CN109608616A - 一种超亲水蓬松型柔软剂及其制备方法 - Google Patents

一种超亲水蓬松型柔软剂及其制备方法 Download PDF

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CN109608616A
CN109608616A CN201811438079.0A CN201811438079A CN109608616A CN 109608616 A CN109608616 A CN 109608616A CN 201811438079 A CN201811438079 A CN 201811438079A CN 109608616 A CN109608616 A CN 109608616A
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徐炜
朱建华
章东升
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Ningbo Run Wo Hi Tech Materials Polytron Technologies Inc
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Abstract

本发明涉及一种超亲水蓬松型柔软剂及其制备方法，其结构通式为：其中R2为R为R1为m，n，p，x，y，z为整数，且31≤m≤50，7≤n≤9，7≤p≤11，1≤x≤2，1≤y≤4，4≤z≤7。

Description

一种超亲水蓬松型柔软剂及其制备方法
技术领域
本发明涉及精细化工领域，尤其涉及一种超亲水蓬松型柔软剂及其制备方法。
背景技术
近年来，市场对柔软剂的性能要求越来越高，不仅需要使整理后织物具有柔软、蓬松的手感，而且要求对织物的亲水性能影响较小，但是市面上的柔软剂通常做不到两者兼顾，并且在合成的过程中需要加入一定量的溶剂，对生产、使用过程以及生态环境都会造成一定的影响。为了得到既具有较好手感，又具有较好亲水性的柔软剂，有研究者采用聚氨酯与端羟基硅油和氨基硅油进行反应，得到嵌段型聚氨酯有机硅柔软剂，由于聚氨酯与端羟基硅油和氨基硅油的相容性较差，在反应过程中仍需要加入一定量溶剂；同时，聚氨酯链段较长，会使柔软剂的柔软性能下降。
发明内容
本发明所要解决的技术问题是针对现有技术的现状提供一种具有超亲水效果，同时能赋予整理后织物较好的蓬松、丰满手感的超亲水蓬松型柔软剂及其制备方法。
本发明解决上述技术问题所采用的技术方案为：1、一种超亲水蓬松型柔软剂，其特征在于结构通式为：
其中R2为R为R1为m，n，p，x，y，z为整数，且31≤m≤50，7≤n≤9，7≤p≤11，1≤x≤2，1≤y≤4，4≤z≤7。
2、用于制备权利要求1所述的超亲水蓬松型柔软剂的制备方法，其特征在于包括如下步骤，以下所述配比均为质量份数：
(1)将100份的双端羟基聚醚硅油和2～4份的N，N-二甲基环己胺加入到装有温度计、搅拌器和冷凝回流的反应釜中，升温至80～100℃，通入N2，并通过恒压滴液漏斗将11～14份的异佛尔酮二异氰酸酯缓慢的加入到反应釜中，保温反应8～10h后，降温至40～50℃，
该步骤的反应式为：
(2)缓慢加入15～20份的仲胺型聚醚胺，保温反应3～4h，该步骤的反应式为：
(3)加入6～10份的碳酸二甲酯，升温至50～60℃，保温反应2～3h后，开启真空，在真空-0.09～-0.1Mpa下抽除0.5～1h，除去低沸物，冷却降温，出料，得到超亲水蓬松型柔软剂，该步骤的反应式为：
上述反应式中的R2为
R为R1为m，n，p，x，y，z为整数，且31≤m≤50，7≤n≤9，7≤p≤11，1≤x≤2，1≤y≤4，4≤z≤7。
优选的，所述双端羟基聚醚硅油的数均分子量为3000～4000。
优选的，所述仲胺型聚醚胺的数均分子量为500～600。
与现有技术相比，本发明的优点在于：
1、本发明得到的柔软剂是将有机硅链段和聚氨酯链段结合，不仅能使整理后织物具有一定柔软手感，还赋予织物较好的丰满手感。
2、本发明得到的柔软剂分子结构中含有季铵盐基团和聚醚链段，能赋予整理后织物瞬时亲水的效果，季铵盐基团的存在不仅在一定程度上提高了柔软剂的亲水性能，同时也使柔软剂具有一定的抗菌效果。
3、本发明选择N，N-二甲基环己胺替代二月桂酸二丁基锡作为聚氨酯反应催化剂，从而避免了有机锡金属对环境的污染和生物体损害。
4、本发明工艺比较简单，反应过程便于控制，适合工业化生产。
附图说明
图1为本发明中实施例1中超亲水蓬松型柔软剂的红外谱图。
图2为本发明中实施例2中超亲水蓬松型柔软剂的红外谱图。
图3为本发明中实施例3中超亲水蓬松型柔软剂的红外谱图。
具体实施方式
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。
下述实施例的超亲水蓬松型柔软剂的结构通式为
其中R2为R为R1为m，n，p，x，y，z为整数，且31≤m≤50，7≤n≤9，7≤p≤11，1≤x≤2，1≤y≤4，4≤z≤7。
实施例1
将100份的双端羟基聚醚硅油和2份的N，N-二甲基环己胺加入到装有温度计、搅拌器和冷凝回流的反应釜中，升温至100℃，通入N2，并通过恒压滴液漏斗将11份的异佛尔酮二异氰酸酯缓慢的加入到反应釜中，保温反应8h后，降温至40℃，缓慢加入15份的仲胺型聚醚胺，保温反应4h后，加入6份的碳酸二甲酯，升温至50℃，保温反应3h后，开启真空，在真空-0.1Mpa下抽除0.5h，除去低沸物，冷却降温，出料，得到超亲水蓬松型柔软剂。
参见附图1，它是本实施例中超亲水蓬松型柔软剂的红外谱图。3325cm-1处为-NHCOO与-NHCON的N-H的特征吸收峰，1634cm-1处-NHCOO的C＝O的特征吸收峰，1562cm-1为C-N的特征吸收峰，在1260cm-1、1030～1085cm-1、802cm-1处出现三个特征吸收峰，分别为有机硅链段中的Si-CH3、Si-O-CH2、Si-O-Si的特征吸收峰，C-O-C的特征吸收峰在1030～1085cm-1处与Si-O-Si的特征吸收峰重合，在红外谱图中出现了-NHCOO与-NHCON的N-H和C-N的吸收特征峰，表明目标产物成功获得。
实施例2
将100份的双端羟基聚醚硅油和3份的N，N-二甲基环己胺加入到装有温度计、搅拌器和冷凝回流的反应釜中，升温至90℃，通入N2，并通过恒压滴液漏斗将12份的异佛尔酮二异氰酸酯缓慢的加入到反应釜中，保温反应9h后，降温至45℃，缓慢加入18份的仲胺型聚醚胺，保温反应3.5h后，加入8份的碳酸二甲酯，升温至55℃，保温反应2.5h后，开启真空，在真空-0.1Mpa下抽除0.75h，除去低沸物，冷却降温，出料，得到超亲水蓬松型柔软剂。
参见附图2，它是本实施例中超亲水蓬松型柔软剂的红外谱图。3407cm-1处为-NHCOO与-NHCON的N-H的特征吸收峰，1645cm-1处-NHCOO的C＝O的特征吸收峰，1548cm-1为C-N的特征吸收峰，在1253cm-1、1023～1096cm-1、794cm-1处出现三个特征吸收峰，分别为有机硅链段中的Si-CH3、Si-O-CH2、Si-O-Si的特征吸收峰，C-O-C的特征吸收峰在1023～1096cm-1处与Si-O-Si的特征吸收峰重合，在红外谱图中出现了-NHCOO与-NHCON的N-H和C-N的吸收特征峰，表明目标产物成功获得。
实施例3
将100份的双端羟基聚醚硅油和4份的N，N-二甲基环己胺加入到装有温度计、搅拌器和冷凝回流的反应釜中，升温至80℃，通入N2，并通过恒压滴液漏斗将14份的异佛尔酮二异氰酸酯缓慢的加入到反应釜中，保温反应10h后，降温至50℃，缓慢加入20份的仲胺型聚醚胺，保温反应3h后，加入10份的碳酸二甲酯，升温至60℃，保温反应2h后，开启真空，在真空-0.1Mpa下抽除1h，除去低沸物，冷却降温，出料，得到超亲水蓬松型柔软剂。
参见附图3，它是本实施例中超亲水蓬松型柔软剂的红外谱图。3426cm-1处为-NHCOO与-NHCON的N-H的特征吸收峰，1633cm-1处-NHCOO的C＝O的特征吸收峰，1530cm-1为C-N的特征吸收峰，在1265cm-1、1012～1101cm-1、806cm-1处出现三个特征吸收峰，分别为有机硅链段中的Si-CH3、Si-O-CH2、Si-O-Si的特征吸收峰，C-O-C的特征吸收峰在1012～1101cm-1处与Si-O-Si的特征吸收峰重合，在红外谱图中出现了-NHCOO与-NHCON的N-H和C-N的吸收特征峰，表明目标产物成功获得。
将上述实施例制得的超亲水蓬松型柔软剂的进行应用：
1.超亲水蓬松型柔软剂的乳液配制：
超亲水蓬松型柔软剂 50份
醋酸 1份
水 199份
注：原料的份数都是质量份数
所用织物：棉针织织物
2.整理工艺
整理工艺流程：浸轧工作液(超亲水蓬松型柔软剂乳液15g/L，轧液率70％)→预烘焙烘(180℃×45s)→回潮24h→测试
3.应用性能测试
手感评价：用手触摸法评定，采用1～5分评判法，1分最差，5分最好，5人同时评定，取平均值。
亲水性评价：用标准滴管(25滴/mL)从距离布面2cm的高度滴一滴水，静态条件下测试织物吸水完毕所用时间，不同位置滴3次以上，取平均值。
抗菌性测试：参照GB/T 20944.2-2007《纺织品抗菌性能的评价第2部分：吸收法》进行测试，测试整理后织物对大肠杆菌得抑菌率。
本发明的超亲水蓬松型柔软剂应用性能测试结果如表1所示：
表1超亲水蓬松型柔软剂应用性能测试结果
蓬松手感/分 亲水性/s 抑菌率/％
原布 1 4.37 --
实施例1 5 1.41 52.7
实施例2 5 1.20 56.4
实施例3 5 0.98 59.7
市售亲水蓬松型硅油 5 6.38 0
本发明利用双端羟基聚醚硅油、异佛尔酮二异氰酸酯在胺类碱性催化作用下，羟基和异氰酸酯基反应，得到双端含有异氰酸酯基的聚氨酯聚醚有机硅共聚物，而后加入的仲胺型聚醚胺可以在低温条件下与异氰酸酯基发生反应，待反应完成后，利用碳酸二甲酯对产物进行季铵化改性，最后得到同时含有聚氨酯链段、季铵盐基团、聚醚链段和有机硅链段的超亲水蓬松型柔软剂。聚氨酯和有机硅链段的存在可以赋予柔软剂蓬松、丰满的性能，季铵盐基团的存在不仅可以赋予柔软剂好的亲水性能，还能赋予柔软剂一定的抗菌性能。

Claims (4)

1.一种超亲水蓬松型柔软剂，其特征在于结构通式为：
其中
R2为R为R1为m，n，p，x，y，z为整数，且31≤m≤50，7≤n≤9，7≤p≤11，1≤x≤2，1≤y≤4，4≤z≤7。
2.用于制备权利要求1所述的超亲水蓬松型柔软剂的制备方法，其特征在于包括如下步骤，以下所述配比均为质量份数：
(1)将100份的双端羟基聚醚硅油和2～4份的N，N-二甲基环己胺加入到装有温度计、搅拌器和冷凝回流的反应釜中，升温至80～100℃，通入N2，并通过恒压滴液漏斗将11～14份的异佛尔酮二异氰酸酯缓慢的加入到反应釜中，保温反应8～10h后，降温至40～50℃，
该步骤的反应式为：
(2)缓慢加入15～20份的仲胺型聚醚胺，保温反应3～4h，该步骤的反应式为：
(3)加入6～10份的碳酸二甲酯，升温至50～60℃，保温反应2～3h后，开启真空，在真空-0.09～-0.1Mpa下抽除0.5～1h，除去低沸物，冷却降温，出料，得到超亲水蓬松型柔软剂，该步骤的反应式为：
上述反应式中的R2为
R为R1为m，n，p，x，y，z为整数，且31≤m≤50，7≤n≤9，7≤p≤11，1≤x≤2，1≤y≤4，4≤z≤7。
3.根据权利要求2所述的超亲水蓬松型柔软剂的制备方法，其特征在于：所述双端羟基聚醚硅油的数均分子量为3000～4000。
4.根据权利要求2所述的超亲水蓬松型柔软剂的制备方法，其特征在于：所述仲胺型聚醚胺的数均分子量为500～600。
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