CN114133514A - 一种应用于纺织品的低环体环保硅油制备方法 - Google Patents
一种应用于纺织品的低环体环保硅油制备方法 Download PDFInfo
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Abstract
本发明公开了一种应用于纺织品的低环体环保硅油制备方法，其步骤包括聚氨酯预聚体的制备和预处理、双端氨基聚硅氧烷的制取和提纯、聚氨酯改性粗成品硅油的制备、聚氨酯改性粗成品硅油的去羟基处理和超声波处理工序，通过该工序的制得的低环体环保硅油，在保留原聚氨酯改性硅油的优良特性的基础上，对聚氨酯改性硅油制备环节中聚氨酯预聚体和双端氨基聚硅氧烷进行了分别独立的除杂提纯，有效的解决了制备中多余试剂的残留问题，同时还在成品环节进行了主链中脱羟基处理，配合超声波处理，得到了性能显著提升的低环体环保硅油，其制备过程简单，效果显著，有利于在纺织品相关行业普及和推广。
Description
技术领域
本发明涉及硅油制备相关领域，具体是一种应用于纺织品的低环体环保硅油制备方法。
背景技术
硅油通常指的是在室温下保持液体状态的线型聚硅氧烷产品，一般分为甲基硅油和改性硅油两类，在各类纺织品的柔软整理剂中存在硅油的广泛使用，其可以赋予纺织品优异的柔软性能，但随着对纺织品要求的不断提高，对原硅油类产品提出了更高的要求。
其中公告号为CN 104628990 B的申请公开了一种用于纺织品的滑弹硅油、制备方法及其应用，其在传统的应用于纺织品的硅油的基础上，应用了聚氨酯分子，聚氨酯分子可赋予纺织品优异的回弹性、滑爽感，同时提升纺织品的耐磨性、耐溶剂性，对纺织品性能进行显著提升。
然而，在应用聚氨酯分子的过程中，其先后制备交联的聚氨酯预聚体和双端氨基聚硅氧烷，再将其混合、催化、搅拌得到聚氨酯改性聚硅氧烷滑弹硅油，在这过程中的使用到多种不同的氧化剂并进过反复的混合反应，在最终的硅油产品上必然会导致氧化剂的残留及其他的附带低挥发性杂质，并且，反应过程中会在一定程度上在主链上形成羟基，引起不必要的交联，引起有效期缩短、抗腐蚀能力减弱等产品质量差异，因此，为了提升其产品力，需要一种进一步改良的应用于纺织品的低环体环保硅油制备方法。
发明内容
本发明的目的在于提供一种应用于纺织品的低环体环保硅油制备方法，以解决上述背景技术中提出的问题。
为实现上述目的，本发明提供如下技术方案：
一种应用于纺织品的低环体环保硅油制备方法，包括以下步骤：
1、添加聚醚二元醇、扩链剂及催化剂制取混合物，在混合物中先后加入异氟尔酮二异氰酸酯和聚醚三元醇和溶剂丁酮，交联反应后得到聚氨酯预聚体，将聚氨酯预聚体处于65-75℃环境中保温静置1小时后，加入与聚氨酯预聚体等量的蒸馏水，向聚氨酯预聚体和蒸馏水混合液中滴入酸性溶液，调节至PH值至6.5-6.7后，停止酸性溶液的添加，改添加碱性溶液，调节PH至8.2-8.5后停止，再改酸性溶液洗至中性，添加酸性溶液和碱性溶液的过程中，保持搅拌的持续进行，减压蒸馏后，去除底部浊液，得到预处理完毕的聚氨酯预聚体；
2、添加八甲基环四硅氧烷及氨基双封头剂及催化剂四甲基氢氧化铵，反应得到双端氨基聚硅氧烷，向双端氨基聚硅氧烷中注入活化剂，在30-38℃条件下预热15min后，通入装有吸附剂的层析柱中，得到提纯后的双端氨基聚硅氧烷；
3、将步骤1和步骤2中的聚氨酯预聚体和双端氨基聚硅氧烷混合，加入催化剂制得聚氨酯改性粗成品硅油；
4、将步骤3中制得聚氨酯改性粗成品硅油中注入聚氨酯改性粗品质量百分比2.4-4.6％的丙醇，加热至沸腾并保持沸腾状态不少于30min，冷却时常温后滴入聚氨酯改性粗品质量百分比6.5-7.8％的醋酐，减压蒸馏后制得准成品；
5、将准成品进行超声波处理，制得成品的低环体环保硅油。
作为本发明进一步的方案：所述步骤1中添加的酸性溶液为硫酸，步骤1中添加的碱性溶液为碳酸钠。
作为本发明再进一步的方案：步骤1的PH检测采用由传感器和二次表组成的PH值测定仪。
作为本发明再进一步的方案：所述步骤2中的活化剂为油酸异辛酯。
作为本发明再进一步的方案：步骤3中的催化剂为二月桂酸二丁基锡。
作为本发明再进一步的方案：所述步骤5中进行超声波处理的时间不低于15min。
与现有技术相比，本发明的有益效果是：
通过该工序的制得的低环体环保硅油，在保留原聚氨酯改性硅油的优良特性的基础上，对聚氨酯改性硅油制备环节中聚氨酯预聚体和双端氨基聚硅氧烷进行了分别独立的除杂提纯，有效的解决了制备中多余试剂的残留问题，同时还在成品环节进行了主链中脱羟基处理，配合超声波处理，得到了性能显著提升的低环体环保硅油，其制备过程简单，效果显著，有利于在纺织品相关行业普及和推广。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明实施例中，一种应用于纺织品的低环体环保硅油制备方法，包括以下步骤；
1、准备聚醚二元醇、扩链剂和催化剂，其中聚醚二元醇预先进行干燥脱水处理，扩链剂可采用4,4′-亚甲基双(3-氯-2,6-二乙基苯胺)，催化剂可采用二月桂酸二丁基锡，其中扩链剂占反应物总质量的1.3-3％，催化剂占反应物总质量的0.03％～0.09％，在具有搅拌、温度监控和冷凝回流功能的反应器中，进行充分的搅拌，后在反应器中加入异氟尔酮二异氰酸酯和适量聚醚三元醇和溶剂丁酮，进行不少于1小时的交联反应，制得聚氨酯预聚体；
将聚氨酯预聚体处于65-75℃环境中保温静置1小时后，加入与聚氨酯预聚体等量的蒸馏水，向聚氨酯预聚体和蒸馏水混合液中滴入酸性溶液，调节至PH值至6.5-6.7后，停止酸性溶液的添加，改添加碱性溶液，调节PH至8.2-8.5后停止，再改酸性溶液洗至中性，添加酸性溶液和碱性溶液的过程中，保持搅拌的持续进行，减压蒸馏后，去除底部浊液，得到预处理完毕的聚氨酯预聚体，其中所用的酸性溶液为硫酸，所添加的碱性溶液为碳酸钠，对制得的聚氨酯预聚体进行酸碱环境的絮凝工序，进行去氧化剂的除杂工序；
2、添加八甲基环四硅氧烷及氨基双封头剂铵，在开启搅拌后，加入占反应物总质量0.02％～0.03％的催化剂四甲基氢氧化铵，升温至100～110℃，反应9～12小时，待反应完全后升温至140～150℃，保温0.5～1小时；在130～140℃、0.09～0.1MPa的条件下除去低沸物，得到双端氨基聚硅氧烷；
向双端氨基聚硅氧烷中注入活化剂，在30-38℃条件下预热15min后，通入装有吸附剂的层析柱中，得到提纯后的双端氨基聚硅氧烷，所添加的活化剂为油酸异辛酯，该成分可以活化双端氨基聚硅氧烷产物中各组分的活性，配合设置有吸附剂的层析柱作用，对双端氨基聚硅氧烷进行有效的提纯；
3、将步骤1中得到的聚氨酯预聚体和步骤2中得到的双端氨基聚硅氧烷，加入装有搅拌器、温度计、冷凝回流装置的反应容器中，再加入占反应物总质量的0.02％～0.03％的催化剂二月桂酸二丁基锡、适量溶剂四氢呋喃降粘，开启搅拌，在氮气保护下升温至60～70℃，反应3～4小时，降温至40～45℃，加入甲乙酮肟封端反应1～1.5小时，减压除去溶剂，得到聚氨酯改性粗成品硅油；
4、将步骤3中制得聚氨酯改性粗成品硅油中注入聚氨酯改性粗品质量百分比2.4-4.6％的丙醇，加热至沸腾并保持沸腾状态不少于30min，冷却时常温后滴入聚氨酯改性粗品质量百分比6.5-7.8％的醋酐，减压蒸馏后制得准成品，通过丙醇并经过沸腾状态作用(必要时可补充酸性溶液，如盐酸等)，可有效的对主链上的芳环的苄位的羟基进行去除作用，同时在后续的醋酐的作用下，将主链上的羟基反应为醋酸酯，醋酸酯是醋酸酯类产品，广泛应用于表面活性剂及聚合物单体等领域，在解决主链羟基对产品性能影响的前提下，还对产品有一定的性能提升作用。
5、将准成品进行超声波处理，制得成品的低环体环保硅油，超声波能改变高分子电解质的结构，从而提高脱水性能。超声波作用高分子电解质一定时间，可以使电解质分支减少，链节变短，更有利于脱水，使得到的硅油产品性能更加优异。
通过该工序的制得的低环体环保硅油，在保留原聚氨酯改性硅油的优良特性的基础上，对聚氨酯改性硅油制备环节中聚氨酯预聚体和双端氨基聚硅氧烷进行了分别独立的除杂提纯，有效的解决了制备中多余试剂的残留问题，同时还在成品环节进行了主链中脱羟基处理，配合超声波处理，得到了性能显著提升的低环体环保硅油，其制备过程简单，效果显著，有利于在纺织品相关行业普及和推广。
在本发明的描述中，术语“第一”、“第二”等仅用于描述目的，而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此，在本发明的描述中，除非另有说明，“多个”的含义是两个或两个以上。限定有“第一”、“第二”等的特征可以明示或者隐含地包括一个或者更多个该特征。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。
此外，应当理解，虽然本说明书按照实施方式加以描述，但并非每个实施方式仅包含一个独立的技术方案，说明书的这种叙述方式仅仅是为清楚起见，本领域技术人员应当将说明书作为一个整体，各实施例中的技术方案也可以经适当组合，形成本领域技术人员可以理解的其他实施方式。
Claims (6)
1.一种应用于纺织品的低环体环保硅油制备方法，其特征在于，包括以下步骤：
1)、添加聚醚二元醇、扩链剂及催化剂制取混合物，在混合物中先后加入异氟尔酮二异氰酸酯和聚醚三元醇和溶剂丁酮，交联反应后得到聚氨酯预聚体，将聚氨酯预聚体处于65-75℃环境中保温静置1小时后，加入与聚氨酯预聚体等量的蒸馏水，向聚氨酯预聚体和蒸馏水混合液中滴入酸性溶液，调节至PH值至6.5-6.7后，停止酸性溶液的添加，改添加碱性溶液，调节PH至8.2-8.5后停止，再改酸性溶液洗至中性，添加酸性溶液和碱性溶液的过程中，保持搅拌的持续进行，减压蒸馏后，去除底部浊液，得到预处理完毕的聚氨酯预聚体；
2)、添加八甲基环四硅氧烷及氨基双封头剂及催化剂四甲基氢氧化铵，反应得到双端氨基聚硅氧烷，向双端氨基聚硅氧烷中注入活化剂，在30-38℃条件下预热15min后，通入装有吸附剂的层析柱中，得到提纯后的双端氨基聚硅氧烷；
3)、将步骤1和步骤2中的聚氨酯预聚体和双端氨基聚硅氧烷混合，加入催化剂制得聚氨酯改性粗成品硅油；
4)、将步骤3中制得聚氨酯改性粗成品硅油中注入聚氨酯改性粗品质量百分比2.4-4.6％的丙醇，加热至沸腾并保持沸腾状态不少于30min，冷却时常温后滴入聚氨酯改性粗品质量百分比6.5-7.8％的醋酐，减压蒸馏后制得准成品；
5)、将准成品进行超声波处理，制得成品的低环体环保硅油。
2.根据权利要求1所述的应用于纺织品的低环体环保硅油制备方法，其特征在于，所述步骤1中添加的酸性溶液为硫酸，步骤1中添加的碱性溶液为碳酸钠。
3.根据权利要求1所述的应用于纺织品的低环体环保硅油制备方法，其特征在于，步骤1的PH检测采用由传感器和二次表组成的PH值测定仪。
4.根据权利要求1所述的应用于纺织品的低环体环保硅油制备方法，其特征在于，所述步骤2中的活化剂为油酸异辛酯。
5.根据权利要求1所述的应用于纺织品的低环体环保硅油制备方法，其特征在于，步骤3中的催化剂为二月桂酸二丁基锡。
6.根据权利要求1所述的应用于纺织品的低环体环保硅油制备方法，其特征在于，所述步骤5中进行超声波处理的时间不低于15min。
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