CN107474720A - 一种聚氨酯/石墨烯复合塑料工艺品表面涂饰剂 - Google Patents

一种聚氨酯/石墨烯复合塑料工艺品表面涂饰剂 Download PDF

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CN107474720A
CN107474720A CN201710951310.5A CN201710951310A CN107474720A CN 107474720 A CN107474720 A CN 107474720A CN 201710951310 A CN201710951310 A CN 201710951310A CN 107474720 A CN107474720 A CN 107474720A
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韩萍
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Huizhou Hailaifu Industrial Co Ltd
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Abstract

本发明揭示一种聚氨酯/石墨烯复合塑料工艺品表面涂饰剂，包括溶剂型聚氨酯和亲油性改性石墨烯，利用亲油改性的石墨烯与溶剂型聚氨酯反应制备了石墨烯/聚氨酯复合塑料工艺品表面涂饰剂，石墨烯添加量在0.025％～0.1％时，材料的耐溶剂性、力学性能及耐磨性得到显著提高，综合性能优越，从而改善塑料工艺品的表面性能，延长工艺品的表观寿命。

Description

一种聚氨酯/石墨烯复合塑料工艺品表面涂饰剂
技术领域
本发明涉及表面涂饰剂技术领域，具体地，涉及一种聚氨酯/石墨烯复合塑料工艺品表面涂饰剂。
背景技术
目前，塑料工艺品因其质轻耐摔而广受欢迎，但其表面容易刮花受损，影响表观。表面涂饰剂是一类用于物品表面装饰和保护的涂料，因此，需要一种可保护塑料工艺品表观的涂饰剂。
发明内容
针对现有技术的不足，本发明提供一种聚氨酯/石墨烯复合塑料工艺品表面涂饰剂。
本发明公开的一种聚氨酯/石墨烯复合塑料工艺品表面涂饰剂，其包括溶剂型聚氨酯和亲油性改性石墨烯，其中溶剂型聚氨酯包括40份聚四氢呋喃醚二醇、20份聚己二酸丁二醇酯二醇、30份4,4-二苯基甲烷二异氰酸酯、6份异佛尔酮二胺、4份1,4-丁二醇、2份异丙醇及120份N,N-二甲基甲酰胺，分数为重量分数，亲油性改性石墨烯的重量为溶剂型聚氨酯重量的0.025％～0.1％，采用以下步骤制作：
合成亲油性改性石墨烯，取50份氧化石墨烯水分散液超声1h；将1份硅烷偶联剂加入到氧化石墨烯水分散液中，反应24h，所得产物用无水乙醇洗涤5次，再用蒸馏水洗涤3次；将洗涤后的产物分散于100份蒸馏水中，超声1h；加入3份水合肼，还原6h；用无水乙醇和蒸馏水洗涤产物，干燥产物，制得固态亲油性改性石墨烯；
合成溶剂型聚氨酯，向反应釜中投入配方量的聚己二酸丁二醇酯二醇、聚四氢呋喃醚二醇、4,4-二苯基甲烷二异氰酸酯、异佛尔酮二胺、1,4-丁二醇及N,N-二甲基甲酰胺，于70～85℃进行反应，2h后补加4,4-二苯基甲烷二异氰酸酯增粘，经过2～3次的稀释、增粘，再加入剩余N,N-二甲基甲酰胺和异丙醇合成溶剂型聚氨酯。
将亲油性改性石墨烯分散于溶剂型聚氨酯中，搅拌均匀，形成分散液；
将分散液在超声波粉碎机中超声2h，形成分散体；
于室温风干分散体，制得涂饰剂。
根据本发明的实施方式，上述硅烷偶联剂为KH-550。
与现有技术相比，本发明可以获得包括以下技术效果：
本申请利用亲油改性的石墨烯制备了石墨烯/聚氨酯复合塑料工艺品表面涂饰剂，石墨烯添加量在0.025％～0.1％时，材料的耐溶剂性、力学性能及耐磨性得到显著提高，综合性能优越，从而改善塑料工艺品的表面性能，延长塑料工艺品的表观寿命。
具体实施方式
以下将揭露本申请的多个实施方式，为明确说明起见，许多实务上的细节将在以下叙述中一并说明。然而，应了解到，这些实务上的细节不应用以限制本申请。也就是说，在本申请的部分实施方式中，这些实务上的细节是非必要的。
根据配方量准备原料，其中溶剂型聚氨酯包括40g聚四氢呋喃醚二醇、20g聚己二酸丁二醇酯二醇、30g4,4-二苯基甲烷二异氰酸酯、6g异佛尔酮二胺、4g1,4-丁二醇、2g异丙醇及120gN,N-二甲基甲酰胺，亲油性改性石墨烯包括50g氧化石墨烯水分散液、1gKH-550及3g水合肼。
分别制备溶剂型聚氨酯树脂和亲油改性石墨烯。
亲油改性石墨烯的制备。取50g氧化石墨烯水分散液超声1h；将1g硅KH-550加入到所述氧化石墨烯水分散液中，反应24h，所得产物用无水乙醇洗涤5次，再用蒸馏水洗涤3次；将洗涤后的产物分散于100ml蒸馏水中，超声1h；加入3g水合肼，还原6h；用无水乙醇和蒸馏水洗涤产物，干燥产物，制得固态亲油性改性石墨烯。
溶剂型聚氨酯树脂的制备。向反应釜中投入配方量的聚己二酸丁二醇酯二醇、聚四氢呋喃醚二醇、4,4-二苯基甲烷二异氰酸酯、异佛尔酮二胺、1,4-丁二醇及N,N-二甲基甲酰胺，于70～85℃进行反应，2h后补加4,4-二苯基甲烷二异氰酸酯增粘，经过2～3次的稀释、增粘，再加入剩余N,N-二甲基甲酰胺和异丙醇合成溶剂型聚氨酯。
将亲油改性石墨烯加入溶剂型聚氨酯树脂中搅拌均匀，形成分散液；将分散液在超声波粉碎机中超声2h，形成分散体；于室温风干分散体，制得涂饰剂。
按亲油改性石墨烯添加质量的不同，制取多个试样，亲油改性石墨烯的添加量分别为0％、0.025％、0.05％、0.075％、0.1％、0.25％、0.5％将多个试样置于50℃烘箱中至质量不再变化，分别测试多个试样的耐溶剂性能、力学性能及耐磨性能。
通过考察试样在水、甲苯等溶剂中的溶胀程度来考察胶膜的耐溶剂性。如下表1所示不同石墨烯的添加量对应的溶胀率。用分析天平称量薄膜的质量，将其分别放至在蒸馏水和甲苯溶剂中，在30℃条件下浸泡12h后取出。用滤纸擦干表面，称重，溶胀率的计算公式如下：
溶胀率＝(m2-m1)/m1×100％
式中：m1—溶剂浸泡前胶膜的质量，g；
m2—溶剂浸泡后胶膜的质量，g。
表1
编号 石墨烯添加量/％ 甲苯溶胀率/％
1 0 32.38
2 0.025 26.39
3 0.05 25.00
4 0.075 23.68
5 0.1 28.00
6 0.25 30.28
7 0.5 32.00
根据测试表明，试样在甲苯中的溶胀率随石墨烯添加量的增加呈现先减小后增大的趋势，说明石墨烯与聚合物间较强的界面相互作用提高了复合胶膜的耐溶剂性能。而当石墨烯添加量超过0.1％时，可能较多的石墨烯发生堆积或聚集，导致耐溶剂性下降。
力学性能测试方法为：用模具裁取哑铃型样品，试样长度为50mm，宽度为10mm。使用电子拉力机进行拉伸强度的测试，运行速度为100mm/min。每个试样至少取两个样品进行平行试验，结果取其平均值。如下表2所示不同石墨烯添加量的试样的拉伸强度和断裂伸长率。
表2
从表2可知，未添加石墨烯的试样拉伸强度很低，仅有2.26MPa，添加石墨烯后，拉伸强度随添加量的增加显著上升，当添加量为0.1％时，拉伸强度达到最大值，其数值为纯PU的接近四倍，当添加量大于0.1％，拉伸强度反而开始下降。断裂伸长率随石墨烯添加量的增大则呈现下降的趋势。拉伸强度的显著改善表明石墨烯在聚氨酯基质中能够良好分散，当添加量较低时，片层结构贯穿于PU大分子之间，起到增强作用；另外，二者间的界面相互作用明显，石墨烯优异的力学性质得以体现。而当添加量超过0.1％时，由于石墨烯片层间较强的范德华力使较多的石墨烯发生堆积或聚集，产生银纹效应，导致机械强度下降。
耐磨性测试方法为：将试样均匀喷涂在塑料表面，厚度约为0.4～0.6mm。将试样截取为直径约为11cm的圆片，使用向科检测仪器有限公司生产的TABER耐磨耗试验机，设定回转速度60r/min，荷重750g，进行磨耗试验。以下表3为各试样的耐磨转数。
表3
编号 石墨烯添加量/％ 转数/r
1 0 1569
2 0.025 2122
3 0.05 2417
4 0.075 2844
5 0.1 3117
6 0.25 4011
7 0.5 4823
从表3中可以看出，纯聚氨酯的耐磨性较差，随着聚氨酯中石墨烯含量的增加，耐磨性逐渐增强，添加量为0.5％时，涂层的耐磨性较纯PU提高约三倍。耐磨性的显著提高，一方面是由于石墨烯密集的层状结构赋予其优异的力学性能，超薄的片层结构使其较易进入摩擦接触面，减少两粗糙表面的直接接触，从而保护聚氨酯大分子；另一方面，石墨烯优良的导热性将减少接触面因剧烈摩擦而产生的热量积累，降低表面温度，从而提高其耐磨性。
综上所述，利用亲油改性的石墨烯制备了石墨烯/聚氨酯复合塑料工艺品表面涂饰剂，石墨烯添加量在0.025％～0.1％时，材料的耐溶剂性、力学性能及耐磨性得到显著提高，综合性能优越，从而改善塑料工艺品的表面性能，延长工艺品的表观寿命。
上所述仅为本发明的实施方式而已，并不用于限制本发明。对于本领域技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原理的内所作的任何修改、等同替换、改进等，均应包括在本发明的权利要求范围之内。

Claims (2)

1.一种聚氨酯/石墨烯复合塑料工艺品表面涂饰剂，其特征在于，包括溶剂型聚氨酯和亲油性改性石墨烯，其中溶剂型聚氨酯包括40份聚四氢呋喃醚二醇、20份聚己二酸丁二醇酯二醇、30份4,4-二苯基甲烷二异氰酸酯、6份异佛尔酮二胺、4份1,4-丁二醇、2份异丙醇及120份N,N-二甲基甲酰胺，所述分数为重量分数，所述亲油性改性石墨烯的重量为溶剂型聚氨酯重量的0.025％～0.1％，采用以下步骤制作：
合成亲油性改性石墨烯，取50份氧化石墨烯水分散液超声1h；将1份硅烷偶联剂加入到所述氧化石墨烯水分散液中，反应24h，所得产物用无水乙醇洗涤5次，再用蒸馏水洗涤3次；将洗涤后的产物分散于100份蒸馏水中，超声1h；加入3份水合肼，还原6h；用无水乙醇和蒸馏水洗涤产物，干燥产物，制得固态亲油性改性石墨烯；
合成溶剂型聚氨酯，向反应釜中投入配方量的聚己二酸丁二醇酯二醇、聚四氢呋喃醚二醇、4,4-二苯基甲烷二异氰酸酯、异佛尔酮二胺、1,4-丁二醇及N,N-二甲基甲酰胺，于70～85℃进行反应，2h后补加4,4-二苯基甲烷二异氰酸酯增粘，经过2～3次的稀释、增粘，再加入剩余N,N-二甲基甲酰胺和异丙醇合成溶剂型聚氨酯；
将所述亲油性改性石墨烯分散于所述溶剂型聚氨酯中，搅拌均匀，形成分散液；
将所述分散液在超声波粉碎机中超声2h，形成分散体；
于室温风干所述分散体，制得所述涂饰剂。
2.根据权利要求1所述的聚氨酯/石墨烯复合塑料工艺品表面涂饰剂，其特征在于，所述硅烷偶联剂为KH-550。
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