CN108755138A - 一种环保型耐水洗的纺织面料用防水剂及其制备方法 - Google Patents
一种环保型耐水洗的纺织面料用防水剂及其制备方法 Download PDFInfo
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
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Abstract
本发明公开了一种环保型耐水洗的纺织面料用防水剂,由以下原料组成:杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶,乙烯基三乙氧基硅烷,改性纳米氧化铝,藻蛋白酸钠,羧甲基纤维素,引发剂;所述杂醚化三聚氰胺树脂是由三聚氰胺和甲醛经缩合,再用甲醇和丁醇醚化得到的树脂。制备的环保型耐水洗的纺织面料用防水剂能够提高耐水洗性能和手感。
Description
技术领域
本发明属于防水技术领域,具体涉及一种环保型耐水洗的纺织面料用防水剂及其制备方法。
背景技术
防水剂是一类降低被处理物表面张力防水的一类物质,防水机理分为透气性防水机理和不透气性防水机理,不透气防水机理是使疏水性防水剂在织物表面开成疏水性薄膜,可阻止水的浸透,从而产生防水性能,这种防水机理,可使织物防水性能优良,但缺乏透气性,妨碍汗气和热量的散失,使人感觉不舒服。
透气性机理是使疏水性防水剂固着在织物表面或内部,而不形成连续的薄膜,织物不失去透气性,一般来说防水性较前者差,这种防水剂又称为拒水剂。由于透气性整理穿着舒适、轻便、无味,并有柔软的手感受,故应用较广。译
国内一般采用石蜡,有机硅,松香胶等防水,但不耐磨,不耐洗,一般不具有水溶性,不一定环保。国外大多采用氟表面活性剂防水,全氟类表面活性剂大多具有高表面活性,高热稳定性,高化学惰性,但全氟类价格很贵。
随着人们生活水平的提高,纸制品,纺织品、木制品、竹制品、建筑体,都在一定程度上需要防水功能,因此防水助剂应用量剧大,传统油溶性防水剂中含有大量有机溶剂,如苯,以及苯类似物容易挥发污染环境损害制造和使用者身体健康,近年来研制出水溶性防水剂主要是利用树脂形成连续膜的机理防水,这样会使纸制品,纺织品透气性严重下降,使木制品,竹制品无法保持原有特色。目前市场上生产的表面活性剂型防水剂大多数功能单一,一般存在不耐磨,不耐洗等缺陷。因此开发出一种无色,无毒,无味,耐性好,价格便宜,工艺简单的水溶性防水剂,符合市场的需求,发展前景广阔,经济效益乐观。
纺织纤维防水剂的组成在本领域早已公知。一般而言,市场份额最多的防水剂是通常是含氟类防水剂。氟类防水剂通常由大量含氟基团的低聚物或聚合物组成,可以赋予纤维材料良好的防水防油性能。但进年来,由于含氟化合物所引发的环境生态问题愈加引发关注,需要寻找一种不含氟并能给纤维提供良好防水性能的替代物。
CN105088796A中公开了一种无氟防水剂,其通过复配疏水聚合物、石蜡和封端聚氨酯组成以获得良好的防水性能和持久性。CN103628324A中公开了一种由甲基丙烯酸烷基酯聚合物和石蜡复配的防水剂,通过长链疏水性聚合物来达到防水性能。上述单纯采用封端聚氨酯复合物或甲基丙烯酸烷基酯聚合物分散液,虽然能带来良好的防水初始效果和一定的耐洗性能,但在使用中运行稳定性不佳,整理后织物手感发硬等缺点。丙烯酸烷基酯系防水剂还有制备工艺复杂,对设备要求较高,产品重现性差等缺点。
因此需要更加优秀的耐水洗且具有高效环保的有机硅防水剂,本发明者通过对防水剂的组合进行配方和改性,得到了性能完全改善的产品,完成了本发明。
发明内容
本发明提供一种环保型耐水洗的纺织面料用防水剂及其制备方法,制备了环保天然的环保型耐水洗的纺织面料用防水剂,具有更好的防水效果和耐水洗性能,整理后织物手感更柔顺,且天然环保。
为解决以上技术问题,本发明采用以下技术方案:
一种环保型耐水洗的纺织面料用防水剂,其特征在于,由以下原料组成:杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶,乙烯基三乙氧基硅烷,改性纳米氧化铝,藻蛋白酸钠,羧甲基纤维素,引发剂;所述杂醚化三聚氰胺树脂是由三聚氰胺和甲醛经缩合,再用甲醇和丁醇醚化得到的树脂;所述杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶的质量比为40-60:20-30:10-15。
进一步地,所述杂醚化三聚氰胺树脂中原料三聚氰胺、甲醛、甲醇、丁醇的摩尔比为1:4-6:2-4:2-4。
进一步地,所述杂醚化三聚氰胺树脂制备方法为用三乙醇胺调节甲醛水溶液的pH至10-11,然后将三聚氰胺、甲醛水溶液按比例混合,加热升温至70-80℃,待混合溶液的颜色由白色逐渐变为澄清透明后,加入甲醇和丁醇继续反应2-4个小时,分别得到杂醚化三聚氰胺树脂。
进一步地,所述液体硅胶为注射成型液态硅橡胶。
进一步地,藻蛋白酸钠与羧甲基纤维素按1:1的比例添加,总加入量为防水剂总量的1-5质量%。
进一步地,所述改性纳米氧化铝为三聚氰酸改性纳米氧化铝,平均粒径为1-100nm。
进一步地,所述改性纳米氧化铝通过纳米氧化铝分散到乙醇溶液中,然后加入1-5g/L的三聚氰酸,加热溶解回流0.5-1小时,过滤即可。
进一步地,所述引发剂为TPO,EDB,BDK中的至少一种。
进一步地,所述引发剂的加入量为防水剂总量的0.1-0.3质量%。
一种上述的环保型耐水洗的纺织面料用防水剂的制备方法,包括:
(1)将藻蛋白酸钠,羧甲基纤维素加入到水中,加热溶解后加入引发剂,改性纳米氧化铝超声分散,冷却;
(2)加入杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶,乙烯基三乙氧基硅烷和一定量的水在高速匀化器中混合均匀;所述加入水的总量为防水剂质量的1-3倍。
杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶经过复配形成的复合水溶性树脂,具有很好的相容性,并且由于具有较多游离的羟甲基和一定量的亚氨基,在分子链之间互相交联,提高成膜的牢固度。杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶的质量比为40-60:20-30:10-15,优选为50:25:12.5。
杂醚化三聚氰胺树脂的醚化程度和游离羟甲基含量,能影响树脂溶解度,以及与底材的结合程度。为了更好的实现本发明的技术效果,提高溶解度和活性末端数量,杂醚化三聚氰胺树脂中原料三聚氰胺、甲醛的摩尔比为1:4-6,优选为1:5。因为甲醚化三聚氰胺树脂的固化速度较快,而丁醚化三聚氰胺树脂的固化速度较慢,通过添加一定比例的甲醇和丁醇含量,从而可以控制树脂的固化和交联速度。
本发明配比中采用了纳米级的氧化铝,使产品易于分散,流动性好,耐水,附着牢固,因为纳米级氧化铝比表面积庞大,使得表面配位严重不足,产生了大量活性中心,与水溶性丙烯酸树脂中羧酸基及纸张,布料等的羟基配位络合,大大增强了附着力,同时还有一部分纳米级氧化硅分布在高分子链间,大大增强了流动性。同时通过添加无机纳米氧化铝,可以在纤维表面一定程度破坏了膜的完整性,使透气性更好。纳米氧化铝通过三聚氰酸进行改性后,利用三聚氰酸与三聚氰胺的范德华力结合作用,可以能使膜层附着力显著增强。
乙烯基三乙氧基硅烷为偶联剂,乙烯基三乙氧基硅烷的加入在引发剂的作用下不仅能够促进有机硅防水剂硅树脂网络的形成,而且能在接触面另外形成一层有机分子吸附构成的配位网络状薄膜。藻蛋白酸钠与羧甲基纤维素作为水溶性高分子助剂,可以在防水剂中调整粘度,同时由于其良好对纤维的亲和作用,能够更好促进膜的形成和附着,提高附着强度。
本发明通过以杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶构成的三元体系为基质,通过添加乙烯基三乙氧基硅烷,改性纳米氧化铝,藻蛋白酸钠,羧甲基纤维素,引发剂,能够协同的有效提高耐水洗性能和手感。
具体实施方式
为便于更好地理解本发明,通过以下实例加以说明,这些实例属于本发明的保护范围,但不限制本发明的保护范围。
水溶性丙烯酸树脂为水溶性丙烯酸树脂apa-518H,购自张家港市白玉兰涂料科技有限公司。液体硅胶为注射成型液态硅橡胶,购自东莞市天桉硅胶科技有限公司。
实施例1
一种环保型耐水洗的纺织面料用防水剂,其特征在于,由以下原料组成:杂醚化三聚氰胺树脂50质量份、水溶性丙烯酸树脂25质量份、注射成型液态硅橡胶12.5质量份,乙烯基三乙氧基硅烷7.5质量份,改性纳米氧化铝3质量份,藻蛋白酸钠,羧甲基纤维素,TPO引发剂。所述引发剂的加入量为防水剂总量的0.2质量%。藻蛋白酸钠与羧甲基纤维素按1:1的比例添加,总加入量为防水剂总量的3质量%。
所述杂醚化三聚氰胺树脂制备方法为用三乙醇胺调节甲醛水溶液的pH至10-11,然后将1质量份三聚氰胺、5质量份甲醛混合,加热升温至70-80℃,待混合溶液的颜色由白色逐渐变为澄清透明后,加入3质量份甲醇和3质量份丁醇继续反应3个小时,分别得到杂醚化三聚氰胺树脂。
所述改性纳米氧化铝通过纳米氧化铝分散到乙醇溶液中,然后加入3g/L的三聚氰酸,加热溶解回流0.5-1小时,过滤即可。
上述的环保型耐水洗的纺织面料用防水剂的制备方法,包括:
(1)将藻蛋白酸钠,羧甲基纤维素加入到水中,加热溶解后加入引发剂,改性纳米氧化铝超声分散,冷却;
(2)加入杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶,乙烯基三乙氧基硅烷和一定量的水在高速匀化器中混合均匀;所述加入水的总量为防水剂质量的2倍。
实施例2
一种环保型耐水洗的纺织面料用防水剂,其特征在于,由以下原料组成:杂醚化三聚氰胺树脂40质量份、水溶性丙烯酸树脂30质量份、注射成型液态硅橡胶10质量份,乙烯基三乙氧基硅烷10质量份,改性纳米氧化铝1质量份,藻蛋白酸钠,羧甲基纤维素,TPO引发剂。所述引发剂的加入量为防水剂总量的0.3质量%。藻蛋白酸钠与羧甲基纤维素按1:1的比例添加,总加入量为防水剂总量的1质量%。
所述杂醚化三聚氰胺树脂制备方法为用三乙醇胺调节甲醛水溶液的pH至10-11,然后将1质量份三聚氰胺、6质量份的甲醛水溶液混合,加热升温至70-80℃,待混合溶液的颜色由白色逐渐变为澄清透明后,加入2质量份的甲醇和4质量份的丁醇继续反应2个小时,分别得到杂醚化三聚氰胺树脂。
所述改性纳米氧化铝通过纳米氧化铝分散到乙醇溶液中,然后加入5g/L的三聚氰酸,加热溶解回流0.5小时,过滤即可。
上述的环保型耐水洗的纺织面料用防水剂的制备方法,包括:
(1)将藻蛋白酸钠,羧甲基纤维素加入到水中,加热溶解后加入引发剂,改性纳米氧化铝超声分散,冷却;
(2)加入杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶,乙烯基三乙氧基硅烷和一定量的水在高速匀化器中混合均匀;所述加入水的总量为防水剂质量的3倍。
实施例3
一种环保型耐水洗的纺织面料用防水剂,其特征在于,由以下原料组成:杂醚化三聚氰胺树脂60质量份、水溶性丙烯酸树脂20质量份、注射成型液态硅橡胶15质量份,乙烯基三乙氧基硅烷5质量份,改性纳米氧化铝5质量份,藻蛋白酸钠,羧甲基纤维素,TPO引发剂。所述引发剂的加入量为防水剂总量的0.1质量%。藻蛋白酸钠与羧甲基纤维素按1:1的比例添加,总加入量为防水剂总量的5质量%。
所述杂醚化三聚氰胺树脂制备方法为用三乙醇胺调节甲醛水溶液的pH至10-11,然后将1质量份三聚氰胺、4质量份甲醛水溶液混合,加热升温至70-80℃,待混合溶液的颜色由白色逐渐变为澄清透明后,加入4质量份的甲醇和2质量份的丁醇继续反应4个小时,分别得到杂醚化三聚氰胺树脂。
所述改性纳米氧化铝通过纳米氧化铝分散到乙醇溶液中,然后加入1g/L的三聚氰酸,加热溶解回流0.5-1小时,过滤即可。
上述的环保型耐水洗的纺织面料用防水剂的制备方法,包括:
(1)将藻蛋白酸钠,羧甲基纤维素加入到水中,加热溶解后加入引发剂,改性纳米氧化铝超声分散,冷却;
(2)加入杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶,乙烯基三乙氧基硅烷和一定量的水在高速匀化器中混合均匀;所述加入水的总量为防水剂质量的1倍。
对比例1
与实施例1的制备工艺基本相同,唯有不同的是制备环保型耐水洗的纺织面料用防水剂的原料中缺少杂醚化三聚氰胺树脂。
对比例2
与实施例1的制备工艺基本相同,唯有不同的是制备环保型耐水洗的纺织面料用防水剂的原料中缺少水溶性丙烯酸树脂。
对比例3
与实施例1的制备工艺基本相同,唯有不同的是制备环保型耐水洗的纺织面料用防水剂的原料中缺少液体硅胶。
对比例4
与实施例1的制备工艺基本相同,唯有不同的是制备环保型耐水洗的纺织面料用防水剂的原料中缺少乙烯基三乙氧基硅烷。
对比例5
与实施例1的制备工艺基本相同,唯有不同的是制备环保型耐水洗的纺织面料用防水剂的原料中缺少改性纳米氧化铝。
对比例6
与实施例1的制备工艺基本相同,唯有不同的是制备环保型耐水洗的纺织面料用防水剂的原料中纳米氧化铝不进行改性。
对比例7
与实施例1的制备工艺基本相同,唯有不同的是制备环保型耐水洗的纺织面料用防水剂的原料中缺少藻蛋白酸钠与羧甲基纤维素。
测试方法与结果
通过国标GB 4745—1997考察防水效果。
国家标准《GB 4745—1997》试验方法如下:截取18×18cm 的试样,用夹持器压紧,并安装于与水平成以45°角的固定座上,用250mL(20±2℃) 的蒸馏水或去离子水迅速而平稳地注入漏斗中,通过与试样中心距离的喷头在25-30s 内,朝试样中心平均而持续不断地喷淋。喷淋完毕,迅速将夹持器拿开,使试样正面向下成水平,轻轻地拍打两下,观察试样润湿程度,评定其等级,l 级为受淋表面全部润湿,5级为受淋表面没有润湿,也无小水珠。
耐洗涤性能是将整理好的纺织品进行20次标准洗涤,然后考察防水性能。
测定织物为纯棉梭织布,分别取50g/L实施例和对比例中样品,一浸一轧, 110℃烘干,170℃培烘,冷却至室温后测试防水效果和手感。
手感为主观评价,由5人独立测评,分为5个等级,等级5为最佳。
由上表可知,本发明通过以杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶构成的三元体系为基质,通过添加乙烯基三乙氧基硅烷,改性纳米氧化铝,藻蛋白酸钠,羧甲基纤维素,引发剂,能够协同的有效提高耐水洗性能和手感。
以上内容不能认定本发明具体实施只局限于这些说明,对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思前提下,还可以做出若干简单推演或替换,都应当视为属于本发明由所提交的权利要求书确定的专利保护范围。
Claims (10)
1.一种环保型耐水洗的纺织面料用防水剂,其特征在于,由以下原料组成:杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶,乙烯基三乙氧基硅烷,改性纳米氧化铝,藻蛋白酸钠,羧甲基纤维素,引发剂;所述杂醚化三聚氰胺树脂是由三聚氰胺和甲醛经缩合,再用甲醇和丁醇醚化得到的树脂;所述杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶的质量比为40-60:20-30:10-15。
2.根据权利要求1所述的环保型耐水洗的纺织面料用防水剂,其中所述杂醚化三聚氰胺树脂中原料三聚氰胺、甲醛、甲醇、丁醇的摩尔比为1:4-6:2-4:2-4。
3.根据权利要求1所述的环保型耐水洗的纺织面料用防水剂,其中所述杂醚化三聚氰胺树脂制备方法为用三乙醇胺调节甲醛水溶液的pH至10-11,然后将三聚氰胺、甲醛水溶液按比例混合,加热升温至70-80℃,待混合溶液的颜色由白色逐渐变为澄清透明后,加入甲醇和丁醇继续反应2-4个小时,分别得到杂醚化三聚氰胺树脂。
4.根据权利要求1所述的环保型耐水洗的纺织面料用防水剂,其中所述液体硅胶为注射成型液态硅橡胶。
5.根据权利要求1所述的环保型耐水洗的纺织面料用防水剂,其中藻蛋白酸钠与羧甲基纤维素按1:1的比例添加,总加入量为防水剂总量的1-5质量%。
6.根据权利要求1所述的环保型耐水洗的纺织面料用防水剂,其中所述改性纳米氧化铝为三聚氰酸改性纳米氧化铝,平均粒径为1-100nm。
7.根据权利要求1所述的环保型耐水洗的纺织面料用防水剂,其中所述改性纳米氧化铝通过纳米氧化铝分散到乙醇溶液中,然后加入1-5g/L的三聚氰酸,加热溶解回流0.5-1小时,过滤即可。
8.根据权利要求1所述的环保型耐水洗的纺织面料用防水剂,其中所述引发剂为TPO,EDB,BDK中的至少一种。
9.根据权利要求1所述的环保型耐水洗的纺织面料用防水剂,其中所述引发剂的加入量为防水剂总量的0.1-0.3质量%。
10.一种如权利要求1-9所述的环保型耐水洗的纺织面料用防水剂的制备方法,包括:
(1)将藻蛋白酸钠,羧甲基纤维素加入到水中,加热溶解后加入引发剂,改性纳米氧化铝超声分散,冷却;
(2)加入杂醚化三聚氰胺树脂、水溶性丙烯酸树脂、液体硅胶,乙烯基三乙氧基硅烷和一定量的水在高速匀化器中混合均匀;所述加入水的总量为防水剂质量的1-3倍。
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