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CN110952307A - 一种石墨烯改性浸渍液及其制备方法 - Google Patents

一种石墨烯改性浸渍液及其制备方法 Download PDF

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CN110952307A
CN110952307A CN201911009258.7A CN201911009258A CN110952307A CN 110952307 A CN110952307 A CN 110952307A CN 201911009258 A CN201911009258 A CN 201911009258A CN 110952307 A CN110952307 A CN 110952307A
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方祥
周业昌
石杰
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Wuhu Huaye New Materials Co ltd
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Abstract

本发明公开了一种石墨烯改性浸渍液的制备方法，包括以下制备步骤：A.将称量好的石墨烯浆料和阴离子乳化剂高速剪切搅拌，制得悬浮液；B.将称量好的氨水加入盛放有去离子水的反应釜中，再加入间苯二酚、糠醛和氯磺化聚乙烯胶乳，得到浸渍液；C.将制得的悬浮液加入到制得的浸渍液中，并将称量好的助剂加入到混合液中，加热搅拌，即制得石墨烯改性浸渍液。其中石墨烯改性浸渍液，包括原料石墨烯浆料、阴离子乳化剂、间苯二酚、糠醛、氯磺化聚乙烯胶乳、氨水、去离子水和助剂。相比于同浓度的RFL浸胶液，其在导热系数、阻燃型以及吸胶量方面均有了较大的提升。

Description

一种石墨烯改性浸渍液及其制备方法
技术领域
本发明涉及帆布浸胶液领域，尤其涉及一种石墨烯改性浸渍液及其制备方法。
背景技术
浸胶是织物通过胶液浸槽，使织物纤维浸上胶浆，以提高织物与胶料的熟结力。浸胶可使人造丝、合成纤维及玻璃纤维帘线表面光滑，浸胶浆后可显著提高胶料与纤维的勃着力。常用的浸液为天然乳胶与间苯二酚甲醛树脂相配合的水乳液。浸胶液通过粘附在帆布织物上能够与橡胶材料进行粘黏。但是，现有的浸胶液通常采用含有易挥发的、带有甲醛的RFL浸胶液，同时RFL浸胶液在提高织布纤维的耐热、耐腐、耐压性能方面亟待改善。
石墨烯是近几年发展迅速的热门新型材料，具有质轻、比强度高、比表面积高、超高导热性能等特点。浸胶帆布是运用在橡胶骨架材料领域的一种产品，特别是高温工况环境下，浸胶帆布良好的导热性能可以快速将来自外部环境的热量传导出去，保证橡胶产品质量稳定。经石墨烯该性后的浸胶帆布可以达到上述要求。
发明内容
本发明的目的在于克服现有技术的不足，提供了一种石墨烯改性浸渍液及其制备方法，以解决现有技术中的浸胶液与织物帆布浸润性能不高、导热性能低不易将胶液分散到织物上等技术问题；本发明能够浸胶液与织物帆布浸润效果好、导热性高、分散性优等特点
为解决以上技术问题，本发明公开了一种石墨烯改性浸渍液，包括原料石墨烯浆料、阴离子乳化剂、间苯二酚、糠醛、氯磺化聚乙烯胶乳、氨水、去离子水和助剂；原料的重量组分为：
Figure BDA0002243694700000011
进一步的，石墨烯浆料为质量浓度为5％的石墨烯分散液，分散剂为DMF与VAE的混合液。DMF能够很好的将石墨烯分散在浸胶液中，同时VAE乳液具有较好的成膜性，在浸胶过程中，能够很好的将浸胶液均匀的粘附在帆布上。
进一步的，氨水为质量浓度为20～25％，高浓度的氨水能够更好的促进树脂的生成，防止自聚反应的发生，同时不至于有效成分过度挥发。
进一步的，助剂包括分散剂、促进剂、抗氧化剂和阻燃剂。抗氧化剂是为了防止浸胶液中的酚类、醛类物质被空气氧化，降低有效成分。
进一步的，分散剂为三硬脂酸甘油酯，促进剂为双-(5-碘乙基水杨醛)缩邻苯二胺双季铵盐，抗氧化剂为苯酚，阻燃剂为磷酸三苯酯。分散剂有助于胶液分散，促进剂有助于浸胶涂层后期与橡胶类物质进行反应，同时高分子铵盐能够与浸胶液发生配位反应，提高胶液分子间黏合力，有机阻燃剂能够防止高温过程中会释放出大量的卤族气体，危害健康。
进一步的，阴离子乳化剂为十二烷基苯磺酸钠、壬基酚聚氧乙烯醚或苯乙烯-马来酸钠。
同时本方案还公开了一种石墨烯改性浸渍液的制备方法，包括以下制备步骤：
A.将称量好的石墨烯浆料和阴离子乳化剂一同加入剪切机中高速剪切搅拌1～1.5h，制得悬浮液，备用；
B.将称量好的氨水缓慢加入盛放有去离子水的反应釜中，再向反应釜中加入称量好的间苯二酚、糠醛和氯磺化聚乙烯胶乳，搅拌，反应8～10h后，得到浸渍液；
C.将制得的悬浮液加入到制得的浸渍液中，并将称量好的助剂加入到混合液中，加热搅拌，即制得石墨烯改性浸渍液。
进一步的，B中氨水采用滴加的方式进行加入，滴加的速度控制在2～3d/s。
进一步的，C中加热的温度控制在35～40℃，搅拌的时间为20～50min。
本发明公开了一种石墨烯改性浸渍液及其制备方法，通过将具有超高导热性能的石墨烯与其他纤维织物进行粘附，能够大大提升浸胶帆布的耐酸耐碱、高导热以及导热均匀的性能。同时在浸胶液中加入其他功能助剂，能够提升浸胶液的分散性以及快速成膜性，加快了生产效率。
具体实施方式
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1
实施例1公开了一种石墨烯改性浸渍液的制备方法，包括以下制备步骤：
A.将称量好的石墨烯浆料和阴离子乳化剂一同加入剪切机中高速剪切搅拌1～1.5h，制得悬浮液，备用；
B.将称量好的氨水缓慢加入盛放有去离子水的反应釜中，再向反应釜中加入称量好的间苯二酚、糠醛和氯磺化聚乙烯胶乳，搅拌，反应8h后，得到浸渍液，氨水采用滴加的方式进行加入，滴加的速度控制在2～3d/s。
C.将制得的悬浮液加入到制得的浸渍液中，并将称量好的助剂加入到混合液中，加热搅拌，加热的温度控制在35℃，搅拌的时间为20min，即制得石墨烯改性浸渍液。
同时本方案还公开了一种石墨烯改性浸渍液，包括原料石墨烯浆料、阴离子乳化剂、间苯二酚、糠醛、氯磺化聚乙烯胶乳、氨水、去离子水和助剂；原料的重量组分为：石墨烯浆料5份、阴离子乳化剂1份、间苯二酚1份、糠醛2份、氯磺化聚乙烯胶乳20份、氨水2份、去离子水70份、助剂3份。石墨烯浆料为质量浓度为5％的石墨烯分散液，分散剂为DMF与VAE的混合液。氨水为质量浓度为20％。助剂包括分散剂、促进剂、抗氧化剂和阻燃剂。分散剂为三硬脂酸甘油酯，促进剂为双-(5-碘乙基水杨醛)缩邻苯二胺双季铵盐，抗氧化剂为苯酚，阻燃剂为磷酸三苯酯。阴离子乳化剂为十二烷基苯磺酸钠。
实施例2
实施例2公开了一种石墨烯改性浸渍液的制备方法，包括以下制备步骤：
A.将称量好的石墨烯浆料和阴离子乳化剂一同加入剪切机中高速剪切搅拌1～1.5h，制得悬浮液，备用；
B.将称量好的氨水缓慢加入盛放有去离子水的反应釜中，再向反应釜中加入称量好的间苯二酚、糠醛和氯磺化聚乙烯胶乳，搅拌，反应10h后，得到浸渍液，氨水采用滴加的方式进行加入，滴加的速度控制在2～3d/s。
C.将制得的悬浮液加入到制得的浸渍液中，并将称量好的助剂加入到混合液中，加热搅拌，加热的温度控制在40℃，搅拌的时间为30min，即制得石墨烯改性浸渍液。
同时本方案还公开了一种石墨烯改性浸渍液，包括原料石墨烯浆料、阴离子乳化剂、间苯二酚、糠醛、氯磺化聚乙烯胶乳、氨水、去离子水和助剂；原料的重量组分为：石墨烯浆料7份、阴离子乳化剂1.5份、间苯二酚1.5份、糠醛2份、氯磺化聚乙烯胶乳20份、氨水2份、去离子水80份、助剂4份。石墨烯浆料为质量浓度为5％的石墨烯分散液，分散剂为DMF与VAE的混合液。氨水为质量浓度为25％。助剂包括分散剂、促进剂、抗氧化剂和阻燃剂。分散剂为三硬脂酸甘油酯，促进剂为双-(5-碘乙基水杨醛)缩邻苯二胺双季铵盐，抗氧化剂为苯酚，阻燃剂为磷酸三苯酯。阴离子乳化剂为壬基酚聚氧乙烯醚。
实施例3
实施例3公开了一种石墨烯改性浸渍液的制备方法，包括以下制备步骤：
A.将称量好的石墨烯浆料和阴离子乳化剂一同加入剪切机中高速剪切搅拌1～1.5h，制得悬浮液，备用；
B.将称量好的氨水缓慢加入盛放有去离子水的反应釜中，再向反应釜中加入称量好的间苯二酚、糠醛和氯磺化聚乙烯胶乳，搅拌，反应10h后，得到浸渍液，氨水采用滴加的方式进行加入，滴加的速度控制在2～3d/s。
C.将制得的悬浮液加入到制得的浸渍液中，并将称量好的助剂加入到混合液中，加热搅拌，加热的温度控制在40℃，搅拌的时间为50min，即制得石墨烯改性浸渍液。
同时本方案还公开了一种石墨烯改性浸渍液，包括原料石墨烯浆料、阴离子乳化剂、间苯二酚、糠醛、氯磺化聚乙烯胶乳、氨水、去离子水和助剂；原料的重量组分为：石墨烯浆料8份、阴离子乳化剂1.5份、间苯二酚1.5份、糠醛3份、氯磺化聚乙烯胶乳25份、氨水3份、去离子水80份、助剂5份。石墨烯浆料为质量浓度为5％的石墨烯分散液，分散剂为DMF与VAE的混合液。氨水为质量浓度为25％。助剂包括分散剂、促进剂、抗氧化剂和阻燃剂。分散剂为三硬脂酸甘油酯，促进剂为双-(5-碘乙基水杨醛)缩邻苯二胺双季铵盐，抗氧化剂为苯酚，阻燃剂为磷酸三苯酯。阴离子乳化剂为苯乙烯-马来酸钠。
通过本发明得到的浸胶液涂覆在不同帆布上面晾干后，相比于同浓度的RFL浸胶液，其在导热系数、阻燃型以及吸胶量方面均有了较大的提升，从而能够成为取代以及改进传统RFL浸胶的一种新思路、新方案。

Claims (9)

1.一种石墨烯改性浸渍液，其特征在于，包括原料石墨烯浆料、阴离子乳化剂、间苯二酚、糠醛、氯磺化聚乙烯胶乳、氨水、去离子水和助剂；所述原料的重量组分为：
Figure FDA0002243694690000011
2.如权利要求1所述的一种石墨烯改性浸渍液，其特征在于，所述石墨烯浆料为质量浓度为5％的石墨烯分散液，分散剂为DMF与VAE的混合液。
3.如权利要求1所述的一种石墨烯改性浸渍液，其特征在于，所述氨水为质量浓度为20～25％。
4.如权利要求1所述的一种石墨烯改性浸渍液，其特征在于，所述助剂包括分散剂、促进剂、抗氧化剂和阻燃剂。
5.如权利要求4所述的一种石墨烯改性浸渍液，其特征在于，所述分散剂为三硬脂酸甘油酯，所述促进剂为双-(5-碘乙基水杨醛)缩邻苯二胺双季铵盐，所述抗氧化剂为苯酚，所述阻燃剂为磷酸三苯酯。
6.如权利要求1所述的一种石墨烯改性浸渍液，其特征在于，所述阴离子乳化剂为十二烷基苯磺酸钠、壬基酚聚氧乙烯醚或苯乙烯-马来酸钠。
7.一种如权利要求1-6任一所述的石墨烯改性浸渍液的制备方法，其特征在于，包括以下制备步骤：
A.将称量好的石墨烯浆料和阴离子乳化剂一同加入剪切机中高速剪切搅拌1～1.5h，制得悬浮液，备用；
B.将称量好的氨水缓慢加入盛放有去离子水的反应釜中，再向反应釜中加入称量好的间苯二酚、糠醛和氯磺化聚乙烯胶乳，搅拌，反应8～10h后，得到浸渍液；
C.将制得的悬浮液加入到制得的浸渍液中，并将称量好的助剂加入到混合液中，加热搅拌，即制得石墨烯改性浸渍液。
8.如权利要求7所述的石墨烯改性浸渍液的制备方法，其特征在于，B中氨水采用滴加的方式进行加入，滴加的速度控制在2～3d/s。
9.如权利要求7所述的石墨烯改性浸渍液的制备方法，其特征在于，C中加热的温度控制在35～40℃，搅拌的时间为20～50min。
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