CN108034400A - 一种含超细滑石粉的聚氨酯乳液胶黏剂 - Google Patents
一种含超细滑石粉的聚氨酯乳液胶黏剂 Download PDFInfo
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Abstract
一种含超细滑石粉的聚氨酯乳液胶黏剂，采用超细滑石粉做封端剂，起到补强和诱导聚氨酯分子链结晶的效果，提高胶黏剂的初粘力，并且利用苯乙酮肟封闭异氰酸酯为潜在可反应基团，可与粘接界面的活性基团进一步反应，提高胶黏剂的粘接强度。制得的聚氨酯胶黏剂具有初粘力高、结晶速度快、结晶度高和粘结强度高等优异性能。
Description
技术领域
本发明涉及聚氨酯胶黏剂领域，特别是涉及具有高初粘力、结晶速度快和结晶度高的高性能水性聚氨酯乳液胶黏剂。
背景技术
水性聚氨酯胶黏剂因其具有无污染、易运输和工作环境友好等优点，逐渐成为了胶黏剂市场的主流。但是，水性聚氨酯胶黏剂存在干燥速度慢、初粘力小和耐水性差等缺点，特别是低的初粘力，严重影响了聚氨酯胶黏剂的施工便利性，限制了水性聚氨酯胶黏剂的进一步发展。
聚氨酯分子链结晶速度是决定聚氨酯初粘力大小的重要因素之一。分子链的结晶速度快，聚氨酯分子链在短时间内内聚力急剧增大，初粘力得到有效提高。不仅如此，高的结晶速度也能提高胶黏剂的最终粘接强度。因此提高聚氨酯分子链结晶速度是同时解决水性聚氨酯初粘力和最终粘结强度的有效方案之一，也是目前水性聚氨酯的研究重点之一。
纳米填料是高分子材料中的重要组成部分之一，能促进高分子材料的结晶性能，提高高分子材料的强度，降低成本，提高产品的竞争力。但是，当纳米填料在水性聚氨酯胶黏剂中应用时，存在严重的团聚问题，以及随之而来的沉降，反而会降低产品的粘结强度及其施工性能。因此，如何解决纳米填料在水性聚氨酯中的团聚，并提高纳米填料对聚氨酯分子链的结晶速度，是目前纳米填料/聚氨酯胶黏剂领域的研究方向。
滑石具有润滑性、抗黏、助流、柔软、光泽好、吸附力强等优良的物理、化学特性，能够增加高分子材料的产品形状的稳定，增加产品的拉伸强度、剪切强度和屈挠强度，是一类优良的天然填料。
发明内容
发明目的：本发明的目的是为了克服现有技术中的不足，提供一种含超细滑石粉的高结晶速度、初粘力大和、粘结强度高的水性聚氨酯乳液胶黏剂。
技术方案：为了解决上述技术问题，本发明所述的一种含超细滑石粉的聚氨酯乳液胶黏剂，它包括以下步骤，
步骤一：在氮气保护下，加入1 mol的聚己二酸已二醇酯二元醇与2 mol的甲苯二异氰酸酯，在温度60~70℃下搅拌2~3 h，加入400g超细滑石粉，加入2wt%的二月桂酸二丁基锡，温度80~90℃下继续搅拌1~2 h，接着降低温度，加入1 mol封闭剂，继续搅拌2 h，得到预聚体A，其中，2wt%是以聚己二酸已二醇酯二元醇和甲苯二异氰酸酯之和为基准；
步骤二：在干燥氮气保护下，在反应釜中加入10 mol分子量为4000的聚己二酸已二醇酯二元醇和20 mol甲苯二异氰酸酯，加热60℃，搅拌2h，加入2 wt%的二月桂酸二丁基锡，继续搅拌2 h，得到预聚体B，其中，2wt%是以聚己二酸已二醇酯二元醇和甲苯二异氰酸酯之和为基准；
步骤三：在步骤二中得到的预聚体B中，加入5 mol二羟甲基丙酸，加热搅拌，最后加入2mol三羟甲基丙烷和1 mol一缩二乙二醇，用丙酮调节体系粘度至2000~4000mPa·s，以40r/min的速率搅拌3 h，降温至50℃，按照体系与预聚体A质量比1:1的加入步骤一中得到的预聚体A，40 r/min继续搅拌1 h，得到聚氨酯溶液；
步骤四：在50 r/min搅拌下，将步骤三得到的聚氨酯溶液以1:0.5质量比加入去离子水中，搅拌1 h后，减压蒸馏脱去溶剂丙酮，得到含超细滑石粉的水性聚氨酯乳液胶黏剂。
步骤一中的超细滑石粉的纵横比为20:1，平均粒径为1μm，比表面积为500m2/g，表面羟基数为3.0 OH/nm2。
步骤一中得到的预聚体A的结构式如下：
。
步骤一中，降低温度到50℃，加入的封闭剂为苯乙酮肟。
步骤三中，加入二羟甲基丙酸后，在60~70℃下搅拌1~2 h。
有益效果：本发明与现有技术相比，其显著优点是：
（1）在聚氨酯乳液胶黏剂中，通过采用特定分子量的聚酯多元醇和特定结构的超细滑石粉相匹配，使得超细滑石粉作为封端剂，稳定地分散在于聚氨酯乳液胶黏剂中，实现了超细滑石粉对聚氨酯胶黏剂的纳米补强效应，提高了胶黏剂的初粘力和粘结强度；
（2）通过超细滑石粉对聚氨酯分子链的诱导结晶作用，有效提高了聚氨酯胶黏剂的结晶速度和结晶度，进一步增大了胶黏剂的初粘力粘结强度，提高胶黏剂的耐热性，得到的胶黏剂具有施工便利性和良好的使用效果。
附图说明
图1是含超细滑石粉的聚氨酯乳液胶黏剂的制备工艺流程图。
具体实施方式
下面结合实施例和对比例对本发明作进一步的说明。
实施例1：
步骤一：在氮气保护下，加入1 mol的聚己二酸已二醇酯二元醇与2 mol的甲苯二异氰酸酯，搅拌均匀，在温度60℃下反应3h，加入400g纵横比为20:1，平均粒径为1μm，比表面积为500m2/g的超细滑石粉，表面羟基数为3.0 OH/nm2，加入2wt%的二月桂酸二丁基锡，温度90℃下继续搅拌1h，接着降低温度到50℃，加入1 mol的苯乙酮肟，继续搅拌2 h，得到预聚体A，其中，2wt%是以聚己二酸已二醇酯二元醇和甲苯二异氰酸酯之和为基准；
步骤二：在干燥氮气保护下，在反应釜中加入10 mol分子量为4000的聚己二酸已二醇酯二元醇和20 mol甲苯二异氰酸酯，加热60℃，搅拌2h，加入2wt%的二月桂酸二丁基锡，继续搅拌2 h，得到预聚体B，其中，2wt%是以聚己二酸已二醇酯二元醇和甲苯二异氰酸酯之和为基准；
步骤三：在步骤二中得到的预聚体B中，加入5 mol二羟甲基丙酸，在70℃下搅拌1 h，最后加入2 mol三羟甲基丙烷和1 mol一缩二乙二醇，用丙酮调节体系粘度至2000mPa·s，以40 r/min的速率搅拌3 h，降温至50℃，按照体系与预聚体A质量比1:1的加入步骤一中得到的预聚体A，40 r/min继续搅拌1 h，得到聚氨酯溶液；
步骤四：在50 r/min搅拌下，将步骤三得到的聚氨酯溶液以1:0.5质量比加入去离子水中，搅拌1 h后，减压蒸馏脱去溶剂丙酮，得到含超细滑石粉的水性聚氨酯乳液胶黏剂。
胶黏剂性能如表1所示。
实施例2：
按指定的各组分含量重复实施例1的方法，但是在步骤一中的第一段温度为70℃，搅拌时间为2 h；第二段温度为80℃，搅拌2 h；步骤三中的第一段温度为60℃，搅拌时间2 h，粘度调节至4000mPa·s。
胶黏剂性能如表1所示。
对比例1：
按指定的各组分含量重复实施例1的方法，但是在步骤一中不添加超细滑石粉。胶黏剂性能如表1所示。
对比例2：
按指定的各组分含量重复实施例1的方法，但是在步骤三中的加入的预聚体A的结构为
。
胶黏剂性能如表1所示。
对比例3：
按指定的各组分含量重复实施例1的方法，但是在步骤三中的加入的预聚体A的结构为：
。
胶黏剂性能如表1所示。
对比例4：
按指定的各组分含量重复实施例1的方法，但是步骤一中没有降低温度。
胶黏剂性能如表1所示。
对比例5：
按指定的各组分含量重复实施例1的方法，但是步骤一中加入的封闭剂为乙二醇乙醚。
胶黏剂性能如表1所示。
由上表1可知，本发明的聚氨酯乳液胶黏剂，具备高初粘力、结晶速度快、结晶度高。
将制得的含超细滑石粉的聚氨酯乳液胶黏剂进行性能测试。
（1）初粘力：
采用GB/T2790胶黏剂180度剥离强度试验方法。将挠性被粘试片的未胶接的一端弯曲180°，将刚性被粘试片夹紧在固定的夹头上，而将挠性试片夹紧在另一夹头上。注意使夹头间试样准确定位，以保证所施加的拉力均匀地分布在试样的宽度上。开动机器，使上下夹头以恒定的速率分离。夹头的分离速率为100±10mm/min。记下夹头的分离速率和当夹头分离运行时所受到的力，直到至少有125 mm的胶接长度被剥离。初粘力越大越好。
注：在剥离过程中，剥开的挠性部分有时会在胶接部分上蹭过去，为了减少摩擦，可使用适当的润滑剂，如甘油或肥皂水，只要它不影响被粘物。
（2）粘结强度：
参照GB 7124-86胶黏剂拉伸剪切强度测定方法对制得的胶黏剂进行测试。用量具测量试样搭接面的长度和宽度，精确到0.05mm。把试样对称地夹在上、下夹持器中，夹持处至搭接端的距离为50±1 mm.开动试验机，在5±1 mm／min内，以稳定速度加载。记录试样剪切破坏的最大负荷。记录胶按破坏的类型(内聚破坏、粘附破坏、金属破坏)。
（3）热稳定性：
采用TG测试法对制得的水性聚氨酯胶黏剂进行热稳定性测试，作出TG曲线，从曲线中得到热失重为5%所对应的温度T 5%其中，失重温度越高，说明胶黏剂的稳定性越好。
（4）结晶性能：
基于DSC的测试数据，将DSC曲线与基线包围的面积转化为热焓值（结晶焓ΔHc）并列表，将结晶峰的温度记为结晶温度Tc，将结晶峰的半峰宽FWHH记为结晶相对速度。Tc越大，说明样品更容易结晶，FWHH越小，说明相对结晶速率越快，ΔHc越大，说明结晶度越高。
Claims (5)
1.一种含超细滑石粉的聚氨酯乳液胶黏剂，其特征在于：它包括以下步骤，
步骤一：在氮气保护下，加入1 mol的聚己二酸已二醇酯二元醇与2 mol的甲苯二异氰酸酯，在温度60~70℃下搅拌2~3 h，加入400g超细滑石粉，加入2 wt%的二月桂酸二丁基锡，温度80~90℃下继续搅拌1~2 h，接着降低温度，加入1 mol封闭剂，继续搅拌2 h，得到预聚体A，其中，2wt%是以聚己二酸已二醇酯二元醇和甲苯二异氰酸酯之和为基准；
步骤二：在干燥氮气保护下，在反应釜中加入10 mol分子量为4000的聚己二酸已二醇酯二元醇和20 mol甲苯二异氰酸酯，加热60℃，搅拌2h，加入2 wt%的二月桂酸二丁基锡，继续搅拌2 h，得到预聚体B，其中，2wt%是以聚己二酸已二醇酯二元醇和甲苯二异氰酸酯之和为基准；
步骤三：在步骤二中得到的预聚体B中，加入5 mol二羟甲基丙酸，加热搅拌，最后加入2mol三羟甲基丙烷和1 mol一缩二乙二醇，用丙酮调节体系粘度至2000~4000mPa·s，以40r/min的速率搅拌3 h，降温至50℃，按照体系与预聚体A质量比1:1加入步骤一中得到的预聚体A，40 r/min继续搅拌1 h，得到聚氨酯溶液；
步骤四：在50 r/min搅拌下，将步骤三得到的聚氨酯溶液以1:0.5质量比加入去离子水中，搅拌1 h后，减压蒸馏脱去溶剂丙酮，得到含超细滑石粉的水性聚氨酯乳液胶黏剂。
2.根据权利要求1所述的含超细滑石粉的聚氨酯乳液胶黏剂，其特征在于：步骤一中的超细滑石粉的纵横比为20:1，平均粒径为1μm，比表面积为500m2/g，表面羟基数为3.0 OH/nm2。
3.根据权利要求1所述的含超细滑石粉的聚氨酯乳液胶黏剂，其特征在于：步骤一中得到的预聚体A的结构式如下：
。
4.根据权利要求1所述的含超细滑石粉的聚氨酯乳液胶黏剂，其特征在于：步骤一中，降低温度到50℃，加入的封闭剂为苯乙酮肟。
5.根据权利要求1所述的含超细滑石粉的聚氨酯乳液胶黏剂，其特征在于：步骤三中，加入二羟甲基丙酸后，在60~70℃下搅拌1~2 h。
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