CN109627747A - 一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备 - Google Patents

一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备 Download PDF

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CN109627747A
CN109627747A CN201811477347.XA CN201811477347A CN109627747A CN 109627747 A CN109627747 A CN 109627747A CN 201811477347 A CN201811477347 A CN 201811477347A CN 109627747 A CN109627747 A CN 109627747A
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易昌凤
程朝
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Hubei University
Tongji Medical College of Huazhong University of Science and Technology
Union Hospital Tongji Medical College Huazhong University of Science and Technology
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Union Hospital Tongji Medical College Huazhong University of Science and Technology
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Abstract

本发明公开了了一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备，依次制备合成水性聚氨酯和水性聚氨酯/二硼化钛复合材料；通过二硼化钛和水性聚氨酯复合，可以很好的提高水性聚氨酯的耐热性，简单高效，合成成本低，同时赋予WPU抗静电的功能，让其在抗静电领域也有很好的应用，本发明将二硼化钛和水性聚氨酯复合，不仅可以提高WPU耐热性能，而且还可以赋予复合材料抗静电的功能，解决了WPU耐热性不好的问题也赋予其抗静电的功能，拓展了其应用。

Description

一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备
技术领域
本发明涉及特殊材料技术领域，尤其涉及一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备。
背景技术
聚氨酯已成为一种用途广泛的特殊材料，广泛应用于涂料、粘合剂、密封剂、弹性体等领域,然而,溶剂型的聚氨酯在这些应用中占主要应用，从而导致了严重的挥发性有机化合物(VOC)排放，污染了环境，危害了人类的健康。所以环保型的低VOC排放的水性聚氨酯(WPU)已成为近几十年来的主要趋势。
但是由于氨基甲酸酯的分解温度在250℃左右，WPU通常展现出相对低的热稳定性；严重的限制了WPU在高温领域的应用，因此提高WPU的耐热性已成为研究热点。
二硼化钛(TiB2)作为一种基础应用材料，正受到人们越来越多的关注。它是一种稳定的准金属化合物，是硼和钛组合成的六方晶系化合物。晶体结构中Ti为六方密堆积结构，B和Ti交替出现，这种特殊的结构使TiB2拥有可类比石墨的物理性能，即良好的导热性65W·m-1·K-1和导电性(电阻率14.4μΩ·cm)，此外有着四倍于钢的硬度(室温约30-35GPa)，良好的抗蠕变性。二硼化钛熔点高达3000℃，其还有着优异的抗氧化性，即使在1000℃的条件下，也不会氧化，它在盐酸和氢氟酸中能稳定存在。
所以将WPU和TiB2复合，不仅可以提高WPU耐热性能，而且还可以赋予复合材料抗静电的功能(水性聚氨酯具有电绝缘性，存在静电积累效应)，解决了WPU耐热性不好的问题也赋予其抗静电的功能，拓展了其应用。
目前改进水性聚氨酯耐热性的主要方法是利用耐热性好的成分对水性聚氨酯进行复合改性，如环氧树脂改性、有机硅改性、硅酸盐改性、丙烯酸酯改性、有机膨润土改性等等，但是都存在合成复杂，成本高，功能单一等缺点，因此，解决这一类的问题显得尤为重要。
发明内容
针对现有技术的不足，本发明提供了一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备，通过二硼化钛和水性聚氨酯复合，可以很好的提高水性聚氨酯的耐热性，简单高效，合成成本低，同时赋予WPU抗静电的功能，让其在抗静电领域也有很好的应用。
为了解决上述问题，本发明提供了一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备，包括以下步骤：
步骤一：合成水性聚氨酯，首先将水性聚氨酯合成在一个250ml的四口烧瓶中，在反应器中加入0.0015mol/3g的聚四氢呋喃、0.0021mol/0.275g的2,2-二羟甲基丙酸以及2ml的1-甲基-2吡咯烷酮，然后升温到80℃时，待体系成为均一稳定溶液之后，加入0.0062mol/1.38g的异佛尔酮二异氰酸酯和0.04g的二丁基氧化锡,反应3h之后，然后降温到40℃，加如0.0025mol/0.2550g的三乙胺反应10min之后,加入12ml的去离子水，并在2min后加入0.0016mol/0.1g的乙二胺反应2h，最后旋蒸除去丙酮溶剂，最终得到30％固含量的水性聚氨酯分散体；
步骤二：制备水性聚氨酯/二硼化钛复合材料，取10g的水性聚氨酯在小烧杯中，然后加3％-7％质量分数的二硼化钛，在超声仪中超声30min，待混合均匀，涂敷在四氟乙烯板上，放在40℃的烘箱12h得到水性聚氨酯/二硼化钛复合薄膜。
进一步改进在于：在步骤一中，所述四口烧瓶配有机械搅拌器、温度计、冷凝器、干燥管和氮气入口。
进一步改进在于：所述聚四氢呋喃在真空度为-0.095MPa、温度为130℃的条件下进行真空除水2h后放入干燥塔储存备用。
本发明的有益效果是：本发明通过二硼化钛和水性聚氨酯复合，可以很好的提高水性聚氨酯的耐热性，简单高效，合成成本低，同时赋予WPU抗静电的功能，让其在抗静电领域也有很好的应用，本发明将二硼化钛和水性聚氨酯复合，不仅可以提高WPU耐热性能，而且还可以赋予复合材料抗静电的功能(水性聚氨酯具有电绝缘性，存在静电积累效应)，解决了WPU耐热性不好的问题也赋予其抗静电的功能，拓展了其应用。
附图说明
图1是本发明的WPU合成路线。
图2是本发明的WPU和WPU/TiB2的XRD曲线。
图3是本发明的WPU和WPU/TiB2的热重曲线。
图4是本发明的WPU/TiB2的表面电阻率。
具体实施方式
为了加深对本发明的理解，下面将结合实施例对本发明做进一步详述，本实施例仅用于解释本发明，并不构成对本发明保护范围的限定。
如图1所示，本实施例提供了一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备，包括以下步骤：
步骤一：合成水性聚氨酯(以下统称WPU)，首先将水性聚氨酯合成在一个250ml的四口烧瓶中，在反应器中加入0.0015mol/3g的聚四氢呋喃、0.0021mol/0.275g的2,2-二羟甲基丙酸以及2ml的1-甲基-2吡咯烷酮，然后升温到80℃时，待体系成为均一稳定溶液之后，加入0.0062mol/1.38g的异佛尔酮二异氰酸酯和0.04g的二丁基氧化锡,反应3h之后，然后降温到40℃，加如0.0025mol/0.2550g的三乙胺反应10min之后,加入12ml的去离子水，并在2min后加入0.0016mol/0.1g的乙二胺反应2h，最后旋蒸除去丙酮溶剂，最终得到30％固含量的水性聚氨酯分散体；
步骤二：制备水性聚氨酯/二硼化钛(以下统称TiB2)复合材料，取10g的水性聚氨酯在小烧杯中，然后加3％-7％质量分数的二硼化钛，在超声仪中超声30min，待混合均匀，涂敷在四氟乙烯板上，放在40℃的烘箱12h得到水性聚氨酯/二硼化钛复合薄膜。
在步骤一中，所述四口烧瓶配有机械搅拌器、温度计、冷凝器、干燥管和氮气入口。所述聚四氢呋喃在真空度为-0.095MPa、温度为130℃的条件下进行真空除水2h后放入干燥塔储存备用。
由图2中WPU曲线可以看出，WPU膜只在2θ为17°～21°处有一个明显的宽而钝的非晶波包，没有明显的结晶峰，即得到的WPU薄膜是非晶结构。WPU/TiB2曲线则为添加有二硼化钛粒子的复合薄膜的XRD衍射图谱，图中可以看到，出现很多尖锐且窄的特征衍射峰，且随着二硼化钛添加量的增多，尖峰的强度随之增加。对比TiB2标准卡片，标准衍射曲线在2θ在27.59°(d 001)、34.14°(d 100)、44.44°(d 101)、56.97°(d 002)、61.12°(d 110)和68.12°(d 102)等有特征峰，与图中特征峰对应。对比纯WPU与复合薄膜的XRD谱图，可以看到WPU自身的大包峰未出现明显改变，TiB2特征峰在复合薄膜在出现，综合红外图谱，可以说明，TiB2已成功引入到复合薄膜中，且没有对WPU的基本结构造成影响。
由图3可知纯的WPU失重50％的温度为364℃，当二硼化钛加入到水性聚氨酯中，WPU/TiB2失重50％的温度为376℃，相对纯的WPU整整提高了12℃，这大大提高了聚氨酯树脂的耐热性能。
图4是WPU和WPU/TiB2的表面电阻率，可知纯的WPU表面电阻率是1.12×1013，明显可以看到，少量添加二硼化钛，复合薄膜电阻率即大幅下降，添加量为5wt％时，复合薄膜表面电阻率为2.31×107Ω·cm，符合抗静电标准(106～109Ω·cm)，使其在抗静电领域具有应用的前景。
本发明通过二硼化钛和水性聚氨酯复合，可以很好的提高水性聚氨酯的耐热性，简单高效，合成成本低，同时赋予WPU抗静电的功能，让其在抗静电领域也有很好的应用，本发明将二硼化钛和水性聚氨酯复合，不仅可以提高WPU耐热性能，而且还可以赋予复合材料抗静电的功能(水性聚氨酯具有电绝缘性，存在静电积累效应)，解决了WPU耐热性不好的问题也赋予其抗静电的功能，拓展了其应用。

Claims (3)

1.一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备，其特征在于，包括以下步骤：
步骤一：合成水性聚氨酯，首先将水性聚氨酯合成在一个250ml的四口烧瓶中，在反应器中加入0.0015mol/3g的聚四氢呋喃、0.0021mol/0.275g的2,2-二羟甲基丙酸以及2ml的1-甲基-2吡咯烷酮，然后升温到80℃时，待体系成为均一稳定溶液之后，加入0.0062mol/1.38g的异佛尔酮二异氰酸酯和0.04g的二丁基氧化锡,反应3h之后，然后降温到40℃，加如0.0025mol/0.2550g的三乙胺反应10min之后,加入12ml的去离子水，并在2min后加入0.0016mol/0.1g的乙二胺反应2h，最后旋蒸除去丙酮溶剂，最终得到30％固含量的水性聚氨酯分散体；
步骤二：制备水性聚氨酯/二硼化钛复合材料，取10g的水性聚氨酯在小烧杯中，然后加3％-7％质量分数的二硼化钛，在超声仪中超声30min，待混合均匀，涂敷在四氟乙烯板上，放在40℃的烘箱12h得到水性聚氨酯/二硼化钛复合薄膜。
2.根据权利要求1所述的一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备，其特征在于：在步骤一中，所述四口烧瓶配有机械搅拌器、温度计、冷凝器、干燥管和氮气入口。
3.根据权利要求1所述的一种耐热及抗静电水性聚氨酯/二硼化钛复合材料的制备，其特征在于：所述聚四氢呋喃在真空度为-0.095MPa、温度为130℃的条件下进行真空除水2h后放入干燥塔储存备用。
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Application publication date: 20190416