CN103641977B - 双组份水性聚氨酯弹性树脂及其涂料 - Google Patents
双组份水性聚氨酯弹性树脂及其涂料 Download PDFInfo
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Abstract
一种气囊用水性弹性涂料，由水性聚氨酯羟基组分与多异氰酸酯固化剂复配制得。合成性能特殊的羟基型水性聚氨酯树脂，并优化选择多异氰酸酯固化剂，得到性能优秀的高韧性弹性涂料，再优选特殊的消光粉，降低光泽的同时保证耐溶剂性，应用于气囊安全组件上，具有良好的装饰及保护作用。
Description
技术领域
本发明涉及一种水性聚氨酯树脂，尤其涉及一种双组份的水性聚氨酯弹性树脂，及以其为主要成膜物制成的涂料，应用于气囊弹性底材表面，起到装饰和保护效果。
背景技术
1953年，DuPont公司的研究人员将端异氰酸酯基预聚体的甲苯溶液分散于水，用乙二胺扩链合成水性PU。60、70年代，对水性聚氨酯的研究、开发迅速发展，进入90年代，随着人们环保意识以及环保法规的加强，环境友好的水性聚氨酯的研究、开发日益受到重视，其应用已由皮革涂饰剂不断扩展到涂料、黏合剂等领域，正在逐步占领溶剂型聚氨酯的市场，代表着涂料、黏合剂的发展方向，在水性树脂中，水性聚氨酯仍然也是优秀树脂的代表,是现代水性树脂研究的热点之一。
水性聚氨酯涂料有单组分和双组分之分，单组分水性聚氨酯涂料的聚合物相对分子质量较大，成膜过程中一般不发生交联，即使引入自交联单元，也不能太多，否则合成困难、贮存稳定性变差，改性空间有限。双组分水性聚氨酯涂料由含羟基的水性树脂和含异氰酸酯基的固化剂组成，施工前将两者混合，成膜过程中发生交联反应，交联密度可调，涂膜性能好。
中国发明专利申请201110210844.5公开了化一种互穿网络丙烯酸聚氨酯乳液的制备方法，以丙烯酸单体作为溶剂，将聚氨酯、甲苯二异氰酸酯TDI、聚醚和催化剂溶于丙烯酸单体中进行充分反应，再加入乳化剂、中和剂和去离子水进行进一步反应，从而形成互穿网络丙烯酸聚氨酯乳液。该技术能够提高聚丙烯酸酯（PA）乳液和聚氨酯（PU）乳液的相容性，从而使这两种聚合物的分子间各自交联、相互渗透，提高所制备丙烯酸聚氨酯乳液成膜后的物化性能和装饰性能。但此方法操作比较复杂，真正产业化生产较难。
发明内容
本发明的一个目的在于提供一种双组份的水性聚氨酯弹性树脂，此树脂配以合适的固化剂能在低温下实现固化，以其为主要成膜物可赋予极高的柔韧性。
本发明的另一个目的在于提供一种涂料，通过添加特殊的消光粉，降低光泽同时具有良好的耐溶剂擦拭性能，能应用于弹性气囊基材上。
本发明提供的一种双组份水性聚氨酯弹性树脂，由如下步骤制得：
步骤一：将20w/w%～40w/w%的分子量1,000～3,000聚酯二元醇、30w/w%～50w/w%多元醇、25w/w%～35w/w%多异氰酸酯单体和5%～10%亲水性单体缩聚聚合，得到水性聚氨酯羟基组分；
步骤二：将制得的所述水性聚氨酯羟基组分与多异氰酸酯固化剂复配，得到性能优秀的双组份水性聚氨酯树脂。
本发明多异氰酸酯单体如：但不仅限于甲苯二异氰酸酯（TDI）、异佛尔酮二异氰酸酯（IPDI）、亚甲基多异氰酸酯（MDI）和六亚甲基多异氰酸酯（HDI）。这些多异氰酸酯单体可单独或同时应用于本发明。
本发明的亲水性单体如：但不仅限于羟基-丙磺酸钠（DHPA）、二羟甲基丁酸（DMPA）和二羟甲基丙酸（DMBA）。这些亲水单体可单独或同时应用于本发明，优先选择二羟甲基丙酸，用量优先选择7w/w%。
本发明还通过对双组份水性聚氨酯树脂分子量的设计，将树脂分子量设定在5,000～10,000，并控制羟基含量在合适的范围内（1w/w%-2w/w%），既能保证良好的强度同时又具有优秀的柔韧性。
本发明固化剂与水性聚氨酯羟基组分发生反应，提高树脂耐水及耐溶剂性能，选择柔韧性良好的固化剂，除提高耐性以外，亦能保证涂料的柔韧性。
无机消光粉由于分散性较差，很难被树脂完全包裹，因此消光的同时伴随着耐溶剂擦拭性能下降；特殊有机消光粉含有羟基官能团，消光的同时能与树脂及固化剂反应，进一步提高耐溶剂性能。
本发明的多异氰酸酯固化剂如：但不仅限于bayer301、bayer2655、Aquolin161和Aquolin160。这些固化剂可单独或同时应用于本发明。
本发明的双组份水性聚氨酯树脂，其特征在于所述的多异氰酸酯固化剂与聚氨酯树脂复配比例为1∶2-1∶5之间，优先选择1∶3。
本发明提供的另一种双组份水性聚氨酯弹性树脂，由如下步骤制得：
步骤一：向带有搅拌装置、温度计、N2入口和冷凝管的四口玻璃烧瓶中加入20w/w%～40w/w%聚酯二元醇、10w/w%～20w/w%丙二醇、5w/w%～10w/w%二羟甲基丁酸、20w/w%～30w/w%三羟甲基丙烷，110℃下真空干燥脱水2小时，降温至80℃加入2%～3%N-甲基吡咯烷酮，搅拌使DMPA全部溶解后，开始滴加25w/w%～35w/w%异佛尔酮二异氰酸酯，约1小时滴完，向其中加入0.3w/w%～0.5w/w%二正丁基锡二月桂酸酯，持续搅拌反应4小时，取样测NCO≤0.1%；冷却至60℃，加入4w/w%～8w/w%TEA中和0.5小时；加水，强烈分散0.5小时，旋出丙酮，得半透明水性聚氨酯羟基组分。
步骤二：多异氰酸酯固化剂按1∶2～1∶5与水性聚氨酯羟基组分复配，得到性能优秀的双组份水性聚氨酯树脂。
本发明提供的树脂，通过选择合适的色浆和有机消光粉，可制得体系稳定的、光泽低且兼顾柔韧性及耐酒精性的水性弹性涂料。
本发明的色浆选自于SM6800、SM6804、SM8809、MO2260、MO2210和DOY1之一种或几种组合
本发明的消光粉如：但不仅限于TS-100、MK-6、SYLOIDC803和OK-500系列。这些消光粉可单独或同时应用于本发明。优先选择MK-6，用量为3w/w%～5w/w%。
本发明提供的各种涂料还包括填料、润湿分散剂、流平剂和消泡剂之一种或几种。本领域普通技术人员，结合弹性塑料的特性和应用的实际需要，选择性的配以适量的颜料、填料、成膜助剂、润湿分散剂、流平剂和消泡剂等组成用于塑料的水性涂料。颜料、填料、成膜助剂、润湿分散剂、流平剂和消泡剂等组分种类和具体用量不得限定本发明。
本发明技术方案实现的有益效果：
本发明双组份水性聚氨酯弹性树脂为主要成膜物，制成水性弹性涂料，可适用于弹性塑料表面涂饰，起到装饰和保护作用。
具体实施方式
以下详细描述本发明的技术方案。本发明实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的精神和范围，其均应涵盖在本发明的权利要求范围中。
本发明所用的试剂若未明确指明，则均购自于西格玛－奥德里奇（Sigma－Aldrich）。
以下各个实施例提供的本发明水性弹性涂料（其中各个组分及按重量计用量参见表1），均按如下方法制得：
步骤一：向带有搅拌装置、温度计、氮气入口和冷凝管的四口玻璃烧瓶中加入PE、CHDM、DMPA、TMP，110℃下真空干燥脱水2小时，降温至80℃加入N-甲基吡咯烷酮，搅拌使DMPA全部溶解后，开始滴加IPDI，约1h滴完，向其中加入二正丁基锡二月桂酸酯，持续搅拌反应4h,取样测NCO≤0.1%；冷却至60℃，加入TEA中和0.5小时；加水，强烈分散0.5小时，旋出丙酮，得半透明水性聚氨酯羟基组分。该产品可以用于水性双组份聚氨酯漆的配制
步骤二：多异氰酸酯固化剂与水性聚氨酯树脂复配，得到性能优秀的双组份水性聚氨酯树脂
步骤三：加入色浆和有机消光粉，制得体系稳定的水性聚氨酯涂料。
表1
经过考察，二羟甲基丙酸用量在7时，水性聚氨酯树脂最为稳定。
实验以稳定的水性聚氨酯树脂为基础，考察固化剂种类对性能的影响，结果见表2。
表2
经比较，固化剂用量越多，耐酒精擦拭越好，相应柔韧性下降。经考察，水性聚氨酯羟基组分（原漆）与固化剂比为3:1时，综合效果最好。
以原漆与固化剂3:1为例，考察消光粉对性能的影响，结果见表3。
表3
由结果可见，有机消光粉MK-6综合性能优越，耐酒精擦拭性良好，以所选择的聚氨酯树脂、固化剂种类及比例和消光粉所得涂料性能结果见表4。同时，还对所得涂料在低温干燥成膜后，所得漆膜各项性能进行检测，结果见表4。
表4漆膜性能指标
根据本发明技术效果，所得弹性涂料，柔韧性优越（弯折不开裂），耐酒精擦拭性能良好（掉色级别3级），用于气囊安全组件上具有良好的装饰及保护作用。
Claims (9)
1.一种双组份水性聚氨酯弹性树脂，由如下步骤制得：
步骤一：将20w/w％的分子量1,000～3,000聚酯二元醇、多元醇、30w/w％多异氰酸酯单体和7w/w％二羟甲基丙酸缩聚聚合，得到水性聚氨酯羟基组分；
步骤二：将制得的所述水性聚氨酯羟基组分与多异氰酸酯固化剂复配，得到双组份水性聚氨酯树脂；
所述的多元醇为14.5w/w％丙二醇和25w/w％三羟甲基丙烷；
所述的多异氰酸酯单体选自于甲苯二异氰酸酯、异佛尔酮二异氰酸酯、亚甲基多异氰酸酯和六亚甲基多异氰酸酯之一种或几种；
所述的多异氰酸酯固化剂与所述的水性聚氨酯树脂复配比例为1∶3。
2.根据权利要求1所述的双组份水性聚氨酯弹性树脂，其特征在于所述的水性聚氨酯树脂分子量为5,000～10,000。
3.根据权利要求1所述的双组份水性聚氨酯弹性树脂，其特征在于所述的水性聚氨酯树脂含有1w/w％-2w/w％的羟基。
4.根据权利要求1所述的双组份水性聚氨酯树脂，其特征在于所述的多异氰酸酯固化剂为bayer301、bayer2655、Aquolin 161和Aquolin160之一种或几种。
5.一种双组份水性聚氨酯弹性树脂，由如下步骤制得：
步骤一：向带有搅拌装置、温度计、N2入口和冷凝管的四口玻璃烧瓶中加入20w/w％聚酯二元醇、14.5w/w％丙二醇、7w/w％二羟甲基丙酸、25w/w％三羟甲基丙烷，110℃下真空干燥脱水2小时，降温至80℃加入3％N-甲基吡咯烷酮，搅拌使二羟甲基丙酸全部溶解后，开始滴加30w/w％异佛尔酮二异氰酸酯，约1小时滴完，向其中加入0.3w/w％～0.5w/w％二正丁基锡二月桂酸酯，持续搅拌反应4小时，取样测NCO≤0.1％；冷却至60℃，加入5w/w％TEA中和0.5小时；加水，强烈分散0.5小时，旋出丙酮，得半透明水性聚氨酯羟基组分；
步骤二：将多异氰酸酯固化剂按1∶3与将制得的所述水性聚氨酯羟基组分复配，得到双组份水性聚氨酯树脂。
6.一种涂料，以权利要求1-5之一所述的双组份水性聚氨酯弹性树脂为主要成膜物，与色浆和消光粉制成，所述的消光粉用量为3w/w％～5w/w％。
7.根据权利要求6所述的涂料，其特征在于所述的色浆选自于SM6800、SM6804、SM8809、MO2260、MO2210和DOY1之一种或几种。
8.根据权利要求6所述的涂料，其特征在于所述消光粉选自于TS-100，MK及SYLOID系列之一种或几种。
9.根据权利要求6所述的涂料，其特征在于所述的涂料还包括填料、润湿分散剂、流平剂和消泡剂之一种或几种。
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