CN115305722A - 一种感光变色面料及其制备方法 - Google Patents
一种感光变色面料及其制备方法 Download PDFInfo
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- CN115305722A CN115305722A CN202210928661.5A CN202210928661A CN115305722A CN 115305722 A CN115305722 A CN 115305722A CN 202210928661 A CN202210928661 A CN 202210928661A CN 115305722 A CN115305722 A CN 115305722A
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- 239000004744 fabric Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title description 2
- 229920002635 polyurethane Polymers 0.000 claims abstract description 56
- 239000004814 polyurethane Substances 0.000 claims abstract description 56
- 229920001778 nylon Polymers 0.000 claims abstract description 34
- 239000004900 Hydrophilic Finishing Agent Substances 0.000 claims abstract description 30
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 23
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 23
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 21
- 150000001412 amines Chemical class 0.000 claims abstract description 21
- 229920000570 polyether Polymers 0.000 claims abstract description 21
- 239000004677 Nylon Substances 0.000 claims abstract description 17
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 15
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 14
- 239000003822 epoxy resin Substances 0.000 claims abstract description 13
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract 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 abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 72
- 239000000243 solution Substances 0.000 claims description 60
- 239000004952 Polyamide Substances 0.000 claims description 50
- 229920002647 polyamide Polymers 0.000 claims description 50
- 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 description 41
- 235000010413 sodium alginate Nutrition 0.000 claims description 41
- 229940005550 sodium alginate Drugs 0.000 claims description 41
- 239000000661 sodium alginate Substances 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 35
- 238000002156 mixing Methods 0.000 claims description 25
- 238000005406 washing Methods 0.000 claims description 24
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 23
- 238000004132 cross linking Methods 0.000 claims description 22
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 21
- 239000012043 crude product Substances 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000835 fiber Substances 0.000 claims description 13
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 10
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 10
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 10
- 229920002614 Polyether block amide Polymers 0.000 claims description 8
- 238000010035 extrusion spinning Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 6
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000009941 weaving Methods 0.000 claims description 6
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 5
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 229940095564 anhydrous calcium sulfate Drugs 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000012047 saturated solution Substances 0.000 claims description 4
- VCMLCMCXCRBSQO-UHFFFAOYSA-N 3h-benzo[f]chromene Chemical compound C1=CC=CC2=C(C=CCO3)C3=CC=C21 VCMLCMCXCRBSQO-UHFFFAOYSA-N 0.000 claims description 2
- DMLAVOWQYNRWNQ-UHFFFAOYSA-N azobenzene Chemical compound C1=CC=CC=C1N=NC1=CC=CC=C1 DMLAVOWQYNRWNQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 230000006750 UV protection Effects 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 abstract description 3
- 229940072056 alginate Drugs 0.000 abstract description 3
- 235000010443 alginic acid Nutrition 0.000 abstract description 3
- 229920000615 alginic acid Polymers 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 16
- 239000000203 mixture Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 125000003368 amide group Chemical group 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001733 carboxylic acid esters Chemical group 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
- D06M15/568—Reaction products of isocyanates with polyethers
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- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
本发明公开了一种感光变色面料及其制备方法,涉及纺织技术领域。本发明在制备感光变色面料时,将母粒与感光变色材料通过挤出纺丝制得锦纶纤维并编织成锦纶面料,再用改性聚氨酯亲水整理剂进行后整理,制得具有防紫外性和亲水性的感光变色面料;其中,母粒上含有具有紫外线屏蔽效果的褐藻酸铁,改性聚氨酯亲水整理剂是由封端聚醚胺、对苯二甲酸、双端羧基聚乙二醇、甲苯二异氰酸酯和环氧树脂反应制得,能够增强面料的热稳定性,与锦纶纤维有较强的亲和力,增强了后整理剂的耐久性,还能够增强面料的亲水性。
Description
技术领域
本发明涉及纺织技术领域,具体为一种感光变色面料及其制备方法。
背景技术
随着人们生活水平的提高,对衣服面料的追求已经不仅仅是为了保暖,人们对其美观和舒适度的要求也不断提高。衣服的颜色基本上由面料的颜色确定,在制作服装时,可以选择单独的一种颜色的面料,也可以使用多种面料进行拼接,但是,无论采用哪种方式,衣服一旦出厂,就再也不能更改颜色。因此,导致无论什么颜色的衣服,长时间穿着之后都会显得单调。
然而现有的光面变色面料大多采用后整理技术,在后续的使用清洗过程中容易导致光敏变色剂从面料上脱落,造成变色效果差;而且锦纶面料的亲水性差,在光照后发生变色后温度也会上升,多面料造成影响;因此本发明制备了一种热稳定性好、抗紫外并且亲水性强的感光变色面料。
发明内容
本发明的目的在于提供一种感光变色面料及其制备方法,以解决上述背景技术中提出的问题。
一种感光变色面料,所述感光变色面料是将母粒与感光变色材料通过挤出纺丝制得锦纶纤维并编织成锦纶面料,再用改性聚氨酯亲水整理剂进行后整理制得。
优选的,所述母粒是由海藻酸钠与超支化聚酰胺反应后再在氯化铁的酸溶液中进行交联制得。
优选的,所述感光变色材料为萘酚吡喃、俘精酸醉或偶氮苯中的一种。
优选的,所述改性聚氨酯亲水整理剂是由封端聚醚胺、对苯二甲酸、双端羧基聚乙二醇、甲苯二异氰酸酯和环氧树脂反应制得。
优选的,所述一种感光变色面料的制备方法,包括以下具体步骤:
(1)向质量分数为8~10%的海藻酸钠溶液中加入海藻酸钠溶液体积0.2~0.4倍的海藻酸钠溶液1~2%的戊二醛溶液,和海藻酸钠溶液体积0.04~0.08倍的质量分数为4~6%的盐酸溶液,升温至60~65℃,在50~100rpm下搅拌反应6~8h,用去离子水洗涤3~5次后,加入海藻酸钠溶液质量3.5~4.8倍的超支化聚酰胺,再在200~400rpm下搅拌反应15~30min,最后用去离子水和乙醇依次洗涤3~5次,制得海藻酸钠改性超支化聚酰胺;
(2)将海藻酸钠改性超支化聚酰胺浸泡在混合交联液中,交联反应24~48h后捞出,用去离子水洗涤3~5次并干燥,制得母粒将母粒与感光变色材料按质量比18:1~30:2混合,用螺杆挤压机挤出,切粒制得锦纶纤维母粒;
(3)在氮气氛围中,将锦纶纤维母粒置于双螺杆挤出机中进行挤出纺丝,控制纺丝计量泵总供量为550~650g/min,纺丝温度为220~240℃,纺丝速度为800~1000m/min,牵伸倍数为2.5~3.0倍,制得锦纶纤维;将锦纶纤维编织为克重120~300g/m3的锦纶面料;
(4)将封端聚酰胺、对苯二甲酸和亚磷酸按质量比1:0.8:0.01~1:1:0.01混合,升温至240~250℃,反应2~3h,然后降温至220~225℃,开始抽真空至真空度为-0.05~-0.08KPa,同时升温至240~250℃,保温反应1~2h,卸真空后降温至160~170℃时出料,制得聚醚酰胺;
(5)将2,2-二羟甲基丙酸与环氧树脂按质量比1:12~1:15混合,加热搅拌至溶解,然后调节温度至60~70℃,加入环氧树脂质量0.4~0.6倍的甲苯二异氰酸酯,密闭条件下在高纯氮气保护下搅拌反应,转速为1000~1500r/min,反应3~4h,制得聚氨酯;向聚氨酯中加入聚氨酯质量1.1~1.3倍的聚醚酰胺和聚氨酯质量0.9~1.4倍的双端羧基聚乙二醇,搅拌均匀后升温至80~90℃,加入聚氨酯质量0.1~0.3倍的碳酸氢钠,在50~100rpm下搅拌反应2~4h,制得改性聚氨酯亲水整理剂;
(6)将锦纶面料用改性聚氨酯亲水整理剂进行后整理,制得感光变色面料。
优选的,上述步骤(1)中:超支化聚酰胺的制备方法为:在氮气氛围下,室温下向三口烧瓶中加入甲醇和甲醇质量0.2~0.4倍的二乙烯三胺,混合均匀后以3~5ml/min的速率滴加甲醇质量0.15~0.18倍的丙烯酸甲酯,反应5~8h后,升温至50~60℃并抽真空,反应20~50min后,再次升温至115~120℃,反应4~6h,再次升温至140~145℃,反应3~4h,制得粗产物,将粗产物分散在粗产物质量5~8倍的甲醇中,搅拌至溶解,再用乙醚沉淀并洗涤,最后置于真空干燥箱中在60~70℃下干燥至恒重,制得超支化聚酰胺。
优选的,上述步骤(2)中:混合交联液是总浓度为1~2%的氯化铁盐酸溶液,氯化铁与盐酸的浓度比例为1.2:1~1.5:1。
优选的,上述步骤(4)中:封端聚醚胺的制备方法为:在氮气氛围下,将聚醚胺加热至200~220℃,加入聚醚胺质量0.02~0.04倍的亚磷酸搅拌均匀后,均匀分3~5次共加入聚醚胺质量0.6~0.8倍的尼龙66盐,间隔时间在20~40min,添加完成后升温至230~235℃,反应3~5h,制得封端聚醚胺。
优选的,上述步骤(5)中:双端羧基聚乙二醇的制备方法为:将聚乙二醇与甲苯按质量比1:15~1:20混合,升温至95~98℃,加入聚乙二醇质量2~3倍的丁二酸酐,升温至105~110℃,保温反应1~1.5h,再减压蒸馏蒸出甲苯,制得固体;将固体溶于固体质量3~5倍的碳酸氢钠饱和溶液中,静置分层后分离出下层溶液,用质量分数为5%的盐酸酸化并用二氯甲烷萃取,最后经去离子水洗涤3~5次,用无水硫酸钙干燥、过滤、浓缩后,用无水乙醚重结晶,再次过滤并真空干燥,制得双端羧基聚乙二醇。
优选的,上述步骤(6)中:后整理时,用改性聚氨酯亲水整理剂进行一浸二轧,压力为0.3~0.5MPa,并在80~90℃下烘干5~10min,最后在170~180℃下焙烘50~60s,冷却至室温。
与现有技术相比,本发明所达到的有益效果是:
本发明在制备感光变色面料时,将母粒与感光变色材料通过挤出纺丝制得锦纶纤维并编织成锦纶面料,再用改性聚氨酯亲水整理剂进行后整理,制得具有防紫外性和亲水性的感光变色面料;
母粒是由海藻酸钠与超支化聚酰胺反应后再在氯化铁的酸溶液中进行交联制得,再将母粒与感光变色材料挤出纺丝制得锦纶纤维;先将海藻酸钠交联在超支化聚酰胺上,增强吸附能力,再在氯化铁的酸溶液中进行交联,铁离子被母粒吸附,并与海藻酸钠上的羧酸酯基和羟基形成离子键,超支化聚酰胺上交联形成具有紫外线屏蔽效果的褐藻酸铁,使得面料具备防紫外线效果;
改性聚氨酯亲水整理剂是由封端聚醚胺、对苯二甲酸、双端羧基聚乙二醇、甲苯二异氰酸酯和环氧树脂反应制得;封端聚醚胺与对苯二甲酸缩聚形成聚醚酰胺,甲苯二异氰酸酯与环氧树脂反应,形成带有环氧基的聚氨酯,双端羧基聚乙二醇将聚醚胺连接在带有环氧基的聚氨酯上,制得长链、含有酰胺基和刚性苯环的改性聚氨酯亲水整理剂,能够穿过并纠缠在锦纶纤维间隙中,共同结晶在锦纶面料表面,增强面料的热稳定性,与锦纶纤维有较强的亲和力,增强了后整理剂的耐久性,还能够增强面料的亲水性。
具体实施方式
下面将结合本发明的实施例,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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
为了更清楚的说明本发明提供的方法通过以下实施例进行详细说明,将实施例和对比例中制备的感光变色面料的各指标测试方法如下:
耐洗性、亲水性:将实施例和对比例中制备的感光变色面料亲水性采用织物的毛细效应表征,在水洗30次后再次进行亲水性测试;
热稳定性:将实施例和对比例中制备的感光变色面料在40℃下纺织5小时后进行亲水性测试;
抗紫外线:将实施例和对比例中制备的感光变色面料参照GB/T18830进行紫外线防护系数(UPF)测定。
实施例1
(1)在氮气氛围下,室温下向三口烧瓶中加入甲醇和甲醇质量0.2倍的二乙烯三胺,混合均匀后以3ml/min的速率滴加甲醇质量0.15倍的丙烯酸甲酯,反应5h后,升温至50℃并抽真空,反应20min后,再次升温至115℃,反应4h,再次升温至140℃,反应3h,制得粗产物,将粗产物分散在粗产物质量5倍的甲醇中,搅拌至溶解,再用乙醚沉淀并洗涤,最后置于真空干燥箱中在60℃下干燥至恒重,制得超支化聚酰胺;向质量分数为8%的海藻酸钠溶液中加入海藻酸钠溶液体积0.2倍的海藻酸钠溶液1%的戊二醛溶液,和海藻酸钠溶液体积0.04倍的质量分数为4%的盐酸溶液,升温至60℃,在50rpm下搅拌反应6h,用去离子水洗涤3次后,加入海藻酸钠溶液质量3.5倍的超支化聚酰胺,再在200rpm下搅拌反应15min,最后用去离子水和乙醇依次洗涤3次,制得海藻酸钠改性超支化聚酰胺;
(2)将海藻酸钠改性超支化聚酰胺浸泡在混合交联液中,交联反应24h后捞出,混合交联液是总浓度为1%的氯化铁盐酸溶液,氯化铁与盐酸的浓度比例为1.2:1,用去离子水洗涤3次并干燥,制得母粒将母粒与感光变色材料按质量比18:1混合,用螺杆挤压机挤出,切粒制得锦纶纤维母粒;
(3)在氮气氛围中,将锦纶纤维母粒置于双螺杆挤出机中进行挤出纺丝,控制纺丝计量泵总供量为550g/min,纺丝温度为220℃,纺丝速度为800m/min,牵伸倍数为2.5倍,制得锦纶纤维;将锦纶纤维编织为克重120g/m3的锦纶面料;
(4)在氮气氛围下,将聚醚胺加热至200℃,加入聚醚胺质量0.02倍的亚磷酸搅拌均匀后,均匀分3次共加入聚醚胺质量0.6倍的尼龙66盐,间隔时间在20min,添加完成后升温至230℃,反应3h,制得封端聚醚胺;将封端聚酰胺、对苯二甲酸和亚磷酸按质量比1:0.8:0.01混合,升温至240℃,反应2h,然后降温至220℃,开始抽真空至真空度为-0.05KPa,同时升温至240℃,保温反应1h,卸真空后降温至160℃时出料,制得聚醚酰胺;
(5)将聚乙二醇与甲苯按质量比1:15混合,升温至95℃,加入聚乙二醇质量2倍的丁二酸酐,升温至105℃,保温反应1h,再减压蒸馏蒸出甲苯,制得固体;将固体溶于固体质量3倍的碳酸氢钠饱和溶液中,静置分层后分离出下层溶液,用质量分数为5%的盐酸酸化并用二氯甲烷萃取,最后经去离子水洗涤3次,用无水硫酸钙干燥、过滤、浓缩后,用无水乙醚重结晶,再次过滤并真空干燥,制得双端羧基聚乙二醇;将2,2-二羟甲基丙酸与环氧树脂按质量比1:12混合,加热搅拌至溶解,然后调节温度至60℃,加入环氧树脂质量0.4倍的甲苯二异氰酸酯,密闭条件下在高纯氮气保护下搅拌反应,转速为1000r/min,反应3h,制得聚氨酯;向聚氨酯中加入聚氨酯质量1.1倍的聚醚酰胺和聚氨酯质量0.9倍的双端羧基聚乙二醇,搅拌均匀后升温至80℃,加入聚氨酯质量0.1倍的碳酸氢钠,在50rpm下搅拌反应2h,制得改性聚氨酯亲水整理剂;
(6)将锦纶面料用改性聚氨酯亲水整理剂进行后整理,后整理时,用改性聚氨酯亲水整理剂进行一浸二轧,压力为0.3MPa,并在80℃下烘干5min,最后在170℃下焙烘50s,冷却至室温,制得感光变色面料。
实施例2
(1)在氮气氛围下,室温下向三口烧瓶中加入甲醇和甲醇质量0.3倍的二乙烯三胺,混合均匀后以4ml/min的速率滴加甲醇质量0.17倍的丙烯酸甲酯,反应6h后,升温至55℃并抽真空,反应40min后,再次升温至118℃,反应5h,再次升温至143℃,反应3.5h,制得粗产物,将粗产物分散在粗产物质量7倍的甲醇中,搅拌至溶解,再用乙醚沉淀并洗涤,最后置于真空干燥箱中在65℃下干燥至恒重,制得超支化聚酰胺;向质量分数为9%的海藻酸钠溶液中加入海藻酸钠溶液体积0.3倍的海藻酸钠溶液1.5%的戊二醛溶液,和海藻酸钠溶液体积0.06倍的质量分数为5%的盐酸溶液,升温至63℃,在80rpm下搅拌反应7h,用去离子水洗涤4次后,加入海藻酸钠溶液质量4倍的超支化聚酰胺,再在300rpm下搅拌反应22min,最后用去离子水和乙醇依次洗涤4次,制得海藻酸钠改性超支化聚酰胺;
(2)将海藻酸钠改性超支化聚酰胺浸泡在混合交联液中,交联反应36h后捞出,混合交联液是总浓度为1.5%的氯化铁盐酸溶液,氯化铁与盐酸的浓度比例为1.4:1,用去离子水洗涤4次并干燥,制得母粒将母粒与感光变色材料按质量比22:1.5混合,用螺杆挤压机挤出,切粒制得锦纶纤维母粒;
(3)在氮气氛围中,将锦纶纤维母粒置于双螺杆挤出机中进行挤出纺丝,控制纺丝计量泵总供量为600g/min,纺丝温度为230℃,纺丝速度为900m/min,牵伸倍数为2.8倍,制得锦纶纤维;将锦纶纤维编织为克重220g/m3的锦纶面料;
(4)在氮气氛围下,将聚醚胺加热至210℃,加入聚醚胺质量0.03倍的亚磷酸搅拌均匀后,均匀分4次共加入聚醚胺质量0.7倍的尼龙66盐,间隔时间在30min,添加完成后升温至233℃,反应4h,制得封端聚醚胺;将封端聚酰胺、对苯二甲酸和亚磷酸按质量比1:0.9:0.01混合,升温至245℃,反应2.5h,然后降温至223℃,开始抽真空至真空度为-0.06KPa,同时升温至245℃,保温反应1.5h,卸真空后降温至165℃时出料,制得聚醚酰胺;
(5)将聚乙二醇与甲苯按质量比1:18混合,升温至96℃,加入聚乙二醇质量2.5倍的丁二酸酐,升温至108℃,保温反应1.3h,再减压蒸馏蒸出甲苯,制得固体;将固体溶于固体质量4倍的碳酸氢钠饱和溶液中,静置分层后分离出下层溶液,用质量分数为5%的盐酸酸化并用二氯甲烷萃取,最后经去离子水洗涤4次,用无水硫酸钙干燥、过滤、浓缩后,用无水乙醚重结晶,再次过滤并真空干燥,制得双端羧基聚乙二醇;将2,2-二羟甲基丙酸与环氧树脂按质量比1:14混合,加热搅拌至溶解,然后调节温度至65℃,加入环氧树脂质量0.5倍的甲苯二异氰酸酯,密闭条件下在高纯氮气保护下搅拌反应,转速为1300r/min,反应3.5h,制得聚氨酯;向聚氨酯中加入聚氨酯质量1.2倍的聚醚酰胺和聚氨酯质量1.2倍的双端羧基聚乙二醇,搅拌均匀后升温至85℃,加入聚氨酯质量0.2倍的碳酸氢钠,在80rpm下搅拌反应3h,制得改性聚氨酯亲水整理剂;
(6)将锦纶面料用改性聚氨酯亲水整理剂进行后整理,后整理时,用改性聚氨酯亲水整理剂进行一浸二轧,压力为0.4MPa,并在85℃下烘干8min,最后在175℃下焙烘55s,冷却至室温,制得感光变色面料。
实施例3
(1)在氮气氛围下,室温下向三口烧瓶中加入甲醇和甲醇质量0.4倍的二乙烯三胺,混合均匀后以5ml/min的速率滴加甲醇质量0.18倍的丙烯酸甲酯,反应8h后,升温至60℃并抽真空,反应50min后,再次升温至120℃,反应6h,再次升温至145℃,反应4h,制得粗产物,将粗产物分散在粗产物质量8倍的甲醇中,搅拌至溶解,再用乙醚沉淀并洗涤,最后置于真空干燥箱中在70℃下干燥至恒重,制得超支化聚酰胺;向质量分数为10%的海藻酸钠溶液中加入海藻酸钠溶液体积0.4倍的海藻酸钠溶液2%的戊二醛溶液,和海藻酸钠溶液体积0.08倍的质量分数为6%的盐酸溶液,升温至65℃,在100rpm下搅拌反应8h,用去离子水洗涤5次后,加入海藻酸钠溶液质量4.8倍的超支化聚酰胺,再在400rpm下搅拌反应30min,最后用去离子水和乙醇依次洗涤5次,制得海藻酸钠改性超支化聚酰胺;
(2)将海藻酸钠改性超支化聚酰胺浸泡在混合交联液中,交联反应48h后捞出,混合交联液是总浓度为2%的氯化铁盐酸溶液,氯化铁与盐酸的浓度比例为1.5:1,用去离子水洗涤5次并干燥,制得母粒将母粒与感光变色材料按质量比30:2混合,用螺杆挤压机挤出,切粒制得锦纶纤维母粒;
(3)在氮气氛围中,将锦纶纤维母粒置于双螺杆挤出机中进行挤出纺丝,控制纺丝计量泵总供量为650g/min,纺丝温度为240℃,纺丝速度为1000m/min,牵伸倍数为3.0倍,制得锦纶纤维;将锦纶纤维编织为克重300g/m3的锦纶面料;
(4)在氮气氛围下,将聚醚胺加热至220℃,加入聚醚胺质量0.04倍的亚磷酸搅拌均匀后,均匀分5次共加入聚醚胺质量0.8倍的尼龙66盐,间隔时间在40min,添加完成后升温至235℃,反应5h,制得封端聚醚胺;将封端聚酰胺、对苯二甲酸和亚磷酸按质量比1:1:0.01混合,升温至250℃,反应3h,然后降温至225℃,开始抽真空至真空度为-0.08KPa,同时升温至250℃,保温反应2h,卸真空后降温至170℃时出料,制得聚醚酰胺;
(5)将聚乙二醇与甲苯按质量比1:20混合,升温至98℃,加入聚乙二醇质量3倍的丁二酸酐,升温至110℃,保温反应1.5h,再减压蒸馏蒸出甲苯,制得固体;将固体溶于固体质量5倍的碳酸氢钠饱和溶液中,静置分层后分离出下层溶液,用质量分数为5%的盐酸酸化并用二氯甲烷萃取,最后经去离子水洗涤5次,用无水硫酸钙干燥、过滤、浓缩后,用无水乙醚重结晶,再次过滤并真空干燥,制得双端羧基聚乙二醇;将2,2-二羟甲基丙酸与环氧树脂按质量比1:15混合,加热搅拌至溶解,然后调节温度至70℃,加入环氧树脂质量0.6倍的甲苯二异氰酸酯,密闭条件下在高纯氮气保护下搅拌反应,转速为1500r/min,反应4h,制得聚氨酯;向聚氨酯中加入聚氨酯质量1.3倍的聚醚酰胺和聚氨酯质量1.4倍的双端羧基聚乙二醇,搅拌均匀后升温至90℃,加入聚氨酯质量0.3倍的碳酸氢钠,在100rpm下搅拌反应4h,制得改性聚氨酯亲水整理剂;
(6)将锦纶面料用改性聚氨酯亲水整理剂进行后整理,后整理时,用改性聚氨酯亲水整理剂进行一浸二轧,压力为0.5MPa,并在90℃下烘干10min,最后在180℃下焙烘60s,冷却至室温,制得感光变色面料。
对比例1
对比例1的处方组成同实施例2。该感光变色面料及其制备方法与实施例2的区别仅在于步骤(1)的不同,将步骤(1)修改为:在氮气氛围下,室温下向三口烧瓶中加入甲醇和甲醇质量0.3倍的二乙烯三胺,混合均匀后以4ml/min的速率滴加甲醇质量0.17倍的丙烯酸甲酯,反应6h后,升温至55℃并抽真空,反应40min后,再次升温至118℃,反应5h,再次升温至143℃,反应3.5h,制得粗产物,将粗产物分散在粗产物质量7倍的甲醇中,搅拌至溶解,再用乙醚沉淀并洗涤,最后置于真空干燥箱中在65℃下干燥至恒重,制得超支化聚酰胺;并在步骤(2)中使用超支化聚酰胺进行母粒的制备。
对比例2
对比例2的处方组成同实施例2。该感光变色面料及其制备方法与实施例2的区别仅在于步骤(5)的不同,将步骤(5)修改为:将2,2-二羟甲基丙酸与环氧树脂按质量比1:14混合,加热搅拌至溶解,然后调节温度至65℃,加入环氧树脂质量0.5倍的甲苯二异氰酸酯,密闭条件下在高纯氮气保护下搅拌反应,转速为1300r/min,反应3.5h,制得聚氨酯;向聚氨酯中加入聚氨酯质量1.2倍的聚醚酰胺,搅拌均匀后升温至85℃,加入聚氨酯质量0.2倍的碳酸氢钠,在80rpm下搅拌反应3h,制得改性聚氨酯亲水整理剂。
对比例3
对比例3的处方组成同实施例2。该感光变色面料及其制备方法与实施例2的区别仅在于不进行步骤(5)的制备,步骤(4)制得的聚醚酰胺为后整理剂。
对比例4
对比例4的处方组成同实施例2。该感光变色面料及其制备方法与实施例2的区别仅在于不进行步骤(4)(5)的处理,步骤(3)制得锦纶面料为感光变色面料。
效果例
下表1给出了采用本发明实施例1、2、3与对比例1-4的感光变色面料的各性能分析结果:
表1
通过表1中实施例与对比例的实验数据比较可以明显发现,实施例1、2、3制备的感光变色面料的抗紫外线、热稳定性、亲水性和耐性性较好。
从实施例和对比例1、2、5的实验数据比较可发现,由海藻酸钠与超支化聚酰胺反应后再在氯化铁的酸溶液中进行交联制得的母粒,在超支化聚酰胺上交联形成具有紫外线屏蔽效果的褐藻酸铁,使得面料具备防紫外线效果;从实施例和对比例3、4的实验数据比较可发现,由封端聚醚胺、对苯二甲酸、双端羧基聚乙二醇、甲苯二异氰酸酯和环氧树脂反应制得的,长链、含有酰胺基和刚性苯环的改性聚氨酯亲水整理剂,能够穿过并纠缠在锦纶纤维间隙中,共同结晶在锦纶面料表面,增强面料的热稳定性,与锦纶纤维有较强的亲和力,增强了后整理剂的耐久性,还能够增强面料的亲水性。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何标记视为限制所涉及的权利要求。
Claims (10)
1.一种感光变色面料,其特征在于,所述感光变色面料是将母粒与感光变色材料通过挤出纺丝制得锦纶纤维并编织成锦纶面料,再用改性聚氨酯亲水整理剂进行后整理制得。
2.根据权利要求1所述的一种感光变色面料,其特征在于,所述母粒是由海藻酸钠与超支化聚酰胺反应后再在氯化铁的酸溶液中进行交联制得。
3.根据权利要求1所述的一种感光变色面料,其特征在于,所述感光变色材料为萘酚吡喃、俘精酸醉或偶氮苯中的一种。
4.根据权利要求1所述的一种感光变色面料,其特征在于,所述改性聚氨酯亲水整理剂是由封端聚醚胺、对苯二甲酸、双端羧基聚乙二醇、甲苯二异氰酸酯和环氧树脂反应制得。
5.一种感光变色面料的制备方法,其特征在于,所述感光变色面料的制备方法,包括以下具体步骤:
(1)向质量分数为8~10%的海藻酸钠溶液中加入海藻酸钠溶液体积0.2~0.4倍的海藻酸钠溶液1~2%的戊二醛溶液,和海藻酸钠溶液体积0.04~0.08倍的质量分数为4~6%的盐酸溶液,升温至60~65℃,在50~100rpm下搅拌反应6~8h,用去离子水洗涤3~5次后,加入海藻酸钠溶液质量3.5~4.8倍的超支化聚酰胺,再在200~400rpm下搅拌反应15~30min,最后用去离子水和乙醇依次洗涤3~5次,制得海藻酸钠改性超支化聚酰胺;
(2)将海藻酸钠改性超支化聚酰胺浸泡在混合交联液中,交联反应24~48h后捞出,用去离子水洗涤3~5次并干燥,制得母粒将母粒与感光变色材料按质量比18:1~30:2混合,用螺杆挤压机挤出,切粒制得锦纶纤维母粒;
(3)在氮气氛围中,将锦纶纤维母粒置于双螺杆挤出机中进行挤出纺丝,控制纺丝计量泵总供量为550~650g/min,纺丝温度为220~240℃,纺丝速度为800~1000m/min,牵伸倍数为2.5~3.0倍,制得锦纶纤维;将锦纶纤维编织为克重120~300g/m3的锦纶面料;
(4)将封端聚酰胺、对苯二甲酸和亚磷酸按质量比1:0.8:0.01~1:1:0.01混合,升温至240~250℃,反应2~3h,然后降温至220~225℃,开始抽真空至真空度为-0.05~-0.08KPa,同时升温至240~250℃,保温反应1~2h,卸真空后降温至160~170℃时出料,制得聚醚酰胺;
(5)将2,2-二羟甲基丙酸与环氧树脂按质量比1:12~1:15混合,加热搅拌至溶解,然后调节温度至60~70℃,加入环氧树脂质量0.4~0.6倍的甲苯二异氰酸酯,密闭条件下在高纯氮气保护下搅拌反应,转速为1000~1500r/min,反应3~4h,制得聚氨酯;向聚氨酯中加入聚氨酯质量1.1~1.3倍的聚醚酰胺和聚氨酯质量0.9~1.4倍的双端羧基聚乙二醇,搅拌均匀后升温至80~90℃,加入聚氨酯质量0.1~0.3倍的碳酸氢钠,在50~100rpm下搅拌反应2~4h,制得改性聚氨酯亲水整理剂;
(6)将锦纶面料用改性聚氨酯亲水整理剂进行后整理,制得感光变色面料。
6.根据权利要求5所述的一种感光变色面料的制备方法,其特征在于,上述步骤(1)中:超支化聚酰胺的制备方法为:在氮气氛围下,室温下向三口烧瓶中加入甲醇和甲醇质量0.2~0.4倍的二乙烯三胺,混合均匀后以3~5ml/min的速率滴加甲醇质量0.15~0.18倍的丙烯酸甲酯,反应5~8h后,升温至50~60℃并抽真空,反应20~50min后,再次升温至115~120℃,反应4~6h,再次升温至140~145℃,反应3~4h,制得粗产物,将粗产物分散在粗产物质量5~8倍的甲醇中,搅拌至溶解,再用乙醚沉淀并洗涤,最后置于真空干燥箱中在60~70℃下干燥至恒重,制得超支化聚酰胺。
7.根据权利要求5所述的一种感光变色面料的制备方法,其特征在于,上述步骤(2)中:混合交联液是总浓度为1~2%的氯化铁盐酸溶液,氯化铁与盐酸的浓度比例为1.2:1~1.5:1。
8.根据权利要求5所述的一种感光变色面料的制备方法,其特征在于,上述步骤(4)中:封端聚醚胺的制备方法为:在氮气氛围下,将聚醚胺加热至200~220℃,加入聚醚胺质量0.02~0.04倍的亚磷酸搅拌均匀后,均匀分3~5次共加入聚醚胺质量0.6~0.8倍的尼龙66盐,间隔时间在20~40min,添加完成后升温至230~235℃,反应3~5h,制得封端聚醚胺。
9.根据权利要求5所述的一种感光变色面料的制备方法,其特征在于,上述步骤(5)中:双端羧基聚乙二醇的制备方法为:将聚乙二醇与甲苯按质量比1:15~1:20混合,升温至95~98℃,加入聚乙二醇质量2~3倍的丁二酸酐,升温至105~110℃,保温反应1~1.5h,再减压蒸馏蒸出甲苯,制得固体;将固体溶于固体质量3~5倍的碳酸氢钠饱和溶液中,静置分层后分离出下层溶液,用质量分数为5%的盐酸酸化并用二氯甲烷萃取,最后经去离子水洗涤3~5次,用无水硫酸钙干燥、过滤、浓缩后,用无水乙醚重结晶,再次过滤并真空干燥,制得双端羧基聚乙二醇。
10.根据权利要求5所述的一种感光变色面料的制备方法,其特征在于,上述步骤(6)中:后整理时,用改性聚氨酯亲水整理剂进行一浸二轧,压力为0.3~0.5MPa,并在80~90℃下烘干5~10min,最后在170~180℃下焙烘50~60s,冷却至室温。
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