CN116396464A - 一种异佛尔酮二异氰酸酯封端嵌段硅油的制备方法 - Google Patents

一种异佛尔酮二异氰酸酯封端嵌段硅油的制备方法 Download PDF

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CN116396464A
CN116396464A CN202310521402.5A CN202310521402A CN116396464A CN 116396464 A CN116396464 A CN 116396464A CN 202310521402 A CN202310521402 A CN 202310521402A CN 116396464 A CN116396464 A CN 116396464A
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isophorone diisocyanate
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伍成凤
敖苏和
沈聪
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HANGZHOU MEIGAO HUAYI CHEMICAL CO Ltd
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Abstract

本发明涉及纺织助剂领域，尤其涉及一种异佛尔酮二异氰酸酯封端嵌段硅油的制备方法，先由端环氧硅油、二乙烯二胺、异丙醇制得哌嗪封端聚硅氧烷，再加入封端剂异佛尔酮二异氰酸酯进行封端，制得异佛尔酮二异氰酸酯封端嵌段硅油。由上述异佛尔酮二异氰酸酯封端嵌段硅油制得的整理剂不仅具有优异的柔滑手感，而且具有低黄变、低色变以及优异的耐阴离子性能。

Description

一种异佛尔酮二异氰酸酯封端嵌段硅油的制备方法
技术领域
本发明涉及一种硅油，尤其是涉及一种异佛尔酮二异氰酸酯封端嵌段硅油的制备方法，属于纺织助剂领域。
背景技术
近年来，硅油领域发展迅速，尤其在嵌段硅油方面可谓日新月异，各种概念型产品应运而生，如嵌段硅油已经由起初的三元共聚发展到多元共聚，但是，其主要合成工艺还是以端环氧硅油与胺反应制得，通过调节环氧硅油的分子量和选择单组分或多组分的胺，可以制得不同结构的多元共聚硅油及不同风格的产品，但是由于制得乳液的离子性多数为强阳离子，当与阴离子硅油复配时往往就会出现离子性冲突等问题。
阳离子嵌段硅油具有优良的使用稳定性、储存稳定性和易回修等特点，其缺点主要为成膜性较差且分子量不易做大，产品风格主要体现为油感柔滑；阴离子硅油具有优良的成膜性并且分子量容易做大的特点，缺点为储存稳定性差和后期不易回修，产品风格主要体现为干爽挺滑。为了结合两者的优点和弥补两者的缺点，目前有少数染厂采用阳离子硅油和阴离子硅油进行复配使用并且获得了较好的风格产品。众所周知，阳离子和阴离子是会发生离子性冲突，所以，为了最大限度的阻碍阴阳离子之间的冲突，往往就需要加入一些稳定剂，如一些两性表面活性剂、分散剂、醇醚羧酸盐表面活性剂等等，虽然此类添加剂具有一定的效果，但是对硅油手感影响较大并且会引起泡沫问题，不宜多加，因此，不能从根本上解决问题，限制了阳离子硅油与阴离子硅油复配的进一步应用。
发明内容
本发明目的是客服现有技术的不足，提供一种采用异佛尔酮二异氰酸酯对哌嗪封端聚硅氧烷进行封端，利用了异佛尔酮二异氰酸酯基对胺基的封端，从而使得封端后的硅油阳离子性大大减弱，从而在保持原有阳离子硅油所具有的手感同时还具有低黄变、低色变以及较好的耐阴离子性能的一种异佛尔酮二异氰酸酯封端嵌段硅油的制备方法。
为了实现上述目的，本发明采用以下技术方案：
一种异佛尔酮二异氰酸酯封端嵌段硅油的制备方法，按如下合成方法进行，按质量份数计算：
先将1000份数均分子量10000～15000双端环氧硅油、11.5～17.5份二乙烯二胺、300～500份异丙醇加入到装有冷凝回流装置的反应容器中，反应容器升温至80～83℃，在此温度范围内保温反应6～9小时，制得哌嗪封端的聚硅氧烷；
反应容器降温至40～60℃，再向应容器中加入15～23份异佛尔酮二异氰酸酯，保温反应2～4小时，制得异佛尔酮二异氰酸酯封端嵌段硅油。
由于上述技术方案的运用，本发明具有如下优点：
本发明用异佛尔酮二异氰酸酯封端自制的哌嗪封端聚硅氧烷中的胺基，封端后的聚硅氧烷呈现出弱阳离子性，从而具有优异的耐阴离子性能，可有效解决目前阳离子硅油与阴离子硅油的复配时所遇到的主要问题，并且，硅油结构中既含哌嗪基团又含脲基基团，哌嗪基团的引入不仅可以提高整理织物的柔软性，而且对整理后织物的黄变影响较小；脲基基团在经过高温烘焙时会发生解封，产生胺基，能与织物上的活性基团发生交联反应，有效增加了硅油链段的吸附。另外，封端后的哌嗪封端聚硅氧烷中的仲胺基基本已被异佛尔酮二异氰酸酯封端完毕，所以封端后的聚硅氧烷中残留仲胺基基本为零，从而又具有极佳的低色变功能。因此，本发明的异佛尔酮二异氰酸酯封端嵌段硅油既保持阳离子嵌段硅油优异的手感，又具有极佳的低黄变、低色变性能和优异的耐阴离子的性能，从而能很好地解决阳离子硅油与阴离子硅油复配所遇到的主要问题，所以，目标产物具有很好的市场前景。
附图说明
图1为本发明中实施例样品与对比样品的耐阴离子测试外观效果对比表格图。
具体实施方式
下面通过具体实施方式，对本发明做进一步的描述。
实施例1：先将1000克数均分子量10000双端环氧硅油、17.5克二乙烯二胺、300克异丙醇加入到装有冷凝回流装置的反应容器中，反应容器升温至80℃，在此温度范围内保温反应6小时，制得哌嗪封端的聚硅氧烷；反应容器降温至45℃，再向应容器中加入23克异佛尔酮二异氰酸酯，保温反应2小时，制得异佛尔酮二异氰酸酯封端嵌段硅油。
实施例2：先将1000克数均分子量13000双端环氧硅油、13.5克二乙烯二胺、400克异丙醇加入到装有冷凝回流装置的反应容器中，反应容器升温至81℃，在此温度范围内保温反应7小时，制得哌嗪封端的聚硅氧烷；反应容器降温至50℃，再向应容器中加入17.5克异佛尔酮二异氰酸酯，保温反应3小时，制得异佛尔酮二异氰酸酯封端嵌段硅油。
实施例3：先将1000克数均分子量15000双端环氧硅油、11.5克二乙烯二胺、450克异丙醇加入到装有冷凝回流装置的反应容器中，反应容器升温至82℃，在此温度范围内保温反应8小时，制得哌嗪封端的聚硅氧烷；反应容器降温至55℃，再向应容器中加入15克异佛尔酮二异氰酸酯，保温反应4小时，制得异佛尔酮二异氰酸酯封端嵌段硅油。
硅油应用评价工艺：
1.硅油的乳液配制
将实施例样品与市售同类型风格的对比样阳离子硅油样品分别与少量的非离子乳化剂搅拌均匀，然后边搅拌边加水，得到含固量为15％的乳液，最后用冰醋酸调pH至4～6。
2.整理工艺
所用织物：白色纯棉梭织布、咖啡色麂皮绒针织布、黑色涤纶针织布。
整理工艺流程：浸轧工作液(异佛尔酮二异氰酸酯封端嵌段硅油乳液50g/L，一浸一轧，轧余率(白色纯棉梭织布80％～90％、咖啡色麂皮绒针织布60％～80％、黑色涤纶针织布60％～80％)→焙烘(白色纯棉梭织布165℃×50s、咖啡色麂皮绒梭织布190℃×80s、黑色涤纶针织布195℃×50s)→冷却回潮24小时→测试性能。
3.应用性能测试
3.1手感评价
用手触摸法评定，采用多人手触评定法，分为1～5级，数值越大，表示柔滑性越好。
3.2耐阴离子性评价
采用硅油乳液与含量15％磺酸开稀液按1:1、1:2进行复配，观察复配物的外观。
3.3黄变评价
用织物白度仪测试整理后的白色纯棉针织布的光谱反射率，以空白织物对比，白度值越大，表示黄变越小。
3.4色变评价
用电脑测色配色仪测试整理后的咖啡色麂皮绒针织布和黑色涤纶针织布的△E值，以空白织物对比，△E值越小，表示色变越小。
3.5乳液电位测试
用Nano-ZS90型Zeta电位分析仪对乳液进行电位测试，电位值越小，表示阳离子性越弱。
本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油乳液与对比样硅油乳液的柔滑性应用性能测试结果如表1所示：
表1实施例样品与对比样品的整理效果对比
Figure BDA0004220985740000061
由表1可以看出，经本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油制成的乳液对织物进行整理后，相比于对比样，织物手感差别不明显，说明本发明产物完全能达到市售同类型风格阳离子硅油产品的性能。
本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油乳液与对比样硅油乳液的耐阴离子性能测试结果如图1所示：
由图1可以看出，本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油制成的乳液与对比样乳液外观基本一致，但是与含量15％磺酸开稀液按1:1、1:2进行复配后，本发明的硅油乳液复配物外观基本无变化，而对比样复配物发白，足以说明本发明产物具有极佳的耐阴离子性能。
本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油乳液与对比样硅油乳液的黄变性能测试结果如表2所示：
表2实施例样品与对比样品的整理效果对比
Figure BDA0004220985740000071
由表2可以看出，本发明的异佛尔酮二异氰酸酯封端嵌段硅油对织物的白度影响较小且要好于对比样，具有优异的抗黄变性能。
本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油乳液与对比样硅油乳液的色变性能测试结果如表3所示：
表3实施例样品与对比样品的整理效果对比
Figure BDA0004220985740000072
Figure BDA0004220985740000081
由表3可以看出，本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油对织物的色变影响较小，要好于对比样。
本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油乳液与对比样硅油乳液的电位测试结果如表4所示：
表4实施例样品与对比样品的电位对比
试验样品 电位/mV
实施例1 5.02
实施例2 4.92
实施例3 5.24
对比样 28.96
由表4可以看出，本发明的一种异佛尔酮二异氰酸酯封端嵌段硅油的电位值明显低于对比样，说明实施例的阳离子性要弱于对比样，从而具有较好的耐阴离子性能。

Claims (1)

1.一种异佛尔酮二异氰酸酯封端嵌段硅油的制备方法，其特征在于按如下合成方法进行，按质量份数计算：
先将1000份数均分子量10000～15000双端环氧硅油、11.5～17.5份二乙烯二胺、300～500份异丙醇加入到装有冷凝回流装置的反应容器中，反应容器升温至80～83℃，在此温度范围内保温反应6～9小时，制得哌嗪封端的聚硅氧烷；
反应容器降温至40～60℃，再向应容器中加入15～23份异佛尔酮二异氰酸酯，保温反应2～4小时，制得异佛尔酮二异氰酸酯封端嵌段硅油。
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