CN115536809B - 低光泽高物性自消光水性uv聚氨酯分散体及其制备方法 - Google Patents
低光泽高物性自消光水性uv聚氨酯分散体及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种低光泽高物性自消光水性UV聚氨酯分散体及其制备方法。制备方法包括以下步骤：a.将40～80份大分子二醇、0～5份小分子二醇、3～7份亲水扩链剂、70～140份二异氰酸酯、催化剂0.1～0.3份混合后，于70～95℃反应2～3h得预聚体；b.往预聚体中加入封端单体25～80份、活性单体0～80份、对甲氧基苯酚0.05～0.1份、丁酮0～50份，于60～85℃反应2～4h，得到UV预聚物；c.加入2～8份中和剂中和30min，然后边搅拌边加入450～600份去离子水乳化；d.乳化完成后加入5～30份扩链剂于20～40℃至反应完全，然后减压蒸馏除去丁酮，得到低光泽高物性自消光水性UV聚氨酯分散体。本发明在保持原有自消光水性聚氨酯低光泽度的同时，提高水性自消光聚氨酯的树脂的成膜强度、附着力等物性，实现低光泽度和高物性的统一。
Description
技术领域
本发明属于聚合物材料领域，具体涉及一种低光泽高物性自消光水性UV聚氨酯分散体及其制备方法。
背景技术
以自消光型水性聚氨酯为代表的消光树脂，无需外添加消光剂即有消光效果，克服了无机消光剂相容性的问题，能提供光泽柔和，高级感强的表面装饰效果，近年来在包装膜、皮革涂饰、油墨、造纸、汽车贴膜等领域越来越流行。但是常规的水性自消光聚氨酯树脂，特别是低光泽度的水性自消光聚氨酯树脂，由于成膜致密性差，导致综合物性不佳，通常需要复配水性树脂搭配使用，但复配后的光泽度通常会提高，被涂物的外观和手感通常会受到较大的影响。
发明内容
针对现有技术中上述的不足，本发明的目的在于提供一种低光泽高物性自消光水性UV聚氨酯分散体及其制备方法，在保持原有自消光水性聚氨酯低光泽度的同时，提高水性自消光聚氨酯的树脂的成膜强度、附着力等物性。
为了实现上述目的，本发明提供了一种低光泽高物性自消光水性UV聚氨酯分散体的制备方法，包括以下步骤：a.将40～80份大分子二醇、0～5份小分子二醇、3～7份亲水扩链剂、70～140份二异氰酸酯、催化剂0.1～0.3份混合后，于70～95℃反应2～3h得预聚体；b.往预聚体中加入封端单体25～80份、活性单体0～80份、对甲氧基苯酚0.05～0.1份、丁酮0～50份，于60～85℃反应2～4h，得到UV预聚物；c.加入2～8份中和剂中和30min，然后边搅拌边加入450～600份去离子水乳化；d.乳化完成后加入5～30份扩链剂于20～40℃至反应完全，然后减压蒸馏除去丁酮，得到低光泽高物性自消光水性UV聚氨酯分散体。
可选的，所述大分子二醇为聚丙二醇(PPG)、聚四氢呋喃二醇(PTMEG)、聚酯二元醇(PEDL)、聚己内酯二元醇(PCL)、聚碳酸酯二元醇(PCDL)中的至少一种，分子量为1000～3000；小分子二元醇为乙二醇(EG)、丁二醇(BDO)、新戊二醇(NPG)、己二醇(HDO)、环己烷二甲醇(CHDM)、三羟甲基丙烷(TMP)中的至少一种；亲水扩链剂为二羟甲基丙酸(DMPA)或二羟甲基丁酸(DMBA)中的至少一种；二异氰酸酯为异佛尔酮二异氰酸酯(IPDI)、六亚甲基二异氰酸酯(HDI)、4,4'-二环己基甲烷二异氰酸酯(HMDI)、甲苯二异氰酸酯(TDI)中的至少一种；所述催化剂为有机铋/锌催化剂，为凡特鲁斯公司的Coscat 8330R或Coscat AC83中的至少一种。
可选的，所所述封端单体为丙烯酸羟乙酯(HEA)、丙烯酸羟丙酯(HPA)、季戊四醇三丙烯酸酯(PETA)、双季戊四醇五丙烯酸酯(DPPA)中的至少一种；活性单体为己二醇二丙烯酸酯(HDDA)、三羟甲基丙烷三丙烯酸酯(TMPTA)、双季戊四醇六丙烯酸酯(DPHA)中的至少一种。
可选的，所所述中和剂为三乙胺(TEA)、N,N-二甲基乙醇胺(DMEA)中的至少一种。
可选的，所所述扩链剂为水合肼(HyHy)、乙二胺(EDA)、异氟尔酮二胺(IPDA)，二乙烯三胺(DETA)中的至少一种。
为了实现上述目的，本发明还提供了一种低光泽高物性自消光水性UV聚氨酯分散体，采用上述任意一项所述的低光泽高物性自消光水性UV聚氨酯分散体的制备方法制备而成。
本发明的有益效果如下：
本发明通过化学反应将可UV固化的丙烯酸酯基团通过化学键接引入水性自消光聚氨酯的分子链结构内，赋予水性自消光聚氨酯可UV固化的功能。经过紫外光的辐照后，分子链能通过化学键接形成致密的三维网络交联结构，能大幅提高树脂的物性；因无需复配常规水性树脂，涂膜的表面粗糙程度几乎不受影响，光泽度能维持在较低水平。得到具有低光泽度、柔和手感同时兼具优异物性的水性自消光聚氨酯，改善现有的水性自消光聚氨酯的树脂成膜强度低，附着力差，物性差等不足，实现低光泽度和高物性的统一。
本发明的低光泽高物性自消光水性UV聚氨酯分散体不含溶剂，绿色环保，适用范围广。
附图说明
为了更清楚地说明本发明的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，对于本领域普通技术人员而言，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1是根据本发明的实施例3的树脂制备的固化膜的扫描电镜图。
具体实施方式
为了更加清楚的呈现本发明的目的，技术方案和优点，下面将进行完整的描述本发明实施例中的技术方案。本发明中为标注具体条件的均可按照常规条件进行。所用的试剂及仪器为标注厂商均可从市售途径购买所得。
在下面的描述中阐述了很多具体细节以便于充分理解本发明，但是本发明还可以采用其它不同于在此描述的其它方式来实施，本领域技术人员可以在不违背本发明内涵的情况下做类似推广，因此本发明不受下面公开的具体实施例的限制。
根据本发明的低光泽高物性自消光水性UV聚氨酯分散体的制备方法包括以下步骤：a.将40～80份大分子二醇、0～5份小分子二醇、3～7份亲水扩链剂、70～140份二异氰酸酯、催化剂0.1～0.3份混合后，于70～95℃反应2～3h得预聚体；b.往预聚体中加入封端单体25～80份、活性单体0～80份、对甲氧基苯酚0.05～0.1份、丁酮0～50份，于60～85℃反应2～4h，得到UV预聚物；c.加入2～8份中和剂中和30min，然后边搅拌边加入450～600份去离子水乳化；d.乳化完成后加入5～30份扩链剂于20～40℃至反应完全，然后减压蒸馏除去丁酮，得到低光泽高物性自消光水性UV聚氨酯分散体。
在根据本发明的低光泽高物性自消光水性UV聚氨酯分散体的制备方法中，所述大分子二醇为聚丙二醇(PPG)、聚四氢呋喃二醇(PTMEG)、聚酯二元醇(PEDL)、聚己内酯二元醇(PCL)、聚碳酸酯二元醇(PCDL)中的至少一种，分子量为1000～3000；小分子二元醇为乙二醇(EG)、丁二醇(BDO)、新戊二醇(NPG)、己二醇(HDO)、环己烷二甲醇(CHDM)、三羟甲基丙烷(TMP)中的至少一种；亲水扩链剂为二羟甲基丙酸(DMPA)或二羟甲基丁酸(DMBA)中的至少一种；二异氰酸酯为异佛尔酮二异氰酸酯(IPDI)、六亚甲基二异氰酸酯(HDI)、4,4'-二环己基甲烷二异氰酸酯(HMDI)、甲苯二异氰酸酯(TDI)中的至少一种；所述催化剂为有机铋/锌催化剂，为凡特鲁斯公司的Coscat 8330R或Coscat AC83中的至少一种。
在根据本发明的低光泽高物性自消光水性UV聚氨酯分散体的制备方法中，所所述封端单体为丙烯酸羟乙酯(HEA)、丙烯酸羟丙酯(HPA)、季戊四醇三丙烯酸酯(PETA)、双季戊四醇五丙烯酸酯(DPPA)中的至少一种；活性单体为己二醇二丙烯酸酯(HDDA)、三羟甲基丙烷三丙烯酸酯(TMPTA)、双季戊四醇六丙烯酸酯(DPHA)中的至少一种。
在根据本发明的低光泽高物性自消光水性UV聚氨酯分散体的制备方法中，所所述中和剂为三乙胺(TEA)、N,N-二甲基乙醇胺(DMEA)中的至少一种。
在根据本发明的低光泽高物性自消光水性UV聚氨酯分散体的制备方法中，所所述扩链剂为水合肼(HyHy)、乙二胺(EDA)、异氟尔酮二胺(IPDA)，二乙烯三胺(DETA)中的至少一种。
根据本发明的低光泽高物性自消光水性UV聚氨酯分散体采用上述低光泽高物性自消光水性UV聚氨酯分散体的制备方法制备而成。
以下结合具体实施例对本发明的低光泽高物性自消光水性UV聚氨酯分散体及其制备方法做具体说明。
所用主要原材料及设备：在未指明情况下，各实施例和对比例的原料和设备相同；未指明具体型号或种类的物料来源于市场采购的常见同一型号，不做具体限制。
实施例1
本实施例提供的低光泽高物性自消光水性UV聚氨酯分散体的制备方法包括以下步骤：
a.将30份PTMEG(分子量2000)、50份PEDL(分子量2000)、5份CHDM、5份DMPA、140份IPDI、0.3份Coscat 8330R混合后，于95℃反应2h得预聚体；
b.往预聚体中加入PETA 80份、TMPTA 50份、对甲氧基苯酚0.1份、丁酮30份，于85℃反应2h，得到UV预聚物；
c.加入4份TEA中和30min，然后边搅拌边加入600份去离子水乳化；
d.乳化完成后加入30份HyHy于40℃至反应完全，然后减压蒸馏除去丁酮，得到低光泽高物性自消光水性UV聚氨酯分散体。
实施例2
本实施例提供的低光泽高物性自消光水性UV聚氨酯分散体的制备方法包括以下步骤：
a.将40份PCDL(分子量1000)、5份EG、7份DMPA、100份HMDI、0.1份Coscat 8330R混合后，于90℃反应3h得预聚体；
b.往预聚体中加入DPPA 80份、HDDA 20份、对甲氧基苯酚0.05份、丁酮50份，于80℃反应2.5h，得到UV预聚物；
c.加入8份TEA中和30min，然后边搅拌边加入500份去离子水乳化；
d.乳化完成后加入25份EDA于20℃至反应完全，然后减压蒸馏除去丁酮，得到低光泽高物性自消光水性UV聚氨酯分散体。
实施例3
本实施例提供的低光泽高物性自消光水性UV聚氨酯分散体的制备方法包括以下步骤：
a.将20份PPG(分子量3000)、40份PCDL(分子量1000)、3份DMBA、100份HMDI、0.1份Coscat AC83混合后，于70℃反应2h得预聚体；
b.往预聚体中加入HEA 20份、PETA 30份、TMPTA 50份、对甲氧基苯酚0.1份，于80℃反应2h，得到UV预聚物；
c.加入2份TEA中和30min，然后边搅拌边加入450份去离子水乳化；
d.乳化完成后加入15份IPDA和份10份DETA于20℃至反应完全，得到低光泽高物性自消光水性UV聚氨酯分散体。
实施例4
本实施例提供的低光泽高物性自消光水性UV聚氨酯分散体的制备方法包括以下步骤：
a.将70份PCL(分子量2000)、2份BDO、2份TMP、3份DMPA、50份TDI、40份HMDI、0.1份Coscat 8330R混合后，于70℃反应3h得预聚体；
b.往预聚体中加入HEA 25份、DPHA 80份对甲氧基苯酚0.08份、丁酮35份，于60℃反应4h，得到UV预聚物；
c.加入2份DMEA中和30min，然后边搅拌边加入500份去离子水乳化；
d.乳化完成后加入4份IPDA、1份DETA于30℃至反应完全，然后减压蒸馏除去丁酮，得到低光泽高物性自消光水性UV聚氨酯分散体。
实施例5
本实施例提供的低光泽高物性自消光水性UV聚氨酯分散体的制备方法包括以下步骤：
a.将40份PCDL(分子量2000)、5份HDO、5份DMPA、70份HDI、0.1份Coscat AC83混合后，于85℃反应2h得预聚体；
b.往预聚体中加入PETA 70份、对甲氧基苯酚0.1份、丁酮40份，于85℃反应3h，得到UV预聚物；
c.加入6份TEA中和30min，然后边搅拌边加入550份去离子水乳化；
d.乳化完成后加入20份HyHy于30℃至反应完全，然后减压蒸馏除去丁酮，得到低光泽高物性自消光水性UV聚氨酯分散体。
性能测试
对上述实施例所得的树脂制备的固化膜和市售常规自消光产品参照相应国家和行业标准进行性能测试，性能测试方法如下：
1.固化膜60°光泽：光泽度仪测试。
2.耐摩擦试验：按照GB/T1768-2006进行。
3.水煮试验：将固化膜放置于80℃热水浸泡30min。
4.基材附着力：按照GBT9286-2021进行。
5.对实施例3的树脂制备的固化膜进行扫描电镜测试。
性能测试结果见表1，扫描电镜图见附图1。
表1性能测试结果
| 测试项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 常规自消光产品 |
| 固化膜60°光泽 | 1.0 | 1.2 | 1.4 | 1.8 | 1.5 | 1.2 |
| 耐摩擦试验 | ＞100次 | ＞100次 | ＞100次 | ＞100次 | ＞100次 | ＜20次 |
| 水煮试验 | 无变化 | 无变化 | 无变化 | 无变化 | 无变化 | 发白且不能恢复 |
| ABS基材附着力 | 0级 | 0级 | 0级 | 0级 | 0级 | 5级 |
| PC基材附着力 | 0级 | 0级 | 0级 | 0级 | 0级 | 3级 |
从表1的性能测试结果可以看出，本发明的实施例可得到60°光泽低于2.0的产品，同时更耐摩擦，水煮性能好，附着力更高。上述结果表明采用本发明的制备方法所制得的自消光水性UV聚氨酯分散体具有低光泽和高物性。
图1是实施例3的树脂制备的固化膜的扫描电镜图，从图1可以清晰看到颗粒状的粒子形成一个粗糙的表面，使得固化膜具有低光泽度；而且颗粒间有相互融合的部分，是微观的分子链之间形成交联网络的宏观表现，保证了固化膜的高物性。
采用本发明制备方法制备得到的低光泽高物性自消光水性UV聚氨酯分散体不含溶剂，绿色环保，适用范围广。
本发明未尽事宜为公知技术。上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。
Claims (6)
1.一种低光泽高物性自消光水性UV聚氨酯分散体的制备方法，其特征在于，包括以下步骤：
a.将40～80份大分子二醇、5份小分子二醇、5～7份亲水扩链剂、100～140份二异氰酸酯、催化剂0.1～0.3份混合后，于70～95℃反应2～3h得预聚体；
b.往预聚体中加入封端单体80份、活性单体20～50份、对甲氧基苯酚0.05～0.1份、丁酮30～50份，于60～85℃反应2～4h，得到UV预聚物；
c.加入4～8份中和剂中和30min，然后边搅拌边加入500～600份去离子水乳化；
d.乳化完成后加入25～30份扩链剂于20～40℃至反应完全，然后减压蒸馏除去丁酮，得到低光泽高物性自消光水性UV聚氨酯分散体；
所述大分子二醇为聚丙二醇(PPG)、聚四氢呋喃二醇(PTMEG)、聚酯二元醇(PEDL)、聚己内酯二元醇(PCL)、聚碳酸酯二元醇(PCDL)中的至少一种，分子量为1000～3000；
所述小分子二醇为乙二醇(EG)、丁二醇(BDO)、新戊二醇(NPG)、己二醇(HDO)、环己烷二甲醇(CHDM)、三羟甲基丙烷(TMP)中的至少一种；
所述活性单体为己二醇二丙烯酸酯(HDDA)、三羟甲基丙烷三丙烯酸酯(TMPTA)、双季戊四醇六丙烯酸酯(DPHA)中的至少一种。
2.根据权利要求1所述的低光泽高物性自消光水性UV聚氨酯分散体的制备方法，其特征在于，亲水扩链剂为二羟甲基丙酸(DMPA)或二羟甲基丁酸(DMBA)中的至少一种；二异氰酸酯为异佛尔酮二异氰酸酯(IPDI)、六亚甲基二异氰酸酯(HDI)、4,4'-二环己基甲烷二异氰酸酯(HMDI)、甲苯二异氰酸酯(TDI)中的至少一种；所述催化剂为有机铋/锌催化剂，为凡特鲁斯公司的Coscat 8330R或Coscat AC83中的至少一种。
3.根据权利要求1所述的低光泽高物性自消光水性UV聚氨酯分散体的制备方法，其特征在于，所述封端单体为丙烯酸羟乙酯(HEA)、丙烯酸羟丙酯(HPA)、季戊四醇三丙烯酸酯(PETA)、双季戊四醇五丙烯酸酯(DPPA)中的至少一种。
4.根据权利要求1所述的低光泽高物性自消光水性UV聚氨酯分散体的制备方法，其特征在于：所述中和剂为三乙胺(TEA)、N,N-二甲基乙醇胺(DMEA)中的至少一种。
5.根据权利要求1所述的低光泽高物性自消光水性UV聚氨酯分散体的制备方法，其特征在于：所述扩链剂为水合肼(HyHy)、乙二胺(EDA)、异氟尔酮二胺(IPDA)，二乙烯三胺(DETA)中的至少一种。
6.一种低光泽高物性自消光水性UV聚氨酯分散体，其特征在于，采用根据权利要求1-5中任意一项所述的低光泽高物性自消光水性UV聚氨酯分散体的制备方法制备而成。
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