CN108914592A - 一种涤纶织物后整理用柔软剂 - Google Patents
一种涤纶织物后整理用柔软剂 Download PDFInfo
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- MRUAUOIMASANKQ-UHFFFAOYSA-O carboxymethyl-[3-(dodecanoylamino)propyl]-dimethylazanium Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC(O)=O MRUAUOIMASANKQ-UHFFFAOYSA-O 0.000 description 1
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Abstract
本发明公开了一种涤纶织物后整理用柔软剂,涉及纺织加工技术领域,包含以下重量份数的组分:三元共聚嵌段氨基硅油35‑45份、PEG‑60氢化蓖麻油5‑10份、丙烯酸‑丙烯酸酯‑膦酸‑磺酸盐四元共聚物1‑5份、白色聚合氯化铝1‑5份、纳米改性粉体0.5‑2份、羟基乙叉二膦酸四钠0.5‑2份、去离子水100‑200份。本发明所制柔软剂温和无刺激,经其处理后的涤纶织物柔软性好且耐水性和耐黄变性能佳,从而显著提高了涤纶织物的使用品质。
Description
技术领域:
本发明涉及纺织加工技术领域,具体涉及一种涤纶织物后整理用柔软剂。
背景技术:
涤纶是合成纤维中的一个重要品种,是我国聚酯纤维的商品名称。它是以聚对苯二甲酸或对苯二甲酸二甲酯和乙二醇为原料,经酯化或酯交换和缩聚反应而制得的成纤高聚物-聚对苯二甲酸乙二醇酯(PET),经纺丝和后处理制成的纤维。
柔软剂是后整理剂中的一个大类,其主要功能是满足涤纶纺织品的不同手感/风格的要求。涤纶纺织品柔软剂主要分为两大类,非硅的脂肪族型和有机硅型,目前应用最广泛的是有机硅型。
有机硅柔软剂的发展大致经历了三个阶段,第一代是甲基硅油乳液,这类柔软剂的最大缺点是与纤维的结合力差,不耐洗;第二代有机硅柔软剂虽然含有能与纤维结合的羟基,但是结合能力差,处理效果不佳;第三代有机硅柔软剂按照官能团可分为单官能团改性硅油和多官能团改性硅油,依靠活性基团增强与纤维的亲和力,可改善织物的耐洗性、柔韧性、亲水性等。
如何在保证柔软性的同时提高织物的耐洗性和耐黄变性成为目前有机硅柔软剂的研究热点,同时还需考虑柔软剂的环境污染性,尽可能减轻所产生废液对环境的污染。
发明内容:
本发明所要解决的技术问题在于提供一种兼具优良耐洗性和耐黄变性能的涤纶织物后整理用柔软剂。
本发明所要解决的技术问题采用以下的技术方案来实现:
一种涤纶织物后整理用柔软剂,包含以下重量份数的组分:
三元共聚嵌段氨基硅油35-45份、PEG-60氢化蓖麻油5-10份、丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物1-5份、白色聚合氯化铝1-5份、纳米改性粉体0.5-2份、羟基乙叉二膦酸四钠0.5-2份、去离子水100-200份;
所述纳米改性粉体由纳米二氧化钛经改性处理制得,其制备方法为:先将纳米二氧化钛置于100-110℃烘箱中干燥至恒重,再加入水解聚马来酸酐,升温至125-135℃保温搅拌5-15min,然后加入三羟甲基丙烷三缩水甘油醚,继续于125-135℃保温搅拌15-30min,并以5℃/min的降温速度降温至0-5℃保温静置0.5-1h,最后将所得固体经粉碎和研磨处理制成纳米粉末,即得纳米改性粉体。
所述纳米二氧化钛、水解聚马来酸酐和三羟甲基丙烷三缩水甘油醚的质量比为1:0.01-0.05:0.05-0.5。
所述柔软剂还包含1-5份丙烯酰胺聚合物。
所述丙烯酰胺聚合物由N-羟甲基丙烯酰胺和多聚谷氨酸经酯化和聚合反应制成,其具体制备方法为:先将N-羟甲基丙烯酰胺和多聚谷氨酸溶于水中,并滴加质量浓度10%的稀硫酸调节体系pH值至5,再加热至75-85℃保温反应,待酯化反应完成后滴加质量浓度5%的碳酸氢钠溶液调节体系pH值至7,然后加入质量浓度10%的过硫酸铵水溶液,继续于75-85℃保温反应,待聚合反应完成后自然冷却至室温,向所得混合物中滴加无水乙醇直至无沉淀析出,过滤,沉淀真空干燥,干燥所得固体经超微粉碎机制成微粉,即得丙烯酰胺聚合物。
所述多聚谷氨酸选用食品级多聚谷氨酸。
所述N-羟甲基丙烯酰胺、多聚谷氨酸、过硫酸铵水溶液的质量比为15-25:5-10:1-5。
本发明的有益效果是:
(1)本发明以三元共聚嵌段氨基硅油为主料,协以PEG-60氢化蓖麻油等辅料制得涤纶织物后整理用柔软剂,所制柔软剂温和无刺激,经其处理后的涤纶织物柔软性好且耐水性和耐黄变性能佳,从而显著提高了涤纶织物的使用品质。
(2)本发明通过对纳米二氧化钛的所述改性处理来提高其耐水洗性能,利用纳米二氧化钛特有的渗透性来增强柔软剂功能成分在涤纶纤维上的附着力,进而提高经柔软剂处理后的涤纶织物耐水洗性能,避免织物经水洗后柔软度骤降。
(3)本发明通过所述丙烯酰胺聚合物的添加来赋予经所制柔软剂处理后涤纶织物优异的耐黄变性能,防止处理后的涤纶织物因出现泛黄现象而影响其使用质量和使用寿命。
具体实施方式:
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
以下实施例和对照例中的三元共聚嵌段氨基硅油选用嘉兴科瑞有机硅有限公司生产的815;丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物选用山东泰和水处理科技股份有限公司生产的TH-241。
实施例1
柔软剂的制备:向160g去离子水中加入40g三元共聚嵌段氨基硅油、8gPEG-60氢化蓖麻油、5g丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物、3g白色聚合氯化铝、0.5g纳米改性粉体、0.5g羟基乙叉二膦酸四钠,搅拌混合均匀,即得柔软剂。
纳米改性粉体的制备:先将1g纳米二氧化钛置于105-110℃烘箱中干燥至恒重,再加入0.05g水解聚马来酸酐,升温至130-135℃保温搅拌10min,然后加入0.25g三羟甲基丙烷三缩水甘油醚,继续于130-135℃保温搅拌15min,并以5℃/min的降温速度降温至0-5℃保温静置30min,最后将所得固体经粉碎和研磨处理制成纳米粉末,即得纳米改性粉体。
实施例2
柔软剂的制备:向160g去离子水中加入40g三元共聚嵌段氨基硅油、8gPEG-60氢化蓖麻油、5g丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物、3g白色聚合氯化铝、1g纳米改性粉体、0.5g羟基乙叉二膦酸四钠,搅拌混合均匀,即得柔软剂。
纳米改性粉体的制备:先将1g纳米二氧化钛置于105-110℃烘箱中干燥至恒重,再加入0.05g水解聚马来酸酐,升温至130-135℃保温搅拌10min,然后加入0.25g三羟甲基丙烷三缩水甘油醚,继续于130-135℃保温搅拌15min,并以5℃/min的降温速度降温至0-5℃保温静置30min,最后将所得固体经粉碎和研磨处理制成纳米粉末,即得纳米改性粉体。
实施例3
柔软剂的制备:向160g去离子水中加入40g三元共聚嵌段氨基硅油、8gPEG-60氢化蓖麻油、5g丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物、3g白色聚合氯化铝、3g丙烯酰胺聚合物、1g纳米改性粉体、0.5g羟基乙叉二膦酸四钠,搅拌混合均匀,即得柔软剂。
纳米改性粉体的制备:先将1g纳米二氧化钛置于105-110℃烘箱中干燥至恒重,再加入0.05g水解聚马来酸酐,升温至130-135℃保温搅拌10min,然后加入0.25g三羟甲基丙烷三缩水甘油醚,继续于130-135℃保温搅拌15min,并以5℃/min的降温速度降温至0-5℃保温静置30min,最后将所得固体经粉碎和研磨处理制成纳米粉末,即得纳米改性粉体。
丙烯酰胺聚合物的制备:先将25g N-羟甲基丙烯酰胺和10g食品级多聚谷氨酸溶于水中,并滴加质量浓度10%的稀硫酸调节体系pH值至5,再加热至75-80℃保温反应,待酯化反应完成后滴加质量浓度5%的碳酸氢钠溶液调节体系pH值至7,然后加入5g质量浓度10%的过硫酸铵水溶液,继续于75-80℃保温反应,待聚合反应完成后自然冷却至室温,向所得混合物中滴加无水乙醇直至无沉淀析出,过滤,沉淀真空干燥,干燥所得固体经超微粉碎机制成微粉,即得丙烯酰胺聚合物。
对照例1
柔软剂的制备:向160g去离子水中加入40g三元共聚嵌段氨基硅油、8gPEG-60氢化蓖麻油、5g丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物、3g白色聚合氯化铝、0.5g纳米二氧化钛、0.5g羟基乙叉二膦酸四钠,搅拌混合均匀,即得柔软剂。
对照例2
柔软剂的制备:向160g去离子水中加入40g三元共聚嵌段氨基硅油、8gPEG-60氢化蓖麻油、5g丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物、0.5g纳米改性粉体、0.5g羟基乙叉二膦酸四钠,搅拌混合均匀,即得柔软剂。
纳米改性粉体的制备:先将1g纳米二氧化钛置于105-110℃烘箱中干燥至恒重,再加入0.05g水解聚马来酸酐,升温至130-135℃保温搅拌10min,然后加入0.25g三羟甲基丙烷三缩水甘油醚,继续于130-135℃保温搅拌15min,并以5℃/min的降温速度降温至0-5℃保温静置30min,最后将所得固体经粉碎和研磨处理制成纳米粉末,即得纳米改性粉体。
对照例3
柔软剂的制备:向160g去离子水中加入40g三元共聚嵌段氨基硅油、8gPEG-60氢化蓖麻油、3g白色聚合氯化铝、0.5g纳米改性粉体、0.5g羟基乙叉二膦酸四钠,搅拌混合均匀,即得柔软剂。
纳米改性粉体的制备:先将1g纳米二氧化钛置于105-110℃烘箱中干燥至恒重,再加入0.05g水解聚马来酸酐,升温至130-135℃保温搅拌10min,然后加入0.25g三羟甲基丙烷三缩水甘油醚,继续于130-135℃保温搅拌15min,并以5℃/min的降温速度降温至0-5℃保温静置30min,最后将所得固体经粉碎和研磨处理制成纳米粉末,即得纳米改性粉体。
实施例4
以实施例1为基础,设置不对纳米二氧化钛进行改性处理的对照例1、不添加白色聚合氯化铝的对照例2、不添加丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物的对照例3。
分别利用实施例1-3、对照例1-3制备柔软剂,并利用所制柔软剂对同批同规格涤纶织物进行后整理,具体操作步骤如下:
(1)后整理液的配制:向100g水中加入15g壳聚糖季铵盐、5g椰油酰胺丙基甜菜碱、2g柔软剂和0.5g抗静电剂SN,搅拌溶解完全,即得后整理液;
(2)浸轧:将涤纶织物完全浸渍于上述后整理液中,浴比1:40,二浸二轧,每次浸渍20min,轧液率75%;
(3)预烘:将经上述浸轧后的涤纶织物于105-110℃预烘2min;
(4)微波固着:将经预烘后的涤纶织物利用微波频率2450MHz、输出功率700W的微波反应器微波处理60s;
(5)水洗:对经微波固着的涤纶织物进行两次水洗,第一次采用45-50℃温水水洗,第二次采用15-20℃冷水水洗,水洗浴比1:20;
(6)烘干:将经水洗后的涤纶织物用50-55℃热风烘干,即完成后整理。
以上述后整理操作步骤为基础,设置不添加柔软剂的空白例。
对经上述后整理后的涤纶织物进行性能测试,结果如表1所示。
硬挺度:参照GB/T 7689.4-2001标准;
耐洗性:参照GB/T 3921-2008标准,测定皂洗50次后硬挺度;
耐黄变:参照ISO 105-X18;2007标准。
表1本发明柔软剂对涤纶织物的性能影响
组别 | 硬挺度 | 耐洗性 | 耐黄变等级 |
空白例 | 4.85 | 5.93 | 2 |
实施例1 | 1.78 | 2.04 | 4 |
实施例2 | 1.43 | 1.63 | 4 |
实施例3 | 1.16 | 1.29 | 4 |
对照例1 | 2.21 | 2.56 | 3-4 |
对照例2 | 2.70 | 3.17 | 3 |
对照例3 | 3.82 | 4.64 | 3 |
未添加柔软剂处理的织物和添加柔软剂处理的织物的硬挺度变化越大,说明添加柔软剂处理的织物柔软性越好;皂洗50次后硬挺度变化越小,说明耐洗性越好;耐黄变等级越高,说明耐黄变性越好。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (6)
1.一种涤纶织物后整理用柔软剂,其特征在于,包含以下重量份数的组分:三元共聚嵌段氨基硅油35-45份、PEG-60氢化蓖麻油5-10份、丙烯酸-丙烯酸酯-膦酸-磺酸盐四元共聚物1-5份、白色聚合氯化铝1-5份、纳米改性粉体0.5-2份、羟基乙叉二膦酸四钠0.5-2份、去离子水100-200份;
所述纳米改性粉体由纳米二氧化钛经改性处理制得,其制备方法为:先将纳米二氧化钛置于100-110℃烘箱中干燥至恒重,再加入水解聚马来酸酐,升温至125-135℃保温搅拌5-15min,然后加入三羟甲基丙烷三缩水甘油醚,继续于125-135℃保温搅拌15-30min,并以5℃/min的降温速度降温至0-5℃保温静置0.5-1h,最后将所得固体经粉碎和研磨处理制成纳米粉末,即得纳米改性粉体。
2.根据权利要求1所述的涤纶织物后整理用柔软剂,其特征在于:所述纳米二氧化钛、水解聚马来酸酐和三羟甲基丙烷三缩水甘油醚的质量比为1:0.01-0.05:0.05-0.5。
3.根据权利要求1所述的涤纶织物后整理用柔软剂,其特征在于:所述柔软剂还包含1-5份丙烯酰胺聚合物。
4.根据权利要求3所述的涤纶织物后整理用柔软剂,其特征在于:所述丙烯酰胺聚合物由N-羟甲基丙烯酰胺和多聚谷氨酸经酯化和聚合反应制成,其具体制备方法为:先将N-羟甲基丙烯酰胺和多聚谷氨酸溶于水中,并滴加质量浓度10%的稀硫酸调节体系pH值至5,再加热至75-85℃保温反应,待酯化反应完成后滴加质量浓度5%的碳酸氢钠溶液调节体系pH值至7,然后加入质量浓度10%的过硫酸铵水溶液,继续于75-85℃保温反应,待聚合反应完成后自然冷却至室温,向所得混合物中滴加无水乙醇直至无沉淀析出,过滤,沉淀真空干燥,干燥所得固体经超微粉碎机制成微粉,即得丙烯酰胺聚合物。
5.根据权利要求4所述的涤纶织物后整理用柔软剂,其特征在于:所述多聚谷氨酸选用食品级多聚谷氨酸。
6.根据权利要求4所述的涤纶织物后整理用柔软剂,其特征在于:所述N-羟甲基丙烯酰胺、多聚谷氨酸、过硫酸铵水溶液的质量比为15-25:5-10:1-5。
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110230149A (zh) * | 2019-04-28 | 2019-09-13 | 安徽柯林医疗用品科技股份有限公司 | 一种可生物降解型医用高吸湿纤维的加工工艺 |
CN117306264A (zh) * | 2023-11-27 | 2023-12-29 | 广东欣薇尔服装有限公司 | 一种超细旦柔软锦纶面料及其制备方法 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1584191A (zh) * | 2004-05-28 | 2005-02-23 | 刘国平 | 纳米柔软平滑剂及其制备方法 |
CN102145943A (zh) * | 2010-09-15 | 2011-08-10 | 杭州英普水处理技术有限公司 | 蒸馏法海水淡化阻垢分散剂及其制备方法 |
CN106835698A (zh) * | 2017-02-14 | 2017-06-13 | 广州天赐高新材料股份有限公司 | 柔顺剂组合物 |
CN107353842A (zh) * | 2017-07-31 | 2017-11-17 | 安徽艺云玻璃有限公司 | 一种中空玻璃加工用外道密封胶抗老化性能增强助剂 |
CN107751258A (zh) * | 2017-11-05 | 2018-03-06 | 茆莉娟 | 一种长效缓释型驱蚊贴的加工方法 |
CN108044840A (zh) * | 2017-12-07 | 2018-05-18 | 马斌祥 | 利用废旧硬质塑料和改性椰糠加工木塑复合材料的装置 |
-
2018
- 2018-07-02 CN CN201810705499.4A patent/CN108914592A/zh active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1584191A (zh) * | 2004-05-28 | 2005-02-23 | 刘国平 | 纳米柔软平滑剂及其制备方法 |
CN102145943A (zh) * | 2010-09-15 | 2011-08-10 | 杭州英普水处理技术有限公司 | 蒸馏法海水淡化阻垢分散剂及其制备方法 |
CN106835698A (zh) * | 2017-02-14 | 2017-06-13 | 广州天赐高新材料股份有限公司 | 柔顺剂组合物 |
CN107353842A (zh) * | 2017-07-31 | 2017-11-17 | 安徽艺云玻璃有限公司 | 一种中空玻璃加工用外道密封胶抗老化性能增强助剂 |
CN107751258A (zh) * | 2017-11-05 | 2018-03-06 | 茆莉娟 | 一种长效缓释型驱蚊贴的加工方法 |
CN108044840A (zh) * | 2017-12-07 | 2018-05-18 | 马斌祥 | 利用废旧硬质塑料和改性椰糠加工木塑复合材料的装置 |
Non-Patent Citations (6)
Title |
---|
刘智安等: "《工业循环冷却水处理》", 30 September 2017, 中国轻工业出版社 * |
周宏湘: "《染整新技术问答》", 30 April 1998, 中国纺织出版社 * |
张宇震: "《中国铝酸盐水泥生产与应用》", 31 January 2014, 中国建材工业出版社 * |
张康夫等: "《防锈油脂与乳化切削油》", 30 May 1983, 国防工业出版社 * |
张建春等: "《化纤仿毛技术原理与生产实践》", 30 September 2003, 中国纺织出版社 * |
李祖德等: "《塑料加工技术应用手册》", 30 October 1997, 中国物资出版社 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110230149A (zh) * | 2019-04-28 | 2019-09-13 | 安徽柯林医疗用品科技股份有限公司 | 一种可生物降解型医用高吸湿纤维的加工工艺 |
CN117306264A (zh) * | 2023-11-27 | 2023-12-29 | 广东欣薇尔服装有限公司 | 一种超细旦柔软锦纶面料及其制备方法 |
CN117306264B (zh) * | 2023-11-27 | 2024-03-29 | 广东欣薇尔服装有限公司 | 一种超细旦柔软锦纶面料及其制备方法 |
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