CN117166113A - Antibacterial skin-friendly fabric - Google Patents
Antibacterial skin-friendly fabric Download PDFInfo
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- CN117166113A CN117166113A CN202311142266.5A CN202311142266A CN117166113A CN 117166113 A CN117166113 A CN 117166113A CN 202311142266 A CN202311142266 A CN 202311142266A CN 117166113 A CN117166113 A CN 117166113A
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- 239000004744 fabric Substances 0.000 title claims abstract description 57
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 97
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 51
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 51
- 241001330002 Bambuseae Species 0.000 claims abstract description 51
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 51
- 239000011425 bamboo Substances 0.000 claims abstract description 51
- 239000003610 charcoal Substances 0.000 claims abstract description 51
- 229920002334 Spandex Polymers 0.000 claims abstract description 49
- 239000004759 spandex Substances 0.000 claims abstract description 49
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 45
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 34
- 239000000835 fiber Substances 0.000 claims abstract description 34
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 32
- 238000002360 preparation method Methods 0.000 claims abstract description 22
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- QAFBDRSXXHEXGB-UHFFFAOYSA-N imidazol-1-ylacetic acid Chemical compound OC(=O)CN1C=CN=C1 QAFBDRSXXHEXGB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000945 filler Substances 0.000 claims abstract description 4
- 238000005576 amination reaction Methods 0.000 claims abstract description 3
- 238000009987 spinning Methods 0.000 claims description 32
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 20
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 20
- 239000004814 polyurethane Substances 0.000 claims description 20
- 229920002635 polyurethane Polymers 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000009941 weaving Methods 0.000 claims description 11
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 230000015271 coagulation Effects 0.000 claims description 10
- 238000005345 coagulation Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 10
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 10
- 238000002166 wet spinning Methods 0.000 claims description 10
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical group CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- BCMYXYHEMGPZJN-UHFFFAOYSA-N 1-chloro-2-isocyanatoethane Chemical compound ClCCN=C=O BCMYXYHEMGPZJN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002131 composite material Substances 0.000 claims description 5
- 238000009832 plasma treatment Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- QOSSAOTZNIDXMA-UHFFFAOYSA-N Dicylcohexylcarbodiimide Chemical compound C1CCCCC1N=C=NC1CCCCC1 QOSSAOTZNIDXMA-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 4
- 235000012239 silicon dioxide Nutrition 0.000 claims 3
- 238000001816 cooling Methods 0.000 claims 2
- 238000002156 mixing Methods 0.000 claims 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims 2
- 239000005543 nano-size silicon particle Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 26
- 230000000694 effects Effects 0.000 abstract description 12
- 230000003712 anti-aging effect Effects 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 3
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 22
- 238000010521 absorption reaction Methods 0.000 description 15
- 238000012360 testing method Methods 0.000 description 12
- 241000238876 Acari Species 0.000 description 7
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- 239000011159 matrix material Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 230000005611 electricity Effects 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- -1 imidazolyl quaternary ammonium salt Chemical class 0.000 description 3
- 125000000879 imine group Chemical group 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 125000004185 ester group Chemical group 0.000 description 2
- 238000007306 functionalization reaction Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 210000004243 sweat Anatomy 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
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- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 238000004113 cell culture Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000005956 quaternization reaction Methods 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical group O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
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- 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
Landscapes
- Artificial Filaments (AREA)
Abstract
本发明涉及面料制备技术领域,公开了一种抗菌亲肤面料,该种抗菌亲肤面料是以抗氧化竹炭微粉与功能化二氧化硅作为填料,制备出氨纶纤维再织造而成;其中,抗氧化竹炭微粉是将竹炭微粉氨基化再接枝3‑(3,5‑二叔丁基‑4‑羟苯基)丙酸制得;功能化二氧化硅是对纳米二氧化硅表面改性后再接枝咪唑‑1‑乙酸制得。本发明所织造的面料具有吸湿性好、排汗透气、柔软亲肤、拉伸强度高的特点,具有极佳的穿着舒适度与易加工性能,该面料还具有优异的杀菌除螨效果、耐老化以及抗静电的性能,并且能够长效稳定的发挥作用,应用领域十分广泛。
The invention relates to the technical field of fabric preparation and discloses an antibacterial and skin-friendly fabric. The antibacterial and skin-friendly fabric is made of spandex fiber prepared using antioxidant bamboo charcoal micropowder and functionalized silica as fillers and then woven into it; wherein, the antibacterial and skin-friendly fabric is Oxidized bamboo charcoal powder is produced by amination of bamboo charcoal powder and then grafted with 3-(3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid; functionalized silica is produced by modifying the surface of nano-silica. Prepared by grafting imidazole-1-acetic acid. The fabric woven by the invention has the characteristics of good hygroscopicity, perspiration and breathability, softness and skin-friendlyness, and high tensile strength. It has excellent wearing comfort and easy processing performance. The fabric also has excellent sterilization and mite removal effect, and is durable and durable. It has anti-aging and anti-static properties and can function stably for a long time. It has a wide range of applications.
Description
技术领域Technical field
本发明涉及面料制备技术领域,具体涉及一种抗菌亲肤面料。The invention relates to the technical field of fabric preparation, and in particular to an antibacterial and skin-friendly fabric.
背景技术Background technique
在历史长河中,面料一直是人类生活不可或缺的一部分,它不仅决定了服装的舒适度和美观度,还反映了时代科技的进步和文化的发展,以往面料大多由天然纤维织造而成,如今化学纤维面料也占据了一席之地,其中,氨纶面料由于其具有独特的高弹性以及柔软性使其成为制作贴身衣物的不二之选,但是贴身衣物直接接触人体很容易就会沾染上汗液,如果不能及时排出会粘在皮肤表面,影响舒适度,并且潮湿的环境中更容易导致细菌和螨虫的滋生,从而影响到皮肤的健康,除了会接触到汗液之外,长时间的摩擦也会导致静电的产生,导致衣物紧贴身体影响美观,静电的存在还容易导致细菌在衣物表面聚集,所以,这就使得氨纶面料需要具备透气吸湿、抗菌除螨以及抗静电的性能,又因为氨纶面料分子中存在氢键,容易被氧化变形,所以,氨纶面料还需要具有抗氧化的性能。Throughout history, fabrics have always been an indispensable part of human life. It not only determines the comfort and beauty of clothing, but also reflects the technological progress and cultural development of the times. In the past, fabrics were mostly woven from natural fibers. Nowadays, chemical fiber fabrics also occupy a place. Among them, spandex fabric has become the best choice for making underwear due to its unique high elasticity and softness. However, underwear can easily be contaminated with sweat if it comes into direct contact with the human body. If it is not discharged in time, it will stick to the surface of the skin, affecting comfort, and a humid environment is more likely to cause bacteria and mites to breed, thus affecting the health of the skin. In addition to contact with sweat, long-term friction can also cause static electricity. The production of clothes causes the clothes to stick closely to the body and affects the appearance. The existence of static electricity can also easily cause bacteria to accumulate on the surface of clothes. Therefore, this requires spandex fabrics to have the properties of breathability, moisture absorption, antibacterial and mite removal, and antistatic properties. Moreover, because the molecules in spandex fabrics There are hydrogen bonds and are easily deformed by oxidation. Therefore, spandex fabrics also need to have antioxidant properties.
公开号为CN112266462B的专利公开了一种耐老化弹性面料及其制备方法,该专利通过对氨纶进行改性,在其结构中引入了由季戊四醇起始的聚醚多元醇,增强所制备氨纶纤维的交联程度,从而使氨纶的分子结构更为稳定,提升氨纶纤维的耐老化性能,同时加入三甘醇,使得制备的氨纶纤维还具有优异的弹性,该专利虽然能够提升氨纶的耐老化性能,但是没有抗菌除螨的能力以及抗静电的效果,在作为贴身衣服使用时,容易造成细菌聚集影响到人的身体健康。The patent with publication number CN112266462B discloses an aging-resistant elastic fabric and its preparation method. The patent modifies spandex and introduces polyether polyol starting from pentaerythritol into its structure to enhance the elasticity of the prepared spandex fiber. The degree of cross-linking makes the molecular structure of spandex more stable and improves the aging resistance of spandex fiber. At the same time, adding triethylene glycol makes the prepared spandex fiber also have excellent elasticity. Although this patent can improve the aging resistance of spandex, However, it does not have antibacterial and mite removal capabilities and antistatic effects. When used as underwear, it can easily cause bacteria to accumulate and affect people's health.
发明内容Contents of the invention
本发明的目的在于提供一种抗菌亲肤面料,解决了以下几点技术问题:(1)传统氨纶面料抗氧化性差,长时间使用时氨纶纤维容易被老化断裂的问题;(2)氨纶面料容易产生静电导致细菌粘附,螨虫滋生的问题;(3)氨纶面料透气吸湿性能差,舒适度不高的问题。The purpose of the present invention is to provide an antibacterial and skin-friendly fabric that solves the following technical problems: (1) The traditional spandex fabric has poor oxidation resistance and the spandex fiber is easily aged and broken when used for a long time; (2) The spandex fabric is easily The generation of static electricity leads to the adhesion of bacteria and the breeding of mites; (3) The problem of poor breathability and moisture absorption of spandex fabrics and low comfort.
本发明的目的可以通过以下技术方案实现:The object of the present invention can be achieved through the following technical solutions:
一种抗菌亲肤面料,是以抗氧化竹炭微粉与功能化二氧化硅作为填料,制备出氨纶纤维再织造而成;所述抗氧化竹炭微粉是将竹炭微粉氨基化再接枝3-(3,5-二叔丁基-4-羟苯基)丙酸制得;所述功能化二氧化硅是对纳米二氧化硅表面改性后再接枝咪唑-1-乙酸制得。An antibacterial and skin-friendly fabric is made from spandex fiber prepared by using antioxidant bamboo charcoal micropowder and functionalized silica as fillers and then woven into it; the antioxidant bamboo charcoal micropowder is made by amination of bamboo charcoal micropowder and then grafted with 3-(3 , 5-di-tert-butyl-4-hydroxyphenyl)propionic acid is prepared; the functionalized silica is prepared by modifying the surface of nano-silica and then grafting imidazole-1-acetic acid.
进一步地,所述抗氧化竹炭微粉的制备方法,包括以下步骤:Further, the preparation method of the antioxidant bamboo charcoal micropowder includes the following steps:
(1)将竹炭微粉置于等离子处理腔中,通入氨气处理10-15min,取出后得到氨基化竹炭微粉;(1) Place the bamboo charcoal powder in the plasma treatment chamber, pass in ammonia gas for 10-15 minutes, and then take it out to obtain the aminated bamboo charcoal powder;
(2)将氨基化竹炭微粉置于乙醇中,超声分散5-10min后,加入3-(3,5-二叔丁基-4-羟苯基)丙酸与复合催化剂,升温至50-70℃反应5-8h,过滤、洗涤、真空干燥后得到抗氧化竹炭微粉。(2) Place aminated bamboo charcoal powder in ethanol, disperse it ultrasonically for 5-10 minutes, add 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid and composite catalyst, and raise the temperature to 50-70 React at ℃ for 5-8 hours, filter, wash, and vacuum dry to obtain antioxidant bamboo charcoal powder.
通过上述技术方案,在等离子处理腔中使用氨气对竹炭微粉表面氨基化,在复合催化剂的作用下,竹炭微粉表面的氨基与3-(3,5-二叔丁基-4-羟苯基)丙酸结构中的羧基发生反应,得到抗氧化竹炭微粉,该种抗氧化竹炭微粉表面接枝有亚胺基团能够使其在氨纶中均匀分散,同时还接枝有具有抗氧化效果的受阻酚基团,能够降低氨纶在长时间使用时由于老化产生断裂的可能性,延长氨纶的使用寿命,并且该种抗氧化竹炭微粉还具有丰富的孔隙结构,能够吸收并蒸发大量的水分,具有良好的吸湿排汗作用,其结构中的竹醌因子具有一定的抗菌除螨作用,能够有效的杀灭细菌与螨虫,并且成分安全不会对皮肤造成刺激性。Through the above technical solution, ammonia gas is used in the plasma treatment chamber to aminate the surface of bamboo charcoal powder. Under the action of the composite catalyst, the amino groups on the surface of bamboo charcoal powder react with 3-(3,5-di-tert-butyl-4-hydroxyphenyl). ) The carboxyl group in the propionic acid structure reacts to obtain antioxidant bamboo charcoal powder. The surface of this antioxidant bamboo charcoal powder is grafted with imine groups to enable it to be evenly dispersed in spandex. At the same time, it is also grafted with hindered substances with antioxidant effects. The phenol group can reduce the possibility of breakage of spandex due to aging during long-term use, extending the service life of spandex. Moreover, this antioxidant bamboo charcoal powder also has a rich pore structure, can absorb and evaporate a large amount of water, and has good It has moisture absorption and perspiration effect, and the bambooquinone factor in its structure has a certain antibacterial and mite removal effect, which can effectively kill bacteria and mites, and the ingredients are safe and will not cause irritation to the skin.
进一步地,步骤(1)中,所述等离子处理腔的功率为100-150W,大气压为2-5Pa。Further, in step (1), the power of the plasma processing chamber is 100-150W, and the atmospheric pressure is 2-5Pa.
进一步地,步骤(2)中,所述复合催化剂为质量比为3-6:1-2的4-二甲氨基吡啶与二环己基碳二亚胺。Further, in step (2), the composite catalyst is 4-dimethylaminopyridine and dicyclohexylcarbodiimide with a mass ratio of 3-6:1-2.
进一步地,所述功能化二氧化硅的制备方法,包括以下步骤:Further, the preparation method of functionalized silica includes the following steps:
S1:将纳米二氧化硅置于去离子水中,超声分散15-20min后,加入氯乙基异氰酸酯与催化剂,升温至65-75℃反应3-5h,过滤、洗涤、真空干燥后得到改性二氧化硅;S1: Place the nanosilica in deionized water, disperse it ultrasonically for 15-20 minutes, add chloroethyl isocyanate and catalyst, raise the temperature to 65-75°C, react for 3-5 hours, filter, wash, and vacuum dry to obtain the modified silicon dioxide. silicon oxide;
S2:将改性二氧化硅置于去离子水中,加入咪唑-1-乙酸并混合均匀,回流反应,降至室温,过滤、洗涤、真空干燥后得到功能化二氧化硅。S2: Place the modified silica in deionized water, add imidazole-1-acetic acid and mix evenly, reflux and react, lower to room temperature, filter, wash, and vacuum dry to obtain functionalized silica.
通过上述技术方案,在催化剂的作用下,使用氯乙基异氰酸酯结构中的异氰酸酯基团对二氧化硅表面进行改性,得到改性二氧化硅,再通过改性二氧化硅表面的活性氯与咪唑-1-乙酸结构中的咪唑基团发生季铵化反应,得到功能化二氧化硅,该种功能化二氧化硅表面具有活性羧基,能够均匀的分散在氨纶的基体中,解决了功能化二氧化硅在基体中容易团聚的问题,使其能够增强氨纶的力学性能,提高氨纶的拉伸强度,该种功能化二氧化硅表面形成的咪唑基季铵盐具有优异的抗菌性能,与氨纶结合后能够显著提高氨纶的抗菌能力和柔软度,即便长时间使用时抗菌物质也不会析出,具有长久的抗菌效果,同时能够在氨纶表面形成吸附膜,有利于静电的逸散,从而使制备的面料还具有优异的抗静电作用,能够防止由于静电的吸附导致细菌聚集,对人体造成的不利影响。Through the above technical solution, under the action of a catalyst, the isocyanate group in the chloroethyl isocyanate structure is used to modify the silica surface to obtain modified silica, and then the active chlorine on the modified silica surface is combined with The imidazole group in the imidazole-1-acetic acid structure undergoes a quaternization reaction to obtain functionalized silica. This functionalized silica has active carboxyl groups on its surface and can be evenly dispersed in the spandex matrix, solving the problem of functionalization. The problem of easy agglomeration of silica in the matrix makes it possible to enhance the mechanical properties of spandex and improve the tensile strength of spandex. The imidazolyl quaternary ammonium salt formed on the surface of this functionalized silica has excellent antibacterial properties and is similar to spandex. After combining, it can significantly improve the antibacterial ability and softness of spandex. Antibacterial substances will not precipitate even when used for a long time, and has a long-lasting antibacterial effect. At the same time, it can form an adsorption film on the surface of spandex, which is conducive to the dissipation of static electricity, thus making the preparation The fabric also has excellent antistatic effect, which can prevent the accumulation of bacteria due to static adsorption and adverse effects on the human body.
进一步地,步骤S1中,所述催化剂为辛酸亚锡、二月桂酸二丁基锡中的任意一种。Further, in step S1, the catalyst is any one of stannous octoate and dibutyltin dilaurate.
进一步地,步骤S2中,所述回流反应温度为80-90℃,时间为24-48h。Further, in step S2, the reflux reaction temperature is 80-90°C and the time is 24-48h.
进一步地,所述抗菌亲肤面料的制备方法,包括以下步骤:Further, the preparation method of the antibacterial skin-friendly fabric includes the following steps:
步骤一、将甲苯二异氰酸酯、聚四氢呋喃醚二醇混合,通入氮气,加入二月桂酸二丁基锡,搅拌至混合均匀,升温至45-55℃反应1-2h,加入1,4-丁二醇,继续升温至70-80℃反应2-3h,降温至40-45℃加入三乙胺、功能化二氧化硅与抗氧化竹炭微粉,反应1-3h后,加入去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix toluene diisocyanate and polytetrahydrofuran ether glycol, add nitrogen, add dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 45-55°C, react for 1-2 hours, and add 1,4-butanediol. , continue to raise the temperature to 70-80℃ and react for 2-3h, then cool to 40-45℃ and add triethylamine, functionalized silica and antioxidant bamboo charcoal powder. After reacting for 1-3h, add deionized water, stir thoroughly and let it cool naturally. After defoaming, polyurethane is obtained;
步骤二、将聚氨酯加入N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速并进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning liquid. Control the flow rate of the spinning liquid and perform wet spinning. After the spinning liquid passes through the spinneret, add it to distilled water. In the coagulation bath, and then through stretching, traction, drying and winding, spandex fiber is obtained;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
进一步地,步骤二中,所述纺丝液流速为0.4-0.8m l/h。Further, in step two, the flow rate of the spinning solution is 0.4-0.8ml/h.
本发明的有益效果:Beneficial effects of the present invention:
本发明通过制备抗氧化竹炭微粉与功能化二氧化硅作为填料制备氨纶纤维并织造成面料,所织造的面料具有吸湿性好、排汗透气、柔软亲肤、拉伸强度高的特点,具有极佳的穿着舒适度与易加工性能,该面料还具有优异的杀菌除螨效果、耐老化以及抗静电的性能,并且能够长效稳定的发挥作用,应用领域十分广泛。In the present invention, spandex fibers are prepared by preparing antioxidant bamboo charcoal micropowder and functionalized silica as fillers and woven into fabrics. The woven fabrics have the characteristics of good hygroscopicity, perspiration wicking, breathability, softness and skin-friendlyness, and high tensile strength, and have extremely high tensile strength. It has excellent wearing comfort and easy processing properties. The fabric also has excellent sterilization and mite removal effects, aging resistance and antistatic properties. It can function stably for a long time and has a wide range of applications.
当然,实施本发明的任一产品并不一定需要同时达到以上所述的所有优点。Of course, any product implementing the present invention does not necessarily need to achieve all the above-mentioned advantages at the same time.
附图说明Description of drawings
为了更清楚地说明本发明实施例的技术方案,下面将对实施例描述所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to explain the technical solutions of the embodiments of the present invention more clearly, the drawings needed to describe the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other drawings can also be obtained based on these drawings without exerting creative efforts.
图1为本发明实施例1中抗氧化竹炭微粉的红外光谱图;Figure 1 is an infrared spectrum of the antioxidant bamboo charcoal micropowder in Example 1 of the present invention;
图2为本发明实施例1中,纳米二氧化硅、改性二氧化硅、功能化二氧化硅的热失重曲线图。Figure 2 is a graph of thermal weight loss curves of nanosilica, modified silica, and functionalized silica in Example 1 of the present invention.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts fall within the scope of protection of the present invention.
实施例1Example 1
一、抗氧化竹炭微粉的制备1. Preparation of antioxidant bamboo charcoal micropowder
(1)将2g竹炭微粉置于功率为100W、大气压为2Pa的等离子处理腔中,通入氨气处理10min,取出后得到氨基化竹炭微粉;(1) Place 2g of bamboo charcoal powder in a plasma treatment chamber with a power of 100W and an atmospheric pressure of 2Pa, and introduce ammonia gas for 10 minutes. After taking it out, aminated bamboo charcoal powder is obtained;
(2)将2g氨基化竹炭微粉置于80m l乙醇中,超声分散5min后,加入1.5g的3-(3,5-二叔丁基-4-羟苯基)丙酸、0.06g的二环己基碳二亚胺与0.02g的4-二甲氨基吡啶,升温至50℃反应5h,过滤、洗涤、真空干燥后得到抗氧化竹炭微粉。(2) Place 2g of aminated bamboo charcoal powder in 80ml of ethanol, disperse it ultrasonically for 5 minutes, then add 1.5g of 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid and 0.06g of di- Cyclohexylcarbodiimide and 0.02g of 4-dimethylaminopyridine were heated to 50°C to react for 5 hours, followed by filtration, washing, and vacuum drying to obtain antioxidant bamboo charcoal micropowder.
通过红外光谱对抗氧化竹炭微粉进行表征,如图1所示,3392cm-1处出现了亚胺基团中氮氢键的吸收峰,3245cm-1处出现羟基的吸收峰,3021cm-1处为苯环中碳氢键的吸收峰,2914cm-1处为甲基中碳氢键的吸收峰,1716cm-1处为酯基中碳氧双键的吸收峰,亚胺基团与酯基吸收峰的出现说明氨基化竹炭微粉表面的氨基与3-(3,5-二叔丁基-4-羟苯基)丙酸结构中的羧基发生了反应。The antioxidant bamboo charcoal micropowder was characterized by infrared spectrum. As shown in Figure 1, the absorption peak of the nitrogen-hydrogen bond in the imine group appeared at 3392cm -1 , the absorption peak of the hydroxyl group appeared at 3245cm -1 , and the absorption peak of benzene appeared at 3021cm -1 The absorption peak of the carbon-hydrogen bond in the ring is the absorption peak of the carbon-hydrogen bond in the methyl group at 2914cm -1 , the absorption peak of the carbon-oxygen double bond in the ester group is at 1716cm -1 , and the absorption peak of the imine group and the ester group is The appearance indicates that the amino group on the surface of aminated bamboo charcoal powder reacted with the carboxyl group in the 3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid structure.
二、功能化二氧化硅的制备2. Preparation of functionalized silica
S1:将1.5g纳米二氧化硅置于100m l去离子水中,超声分散15min后,加入1g氯乙基异氰酸酯与0.1g辛酸亚锡,升温至65℃反应3h,过滤、洗涤、真空干燥后得到改性二氧化硅;S1: Place 1.5g nanometer silica in 100ml deionized water, disperse it ultrasonically for 15 minutes, add 1g chloroethyl isocyanate and 0.1g stannous octoate, raise the temperature to 65°C, react for 3 hours, filter, wash and vacuum dry to obtain modified silica;
S2:将2g改性二氧化硅置于150m l去离子水中,加入1g咪唑-1-乙酸并混合均匀,升温至80℃回流反应24h,降至室温,过滤、洗涤、真空干燥后得到功能化二氧化硅。S2: Place 2g modified silica in 150ml deionized water, add 1g imidazole-1-acetic acid and mix evenly, raise the temperature to 80°C and reflux for 24 hours, lower to room temperature, filter, wash and vacuum dry to obtain functionalization Silica.
通过热失重分析法对纳米二氧化硅、改性二氧化硅、功能化二氧化硅进行表征,由图2可以看出,纳米二氧化硅在800℃的高温下最终质量保持率为98.2%,损失的部分是由于其结构中的结晶水蒸发导致;改性二氧化硅最终质量保持率为56.7%,损失的部分是由于其表面接枝的氯乙基异氰酸酯分解导致;功能化二氧化硅最终质量保持率为37.6%,损失的部分是由于二氧化硅表面接枝的有机物分解导致。Nano-silica, modified silica, and functionalized silica were characterized by thermogravimetric analysis. As can be seen from Figure 2, the final mass retention rate of nano-silica at a high temperature of 800°C was 98.2%. Part of the loss is due to the evaporation of crystal water in its structure; the final quality retention rate of modified silica is 56.7%, and part of the loss is due to the decomposition of chloroethyl isocyanate grafted on its surface; the final quality of functionalized silica The mass retention rate is 37.6%, and part of the loss is due to the decomposition of organic matter grafted on the silica surface.
三、抗菌亲肤面料的制备3. Preparation of antibacterial and skin-friendly fabrics
步骤一、将10m l甲苯二异氰酸酯、8m l聚四氢呋喃醚二醇混合,通入氮气,加入0.1g二月桂酸二丁基锡,搅拌至混合均匀,升温至45℃反应1h,加入1m l的1,4-丁二醇,继续升温至70℃反应2h,降温至40℃加入1.5m l三乙胺、1.5g功能化二氧化硅与2g抗氧化竹炭微粉,反应1h后,加入10m l去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix 10ml of toluene diisocyanate and 8ml of polytetrahydrofuran ether glycol, add nitrogen, add 0.1g of dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 45°C and react for 1 hour, add 1ml of 1, 4-Butanediol, continue to raise the temperature to 70°C for 2 hours, then cool to 40°C and add 1.5ml triethylamine, 1.5g functionalized silica and 2g antioxidant bamboo charcoal powder. After 1 hour of reaction, add 10ml deionized water. Polyurethane is obtained after thorough stirring and natural defoaming;
步骤二、将聚氨酯加入50m l的N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速为0.4m l/h进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to 50ml of N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning solution. Control the flow rate of the spinning solution to 0.4ml/h for wet spinning. The spinning solution is sprayed After the silk board is formed, it is added to the distilled water coagulation bath, and then stretched, dried, and wound to obtain spandex fiber;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
实施例2Example 2
抗菌亲肤面料的制备Preparation of antibacterial and skin-friendly fabrics
步骤一、将12m l甲苯二异氰酸酯、10m l聚四氢呋喃醚二醇混合,通入氮气,加入0.2g二月桂酸二丁基锡,搅拌至混合均匀,升温至50℃反应1.5h,加入1.5m l的1,4-丁二醇,继续升温至75℃反应2.5h,降温至42℃加入2m l三乙胺、2g功能化二氧化硅与2.5g抗氧化竹炭微粉,反应2h后,加入12m l去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix 12ml of toluene diisocyanate and 10ml of polytetrahydrofuran ether glycol, add nitrogen, add 0.2g of dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 50°C and react for 1.5h, add 1.5ml of 1 , 4-butanediol, continue to raise the temperature to 75°C and react for 2.5h, then cool to 42°C and add 2ml triethylamine, 2g functionalized silica and 2.5g antioxidant bamboo charcoal powder. After 2h of reaction, add 12ml deionized water, stir thoroughly and defoam naturally to obtain polyurethane;
步骤二、将聚氨酯加入60m l的N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速为0.6m l/h,并进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to 60ml of N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning solution. Control the flow rate of the spinning solution to 0.6ml/h, and perform wet spinning. The spinning solution After passing through the spinneret, it is added to the distilled water coagulation bath, and then stretched, dried, and wound to obtain spandex fiber;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
其中,抗氧化竹炭微粉与功能化二氧化硅的制备方法与实施例1相同。Among them, the preparation method of antioxidant bamboo charcoal micropowder and functionalized silica is the same as in Example 1.
实施例3Example 3
抗菌亲肤面料的制备Preparation of antibacterial and skin-friendly fabrics
步骤一、将15m l的甲苯二异氰酸酯、12m l聚四氢呋喃醚二醇混合,通入氮气,加入0.3g二月桂酸二丁基锡,搅拌至混合均匀,升温至55℃反应2h,加入2m l的1,4-丁二醇,继续升温至80℃反应3h,降温至45℃加入2.5m l三乙胺、2.5g功能化二氧化硅与3g抗氧化竹炭微粉,反应3h后,加入15m l去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix 15ml of toluene diisocyanate and 12ml of polytetrahydrofuran ether glycol, add nitrogen, add 0.3g of dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 55°C and react for 2 hours, add 2ml of 1 , 4-butanediol, continue to raise the temperature to 80°C for 3 hours, then cool to 45°C and add 2.5ml triethylamine, 2.5g functionalized silica and 3g antioxidant bamboo charcoal powder. After 3 hours of reaction, add 15ml deionized water. , polyurethane is obtained after thorough stirring and natural defoaming;
步骤二、将聚氨酯加入80m l的N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速为0.8m l/h,并进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to 80ml of N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning solution. Control the flow rate of the spinning solution to 0.8ml/h, and perform wet spinning. The spinning solution After passing through the spinneret, it is added to the distilled water coagulation bath, and then stretched, dried, and wound to obtain spandex fiber;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
其中,抗氧化竹炭微粉与功能化二氧化硅的制备方法与实施例1相同。Among them, the preparation method of antioxidant bamboo charcoal micropowder and functionalized silica is the same as in Example 1.
对比例1Comparative example 1
面料的制备fabric preparation
步骤一、将12m l甲苯二异氰酸酯、10m l聚四氢呋喃醚二醇混合,通入氮气,加入0.2g二月桂酸二丁基锡,搅拌至混合均匀,升温至50℃反应1.5h,加入1.5m l的1,4-丁二醇,继续升温至75℃反应2.5h,降温至42℃加入2m l三乙胺、2g功能化二氧化硅,反应2h后,加入12m l去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix 12ml of toluene diisocyanate and 10ml of polytetrahydrofuran ether glycol, add nitrogen, add 0.2g of dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 50°C and react for 1.5h, add 1.5ml of 1 , 4-butanediol, continue to raise the temperature to 75°C and react for 2.5 hours. Cool to 42°C and add 2ml triethylamine and 2g functionalized silica. After 2 hours of reaction, add 12ml deionized water, stir thoroughly and naturally eliminate After soaking, polyurethane is obtained;
步骤二、将聚氨酯加入60m l的N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速为0.6m l/h,并进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to 60ml of N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning solution. Control the flow rate of the spinning solution to 0.6ml/h, and perform wet spinning. The spinning solution After passing through the spinneret, it is added to the distilled water coagulation bath, and then stretched, dried, and wound to obtain spandex fiber;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
其中,功能化二氧化硅的制备方法与实施例1相同。The preparation method of functionalized silica is the same as in Example 1.
对比例2Comparative example 2
步骤一、将12m l甲苯二异氰酸酯、10m l聚四氢呋喃醚二醇混合,通入氮气,加入0.2g二月桂酸二丁基锡,搅拌至混合均匀,升温至50℃反应1.5h,加入1.5m l的1,4-丁二醇,继续升温至75℃反应2.5h,降温至42℃加入2m l三乙胺、2.5g抗氧化竹炭微粉,反应2h后,加入12m l去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix 12ml of toluene diisocyanate and 10ml of polytetrahydrofuran ether glycol, add nitrogen, add 0.2g of dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 50°C and react for 1.5h, add 1.5ml of 1 , 4-butanediol, continue to raise the temperature to 75°C and react for 2.5h, cool to 42°C and add 2ml triethylamine and 2.5g antioxidant bamboo charcoal powder. After reacting for 2h, add 12ml deionized water, stir thoroughly and naturally sterilize. After soaking, polyurethane is obtained;
步骤二、将聚氨酯加入60m l的N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速为0.6m l/h,并进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to 60ml of N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning solution. Control the flow rate of the spinning solution to 0.6ml/h, and perform wet spinning. The spinning solution After passing through the spinneret, it is added to the distilled water coagulation bath, and then stretched, dried, and wound to obtain spandex fiber;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
其中,抗氧化竹炭微粉的制备方法与实施例1相同。Among them, the preparation method of antioxidant bamboo charcoal micropowder is the same as that in Example 1.
对比例3Comparative example 3
步骤一、将12m l甲苯二异氰酸酯、10m l聚四氢呋喃醚二醇混合,通入氮气,加入0.2g二月桂酸二丁基锡,搅拌至混合均匀,升温至50℃反应1.5h,加入1.5m l的1,4-丁二醇,继续升温至75℃反应2.5h,降温至42℃加入2m l三乙胺,反应2h后,加入12m l去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix 12ml of toluene diisocyanate and 10ml of polytetrahydrofuran ether glycol, add nitrogen, add 0.2g of dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 50°C and react for 1.5h, add 1.5ml of 1 , 4-butanediol, continue to raise the temperature to 75°C and react for 2.5h, cool to 42°C and add 2ml triethylamine. After reacting for 2h, add 12ml deionized water, stir thoroughly and defoam naturally to obtain polyurethane;
步骤二、将聚氨酯加入60m l的N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速为0.6m l/h,并进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to 60ml of N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning solution. Control the flow rate of the spinning solution to 0.6ml/h, and perform wet spinning. The spinning solution After passing through the spinneret, it is added to the distilled water coagulation bath, and then stretched, dried, and wound to obtain spandex fiber;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
对比例4Comparative example 4
步骤一、将12m l甲苯二异氰酸酯、10m l聚四氢呋喃醚二醇混合,通入氮气,加入0.2g二月桂酸二丁基锡,搅拌至混合均匀,升温至50℃反应1.5h,加入1.5m l的1,4-丁二醇,继续升温至75℃反应2.5h,降温至42℃加入2m l三乙胺、2g功能化二氧化硅与2.5g竹炭微粉,反应2h后,加入12m l去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix 12ml of toluene diisocyanate and 10ml of polytetrahydrofuran ether glycol, add nitrogen, add 0.2g of dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 50°C and react for 1.5h, add 1.5ml of 1 , 4-butanediol, continue to raise the temperature to 75°C and react for 2.5h, cool to 42°C and add 2ml triethylamine, 2g functionalized silica and 2.5g bamboo charcoal powder. After 2h of reaction, add 12ml deionized water. Polyurethane is obtained after thorough stirring and natural defoaming;
步骤二、将聚氨酯加入60m l的N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速为0.6m l/h,并进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to 60ml of N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning solution. Control the flow rate of the spinning solution to 0.6ml/h, and perform wet spinning. The spinning solution After passing through the spinneret, it is added to the distilled water coagulation bath, and then stretched, dried, and wound to obtain spandex fiber;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
其中,功能化二氧化硅的制备方法与实施例1相同。The preparation method of functionalized silica is the same as in Example 1.
对比例5Comparative example 5
步骤一、将12m l甲苯二异氰酸酯、10m l聚四氢呋喃醚二醇混合,通入氮气,加入0.2g二月桂酸二丁基锡,搅拌至混合均匀,升温至50℃反应1.5h,加入1.5m l的1,4-丁二醇,继续升温至75℃反应2.5h,降温至42℃加入2m l三乙胺、2g纳米二氧化硅与2.5g抗氧化竹炭微粉,反应2h后,加入12m l去离子水,充分搅拌并自然消泡后得到聚氨酯;Step 1. Mix 12ml of toluene diisocyanate and 10ml of polytetrahydrofuran ether glycol, add nitrogen, add 0.2g of dibutyltin dilaurate, stir until evenly mixed, raise the temperature to 50°C and react for 1.5h, add 1.5ml of 1 , 4-butanediol, continue to raise the temperature to 75°C and react for 2.5h, then cool to 42°C and add 2ml triethylamine, 2g nano-silica and 2.5g antioxidant bamboo charcoal powder. After 2h of reaction, add 12ml deionized water. , polyurethane is obtained after thorough stirring and natural defoaming;
步骤二、将聚氨酯加入60m l的N,N-二甲基乙酰胺中,充分搅拌静置形成纺丝液,控制纺丝液流速为0.6m l/h,并进行湿法纺丝,纺丝液经过喷丝板后,加入至蒸馏水凝固浴中,然后经过拉伸牵引、干燥、卷绕,得到氨纶纤维;Step 2: Add polyurethane to 60ml of N,N-dimethylacetamide, stir thoroughly and let it stand to form a spinning solution. Control the flow rate of the spinning solution to 0.6ml/h, and perform wet spinning. The spinning solution After passing through the spinneret, it is added to the distilled water coagulation bath, and then stretched, dried, and wound to obtain spandex fiber;
步骤三、将氨纶纤维经过加捻、定捻、整经、穿综后上机织造,完成后得到面料。Step 3: The spandex fiber is twisted, fixed, warped, and drawn on the machine for weaving, and the fabric is obtained after completion.
其中,抗氧化竹炭微粉的制备方法与实施例1相同。Among them, the preparation method of antioxidant bamboo charcoal micropowder is the same as that in Example 1.
性能检测Performance testing
①将实施例1-实施例3,对比例1-对比例5制备出来的面料制成符合规格的样品,参考标准GB/T5453-1997《纺织品织物透气性测试》对样品进行透气性的测试;参考标准GB/T12704.1-2009《纺织品织物透湿性试验方法第1部分:吸湿法》测试样品吸湿性能;使用DRK321 B-I I表面电阻率测试仪测试样品表面的电阻率,判断其抗静电能力;参考标准GB/T14337-2022《化学纤维短纤维拉伸性能试验方法》,将样品和经过90℃老化箱高温处理24h后的样品,通过万能材料试验机测试其拉伸强度,判断其力学性能以及抗老化能力,具体检测结果见下表:①Make the fabrics prepared in Example 1 to Example 3 and Comparative Example 1 to Comparative Example 5 into samples that meet the specifications, and conduct a breathability test on the samples with reference to the standard GB/T5453-1997 "Textile Fabric Breathability Test"; Refer to the standard GB/T12704.1-2009 "Test Method for Moisture Permeability of Textile Fabrics Part 1: Moisture Absorption Method" to test the moisture absorption performance of the sample; use the DRK321 B-I I surface resistivity tester to test the resistivity of the sample surface to determine its antistatic ability; Referring to the standard GB/T14337-2022 "Test Method for Tensile Properties of Chemical Fiber Short Fibers", test the tensile strength of the sample and the sample after high temperature treatment in a 90°C aging oven for 24 hours through a universal material testing machine to determine its mechanical properties and Anti-aging ability, specific test results are shown in the table below:
由上表可知,实施例1-实施例3制备的样品在透气、吸湿、抗静电、抗老化以及力学性能上均处于较高的水平,对比例1制备的样品没有添加抗氧化竹炭微粉,所以在抗老化、透气、吸湿性能上处于较低的水平,对比例2制备的样品没有添加功能化二氧化硅,所以在抗静电以及拉伸强度方面性能很低,对比例3制备出来的样品不管是抗老化、透气、吸湿还是抗静电和拉伸强度方面均处在很低的水平,对比例4制备的样品直接添加竹炭微粉,没有对其进行表面处理,竹炭微粉在基体中出现了团聚现象,所以导致面料的力学性能很差,透气、吸湿、抗静电、抗老化效果一般,对比例5制备出来的样品直接添加纳米二氧化硅,纳米二氧化硅在基体中同样出现团聚现象,导致面料的力学性能较差,其余效果也一般。It can be seen from the above table that the samples prepared in Examples 1 to 3 are at a relatively high level in terms of breathability, moisture absorption, antistatic, anti-aging and mechanical properties. The sample prepared in Comparative Example 1 did not add antioxidant bamboo charcoal powder, so The anti-aging, air permeability, and moisture absorption properties are at a low level. The sample prepared in Comparative Example 2 did not add functionalized silica, so its antistatic and tensile strength properties are very low. The sample prepared in Comparative Example 3 has no Anti-aging, breathable, hygroscopic, antistatic and tensile strength are all at very low levels. The sample prepared in Comparative Example 4 was directly added with bamboo charcoal powder without surface treatment. The bamboo charcoal powder agglomerated in the matrix. , so the mechanical properties of the fabric are very poor, and the breathability, moisture absorption, antistatic, and anti-aging effects are average. Nano-silica is added directly to the sample prepared in Comparative Example 5. Nano-silica also agglomerates in the matrix, resulting in fabric The mechanical properties are poor, and the other effects are average.
②将实施例1-实施例3,对比例1-对比例5制备出来的面料裁剪成符合规格的样品,参考标准GB/T20944.3-2008《纺织品抗菌性能的评价第3部分:振荡法》对样品进行抗菌性能检测;使用点滴法测试样品杀螨活性,在孔细胞培养板上放置样品,滴入2滴去离子水浸润,同时在上面放置三只螨虫,使用倒置显微镜进行观察,每隔一分钟观察一次,直至三只螨虫全部死亡,记录死亡时间,每个样品做三次试验,实验结果取平均值,判断样品的除螨效果;具体检测结果见下表:② Cut the fabrics prepared in Examples 1 to 3 and Comparative Examples 1 to 5 into samples that meet the specifications. Refer to the standard GB/T20944.3-2008 "Evaluation of Antibacterial Performance of Textiles Part 3: Oscillation Method" Test the antibacterial properties of the samples; use the drip method to test the acaricidal activity of the samples. Place the sample on a well cell culture plate, add 2 drops of deionized water to infiltrate it, and place three mites on it at the same time. Use an inverted microscope to observe. Every other Observe once a minute until all three mites are dead, record the time of death, do three tests for each sample, and average the test results to judge the mite removal effect of the sample; the specific test results are shown in the table below:
由上表可知,实施例1-实施例3制备出来的样品具有优异的抗菌除螨效果,对比例1制备的样品没有加入抗氧化竹炭微粉,只有咪唑基季铵盐发挥作用,所以抗菌效果较好但比不上实施例,而除螨效果一般,对比例2制备的样品没有加入功能化二氧化硅,只有抗氧化竹炭微粉发挥作用,除螨效果较好,但是抗菌效果一般,对比例3制备的样品既没有加入抗氧化竹炭微粉也没有加入功能化二氧化硅,所以几乎没有抗菌除螨的能力,对比例4与对比例5制备出来的样品均在基体中产生了团聚现象,所以在抗菌以及除螨的性能上均处在较差的水平。As can be seen from the table above, the samples prepared in Examples 1 to 3 have excellent antibacterial and mite removal effects. The sample prepared in Comparative Example 1 did not add antioxidant bamboo charcoal micropowder, and only the imidazolyl quaternary ammonium salt played a role, so the antibacterial effect was relatively low. Good but not as good as the examples, and the effect of removing mites is average. The sample prepared in Comparative Example 2 did not add functionalized silica, and only the antioxidant bamboo charcoal micro powder played a role. The effect of removing mites was good, but the antibacterial effect was average. Comparative Example 3 The prepared samples did not add antioxidant bamboo charcoal micropowder or functionalized silica, so they had almost no antibacterial and mite removal capabilities. The samples prepared in Comparative Examples 4 and 5 both had agglomeration in the matrix, so in The antibacterial and mite-removing properties are both at a poor level.
在本说明书的描述中,参考术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不必须针对的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任一个或多个实施例或示例中以合适的方式结合。此外,在不相互矛盾的情况下,本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。In the description of this specification, reference to the terms "one embodiment," "some embodiments," "an example," "specific examples," or "some examples" or the like means that specific features are described in connection with the embodiment or example. , structures, materials or features are included in at least one embodiment or example of the invention. In this specification, the schematic expressions of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the specific features, structures, materials or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, those skilled in the art may combine and combine different embodiments or examples and features of different embodiments or examples described in this specification unless they are inconsistent with each other.
以上内容仅仅是对本发明的构思所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明的构思所定义的范围,均应属于本发明的保护范围。The above contents are only examples and explanations of the concept of the invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or substitute them in similar ways, as long as they do not deviate from the concept of the invention. The defined scope shall all belong to the protection scope of the present invention.
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