.4 | 5.4 |
| Example 5 | 4.7 | 4.7 |
| Comparative example 1 | 12.3 | 13.5 |
| Comparative example 2 | 10.8 | 12.6 |
As can be seen from table 1, the antistatic functional fiber material disclosed in the example of the present invention has more excellent antistatic property and washing resistance than the comparative example product; the addition of the glycerol triglycidyl ether modified aniline trimer, the sodium salt of 2-ethylhexyl sulfate and sodium alginate is beneficial to improving the above properties.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention in any way; those of ordinary skill in the art will readily implement the invention as described above; however, those skilled in the art will appreciate that many modifications, adaptations, and variations of the present invention are possible in light of the above teachings without departing from the scope of the invention; meanwhile, any equivalent changes, modifications and evolution of the above embodiments according to the essential technology of the present invention still fall within the scope of the present invention.
Claims (6)
1. The antistatic functional fiber material is characterized by being prepared from the following raw materials in parts by weight: 15-25 parts of fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, 35-45 parts of polyester chips, 5-8 parts of nano bamboo charcoal powder, 1-3 parts of coupling agent, 3-5 parts of glycerol triglycidyl ether modified aniline trimer, 1-3 parts of 2-ethylhexyl sulfate sodium salt and 2-4 parts of sodium alginate;
the preparation method of the glycerol triglycidyl ether modified aniline trimer comprises the following steps: adding aniline tetramer and glycerol triglycidyl ether into an organic solvent, stirring and reacting for 4-6 hours at 70-80 ℃, and then removing the solvent by rotary evaporation to obtain glycerol triglycidyl ether modified aniline trimer; the molar ratio of the aniline tetramer to the glycerol triglycidyl ether to the organic solvent is 3:1 (15-20);
the preparation method of the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate comprises the following steps:
s1, uniformly mixing 3, 5-isoxazole dicarboxylic acid, N-butyldiethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and a high boiling point solvent, adding into a closed reaction kettle provided with a condensation reflux device, replacing air in the kettle with inert gas, reacting for 3-5 hours at the normal pressure of 110-120 ℃, heating to 240-250 ℃, performing polycondensation reaction for 12-18 hours at 300-500Pa, cooling to room temperature, adjusting to normal pressure, washing the precipitated product with ethanol for 3-6 times, and performing rotary evaporation to remove ethanol to obtain a 3, 5-isoxazole dicarboxylic acid/N-butyldiethanolamine polycondensate; the mol ratio of the 3, 5-isoxazole dicarboxylic acid, N-butyl diethanolamine, N-diisopropylethylamine, 4-dimethylaminopyridine and the high boiling point solvent is 1:1 (0.8-1.2): (0.4-0.6): (10-15);
s2, adding the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate and m-fluorobenzyl fluoride prepared in the step S1 into dimethyl sulfoxide, stirring at 60-80 ℃ for reaction for 4-6 hours, discharging and precipitating in water, washing the precipitated polymer with ethanol for 3-7 times, and drying in a vacuum drying oven at 85-95 ℃ to constant weight to obtain the fluorine-containing phenyl ionization modified 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate; the mass ratio of the 3, 5-isoxazole dicarboxylic acid/N-butyl diethanolamine polycondensate, m-fluorochlorobenzyl and dimethyl sulfoxide is 1 (0.2-0.4) (4-6);
the preparation method of the antistatic functional fiber material comprises the following steps: uniformly mixing all the raw materials except the 2-ethylhexyl sulfate sodium salt and the sodium alginate according to parts by weight, adding the raw materials into a double-screw extruder for extrusion, carrying out melt spinning to obtain a crude fiber material, soaking the crude fiber material into a mixed aqueous solution of the 2-ethylhexyl sulfate sodium salt and the sodium alginate at 50-60 ℃ for 10-20 hours, taking out, washing with water for 3-7 times, and finally drying in a vacuum drying oven at 90-100 ℃ to constant weight to obtain the antistatic functional fiber material.
2. An antistatic functional fibrous material according to claim 1 wherein said organic solvent is at least one of N, N-dimethylformamide, N-dimethylacetamide.
3. The antistatic functional fiber material of claim 1, wherein said coupling agent is at least one of silane coupling agent KH550, silane coupling agent KH560, and silane coupling agent KH570; the granularity of the nano bamboo charcoal powder is 300-500nm; the polyester chip is a special chip FC510A for polyester fine denier composite spinning.
4. An antistatic functional fibrous material according to claim 1, wherein said high boiling point solvent is sulfolane; the inert gas is any one of nitrogen, helium, neon and argon.
5. An antistatic functional fiber material according to any one of claims 1 to 4, wherein the mass ratio of the sodium 2-ethylhexyl sulfate to water in the mixed aqueous solution of the sodium 2-ethylhexyl sulfate and sodium alginate is 1 (20 to 30); the spinning temperature of the melt spinning is 250-260 ℃ and the spinning speed is 1500-2000m/min.
6. Use of an antistatic functional fiber material according to any one of claims 1-4 for making antistatic workwear.
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