CN110591040A - 一种环保型抗菌特性面巾纸用柔软剂的制备方法 - Google Patents
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Abstract
本发明提出了一种环保型抗菌特性面巾纸用柔软剂的制备方法，公开了通过将壳聚糖改性引入季铵盐和有机硅柔软剂合成过程引入铵根离子并对铵根进行季铵化处理的两个过程相合并，既减少了有机硅季铵化处理过程带来的资源消耗，又增加了柔软剂的抗菌特性。壳聚糖作为天然抗菌剂具有良好的生物降解性、环境相容性等诸多优点，使得合成的柔软剂更加环保安全，且柔软剂的合成过程不需要乳化，二者结合简化了生产过程，丰富了产品功能，更利于工厂化生产。
Description
技术领域
本发明涉及面巾纸助剂领域，尤其涉及一种环保型抗菌特性面巾纸用柔软剂的制备方法。
技术背景
第四代有机硅柔软剂即聚醚嵌段氨基改性有机硅柔软剂以其柔软、爽滑和成膜性强等突出特点，广泛应用于各种纤维后处理中，是传统有机硅柔软剂的主流。作为单一结构的高分子，氨基改性有机硅柔软剂在合成过程中添加有大量有机溶剂，因此产品需要乳化过程，且不同配方的氨基硅油柔软剂需要特定乳化剂乳化方能使用，乳化剂的使用使得该类柔软剂成本增加，且产品稳定性和亲水性较差限制了其应用。
本文先在改性封端剂的合成过程中，以壳聚糖代替传统的封端改性剂，在引入铵根离子的过程中引入了具有天然的具有广谱抗菌作用的壳聚糖，既减少了简化处理过程带来的能量消费，又增加了柔软剂的抗菌特性；合成的氨基改性硅油与水性聚氨酯共聚，实现了硅油的自乳化，同时保留了有机硅柔软剂的柔软、爽滑等特性。
发明内容
本发明提出一种环保型抗菌特性面巾纸用柔软剂的制备方法，面巾纸经本柔软剂后处理后，手感柔软、纸巾平滑、亲水性提高、具有抗菌性、且不易变黄等多重优良性能，其生产成本大大降低，易于工业化操作生产。
本发明所采用的技术方案是：
一种环保型抗菌特性面巾纸用柔软剂的制备方法，包括以下步骤：
1)在装有温度计、滴液漏斗和冷凝回流装置的三口烧瓶中加入计量的环氧双封头和壳聚糖，控制反应温度为60-80℃，反应10-12小时，得壳聚糖改性的封端剂，加入适量的八甲基环四硅氧烷(D4)及适量的催化剂四甲基氢氧化铵，并调整温度为120℃，通过改变D4的量得不同相对分子质量的壳聚糖改性的端羟基硅油；
2)将聚乙二醇真空干燥除水置于三口烧瓶中，控制温度为60-80℃，取不同量的多异氰酸酯及适量的催化剂二丁基二月桂酸锡，使得R＝n(-NCO)/n(-OH)的值在1.2-1.8之间，反应得不同R值的聚氨酯预聚体；
3)将步骤1)得到的壳聚糖改性的端羟基硅油和步骤2)得到的聚氨酯预聚体以1:1的摩尔比反应，控制反应温度为80℃，反应2小时，得到环保型抗菌特性面巾纸用柔软剂。
所述壳聚糖分子质量为2×104，脱乙酰度为85％。
所述环氧双封头与壳聚糖的摩尔比为1:1。
所述合成端羟基硅油过程中催化剂四甲基氢氧化铵用量为D4质量的0.05-0.1％。
所述聚乙二醇分子量为1450。
所述多异氰酸酯为异佛尔酮二异氰酸酯。
所述在合成聚氨酯预聚体过程中催化剂二丁基二月桂酸锡用量占体系总质量的0.1-0.2％。
与背景技术相比，本发明具有的有益效果是：
采用上述技术方案，本申请采用壳聚糖代替传统的封端改性剂与环氧双封头反应，再与聚硅氧烷共聚的形式，合成壳聚糖改性端羟基硅油，然后通过与聚氨酯预聚体的共聚，使产品同时具备壳聚糖、聚硅氧烷柔软剂和聚氨酯的多重特性，既具有有机硅柔软剂的高柔软性又增加了产品的亲水性、稳定性和吸附性，通过引入壳聚糖，可有效改善柔软剂的引起面巾纸黄变的缺点，同时壳聚糖作为天然抗菌剂具有良好的生物降解性、环境相容性等诸多优点，使得合成的柔软剂更加环保安全，符合目前大众消费理念，同时该合成过程避免了多功能带来的合成步骤增加，且该合成过程简单，易于实现工业化。
具体实施方式
为了更好的理解本发明，下面通过实施案例对本发明进一步说明，实施例只用于解释本发明，不会对本发明构成任何的限定。
实施例1:
1)在装有温度计、滴液漏斗和冷凝回流装置的三口烧瓶中加入摩尔比为1:1的环氧双封头和分子质量为2×104、脱乙酰度为85％的壳聚糖，控制反应温度为60℃，反应10小时，得壳聚糖改性的封端剂，加入适量的八甲基环四硅氧烷(D4)及适量的催化剂四甲基氢氧化铵，催化剂四甲基氢氧化铵用量为D4质量的0.05％，并调整温度为120℃，通过改变D4的量得不同相对分子质量的壳聚糖改性的端羟基硅油；
2)将分子量为1450的聚乙二醇真空干燥除水置于三口烧瓶中，控制温度为60℃，取不同量的异佛尔酮二异氰酸酯及适量的催化剂二丁基二月桂酸锡，催化剂二丁基二月桂酸锡用量占体系总质量的0.1％，使得R＝n(-NCO)/n(-OH)的值在1.2之间，反应得到聚氨酯预聚体；
3)将步骤1)得到的壳聚糖改性的端羟基硅油和步骤2)得到的聚氨酯预聚体以1:1的摩尔比反应，控制反应温度为80℃，反应2小时，得到环保型抗菌特性面巾纸用柔软剂。
实施例2:
1)在装有温度计、滴液漏斗和冷凝回流装置的三口烧瓶中加入摩尔比为1:1的环氧双封头和分子质量为2×104、脱乙酰度为85％的壳聚糖，控制反应温度为80℃，反应12小时，得壳聚糖改性的封端剂，加入适量的八甲基环四硅氧烷(D4)及适量的催化剂四甲基氢氧化铵，催化剂四甲基氢氧化铵用量为D4质量的0.1％，并调整温度为120℃，通过改变D4的量得不同相对分子质量的壳聚糖改性的端羟基硅油；
2)将分子量为1450的聚乙二醇真空干燥除水置于三口烧瓶中，控制温度为80℃，取不同量的异佛尔酮二异氰酸酯及适量的催化剂二丁基二月桂酸锡，催化剂二丁基二月桂酸锡用量占体系总质量的0.2％，使得R＝n(-NCO)/n(-OH)的值在1.8之间，反应得到聚氨酯预聚体；
3)将步骤1)得到的壳聚糖改性的端羟基硅油和步骤2)得到的聚氨酯预聚体以1:1的摩尔比反应，控制反应温度为80℃，反应2小时，得到环保型抗菌特性面巾纸用柔软剂。
实施例3:
1)在装有温度计、滴液漏斗和冷凝回流装置的三口烧瓶中加入摩尔比为1:1的环氧双封头和分子质量为2×104、脱乙酰度为85％的壳聚糖，控制反应温度为60℃，反应12小时，得壳聚糖改性的封端剂，加入适量的八甲基环四硅氧烷(D4)及适量的催化剂四甲基氢氧化铵，催化剂四甲基氢氧化铵用量为D4质量的0.05％，并调整温度为120℃，通过改变D4的量得不同相对分子质量的壳聚糖改性的端羟基硅油；
2)将分子量为1450的聚乙二醇真空干燥除水置于三口烧瓶中，控制温度为60℃，取不同量的异佛尔酮二异氰酸酯及适量的催化剂二丁基二月桂酸锡，催化剂二丁基二月桂酸锡用量占体系总质量的0.2％，使得R＝n(-NCO)/n(-OH)的值在1.8之间，反应得到聚氨酯预聚体；
3)将步骤1)得到的壳聚糖改性的端羟基硅油和步骤2)得到的聚氨酯预聚体以1:1的摩尔比反应，控制反应温度为80℃，反应2小时，得到环保型抗菌特性面巾纸用柔软剂。
实施例4:
1)在装有温度计、滴液漏斗和冷凝回流装置的三口烧瓶中加入摩尔比为1:1的环氧双封头和分子质量为2×104、脱乙酰度为85％的壳聚糖，控制反应温度为80℃，反应10小时，得壳聚糖改性的封端剂，加入适量的八甲基环四硅氧烷(D4)及适量的催化剂四甲基氢氧化铵，催化剂四甲基氢氧化铵用量为D4质量的0.1％，并调整温度为120℃，通过改变D4的量得不同相对分子质量的壳聚糖改性的端羟基硅油；
2)将分子量为1450的聚乙二醇真空干燥除水置于三口烧瓶中，控制温度为80℃，取不同量的异佛尔酮二异氰酸酯及适量的催化剂二丁基二月桂酸锡，催化剂二丁基二月桂酸锡用量占体系总质量的0.1％，使得R＝n(-NCO)/n(-OH)的值在1.2之间，反应得到聚氨酯预聚体；
3)将步骤1)得到的壳聚糖改性的端羟基硅油和步骤2)得到的聚氨酯预聚体以1:1的摩尔比反应，控制反应温度为80℃，反应2小时，得到环保型抗菌特性面巾纸用柔软剂。
实施例5:
1)在装有温度计、滴液漏斗和冷凝回流装置的三口烧瓶中加入摩尔比为1:1的环氧双封头和分子质量为2×104、脱乙酰度为85％的壳聚糖，控制反应温度为70℃，反应11小时，得壳聚糖改性的封端剂，加入适量的八甲基环四硅氧烷(D4)及适量的催化剂四甲基氢氧化铵，催化剂四甲基氢氧化铵用量为D4质量的0.08％，并调整温度为120℃，通过改变D4的量得不同相对分子质量的壳聚糖改性的端羟基硅油；
2)将分子量为1450的聚乙二醇真空干燥除水置于三口烧瓶中，控制温度为70℃，取不同量的异佛尔酮二异氰酸酯及适量的催化剂二丁基二月桂酸锡，催化剂二丁基二月桂酸锡用量占体系总质量的0.15％，使得R＝n(-NCO)/n(-OH)的值在1.5之间，反应得到聚氨酯预聚体；
3)将步骤1)得到的壳聚糖改性的端羟基硅油和步骤2)得到的聚氨酯预聚体以1:1的摩尔比反应，控制反应温度为80℃，反应2小时，得到环保型抗菌特性面巾纸用柔软剂。
面巾纸经制备的柔软剂进行柔软后处理后，手感爽滑、柔软、具有高抗菌性和广谱抗菌性、保湿性好且不会出现黄变现象。
以上列举的仅是本发明的具体实施例。本发明不限于以上实施例，还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形，均应认为是本发明的保护范围。
Claims (7)
1.一种环保型抗菌特性面巾纸用柔软剂的制备方法，其特征在于，包括以下步骤：
1)在装有温度计、滴液漏斗和冷凝回流装置的三口烧瓶中加入计量的环氧双封头和壳聚糖，控制反应温度为60-80℃，反应10-12小时，得壳聚糖改性的封端剂，加入适量的八甲基环四硅氧烷(D4)及适量的催化剂四甲基氢氧化铵，并调整温度为120℃，通过改变D4的量得不同相对分子质量的壳聚糖改性的端羟基硅油；
2)将聚乙二醇真空干燥除水置于三口烧瓶中，控制温度为60-80℃，取不同量的多异氰酸酯及适量的催化剂二丁基二月桂酸锡，使得R＝n(-NCO)/n(-OH)的值在1.2-1.8之间，反应得不同R值的聚氨酯预聚体；
3)将步骤1)得到的壳聚糖改性的端羟基硅油和步骤2)得到的聚氨酯预聚体以1:1的摩尔比反应，控制反应温度为80℃，反应2小时，得到环保型抗菌特性面巾纸用柔软剂。
2.根据权利要求1所述的一种环保型抗菌特性面巾纸用柔软剂的制备方法，其特征在于：所述壳聚糖分子质量为2×104，脱乙酰度为85％。
3.根据权利要求1所述的一种环保型抗菌特性面巾纸用柔软剂的制备方法，其特征在于：所述环氧双封头与壳聚糖的摩尔比为1:1。
4.根据权利要求1所述的一种环保型抗菌特性面巾纸用柔软剂的制备方法，其特征在于：所述合成端羟基硅油过程中催化剂四甲基氢氧化铵用量为D4质量的0.05-0.1％。
5.根据权利要求1所述的一种环保型抗菌特性面巾纸用柔软剂的制备方法，其特征在于：所述聚乙二醇分子量为1450。
6.根据权利要求1所述的一种环保型抗菌特性面巾纸用柔软剂的制备方法，其特征在于：所述多异氰酸酯为异佛尔酮二异氰酸酯。
7.根据权利要求1所述的一种环保型抗菌特性面巾纸用柔软剂的制备方法，其特征在于：所述在合成聚氨酯预聚体过程中催化剂二丁基二月桂酸锡用量占体系总质量的0.1-0.2％。
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