CN112142947A - 多功能吸湿速干型水性抗菌聚氨酯整理剂制备方法及应用 - Google Patents
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Abstract
本发明公开了多功能吸湿速干型水性抗菌聚氨酯整理剂制备方法及应用,以甲苯二异氰酸酯(TDI)、聚酯聚醚多元醇(PCI,PEG)三乙醇胺、二已醇胺等为原料,加成反应制成预聚体,在预聚体中预留NCO/OH的反应基团位置;在特定催化剂的作用下,预聚体与小分子的抗菌单体聚合反应,将抗菌单体接入聚氨酯链中,本发明整理剂在纺织品应用,对全棉,化纤及其混纺织物,在后整处理工艺中在布面行维交联形成可以吸湿、速干、抗菌、耐洗等功能膜,使纺织品具备吸湿速干抗菌等功效。
Description
技术领域
本发明属于织物整理剂技术领域,具体地说,涉及多功能吸湿速干型水性抗菌聚氨酯整理剂制备方法及应用。
背景技术
织物整理是在织物上施加一种整理剂,它能改变织物的表面性能,从而赋予织物特殊的功能,例如防水防油整理是以具有低表面张力的整理剂处理织物,改变纤维的表面特性,使织物表面不易被水或油润湿和铺展,从而达到憎水憎油的目的;防污整理和易去污整理是通过改变纤维的表面性能或表面状态,使织物在穿着、使用条件下不易沾附污垢,或将已沾附的污垢易于洗涤并不再沾污。目前市面上还没有出现具备抗菌、吸湿、速干等功能的整理剂。
有鉴于此特提出本发明。
发明内容
本发明要解决的技术问题在于克服现有技术的不足,提供多功能吸湿速干型水性抗菌聚氨酯整理剂制备方法及应用,为解决上述技术问题,本发明采用技术方案的基本构思是:
多功能吸湿速干型水性抗菌聚氨酯整理剂的制备方法,包括以下步骤:
步骤1,预留可反应基团聚氨酯预聚体的制备:
将甲苯二异氰酸酯(TDI)、聚酯多元醇、聚乙二醇、二丁基二月桂酸锡加入磁力搅拌三口瓶中,升温至80℃反应3h;尔后继续加入1,4一丁二醇、二羟甲基丁酸、NaN3、亲水扩链剂进行扩链,继续反应6h后降温至40℃;滴加入二乙醇胺中和40min,制得可接入的聚氨酯亲水预聚体(PV-N3);
步骤2,小分子抗菌单体的制备:
2-炔丙基-1,1,3,3-四甲基胍(TMGD)的合成:三口瓶中加入 TMG、EA,搅拌均匀;在三口瓶上方置一恒压漏斗,加入溴丙炔、EA,混合均匀后,以恒定速率缓慢滴加至三口瓶中,常温反应16h;产物进行抽滤操作分离出下层液体,加入二氯甲烷并饱和食盐水萃取5次后合并有机相,旋蒸得棕褐色液态产物2-炔丙基-1,1,3,3-四甲基胍(TMGD);
2,2-双(叠氮甲基)丙烷-1,3-二醇(DAED)的制备:三口瓶中依次加入2,2-双(溴甲基)-1,3-丙二醇、二甲基亚砜(DMSO)溶剂,搅拌均匀后再缓慢小心加入NaN3,冷凝回流,干燥,升温至110℃,反应24h后降至室温,萃取得黄色粘稠液体2,2-双(叠氮甲基)丙烷-1,3-二醇(DAED);
步骤3,小分子抗菌单体与预聚体的聚合反应:
取二甲基甲酰胺,开搅拌通氮气1h,排尽空气;滴加二乙胺基三胺,慢加入CuBr 催化剂,以抗菌单体(TMGD)作变量与聚氨酯预聚体,搅拌均匀;在催化剂CuBr催化下,常温条件,聚氨酯亲水预聚体(PV-N3)、DAED、TMGD按一定质量比,制得所需预聚体。
多功能吸湿速干型水性抗菌聚氨酯整理剂在纺织物上的应用。
采用上述技术方案后,本发明与现有技术相比具有以下有益效果。
本发明整理剂是以甲苯二异氰酸酯(TDI)、聚酯聚醚多元醇(PCI,PEG)三乙醇胺、二已醇胺等为原料,加成反应制成预聚体,在预聚体中预留 NCO/OH的反应基团位置;在特定催化剂的作用下,预聚体与小分子的抗菌单体聚合反应,将抗菌单体接入聚氨酯链中,本发明整理剂在纺织品应用,对全棉,化纤及其混纺织物,在后整处理工艺中在布面行维交联形成可以吸湿、速干、抗菌、耐洗等功能膜,使纺织品具备吸湿速干抗菌等功效。
下面结合附图对本发明的具体实施方式作进一步详细的描述。
附图说明
附图作为本申请的一部分,用来提供对本发明的进一步的理解,本发明的示意性实施例及其说明用于解释本发明,但不构成对本发明的不当限定。显然,下面描述中的附图仅仅是一些实施例,对于本领域普通技术人员来说,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附图。在附图中:
图1是本发明亲水性预聚体的合成反应过程;
需要说明的是,这些附图和文字描述并不旨在以任何方式限制本发明的构思范围,而是通过参考特定实施例为本领域技术人员说明本发明的概念。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,对实施例中的技术方案进行清楚、完整地描述,以下实施例用于说明本发明,但不用来限制本发明的范围。
实施例
1 主要原料和试剂
甲苯二异氰酸酯(TDI)、聚酯多元醇(N210,Mn1200)、聚乙二醇(PEG1000)、胺类扩链剂、1,4一丁二醇、二甲基二月桂酸锡(DBTDL)、二羟甲基丁酸、NaN3叠氮化钠、1,1,3,3-四甲基胍(TMG)、3-溴丙炔、溴化亚铜(CuBr)、丙二醇、去离子水。
2 亲水性预聚体的合成
步骤1,预留可反应基团聚氨酯预聚体的制备:
将TDI、聚酯多元醇、聚乙二醇、二丁基二月桂酸锡(1滴),加入磁力搅拌三口瓶中,升温至80℃,反应3h。后继续加入1,4一丁二醇、二羟甲基丁酸、NaN3、亲水扩链剂进行扩链,继续反应6h后降温至40℃;滴加入二乙醇胺中和40min,制得可接入的聚氨酯亲水预聚体备用(PV-N3)。
步骤2,小分子抗菌单体的制备:
2-炔丙基-1,1,3,3-四甲基胍(TMGD)的合成:三口瓶中,加入30g TMG及 50ml EA,搅拌均匀。在三口瓶上方置一恒压漏斗,加入9ml溴丙炔及40ml EA,混合均匀后以恒定速率缓慢滴加至三口瓶中,常温反应16h。产物进行抽滤操作分离出下层液体,加入160ml二氯甲烷并以 80mL饱和食盐水萃取5次后合并有机相,旋蒸得6.72g棕褐色液态产物(TMGD)。
2,2-双(叠氮甲基)丙烷-1,3-二醇(DAED)的制备:三口瓶中依次加入2,2-双(溴甲基)-1,3-丙二醇60g及180mL二甲基亚砜(DMSO)溶剂,搅拌均匀后再缓慢小心加入NaN3,冷凝回流,干燥,升温至110℃,反应24h后降至室温,萃取得黄色粘稠液体DAED,真空干燥备用。
步骤3,.小分子抗菌单体与预聚体的聚合反应:
取10ml二甲基甲酰胺,开搅拌,通氮气1h排尽空气,滴加二乙胺基三胺380mL,慢加入CuBr 0.2g催化剂,以抗菌单体(TMGD)作变量与聚氨酯预聚体,搅拌均匀。在催化剂CuBr催化下,常温条件,聚氨酸预聚体,DAED,TMGD,按一定质量比,制得所需预聚体。反应过程参见图1示出。
3 亲水性预聚体水分散
将上面的得聚合反应成品,加30%去离子水,在变频高速分散器中,以1000转/分高速中剪切分散30min,得到含固量为35%的水性聚氨酯乳液。
3.1聚氨酯乳液在纺织物上应用,功能性能的整理和测试,结果表明,此乳液效果能达到国家标准,特别是在亲水性,速干性,吸湿性能与及抗菌性能上。
3.2.TMGD及其聚合物预聚体结构表征,红外表征图显示:与空白预聚体相比,在聚氨酯预聚体中含有一定浓度TMGD,表明DAED成功接入聚氨酯高分子主链中。
3.3.聚氨酯聚合物乳液稳定性,在转速为4500转/min离心加速器中离心30min,乳液无沉淀分层现象,表明此乳液具有良好稳定性。
4. 结论:
以甲苯二异氰酸酯(TDI)作为主链原料合成,预留可接入基团位置的聚氨酯预聚体链上,聚合引入小分子胍盐类单体,获得一种在纺织品应用上的多功能具有亲水性,吸湿速干,兼顾有抗菌性能,具备耐洗性的功能整理剂。
以上所述仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专利的技术人员在不脱离本发明技术方案范围内,当可利用上述提示的技术内容作出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与修饰,均仍属于本发明方案的范围内。
Claims (2)
1.多功能吸湿速干型水性抗菌聚氨酯整理剂的制备方法,其特征在于,包括以下步骤:
步骤1,预留可反应基团聚氨酯预聚体的制备:
将甲苯二异氰酸酯(TDI)、聚酯多元醇、聚乙二醇、二丁基二月桂酸加入磁力搅拌三口瓶中,升温至80℃反应3h;尔后继续加入1,4一丁二醇、二羟甲基丁酸、NaN3、亲水扩链剂进行扩链,继续反应6h后降温至40℃;滴加入二乙醇胺中和40min,制得可接入的聚氨酯亲水预聚体(PV-N3);
步骤2,小分子抗菌单体的制备:
2-炔丙基-1,1,3,3-四甲基胍(TMGD)的合成:三口瓶中加入 TMG、EA,搅拌均匀;在三口瓶上方置一恒压漏斗,加入溴丙炔、EA,混合均匀后,以恒定速率缓慢滴加至三口瓶中,常温反应16h;产物进行抽滤操作分离出下层液体,加入二氯甲烷并饱和食盐水萃取5次后合并有机相,旋蒸得棕褐色液态产物2-炔丙基-1,1,3,3-四甲基胍(TMGD);
2,2-双(叠氮甲基)丙烷-1,3-二醇(DAED)的制备:三口瓶中依次加入2,2-双(溴甲基)-1,3-丙二醇、二甲基亚砜(DMSO)溶剂,搅拌均匀后再缓慢小心加入NaN3,冷凝回流,干燥,升温至110℃,反应24h后降至室温,萃取得黄色粘稠液体2,2-双(叠氮甲基)丙烷-1,3-二醇(DAED);
步骤3,小分子抗菌单体与预聚体的聚合反应:
取二甲基甲酰胺,开搅拌通氮气1h,排尽空气;滴加二乙胺基三胺,慢加入CuBr 催化剂,以抗菌单体(TMGD)作变量与聚氨酯预聚体,搅拌均匀;在催化剂CuBr催化下,常温条件,聚氨酯亲水预聚体(PV-N3)、DAED、TMGD按一定质量比,制得所需预聚体。
2.如权利要求1所述方法制得的多功能吸湿速干型水性抗菌聚氨酯整理剂在纺织物上的应用。
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