CN106009903A - 一种低结晶水性聚氨酯油墨连接料的制备方法 - Google Patents
一种低结晶水性聚氨酯油墨连接料的制备方法 Download PDFInfo
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Abstract
本发明提供了一种低结晶水性聚氨酯油墨连接料的制备方法。以聚四氢呋喃醚二醇、聚丙二醇、聚碳酸酯二醇、1，4丁二醇、六亚甲基二异氰酸酯和异氟尔酮二异氰酸酯、二羟甲基丙酸、三乙胺为原料制得水性聚氨酯分散体。将制备好的分散体在去离子水中分散的同时滴加亲水扩链剂2‑[(2‑氨基乙基)氨基]乙磺酸钠水溶液进行内交联。再脱去体系内丙酮或丁酮，制得低结晶水性聚氨酯油墨连接料。本制备方法工艺简单。所得的低结晶水性聚氨酯油墨连接料的胶膜性的强度，稳定性和耐热性都有较大的提高。制得的水性聚氨酯油墨连接料稳定性好，乳液粘度低，固含高，干燥速度快，胶膜具有较高的强度及耐高温性能，耐水解性能，光泽度及透光率均可调。
Description
技术领域
本发明属于油墨技术领域，涉及一种低结晶水性聚氨酯油墨连接料的制备方法。
背景技术
水性聚氨酯油墨采取水作为溶剂，减少VOC的排放，可以保护环境，降减少有毒物质的使用，已经广泛的应用在印刷和包装工业中。水性聚氨酯油墨跟溶剂型聚氨酯油墨相似，包含颜料，连接料和其它一些助剂。连接料主要由碱溶性树脂组成，印刷时赋予油墨很好的流动性和附着力，在承印物表面形成坚固的膜层。油墨连接料直接影响油墨的使用性能，比如粘度，附着力，光泽和干燥速度。所以，性能优异水性聚氨酯油墨必须采用好的聚氨酯树脂连接料。现有的一些油墨生产技术存在一些缺陷：（1）溶剂型油墨在制备及使用过程中不安全，对人体的健康产生危害，对环境造成污染。（2）普通的聚氨酯油墨在高温高湿的环境中易水解，粘度高，干燥速度慢，增加施工成本，影响产品质量。
发明内容
为了克服已有水性聚氨酯油墨连接料制备技术上的缺陷，本发明提供了一种低结晶水性聚氨酯油墨连接料的制备方法。
本发明的一种低结晶水性聚氨酯油墨连接料的制备方法如下：
材料和质量百分比如下:聚醚多元醇为65.8%—74%；二异氰酸酯为18.4%—25.3%；催化剂为0.7%-1.17%；羧酸型亲水扩链剂为1.1%—3.29%；前扩链剂为1.2%-3.42%；中和剂为0.84%-1.7%；后扩链剂为0.5%—1.27%；
所述的多元醇为聚丙二醇和聚四氢呋喃醚二醇中的一种或两种，分子量均为Mn =2000；
所述的二异氰酸酯为六亚甲基二异氰酸酯和异氟尔酮二异氰酸酯中的一种或两种；
所述的催化剂为有机铋；
所述的羧酸型亲水扩链剂为二羟甲基丙酸和二羟甲基丁酸中的一种或两种；
所述的前扩链剂为1,4丁二醇和乙二醇中的一种或两种；
所述的后扩链剂为质量浓度为50%的2-[(2-氨基乙基)氨基]乙磺酸钠水溶液；
制备的步骤和条件如下：按配比加料；
（1）将聚醚多元醇在60℃水浴下，搅拌10min，搅拌速度180rd/min，再将水浴温度升至80℃，向反应体系中加入六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯及有机铋催化剂，保温反应1.5小时；
（2）继续向反应体系中加入羧酸型亲水扩链剂及小分子二元醇扩链剂，保温反应2小时，搅拌，搅拌速度250rd/min，当反应体系中剩余NCO的质量分数达到9%-33%时，将反应体系温度降至50℃，向体系中加预聚体的质量的20%的丙酮稀释，并加入三乙胺中和剂，继续保温反应30min，得到NCO端基的预聚体；
（3）将水浴温度降至40℃，使预聚体在水中分散的同时，将质量浓度为50%的磺酸盐型亲水扩链剂2-[(2-氨基乙基)氨基]乙磺酸钠稀释至质量浓度为5%水溶液，以2-3g/min的滴加速度滴入水性聚氨酯分散体中进行后扩链和内交联；
（4）在50℃，-0.05MP条件下脱除体系内丙酮，得到低结晶水性聚氨酯油墨连接料。
有益效果：本发明提供的一种低结晶水性聚氨酯油墨连接料的制备方法的优点是：（1）使用低结晶的聚醚多元醇作为合成水性聚氨酯连接料的多元醇组份，使制得的水性聚氨酯油墨连接料具有很好的耐候性和耐水解性能。（2）将羧酸型亲水扩链剂和磺酸型亲水扩链剂分别作为制备水性聚氨酯油墨连接料的前扩链剂和后扩链剂，由于氨基磺酸盐的亲水性基团为磺酸根离子，其亲水性强于羧酸盐，具有更高离子化程度，因此可以降低羧酸盐亲水基团的用量，且磺酸盐呈电中性，无需加胺类物质中和，还可以通过控制羧酸盐与磺酸盐的用量比调节水性聚氨酯油墨连接料的光泽度和透光率。因此使用羧酸盐扩链剂与磺酸盐扩链剂最终得到的水性聚氨酯连接料能够提高印刷施工的效率，节省生产成本，对工人的身体健康及施工环境均无危害。（3）使用磺酸盐亲水扩链剂替代一般的小分子胺类扩链剂进行后扩链和内交联，避免了由于小分子胺类扩链剂挥发带来的不利影响。（4）采用六亚甲基二异氰酸酯和异氟尔酮二异氰酸酯混合异氰酸酯与多元醇反应，由于这两种异氰酸酯结构对称性促使软硬段相分离程度提高，所得的低结晶水性聚氨酯油墨连接料的胶膜性的强度，稳定性和耐热性都有较大的提高。所得的低结晶水性聚氨酯油墨连接料的胶膜性的粘度为21.8-38.4 mpas，粒径为54.3-67.6 nm，固含量40.5-42.6%，储存稳定性六个月以上，拉伸强度为40.2-43.8 MPa，断裂伸长率为
812-860%，吸水率0.48-0.89。
具体实施方式
实施例1 一种低结晶水性聚氨酯油墨连接料的制备方法如下：
材料和质量百分比如下:聚醚多元醇为73.6%；二异氰酸酯为20%；催化剂为0.7%；羧酸型亲水扩链剂为2.3%；前扩链剂为1.2%；中和剂为1.7%；后扩链剂为0.5%；
所述的多元醇为聚丙二醇, 分子量Mn =2000，质量为55g，；
二异氰酸酯为六亚甲基二异氰酸酯，质量为5.21g；异氟尔酮二异氰酸酯，质量为9.77g；催化剂为有机铋,质量为0.5g，羧酸型亲水扩链剂为二羟甲基丙酸,质量为1.69；前扩链剂为1,4丁二醇，质量为0.91g；中和剂为三乙胺，质量为1.27g；后扩链剂为质量浓度为50%的2-[(2-氨基乙基)氨基]乙磺酸钠水溶液，2-[(2-氨基乙基)氨基]乙磺酸钠质量为0.38g；
制备的步骤和条件如下，按配比加料：（1）将聚丙二醇55g在60℃水浴下，搅拌10min，搅拌速度180rd/min，再将水浴温度升至80℃，向反应体系中加入六亚甲基二异氰酸酯5.21g,异氟尔酮二异氰酸酯9.77g及有机铋催化剂0.5g，保温反应1.5小时；
（2）继续向反应体系中加入羧酸型亲水扩链剂1.69g及1,4丁二元醇扩链剂0.91g，保温反应2小时，搅拌速度250rd/min，当反应体系中剩余NCO的质量分数达到33%时，将反应体系温度降至50℃，向体系中加15g丙酮稀释，并加入三乙胺中和剂1.27g，继续保温反应30min，得到NCO端基的预聚体；
（3）将水浴温度降至40℃，使预聚体在水中分散的同时，将质量浓度为50%的磺酸盐型亲水扩链剂2-[(2-氨基乙基)氨基]乙磺酸钠稀释至质量浓度为5%水溶液，以2-3g/min的滴加速度滴入水性聚氨酯分散体中进行后扩链和内交联；
（4）在50℃，-0.05MPa条件下脱除体系内丙酮，得到低结晶水性聚氨酯油墨连接料。
实施例2 一种低结晶水性聚氨酯油墨连接料的制备方法如下：
材料和质量百分比如下:聚醚多元醇为74%；二异氰酸酯为18.4%；催化剂为0.93%；羧酸型亲水扩链剂为1.1%；前扩链剂为3.42%；中和剂为0.88%；后扩链剂为1.27%；
所述的多元醇为聚四氢呋喃醚二醇,质量为64g, 分子量Mn =2000；二异氰酸酯为六亚甲基二异氰酸酯（HDI），质量为5.27g；异氟尔酮二异氰酸酯(IPDI)，质量为10.66g；催化剂为有机铋,质量为0.8g；羧酸型亲水扩链剂为二羟甲基丙酸,质量为0.95g；前扩链剂为1,4丁二醇，质量为2.96g；中和剂为三乙胺，质量为0.76g；后扩链剂为质量分数为50%的2-[(2-氨基乙基)氨基]乙磺酸钠水溶液，2-[(2-氨基乙基)氨基]乙磺酸钠质量为1.1g；
制备的步骤和条件如下，均按配比加料：（1）将聚四氢呋喃醚二醇64g在60℃水浴下，搅拌10min，搅拌速度180rd/min，再将水浴温度升至80℃，向反应体系中加入六亚甲基二异氰酸酯（HDI）5.27g，异氟尔酮二异氰酸酯（IPDI）10.66g及有机铋催化剂0.8g，保温反应1.5小时；
（2）继续向反应体系中加入羧酸型亲水扩链剂0.95g及1,4丁二元醇扩链剂2.96g，保温反应2小时，搅拌速度250rd/min，当反应体系中剩余NCO的质量分数达到9%时，将反应体系温度降至50℃，向体系中加17g丙酮稀释，并加入三乙胺中和剂，继续保温反应30min，得到NCO端基的预聚体；
（3）将水浴温度降至40℃，使预聚体在水中分散的同时，将质量浓度为50%的磺酸盐型亲水扩链剂2-[(2-氨基乙基)氨基]乙磺酸钠稀释至质量浓度为5%的水溶液，以2-3g/min的滴加速度滴入水性聚氨酯分散体中进行后扩链和内交联；
实施例3 一种低结晶水性聚氨酯油墨连接料的制备方法如下：
材料和质量百分比如下:聚醚多元醇为65.8%；二异氰酸酯为25.3%；
催化剂为1.17%；羧酸型亲水扩链剂3.29%；前扩链剂为2.65%；中和剂为0.84%；后扩链剂为0.95%；
所述的多元醇为聚四氢呋喃醚二醇,质量为43g, 分子量Mn =2000；二异氰酸酯为异氟尔酮二异氰酸酯(IPDI)，质量为16.56g，
催化剂为有机铋,质量为0.76g；羧酸型亲水扩链剂为二羟甲基丙酸,质量为2.1g；前扩链剂为1,4丁二醇，质量为1.73g；中和剂为三乙胺，质量为0.55g；后扩链剂为质量分数为50%的2-[(2-氨基乙基)氨基]乙磺酸钠水溶液，2-[(2-氨基乙基)氨基]乙磺酸钠质量为0.62g；
制备的步骤和条件如下，均按配比加料：（1）将聚四氢呋喃醚二醇43g在60℃水浴下，搅拌10min，搅拌速度180rd/min，再将水浴温度升至80℃，向反应体系中加入异氟尔酮二异氰酸酯16.56g及有机铋催化剂0.76g，保温反应1.5小时；
（2）继续向反应体系中加入羧酸型亲水扩链剂2.1g及1,4丁二元醇扩链剂1.73g，保温反应2小时，搅拌速度250rd/min，当反应体系中剩余NCO的质量分数达到24%时，将反应体系温度降至50℃，向体系中加13g丙酮稀释，并加入三乙胺中和剂，继续保温反应30min，得到NCO端基的预聚体；
（3）将水浴温度降至40℃，使预聚体在水中分散的同时，将质量浓度为50%的磺酸盐型亲水扩链剂2-[(2-氨基乙基)氨基]乙磺酸钠稀释至质量浓度为5%的水溶液，以2-3g/min的滴加速度滴入水性聚氨酯分散体中进行后扩链和内交联；
测定实施例1至3的一种低结晶水性聚氨酯油墨连接料的物性和胶膜性能。结果见表1、2.
检测方法如下：
粘度测定：将乳液倒入200ml的烧杯中，将烧杯置于25℃恒温水浴中，恒温20分钟。然后将旋转粘度计的转子置于液面以下，打开开关，旋转60s读数，反复测量三次，取平均值即为乳液粘度。
固含量测定：称取一定质量的乳液M1于一干燥的表面皿中，让其铺展于表面皿上，放进（60±5）℃ 的烘箱中干燥，称表面皿中剩余固形物的总质量至恒重M2。按照下式计算固含量：
C(%)=M2/ M1×100%
式中：C—固含量(%)；M1—试样的质量（g）；M2—固形物质量（g）
离心稳定性测定：取一定质量的乳液装在离心管里，放入离心机内，在25℃、转速为3000 r/min的条件下离心15 min，观察有无分层和沉淀，评价乳液的稳定性，若乳液无分层或沉淀则可认为在常温下放置6个月稳定。
乳液粒径测试：用粒径分析仪采用动态光散射法测试粒径。取适量的乳液，用去离子水将其稀释至固含量为3‰的稀乳液。取稀释好的样品1ml，转移至石英比色皿中，再将装有稀释乳液的比色皿放入仪器光路中，在25℃的条件下，进行乳液粒径测试。
力学性能测试：将聚氨酯胶膜剪成标准样品（哑铃状），测试温度为25℃，在电子拉伸试验机上进行测试，拉伸速度为200mm/min，每个样品测试3次取平均值。
耐热性测试：采用热重分析仪进行测试，测试温度范围为25-600℃,升温速度为10℃/min。
吸水率测试：把干燥好的聚氨酯胶膜剪成1cm × 1cm的小方块，在25℃的室温下测定样品小方块膜的质量，然后把小方块膜浸泡于25℃室温下的去离子水中24h后，用滤纸吸干其表面的水分，再称量其质量，依据两者的质量差求吸水率 ：
W =［(M2 －M1) / M1］× 100%
式中W为样品膜的吸水率（%），M1为样品膜浸泡前质量（g），M2为样品膜浸泡后的质量(g)。每张膜取3个小方块，取其平均值。
表1 为一种低结晶水性聚氨酯油墨连接料乳液性能表。
表2 为一种低结晶水性聚氨酯油墨连接料胶膜性能表。
Claims (4)
1.一种低结晶水性聚氨酯油墨连接料的制备方法，其特征在于，材料和质量百分比如下:聚醚多元醇为65.8%—74%；二异氰酸酯为18.4%—25.3%；催化剂为0.7%-1.17%；羧酸型亲水扩链剂为1.1%—3.29%；前扩链剂为1.2%-3.42%；中和剂为0.84%-1.7%；后扩链剂为0.5%—1.27%；
所述的多元醇为聚丙二醇和聚四氢呋喃醚二醇中的一种或两种，分子量均为Mn =2000；
所述的二异氰酸酯为六亚甲基二异氰酸酯和异氟尔酮二异氰酸酯中的一种或两种；
所述的催化剂为有机铋；
所述的羧酸型亲水扩链剂为二羟甲基丙酸和二羟甲基丁酸中的一种或两种；
所述的前扩链剂为1,4丁二醇和乙二醇中的一种或两种；
所述的后扩链剂为质量浓度为50%的2-[(2-氨基乙基)氨基]乙磺酸钠水溶液；
制备的步骤和条件如下：按配比加料；
（1）将聚醚多元醇在60℃水浴下，搅拌10min，搅拌速度180rd/min，再将水浴温度升至80℃，向反应体系中加入六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯及有机铋催化剂，保温反应1.5小时；
（2）继续向反应体系中加入羧酸型亲水扩链剂、小分子二元醇扩链剂，保温反应2小时，搅拌，搅拌速度250rd/min，当反应体系中剩余NCO的质量分数达到9%-33%时，将反应体系温度降至50℃，向体系中加预聚体的质量的20%的丙酮稀释，并加入三乙胺中和剂，继续保温反应30min，得到NCO端基的预聚体；
（3）将水浴温度降至40℃，使预聚体在水中分散的同时，将质量浓度为50%的磺酸盐型亲水扩链剂2-[(2-氨基乙基)氨基]乙磺酸钠稀释至质量浓度为5%水溶液，以2-3g/min的滴加速度滴入水性聚氨酯分散体中进行后扩链和内交联；
（4）在50℃，-0.05MP条件下脱除体系内丙酮，得到低结晶水性聚氨酯油墨连接料。
2.如权利要求1所述的一种低结晶水性聚氨酯油墨连接料的制备方法，其特征在于，所述的材料和质量百分比如下:
聚醚多元醇为73.6%；二异氰酸酯为20%；催化剂为0.7%；羧酸型亲水扩链剂为2.3%；前扩链剂为1.2%；中和剂为1.7%；后扩链剂为0.5%；
所述的制备的步骤（1）将聚丙二醇在60℃水浴下，搅拌10min，搅拌速度180rd/min，再将水浴温度升至80℃，向反应体系中加入六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯及有机铋催化剂，保温反应1.5小时；
所述的制备的步骤（2）继续向反应体系中加入羧酸型亲水扩链剂及1,4丁二元醇扩链剂，保温反应2小时，搅拌速度250rd/min，当反应体系中剩余NCO的质量分数达到33%时，将反应体系温度降至50℃，向体系中加预聚体的质量的20%的丙酮稀释，并加入三乙胺中和剂，继续保温反应30min，得到NCO端基的预聚体；
所述的制备的步骤（3）将水浴温度降至40℃，使预聚体在水中分散的同时，将质量浓度为50%的磺酸盐型亲水扩链剂2-[(2-氨基乙基)氨基]乙磺酸钠稀释至质量浓度为5%水溶液，以2-3g/min的滴加速度滴入水性聚氨酯分散体中进行后扩链和内交联。
3.如权利要求1所述的一种低结晶水性聚氨酯油墨连接料的制备方法，其特征在于，所述的材料和质量百分比如下:聚醚多元醇为74%；二异氰酸酯为18.4%；催化剂为0.93%；羧酸型亲水扩链剂为1.1%；前扩链剂为3.42%；中和剂为0.88%；后扩链剂为1.27%；
所述的制备的步骤（1）将聚四氢呋喃醚二醇在60℃水浴下，搅拌10min，搅拌速度180rd/min，再将水浴温度升至80℃，向反应体系中加入六亚甲基二异氰酸酯、异氟尔酮二异氰酸酯及有机铋催化剂，保温反应1.5小时；
所述的制备的步骤（2）继续向反应体系中加入羧酸型亲水扩链剂及1,4丁二元醇扩链剂，保温反应2小时，搅拌速度250rd/min，当反应体系中剩余NCO的质量分数达到9%时，将反应体系温度降至50℃，向体系中加预聚体的质量的20%的丙酮稀释，并加入三乙胺中和剂，继续保温反应30min，得到NCO端基的预聚体；
所述的制备的步骤（3）将水浴温度降至40℃，使预聚体在水中分散的同时，将质量浓度为50%的磺酸盐型亲水扩链剂2-[(2-氨基乙基)氨基]乙磺酸钠稀释至质量浓度为5%水溶液，以2-3g/min的滴加速度滴入水性聚氨酯分散体中进行后扩链和内交联。
4.如权利要求1所述的一种低结晶水性聚氨酯油墨连接料的制备方法，其特征在于，所述的步材料和质量百分比如下:聚醚多元醇为65.8%；二异氰酸酯为25.3%；催化剂为1.17%；羧酸型亲水扩链剂3.29%；前扩链剂为2.65%；中和剂为0.84%；后扩链剂为0.95%；
所述的制备的步骤（1）将聚四氢呋喃醚二醇在60℃水浴下，搅拌10min，搅拌速度180rd/min，再将水浴温度升至80℃，向反应体系中加入异氟尔酮二异氰酸酯及有机铋催化剂，保温反应1.5小时；
所述的制备的步骤（2）继续向反应体系中加入羧酸型亲水扩链剂及1,4丁二元醇扩链剂，保温反应2小时，搅拌速度250rd/min，当反应体系中剩余NCO的质量分数达到24%时，将反应体系温度降至50℃，向反应体系中加预聚体的质量的20%的丙酮稀释，并入三乙胺中和剂，继续保温反应30min，得到NCO端基的预聚体；
所述的制备的步骤（3）将水浴温度降至40℃，使预聚体在水中分散的同时，将质量浓度为50%的磺酸盐型亲水扩链剂2-[(2-氨基乙基)氨基]乙磺酸钠稀释至质量浓度为5%水溶液，以2-3g/min的滴加速度滴入水性聚氨酯分散体中进行后扩链和内交联。
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