CN109517134A - 一种水性弹性聚酯乳液的制备方法 - Google Patents
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Abstract
本发明提供一种水性弹性聚酯乳液的制备方法,包括下列步骤:一种水性弹性聚酯乳液的制备方法,包括下列步骤:首先,通过不同的酸与不同的醇发生酯化反应,再在高温低压的环境下完成缩聚反应,分别得到水性端羟基硬段聚酯预聚体和水性端羟基软段聚酯预聚体;其次,由所述水性端羟基硬段聚酯预聚体与所述水性端羟基软段聚酯预聚体混合再加入异佛尔酮二异氰酸酯发生偶合反应得到偶合聚酯分子;再次,所述偶合产物冷却后经过机械粉碎,用40目筛网过筛;最后,形成所述的弹性聚酯乳液,本发明特别适合于针织物变形度大和弹性恢复大的要求,同时赋予涂料印花粘合剂柔软和的手感,克服了丙烯酸酯粘合剂发黏吸尘的缺点。
Description
技术领域
本发明涉及一种水性弹性聚酯乳液的制备方法,用该聚酯乳液作为涂料印花粘合剂,改善印花针织物的手感,属于纺织品涂料印花粘合剂技术领域。
背景技术
涂料印花是将粒径小于1μm的颜料色素微粒借助印花粘合剂在织物表面印花,干燥成膜焙烘后,印花色素被机械固着于纤维表面的一种印花方法。涂料印花适应所有类型纤维织物、印花工艺简单、不需要印花后水洗工序,因而生产效率高,不产生废水,印花色彩鲜艳,轮廓清晰,各项牢度好,是纺织印染行业节能减排的重要发展方向之一。目前,丙烯酸酯共聚乳液是最常用的机织物印花粘合剂,但是不适应于针织品印花。因为针织品的弹性好、服用过程中变形程度大,要求涂料印花粘合剂柔软有弹性;尽管聚丙烯酸酯可通过选择共聚单体的得到柔软的皮膜,但是该皮膜常常发黏吸尘,而且皮膜伸长后弹性回复差。发明专利CN103526580A和CN103541235A采用硅烷偶联剂KH-570对聚丙烯酸酯改性,可改善聚酯丙烯酸酯的发黏吸尘缺点,但是仍然缺乏弹性。因此,针织品涂料印花急需一种柔软有弹性的印花粘合剂。
发明内容
针对聚丙烯酸酯印花粘合剂发黏吸尘和缺乏弹性的不足,本发明的目的在于提供一种水性弹性聚酯乳液的制备方法,根据该方法所获得的弹性聚酯乳液用于针织品涂料印花,具有柔软不发黏和弹性手感。
本发明提供一种水性弹性聚酯乳液的制备方法,其特征在于包括下列步骤。
首先,通过不同的酸与不同的醇发生酯化反应,再在高温低压的环境下完成缩聚反应,分别得到水性端羟基硬段聚酯预聚体和水性端羟基软段聚酯预聚体;
其次,由所述水性端羟基硬段聚酯预聚体与所述水性端羟基软段聚酯预聚体混合再加入异佛尔酮二异氰酸酯发生偶合反应得到偶合聚酯分子,所述异佛尔酮二异氰酸酯克分子数与所述水性端羟基硬段聚酯预聚体、所述水性端羟基软段聚酯预聚体这两种聚酯预聚体的克分子数之和的比率为1/1.4;
再次,所述偶合产物冷却后经过机械粉碎,用40目筛网过筛;
最后,在反应釜内加入软水70-80质量份数,升温至80-95℃,在搅拌下加入粉碎过筛的所述弹性聚酯,30-60分钟后停止搅拌,过100目筛网出料,成为所述的弹性聚酯乳液,所述弹性聚酯乳液固体含量20-30%。
作为本发明水性弹性聚酯乳液的制备方法的改进,本发明水性弹性聚酯乳液的制备方法中的所述水性端羟基硬段聚酯预聚体的制备过程如下:在不锈钢聚酯釜加入对苯二甲酸、间苯二甲酸、间苯二甲酸-5-磺酸钠和乙二醇,以及抗氧化剂和单丁基氧化锡,在氮气的保护下,开启搅拌器完成酯化反应,保持温度不变,关闭氮气并抽真空,内压下降,完成缩聚反应得到所述水性端羟基硬段聚酯预聚体,所述乙二醇与包含所述对苯二甲酸、所述间苯二甲酸和所述间苯二甲酸-5-磺酸钠的芳香族二羧酸的克分子比为1.2:1;所述水性端羟基软段聚酯预聚体的制备过程如下:在不锈钢聚酯釜加入1,6-己二酸、对苯二甲酸、间苯二甲酸、间苯二甲酸-5-磺酸钠、新戊二醇、1,4-丁二醇和乙二醇,以及抗氧化剂和单丁基氧化锡,在氮气的保护下,开启搅拌器完成酯化反应,降低温度,关闭氮气并抽真空,内压下降,完成缩聚反应得到所述水性端羟基软段聚酯预聚体,包含所述对苯二甲酸、所述间苯二甲酸和所述间苯二甲酸-5-磺酸钠的芳香族二羧酸与包含所述乙二醇、所述1,4-丁二醇、所述新戊二醇中的二元醇的克分子比为1.2:1。
作为本发明水性弹性聚酯乳液的制备方法的改进,本发明水性弹性聚酯乳液的制备方法中的所述偶合反应的具体过程如下,所述的水性端羟基硬段聚酯预聚体100公斤放入到2.5升不锈钢反应釜,充氮气并加热至150℃;停止充氮气,抽真空至 ‒0.095 MPa,10分钟后停止真空;再次充氮气并升温至250℃软化,开动搅拌器直至完全熔融后,加入900公斤所述的水性端羟基软段聚酯预聚体,温度下降至150℃;再次抽真空至 ‒0.095 MPa,10分钟后停止真空;反应釜内第三次充氮气并升温至200℃,在搅拌下立刻加入所述异佛尔酮二异氰酸酯33.98公斤,所述异佛尔酮二异氰酸酯克分子数与所述水性端羟基硬段聚酯预聚体、所述水性端羟基软段聚酯预聚体这两种聚酯预聚体的克分子数之和的比率为1/1.4,反应20分钟;用氮气压出反应产物。
与现有丙烯酸酯涂料印花粘合剂的制备方法相比,本发明的有益效果为。
本发明的目的在于提供一种水性弹性聚酯乳液的制备方法,根据该方法所获得的水性弹性聚酯乳液赋予涂料印花粘合剂柔软和的手感,并且克服了丙烯酸酯粘合剂发黏吸尘的缺点,这是因为丙烯酸酯聚合物的柔软性来自于其脂肪侧链,由此也带来了发黏的弊端,而本发明中的的聚酯主链含脂肪族聚酯嵌段,不会产生发黏的问题,本发明的水性弹性聚酯具有软段和硬段嵌段结构,经过涂料印花后在针织物表面成膜后,所述的聚酯膜本体中软硬链段微相分离,赋予针织物印花部分良好的弹性和力学性能,特别适合于针织物变形度大和弹性回复大的要求,而丙烯酸酯印花粘合剂通过无规共聚,软硬单元无规分布,无法为印花针织物提供弹性回复性能。
附图说明
图1为本发明水性弹性聚酯乳液的制备方法中的水性弹性聚酯乳液的结构和性能参数。
图2为本发明水性弹性聚酯乳液的制备方法中的水性端羟基软段聚酯预聚体、水性端羟基硬段聚酯预聚体、以及由所述的软段与硬段预聚体的以90/10质量份数比混合,通过异佛尔酮二异氰酸酯偶合后形成软段和硬段嵌段结构的较高分子量的聚酯,经过在水中乳化、成膜后,用电子强力仪测定的断裂拉伸曲线流程图。
图3本发明水性弹性聚酯乳液的制备方法中第一次和第五次拉伸-回复的瞬时弹性回复率的平均值的计算公式1。
具体实施方式
本实施中按列出的单体和原料数量,用本发明的合成方法制备,分为酯化缩聚和偶合两个反应阶段,均在2.5升不锈钢聚酯反应釜中进行。
在2.5升不锈钢聚酯釜中加入对苯二甲酸531.62公斤、间苯二甲酸73.10公斤、间苯二甲酸-5-磺酸钠95.55公斤和乙二醇297.93公斤,以及1.5公斤抗氧化剂1010和1.0公斤单丁基氧化锡,氮气保护,开动搅拌器同时升温,控制升温速率使回流冷凝管顶温不高于103℃,体系逐渐升温至260℃,保持该温度5小时直至回流冷凝管顶温小于60℃,完成酯化反应;保持体系温度260℃,关闭氮气并抽真空,反应体系内压逐步降低,30分钟后使内压降低至 –0.095 MPa,并维持此温度和真空度2小时,缩聚反应完成;关闭真空泵并用氮气解除真空并加压出料。得到水性端羟基硬段聚酯预聚体。
在2.5升不锈钢聚酯釜中加入1,6-己二酸350.74公斤、对苯二甲酸166.13公斤、间苯二甲酸66.45公斤、间苯二甲酸-5-磺酸钠26.82公斤、乙二醇198.62公斤、新戊二醇124.98公斤和1,4-丁二醇9.01公斤,以及1.5公斤抗氧化剂1010和1.0公斤单丁基氧化锡,充氮气,开动搅拌器同时升温,控制升温速率使回流冷凝管顶温不高于103℃,体系逐渐升温至240℃,保持该温度3小时直至回流冷凝管顶温小于60℃,完成酯化反应;降低体系温度至230℃,关闭氮气并抽真空,反应体系内压逐步降低,30分钟后使内压降低至 ‒0.095MPa,并维持此温度和真空度2小时,缩聚反应完成;然后关闭真空泵并用氮气解除真空并加压出料。得到水性端羟基软段聚酯预聚体。
在所述的水性端羟基硬段聚酯预聚体100公斤放入到2.5升不锈钢反应釜,充氮气并加热至150℃;停止充氮气,抽真空至 ‒0.095 MPa,10分钟后停止真空;再次充氮气并升温至250℃软化,开动搅拌器直至完全熔融后,加入900公斤所述的水性端羟基软段聚酯预聚体,温度下降至150℃;再次抽真空至 ‒0.095 MPa,10分钟后停止真空;反应釜内第三次充氮气并升温至200℃,在搅拌下立刻加入所述异佛尔酮二异氰酸酯33.98公斤,所述异佛尔酮二异氰酸酯克分子数与所述水性端羟基硬段聚酯预聚体、所述水性端羟基软段聚酯预聚体这两种聚酯预聚体的克分子数之和的比率为1/1.4,反应20分钟;用氮气压出反应产物,所述偶合产物冷却后经过机械粉碎,用40目筛网过筛。
在反应釜内加入软水70-80质量份数,升温至80-95℃,在搅拌下加入粉碎过筛的所述弹性聚酯,30-60分钟后停止搅拌,过100目筛网出料,成为所述的水性弹性聚酯乳液,所述水性弹性聚酯乳液固体含量20-30%,所得到的水性弹性聚酯乳液的结构和性能参数由附图1列出。
附图1的来源如下:取样品膜5个样条在电子强力仪测定进行定伸长20%的弹性测试,间距100 mm,速率30 mm/min,定伸长拉伸后停滞10s,释放应力10s后,测定弹性回复率;第二次定伸长20%拉伸,释放应力,测定弹性回复率;如此重复拉伸5次;计算第一次和第五次拉伸-回复的瞬时弹性回复率的平均值,如图3公式1所示。
上式中,L0为拉伸-回复循环前样条长度, ΔL为拉伸-回复循环后样条增长量,ER为拉伸回复循环后样条的瞬时弹性回复率。
与现有丙烯酸酯涂料印花粘合剂的制备方法相比,本发明的有益效果为:
本发明的目的在于提供一种水性弹性聚酯乳液的制备方法,根据该方法所获得的弹性聚酯乳液赋予涂料印花粘合剂柔软和的手感,并且克服了丙烯酸酯粘合剂发黏吸尘的缺点,这是因为丙烯酸酯聚合物的柔软性来自于其脂肪侧链,由此也带来了发黏的弊端,而本发明中的的聚酯主链含脂肪族聚酯嵌段,不会产生发黏的问题,本发明的水性弹性聚酯具有软段和硬段嵌段结构,经过涂料印花后在针织物表面成膜后,所述的聚酯膜本体中软硬链段微相分离,赋予针织物印花部分良好的弹性和力学性能,特别适合于针织物变形度大和弹性回复大的要求,而丙烯酸酯印花粘合剂通过无规共聚,软硬单元无规分布,无法为印花针织物提供弹性回复性能。
虽然本发明已经参考具体的实施方式进行描述,但是本领域技术人员通过阅读上述描述后,将可以对本发明做出显而易见的修改和修饰,而不违背本发明的意图和本质。本发明有意将这些修改和修饰包括在权利要求的范围内。
Claims (3)
1.一种水性弹性聚酯乳液的制备方法,其特征在于包括下列步骤:
首先,通过不同的酸与不同的醇发生酯化反应,再在高温低压的环境下完成缩聚反应,分别得到水性端羟基硬段聚酯预聚体和水性端羟基软段聚酯预聚体;
其次,由所述水性端羟基硬段聚酯预聚体与所述水性端羟基软段聚酯预聚体混合再加入异佛尔酮二异氰酸酯发生偶合反应得到偶合聚酯分子,所述异佛尔酮二异氰酸酯克分子数与所述水性端羟基硬段聚酯预聚体、所述水性端羟基软段聚酯预聚体这两种聚酯预聚体的克分子数之和的比率为1/1.4;
再次,所述偶合产物冷却后经过机械粉碎,用40目筛网过筛;
最后,在反应釜内加入软水70-80质量份数,升温至80-95℃,在搅拌下加入粉碎过筛的所述弹性聚酯,30-60分钟后停止搅拌,过100目筛网出料,成为所述的水性弹性聚酯乳液,所述水性弹性聚酯乳液固体含量20-30%。
2.根据权利要求1所述的水性弹性聚酯乳液的制备方法,其特征在于:所述水性端羟基硬段聚酯预聚体的制备过程如下:在不锈钢聚酯釜加入对苯二甲酸、间苯二甲酸、间苯二甲酸-5-磺酸钠和乙二醇,以及抗氧化剂和单丁基氧化锡,在氮气的保护下,开启搅拌器完成酯化反应,保持温度不变,关闭氮气并抽真空,内压下降,完成缩聚反应得到所述水性端羟基硬段聚酯预聚体,所述乙二醇与包含所述对苯二甲酸、所述间苯二甲酸和所述间苯二甲酸-5-磺酸钠的芳香族二羧酸的克分子比为1.2:1;所述水性端羟基软段聚酯预聚体的制备过程如下:在不锈钢聚酯釜加入1,6-己二酸、对苯二甲酸、间苯二甲酸、间苯二甲酸-5-磺酸钠、新戊二醇、1,4-丁二醇和乙二醇,以及抗氧化剂和单丁基氧化锡,在氮气的保护下,开启搅拌器完成酯化反应,降低温度,关闭氮气并抽真空,内压下降,完成缩聚反应得到所述水性端羟基软段聚酯预聚体,包含所述对苯二甲酸、所述间苯二甲酸和所述间苯二甲酸-5-磺酸钠的芳香族二羧酸与包含所述乙二醇、所述1,4-丁二醇、所述新戊二醇中的二元醇的克分子比为1.2:1。
3.根据权利要求2所述的水性弹性聚酯乳液的制备方法,其特征在于:所述偶合反应的具体过程如下,所述的水性端羟基硬段聚酯预聚体100公斤放入到2.5升不锈钢反应釜,充氮气并加热至150℃;停止充氮气,抽真空至 ‒0.095 MPa,10分钟后停止真空;再次充氮气并升温至250℃软化,开动搅拌器直至完全熔融后,加入900公斤所述的水性端羟基软段聚酯预聚体,温度下降至150℃;再次抽真空至 ‒0.095 MPa,10分钟后停止真空;反应釜内第三次充氮气并升温至200℃,在搅拌下立刻加入所述异佛尔酮二异氰酸酯33.98公斤,所述异佛尔酮二异氰酸酯克分子数与所述水性端羟基硬段聚酯预聚体、所述水性端羟基软段聚酯预聚体这两种聚酯预聚体的克分子数之和的比率为1/1.4,反应20分钟;用氮气压出反应产物。
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