CN106519243A - 端‑侧基氨基聚醚改性硅油乳液的制备方法 - Google Patents

端‑侧基氨基聚醚改性硅油乳液的制备方法 Download PDF

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CN106519243A
CN106519243A CN201611007952.1A CN201611007952A CN106519243A CN 106519243 A CN106519243 A CN 106519243A CN 201611007952 A CN201611007952 A CN 201611007952A CN 106519243 A CN106519243 A CN 106519243A
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silicone oil
modified silicone
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王耀斌
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Shaanxi Shengmai Petroleum Co Ltd
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Abstract

本发明涉及功能材料技术领域，具体涉及一种端‑侧基氨基聚醚改性硅油乳液的制备方法。端‑侧基氨基聚醚改性硅油乳液的制备方法，包括如下步骤：（1）端‑侧基环氧改性硅油的制备；（2）端‑侧基氨基聚醚改性硅油的制备；（3）端‑侧基氨基聚醚改性硅油乳液的制备。本发明通过封端剂、D4。及环氧偶联剂在碱性催化剂下反应，合成环氧改性硅油，再与聚醚胺(D‑400)反应合成一种双端及侧链同时含有氨基聚醚的改性硅油，并对其乳化。乳液粒径低至十几纳米，透光率高达98％，达到微乳液级别，硅油亲水性以及柔顺性进一步提高。

Description

端-侧基氨基聚醚改性硅油乳液的制备方法
技术领域
本发明涉及功能材料技术领域，具体涉及一种端-侧基氨基聚醚改性硅油乳液的制备方法。
背景技术
高性能碳纤维原丝上油多为硅系油剂，特别是以聚二甲基硅氧烷(PDMS)为母体的改性油剂。氨基硅油是二甲基硅油分子中的部分甲基被氨烃基取代后的产物，由于氨基能与纤维表面的羟基、羧基等相互作用，使硅氧烷主链定向地附着于纤维的表面，可以赋予纤维特殊的反应性、吸附性和柔顺性。但氨基改性硅油亲水性差，制备成乳液时稳定性不好，易出现漂油破乳的现象。而氨基聚醚硅油在兼有氨基改性硅油特性的同时，又有亲水性、抗静电性，其乳液稳定，为贮存、运输及应用创造了便利条件。
目前，氨基聚醚改性硅油的研究主要是端基和侧链两种类型。在碱催化下，以羟基封端的聚二甲基硅油、氨乙基氨丙基甲基二甲氧基硅烷(KH-602)和聚乙二醇为原料，在一定温度下经聚合、缩合反应数小时，减压除去挥发性组分，得侧链型氨基聚醚硅油。以八甲基环四硅氧烷、四甲基二氢二硅氧烷为原料在浓硫酸催化下，制得端基含氢硅油中间体，通过硅氢加成反应将烯丙基环氧聚醚引入，最后通过氨解开环反应将端氨基聚醚引入分子链中制得高固含量双端型氨基聚醚嵌段共聚物。
发明内容
本发明旨在针对上述问题，提出一种端-侧基氨基聚醚改性硅油乳液的制备方法。
本发明的技术方案在于：
端-侧基氨基聚醚改性硅油乳液的制备方法，包括如下步骤：
（1）端-侧基环氧改性硅油的制备：
将D4，3-缩水甘油丙基甲基硅烷及封端剂置于三口烧瓶中，氮气条件下，升温至70℃，加入四甲基氢氧化铵催化剂，反应4 h，反应结束后，抽除低沸物，得到淡黄色端一侧基环氧改性硅油；
（2）端-侧基氨基聚醚改性硅油的制备：
将端-侧基环氧改性硅油、聚醚胺及异丙醇置于三口烧瓶中，氮气条件下，70℃下反应4h，真空旋蒸除去低沸物，得淡黄色端-侧基氨基聚醚改性硅油；
（3）端-侧基氨基聚醚改性硅油乳液的制备：
在30℃下将硅油、AEO-3及蒸馏水置于烧杯中，用高速均质机以10000 r／min搅拌30min使其均匀分散，将乳液置于2000r／min的磁力搅拌器中，将乳化剂加入到乳液中，蒸馏水缓慢滴加到乳液中，搅拌1 h，搅拌结束后用冰醋酸调节乳液pH值在6.0～7.0，即得到半透明到透明的端-侧基氨基聚醚改性硅油乳液。
本发明的技术效果在于：
本发明通过封端剂、D4。及环氧偶联剂在碱性催化剂下反应，合成环氧改性硅油，再与聚醚胺(D-400)反应合成一种双端及侧链同时含有氨基聚醚的改性硅油，并对其乳化。乳液粒径低至十几纳米，透光率高达98％，达到微乳液级别，硅油亲水性以及柔顺性进一步提高。
具体实施方式
端-侧基氨基聚醚改性硅油乳液的制备方法，包括如下步骤：
（1）端-侧基环氧改性硅油的制备：
将D4，3-缩水甘油丙基甲基硅烷及封端剂置于三口烧瓶中，氮气条件下，升温至70℃，加入四甲基氢氧化铵催化剂，反应4 h，反应结束后，抽除低沸物，得到淡黄色端一侧基环氧改性硅油；
（2）端-侧基氨基聚醚改性硅油的制备：
将端-侧基环氧改性硅油、聚醚胺及异丙醇置于三口烧瓶中，氮气条件下，70℃下反应4h，真空旋蒸除去低沸物，得淡黄色端-侧基氨基聚醚改性硅油；
（3）端-侧基氨基聚醚改性硅油乳液的制备：
在30℃下将硅油、AEO-3及蒸馏水置于烧杯中，用高速均质机以10000 r／min搅拌30min使其均匀分散，将乳液置于2000r／min的磁力搅拌器中，将乳化剂加入到乳液中，蒸馏水缓慢滴加到乳液中，搅拌1 h，搅拌结束后用冰醋酸调节乳液pH值在6.0～7.0，即得到半透明到透明的端-侧基氨基聚醚改性硅油乳液。

Claims (1)

1.端-侧基氨基聚醚改性硅油乳液的制备方法，其特征在于：包括如下步骤：
（1）端-侧基环氧改性硅油的制备：
将D4，3-缩水甘油丙基甲基硅烷及封端剂置于三口烧瓶中，氮气条件下，升温至70℃，加入四甲基氢氧化铵催化剂，反应4 h，反应结束后，抽除低沸物，得到淡黄色端一侧基环氧改性硅油；
（2）端-侧基氨基聚醚改性硅油的制备：
将端-侧基环氧改性硅油、聚醚胺及异丙醇置于三口烧瓶中，氮气条件下，70℃下反应4h，真空旋蒸除去低沸物，得淡黄色端-侧基氨基聚醚改性硅油；
（3）端-侧基氨基聚醚改性硅油乳液的制备：
在30℃下将硅油、AEO-3及蒸馏水置于烧杯中，用高速均质机以10000 r／min搅拌30min使其均匀分散，将乳液置于2000r／min的磁力搅拌器中，将乳化剂加入到乳液中，蒸馏水缓慢滴加到乳液中，搅拌1 h，搅拌结束后用冰醋酸调节乳液pH值在6.0～7.0，即得到半透明到透明的端-侧基氨基聚醚改性硅油乳液。
CN201611007952.1A 2016-11-16 2016-11-16 端‑侧基氨基聚醚改性硅油乳液的制备方法 Pending CN106519243A (zh)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107759794A (zh) * 2017-09-06 2018-03-06 四川省纺织科学研究院 一种侧链含叔胺基的主链嵌端氨基硅油的制备方法及应用
CN107814730A (zh) * 2017-09-06 2018-03-20 四川益欣科技有限责任有限公司 一种含侧叔胺基的线型梳状环氧多胺化合物的制备方法
CN108219144A (zh) * 2018-01-04 2018-06-29 佛山市三水古闰纺织印染研究院有限公司 一种双端环氧基硅油的制备方法
CN108219147A (zh) * 2018-01-04 2018-06-29 佛山市三水古闰纺织印染研究院有限公司 一种亲水硅油的制备方法
CN110229341A (zh) * 2019-05-31 2019-09-13 丽王化工(南通)有限公司 一种有机硅树脂基非离子型超分散剂及其制备方法
CN111088702A (zh) * 2019-12-19 2020-05-01 广东轻工职业技术学院 一种新型亲水性聚醚胺改性有机硅柔软剂的制备方法
CN112832029A (zh) * 2021-03-01 2021-05-25 陕西工业职业技术学院 一种用于织物柔软整理的整理剂的制备方法
CN114214124A (zh) * 2021-12-29 2022-03-22 威莱(广州)日用品有限公司 一种柔顺护色洗衣液及其制备方法

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107759794A (zh) * 2017-09-06 2018-03-06 四川省纺织科学研究院 一种侧链含叔胺基的主链嵌端氨基硅油的制备方法及应用
CN107814730A (zh) * 2017-09-06 2018-03-20 四川益欣科技有限责任有限公司 一种含侧叔胺基的线型梳状环氧多胺化合物的制备方法
CN107759794B (zh) * 2017-09-06 2020-04-28 四川省纺织科学研究院 一种侧链含叔胺基的主链嵌段氨基硅油的制备方法及应用
CN108219144A (zh) * 2018-01-04 2018-06-29 佛山市三水古闰纺织印染研究院有限公司 一种双端环氧基硅油的制备方法
CN108219147A (zh) * 2018-01-04 2018-06-29 佛山市三水古闰纺织印染研究院有限公司 一种亲水硅油的制备方法
CN110229341A (zh) * 2019-05-31 2019-09-13 丽王化工(南通)有限公司 一种有机硅树脂基非离子型超分散剂及其制备方法
CN111088702A (zh) * 2019-12-19 2020-05-01 广东轻工职业技术学院 一种新型亲水性聚醚胺改性有机硅柔软剂的制备方法
CN112832029A (zh) * 2021-03-01 2021-05-25 陕西工业职业技术学院 一种用于织物柔软整理的整理剂的制备方法
CN114214124A (zh) * 2021-12-29 2022-03-22 威莱(广州)日用品有限公司 一种柔顺护色洗衣液及其制备方法

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