CN108794723A - 一种生物基哑光水性聚氨酯分散体及其制备方法 - Google Patents
一种生物基哑光水性聚氨酯分散体及其制备方法 Download PDFInfo
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- CN108794723A CN108794723A CN201810364190.3A CN201810364190A CN108794723A CN 108794723 A CN108794723 A CN 108794723A CN 201810364190 A CN201810364190 A CN 201810364190A CN 108794723 A CN108794723 A CN 108794723A
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Classifications
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- Chemical Kinetics & Catalysis (AREA)
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- Polyurethanes Or Polyureas (AREA)
Abstract
本发明提供一种生物基哑光水性聚氨酯分散体及其制备方法，生物基哑光水性聚氨酯分散体包括：大分子多元醇20～50份；生物基多元醇5～30份；异氰酸酯10～30份；羧酸型亲水扩链剂0.5～10份；中和剂3～5份；多元醇扩链剂1～10份；磺酸型亲水扩链剂0.5～5份；小分子胺后扩链剂0.5～10份；本发明制备的生物基哑光水性聚氨酯分散体在后扩链的过程中加入磺酸型亲水扩链剂2‑[(2‑氨乙基)氨基]乙磺酸钠，提高乳液的稳定性而不过多的降低乳液的粒径，保持乳液成膜的哑光特性；水合肼与异氰酸酯有极高的反应活性，在扩链反应时，不仅与乳胶粒内部的NCO反应，还可以与周围乳胶粒中的NCO基团反应，使两个乳胶粒相互融合而增大粒径，降低乳液成膜平整度，使表面具有哑光特性。
Description
技术领域
本发明涉及高分子树脂技术领域，具体公开了一种生物基哑光水性聚氨酯分散体及其制备方法。
背景技术
水性聚氨酯以水为分散介质，根据粒子尺寸，可分为水乳化型、水分散型和水溶型三种。它不含或少含有机溶剂、不燃、无毒、不污染环境、易运输、易运输、易保存、使用方便，且具有聚氨酯固有的高强度、耐磨损等优良特性。
随着时代的发展，以哑光为表面装饰的产品越来越受到追捧，哑光材料也从一般自然界中存在的高填充料，发展到微粉蜡，进而到无机消光粉。它们虽然具备消光性，但其缺点也是明显的：填料的添加导致涂层脆性增加，物理性能大幅度降低，传统材料使用废弃后很难在自然环境中降解，会对环境造成一定的污染，且生物基哑光水性聚氨酯分散体的稳定性也是需要进一步的提高。因此，研发一种储存稳定性好、哑光性、机械性能优异，且环保的水性聚氨酯分散体具有良好的应用前景。
发明内容
本发明的目的在于克服现有的缺陷，提供一种生物基哑光水性聚氨酯分散体及其制备方法，该水性聚氨酯分散体储存稳定性好，耐水性佳，耐黄变性好，机械性能优异。且在大分子链中引入生物基成分可以有效提高成品的自然降解性。
为解决上述问题，本发明是通过以下技术方案实现的；
一种生物基哑光水性聚氨酯分散体，包括以下原料组分及重量百分比：
优选地，所述大分子多元醇为聚己内酯二醇、聚四氢呋喃二醇、聚碳酸酯二醇和聚己二酸丁二醇酯二醇中的任意一种或多种。
优选地，所述生物基多元醇为大豆油多元醇、棕榈油多元醇、松香酯多元醇和松节油酯二醇中的任意一种或多种。
优选地，所述异氰酸酯为六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯和二环己基甲烷二异氰酸酯中的任意一种或多种。
优选地，所述中和剂包括三乙胺、二乙醇胺和三乙醇胺中的任意一种或多种。
优选地，所述羧酸型亲水扩链剂选择为DMPA。
优选地，所述多元醇扩链剂为1.4-二羟基丁烷、新戊二醇、甲基丙二醇或1.4-环己基二甲醇中的一种或者两种的混合。
优选地，所述磺酸型亲水扩链剂为2-[(2-氨乙基)氨基]乙磺酸钠；后扩链的过程中加入亲水扩链剂2-[(2-氨乙基)氨基]乙磺酸钠可以提高乳液的稳定性而不过多的降低乳液的粒径，保持乳液成膜的哑光特性。
优选地，所述小分子胺后扩链剂包括乙二胺、异氟尔酮二胺、水合肼和二氨基二环己基甲烷中的任意一种或多种；小分子胺后扩链剂优选为水合肼，水合肼与异氰酸酯有极高的反应活性，在扩链反应时，不仅与乳胶粒内部的NCO反应，还可以与周围乳胶粒中的NCO基团反应，使两个乳胶粒相互融合而增大粒径，降低乳液成膜平整度，使表面具有哑光特性。
本发明还公开了制备如上述生物基哑光水性聚氨酯分散体的方法，包括以下步骤：
1)将所述量的大分子多元醇、所述量的生物基多元醇与所述量的异氰酸酯加入反应器，在80～100℃下搅拌1～3h，然后在搅拌下加入所述量的羧酸型亲水扩链剂，以及10～15份的蓖麻油，并在80～100℃下继续搅拌1～2h，再加入所述量的多元醇扩链剂，继续在80～100℃下搅拌1～2h，加入催化剂和份量为蓖麻油两倍的丙酮，恒温反应2～4小时，获得水性聚氨酯预聚体；
2)将所述水性聚氨酯预聚体降温至1～20℃，加入所述量的中和剂后转移至高速分散机内，高速搅拌下加入磺酸型亲水扩链剂和去离子水；然后加入所述量的小分子胺后扩链剂，获得生物基哑光水性聚氨酯分散体。
本发明与现有技术相比具有以下优点：
本发明中，首先使得异氰酸酯单体与生物基多元醇及大分子多元醇进行反应，得到低粘度的反应物，然后依次加入羧酸型亲水扩链剂、多元醇扩链剂搅拌均匀，充分反映后，乳化分散，从而制备出储存稳定性好，耐热、耐冷、耐水性能优良，且具有哑光特性的水性聚氨酯分散体。
本发明的有益效果为，本专利水性聚氨酯采用生物基多元醇替代部分石油基多元醇，有效的提高了产品的自然降解性，并且产品具有很好的哑光特性。
具体实施方式
下面结合实施例进一步阐述本发明。应理解，实施例仅用于说明本发明，而非限制本发明的范围。
实施例1-4是生物基哑光水性聚氨酯分散体的具体配方以及制备方法的实施例，实施例中的各原料的组分和配比分别参见表1，表中各原料组分的含量为重量份。
表1实施例1～4中各原料组分的重量配比
为了进一步的增加磺酸型亲水扩链剂2-[(2-氨乙基)氨基]乙磺酸钠对乳液稳定性的影响，以及水合肼对哑光性的影响，增加对比例1至对比例4，其中对比例1和对比例2中的的制备方法同实施例1和实施例2，但是其中不添加磺酸型亲水扩链剂2-[(2-氨乙基)氨基]乙磺酸钠，对比例3和对比例4的制备方法同实施例1和实施例2，只是将小分子扩链剂选择为乙二胺。
表2对比例1～4中各原料组分的重量配比
实施例1
一种生物基哑光水性聚氨酯分散体，包括以下步骤：
称取43g聚己内酯二醇(PCL2000，相对分子质量为2000)和7.4g生物基多元醇(HM10100，相对分子质量为2500)，放入反应器中，搅拌下加入25g异氟尔酮二异氰酸酯，保持温度90℃，搅拌2小时。降温至80℃加入2g二羟甲基丙酸(DMPA)，11g蓖麻油，2g甲基丙二醇，并保持80℃搅拌2小时，然后降温到65℃加入催化剂和20g丙酮，恒温反应3h，制得水性聚氨酯预聚体。
将水性聚氨酯预聚体降温至15℃，加入1.5g三乙胺，搅拌1分钟，然后转移至高速乳化机内，在1400r/min的转速下加入1g2-[(2-氨乙基)氨基]乙磺酸钠和184g去离子水，相转变后缓慢加入0.8g水合肼后扩链试剂，制得生物基哑光水性聚氨酯分散体。
实施例2
一种生物基哑光水性聚氨酯分散体，包括以下步骤：
称取30g聚己内酯二醇(PCL2000，相对分子质量为2000)和14.7g生物基多元醇(HM10100，相对分子质量为2500)，放入反应器中，搅拌下加入25g异氟尔酮二异氰酸酯，保持温度90℃，搅拌2小时。降温至80℃加入2g二羟甲基丙酸(DMPA)，11g蓖麻油，2g甲基丙二醇，并保持80℃搅拌2小时，然后降温到65℃加入催化剂和20g丙酮，恒温反应3h，制得水性聚氨酯预聚体。
将水性聚氨酯预聚体降温至15℃，加入1.5g三乙胺，搅拌1分钟，然后转移至高速乳化机内，在1400r/min的转速下加入1g2-[(2-氨乙基)氨基]乙磺酸钠和180g去离子水，相转变后缓慢加入0.8g水合肼后扩链试剂，制得生物基哑光水性聚氨酯分散体。
实施例3
一种生物基哑光水性聚氨酯分散体，包括以下步骤：
称取30g聚四氢呋喃二醇(PTMG2000，相对分子质量为2000)和14.7g生物基多元醇(HM10100，相对分子质量为2500)，放入反应器中，搅拌下加入25g异氟尔酮二异氰酸酯，保持温度90℃，搅拌2小时。降温至80℃加入2g二羟甲基丙酸(DMPA)，11g蓖麻油，2g甲基丙二醇，并保持80℃搅拌2小时，然后降温到65℃加入催化剂和20g丙酮，恒温反应3h，制得水性聚氨酯预聚体。
将水性聚氨酯预聚体降温至15℃，加入1.5g三乙胺，搅拌1分钟，然后转移至高速乳化机内，在1400r/min的转速下加入1g2-[(2-氨乙基)氨基]乙磺酸钠和180g去离子水，相转变后缓慢加入1.6g水合肼后扩链试剂，制得生物基哑光水性聚氨酯分散体。
实施例4
一种生物基哑光水性聚氨酯分散体，包括以下步骤：
称取30g聚己二酸丁二醇酯二醇(PAA2000，相对分子质量为2000)和14.7g生物基多元醇(HM10100，相对分子质量为2500)，放入反应器中，搅拌下加入25g异氟尔酮二异氰酸酯，保持温度90℃，搅拌2小时。降温至80℃加入2g二羟甲基丙酸(DMPA)，11g蓖麻油，2g甲基丙二醇，并保持80℃搅拌2小时，然后降温到65℃加入催化剂和20g丙酮，恒温反应3h，制得水性聚氨酯预聚体。
将水性聚氨酯预聚体降温至15℃，加入1.5g三乙胺，搅拌1分钟，然后转移至高速乳化机内，在1400r/min的转速下加入1g2-[(2-氨乙基)氨基]乙磺酸钠和180g去离子水，相转变后缓慢加入1.6g水合肼后扩链试剂，制得生物基哑光水性聚氨酯分散体。
对比例1
一种生物基哑光水性聚氨酯分散体，包括以下步骤：
称取43g聚己内酯二醇(PCL2000，相对分子质量为2000)和7.4g生物基多元醇(HM10100，相对分子质量为2500)，放入反应器中，搅拌下加入25g异氟尔酮二异氰酸酯，保持温度90℃，搅拌2小时。降温至80℃加入2g二羟甲基丙酸(DMPA)，11g蓖麻油，2g甲基丙二醇，并保持80℃搅拌2小时，然后降温到65℃加入催化剂和20g丙酮，恒温反应3h，制得水性聚氨酯预聚体。
将水性聚氨酯预聚体降温至15℃，加入1.5g三乙胺，搅拌1分钟，然后转移至高速乳化机内，在1400r/min的转速下加入184g去离子水，相转变后缓慢加入0.8g水合肼后扩链试剂，制得生物基哑光水性聚氨酯分散体。
对比例2
一种生物基哑光水性聚氨酯分散体，包括以下步骤：
称取30g聚己内酯二醇(PCL2000，相对分子质量为2000)和14.7g生物基多元醇(HM10100，相对分子质量为2500)，放入反应器中，搅拌下加入25g异氟尔酮二异氰酸酯，保持温度90℃，搅拌2小时。降温至80℃加入2g二羟甲基丙酸(DMPA)，11g蓖麻油，2g甲基丙二醇，并保持80℃搅拌2小时，然后降温到65℃加入催化剂和20g丙酮，恒温反应3h，制得水性聚氨酯预聚体。
将水性聚氨酯预聚体降温至15℃，加入1.5g三乙胺，搅拌1分钟，然后转移至高速乳化机内，在1400r/min的转速下加入180g去离子水，相转变后缓慢加入0.8g水合肼后扩链试剂，制得生物基哑光水性聚氨酯分散体。
对比例3
一种生物基哑光水性聚氨酯分散体，包括以下步骤：
称取43g聚己内酯二醇(PCL2000，相对分子质量为2000)和7.4g生物基多元醇(HM10100，相对分子质量为2500)，放入反应器中，搅拌下加入25g异氟尔酮二异氰酸酯，保持温度90℃，搅拌2小时。降温至80℃加入2g二羟甲基丙酸(DMPA)，11g蓖麻油，2g甲基丙二醇，并保持80℃搅拌2小时，然后降温到65℃加入催化剂和20g丙酮，恒温反应3h，制得水性聚氨酯预聚体。
将水性聚氨酯预聚体降温至15℃，加入1.5g三乙胺，搅拌1分钟，然后转移至高速乳化机内，在1400r/min的转速下加入1g2-[(2-氨乙基)氨基]乙磺酸钠和184g去离子水，相转变后缓慢加入0.8g乙二胺后扩链试剂，制得生物基哑光水性聚氨酯分散体。
对比例4
一种生物基哑光水性聚氨酯分散体，包括以下步骤：
称取30g聚己内酯二醇(PCL2000，相对分子质量为2000)和14.7g生物基多元醇(HM10100，相对分子质量为2500)，放入反应器中，搅拌下加入25g异氟尔酮二异氰酸酯，保持温度90℃，搅拌2小时。降温至80℃加入2g二羟甲基丙酸(DMPA)，11g蓖麻油，2g甲基丙二醇，并保持80℃搅拌2小时，然后降温到65℃加入催化剂和20g丙酮，恒温反应3h，制得水性聚氨酯预聚体。
将水性聚氨酯预聚体降温至15℃，加入1.5g三乙胺，搅拌1分钟，然后转移至高速乳化机内，在1400r/min的转速下加入1g2-[(2-氨乙基)氨基]乙磺酸钠和180g去离子水，相转变后缓慢加入0.8g乙二胺后扩链试剂，制得生物基哑光水性聚氨酯分散体。
检测结果：
1、对上述实施例1～4和对比例1～4中制备的生物基哑光水性聚氨酯分散体进行性能测试：
(1)粘度：用涂料4号杯进行测试。粘度测试结果如表1所示。
(2)储存稳定性：将乳液放置在50℃的环境中，三周后，观察粘度及外观有无异常，比如粘度是否增大，外观是否变的更白更倾向不透明，是否有渣滓出现等异常情况。储存稳定性的测试结果如表1所示。
2、水性聚氨酯的光泽，指对入射角为60度的试样表面的镜面反射光强度与相同条件下折射率为定值的白瓷板表面的镜面反射光强之比。
表1实施例1～4和对比例1～4制得的生物基哑光水性聚氨酯分散体的性能结果
表2实施例1～4和对比例1～4制得的生物基哑光水性聚氨酯分散体的光泽
| 实施例1 | 实施例2 | 实施例3 | 实施例4 | 对比例1 | 对比例2 | 对比例3 | 对比例4 | |
| 光泽 | 20 | 23 | 12 | 15 | 20 | 23 | 25 | 27 |
从表1、表2可以看出，实施例1～4制得的生物基哑光水性聚氨酯分散体的外观、粘度正常，还具有优良的机械性能、储存稳定性，并且有较好的哑光特性。对比例1-2中不添加磺酸型亲水扩链剂2-[(2-氨乙基)氨基]乙磺酸钠时，制得的生物基哑光水性聚氨酯分散体的稳定性降低，50℃储存3周稳定性有异常；而添加磺酸型亲水扩链剂2-[(2-氨乙基)氨基]乙磺酸钠的实施例1-2中，制得的生物基哑光水性聚氨酯分散体在50℃储存3周稳定性无异常。而对比例3和对比例4，将小分子扩链剂选择为乙二胺，制得的生物基哑光水性聚氨酯分散体的哑光性变差，其光泽分别是25和27，较实施例1和实施例2中，小分子扩链剂选择为水合肼的光泽为20和23，可见水合肼与异氰酸酯有极高的反应活性，经扩链反应使与预聚体的分子结构更为复杂，成膜平整度降低，光泽降低。
以上，仅为本发明的较佳实施例，并非对本发明任何形式上和实质上的限制，应当指出，对于本技术领域的普通技术人员，在不脱离本发明方法的前提下，还将可以做出若干改进和补充，这些改进和补充也应视为本发明的保护范围。凡熟悉本专业的技术人员，在不脱离本发明的精神和范围的情况下，当可利用以上所揭示的技术内容而做出的些许更动、修饰与演变的等同变化，均为本发明的等效实施例；同时，凡依据本发明的实质技术对上述实施例所作的任何等同变化的更动、修饰与演变，均仍属于本发明的技术方案的范围内。
Claims (10)
1.一种生物基哑光水性聚氨酯分散体，其特征在于，包括以下原料组分及重量百分比：
2.如权利要求1所述的生物基哑光水性聚氨酯分散体，其特征在于：所述大分子多元醇为聚己内酯二醇、聚四氢呋喃二醇、聚碳酸酯二醇和聚己二酸丁二醇酯二醇中的任意一种或多种。
3.如权利要求1所述的生物基哑光水性聚氨酯分散体，其特征在于：所述生物基多元醇为大豆油多元醇、棕榈油多元醇、松香酯多元醇和松节油酯二醇中的任意一种或多种。
4.如权利要求1所述的生物基哑光水性聚氨酯分散体，其特征在于：所述异氰酸酯为六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯和二环己基甲烷二异氰酸酯中的任意一种或多种。
5.如权利要求1～4任意所述的生物基哑光水性聚氨酯分散体，其特征在于：所述中和剂包括三乙胺、二乙醇胺和三乙醇胺中的任意一种或多种。
6.如权利要求5所述的生物基哑光水性聚氨酯分散体，其特征在于：所述羧酸型亲水扩链剂选择为DMPA；所述多元醇扩链剂为1.4-二羟基丁烷、新戊二醇、甲基丙二醇或1.4-环己基二甲醇中的一种或者两种的混合。
7.如权利要求5所述的生物基哑光水性聚氨酯分散体，其特征在于：所述磺酸型亲水扩链剂为2-[(2-氨乙基)氨基]乙磺酸钠。
8.如权利要求5所述的生物基哑光水性聚氨酯分散体，其特征在于：所述小分子胺后扩链剂包括乙二胺、异氟尔酮二胺、水合肼和二氨基二环己基甲烷中的任意一种或多种。
9.如权利要求5所述的生物基哑光水性聚氨酯分散体，其特征在于：所述小分子胺后扩链剂为水合肼。
10.一种制备如权利要求1～9任一所述的生物基哑光水性聚氨酯分散体的方法，其特征在于：包括以下步骤：
1)将所述量的大分子多元醇、所述量的生物基多元醇与所述量的异氰酸酯加入反应器，在80～100℃下搅拌1～3h，然后在搅拌下加入所述量的羧酸型亲水扩链剂，以及10～15份的蓖麻油，并在80～100℃下继续搅拌1～2h，再加入所述量的多元醇扩链剂，继续在80～100℃下搅拌1～2h，加入催化剂和份量为蓖麻油两倍的丙酮，恒温反应2～4小时，获得水性聚氨酯预聚体；
2)将所述水性聚氨酯预聚体降温至1～20℃，加入所述量的中和剂后转移至高速分散机内，高速搅拌下加入磺酸型亲水扩链剂和去离子水；然后加入所述量的小分子胺后扩链剂，获得生物基哑光水性聚氨酯分散体。
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