CN106543475B - 一种改性石墨烯的制备及其在可发性聚苯乙烯中的应用 - Google Patents
一种改性石墨烯的制备及其在可发性聚苯乙烯中的应用 Download PDFInfo
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Abstract
一种改性石墨烯制备复合EPS的方法:将石墨烯、活化剂在去离子水或有机溶剂中进行预分散,然后加入改性剂、活性分散剂、助分散剂进行石墨烯的改性分散,改性结束后过滤干燥得改性石墨烯粉末,改性石墨烯即可添加到白料EPS中进行悬浮聚合。本发明改性石墨烯的制备以石墨烯为基础材料,专为EPS应用而开发。本发明改性石墨烯主要用于EPS应用中,重点在石墨烯的改性,改性石墨烯EPS模塑聚苯板强度比国家标准提高150%‑190%,导热系数比032级国家标准降低8%‑12%,具有更优异的综合力学性能。本发明提供的方法工艺简单,成本低,对环境污染小,易于工业化生产。
Description
技术领域
本发明涉及改性石墨烯材料技术领域,尤其是涉及一种改性石墨烯的制备方法和应用方法。
背景技术
石墨烯是一种由碳原子紧密堆积而成的二维晶体材料,因其具有独特的结构,优异的电学、力学、光学、化学及热学等性能成为许多人研究的热点。石墨烯的制备方法有许多,具备工业化大生产的目前只有氧化还原法,其生产效率高,工艺流程化规模化。氧化还原方法是将天然石墨与强酸强氧化物反应生成氧化石墨,经过超声或微波膨化处理成氧化石墨烯,再进行还原去除氧化石墨烯表面的含氧官能团,即得石墨烯。但氧化还原石墨烯在工业化的应用过程中,总遇到分散效果不佳、应用效果不明显、添加量大成本高等问题。
因此,针对特定的行业,有必要对石墨烯进行改性,再进行工业化应用,特别在EPS(EPS即可发性聚苯乙烯)行业中。目前有白料EPS、石墨EPS两种产品。国家标准GB/T 29906-2013《模塑聚苯板薄抹灰外墙外保温系统材料》中EPS模塑聚苯板抗拉强度≥0.1Mpa,039级导热系数≤0.039W/(m·K),032级导热系数≤0.032W/(m·K),其中,白料EPS导热系数为039级,石墨EPS导热系数为032级。可发性聚苯乙烯因其优异的保温隔热性而被用作建筑保温隔热材料,且每年数十万吨的可发性聚苯乙烯用于商品包装,石墨EPS中石墨添加量占聚合反应体系的3%-5%,易导致反应不可控,爆聚结釜等问题。
石墨烯的改性是一个复杂的化学反应过程,通过对石墨烯的活化分散,达到提高石墨烯EPS综合性能的要求。石墨烯EPS凭借其抗压抗拉强度高、低导热、耐久性、抗老化等优异性能,将在包装、建筑节能、军工等领域发挥其巨大的应用价值。
发明内容
针对现有技术存在的上述问题,本申请人提供了一种改性石墨烯的制备及其在可发性聚苯乙烯中的应用。本发明生产效率高,绿色环保,成本低,适用于EPS行业的改性石墨烯,为石墨烯在EPS领域中的应用开发了一种新的思路。
本发明的技术方案如下:
一种改性石墨烯的制备方法,包括以下步骤:
(1)预分散:将氧化还原石墨烯粉末、活化剂在去离子水或有机溶剂中进行预分散;
(2)石墨烯的改性:然后加入改性剂、活性分散剂、助分散剂进行石墨烯的改性分散;
(3)过滤干燥:改性结束后进行过滤干燥得到所述改性石墨烯粉末;
上述各原料的用量为:石墨烯为去离子水或有机溶剂的5~20wt%、活化剂为石墨烯的1~5wt%、改性剂为石墨烯的1~5wt%、活性分散剂为石墨烯的3~10wt%,助分散剂为石墨烯的0.5-1wt%。
所述氧化还原石墨烯为各种氧化还原法生产的石墨烯,石墨烯层数在10层以下。
所述活化剂为烷基苯磺酸钠、R-C6H4-SO3Na中的一种或多种。优选的,所述活化剂为十二烷基苯磺酸钠、十六烷基苯磺酸钠、十八烷基苯磺酸钠中的一种或多种。
所述有机溶剂为乙醇、丁醇、丙醇、甘油,或乙二醇中的一种。
所述改性剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂,或复合偶联剂中的一种或多种。
所述活性分散剂为活性磷酸钙、活性碳酸钙中的一种或多种。
所述助分散剂为各种分子量的聚乙二醇中的一种或多种。
一种所述的改性石墨烯的应用方法,将改性石墨烯加入到白料EPS体系中进行悬浮聚合,所述白料EPS聚合体系包括纯水、苯乙烯、引发剂BPO、分散剂活性磷酸钙、发泡剂戊烷;其中纯水与苯乙烯的重量比为1~4:1,石墨烯为苯乙烯的0.5%wt,引发剂为苯乙烯的0.2~0.5wt%、分散剂为苯乙烯的0.5~1wt%、发泡剂戊烷为苯乙烯的7~10wt%;然后发泡打板,制备得到可发性聚苯乙烯模塑聚苯板。
优选的,所述硅烷偶联剂可以是KH550、KH560,所述钛酸酯偶联剂可以是101、201。
所述的干燥方法为微波干燥,红外干燥,真空干燥,常压鼓风干燥中的一种。
本发明有益的技术效果在于:
(1)开发了一种新的改性石墨烯的制备方法与应用;(2)实现了石墨烯在EPS领域中的应用,为包装、建筑节能等领域做贡献(3)石墨烯制备工艺绿色环保,制造成本低;(4)改性石墨烯的制备技术路线成熟,生产效率高,适合工业化大生产;(5)提高了可发性聚苯乙烯的力学强度与保温性能,拓宽了EPS的应用范围。
石墨烯不经改性直接添加到EPS体系中聚合,易导致阻聚效应甚至出现结釜现象,勉强聚合出EPS粒子后,经发泡打板测性能,抗拉强度比国家标准0.1Mpa能提高5%-20%,导热系数基本无明显降低。而本发明制备得到的改性石墨烯添加到EPS体系中聚合,能解决阻聚效应克服结釜问题,改性石墨烯EPS模塑聚苯板强度比国家标准提高150-190%,导热系数比032级国家标准降低8%-12%且石墨烯经改性后,与苯乙烯单体充分接枝,提高了石墨烯聚苯板的力学强度,改性后石墨烯在发泡打板时被EPS发泡微孔充分包裹,石墨烯的片状结构均匀分布在EPS微孔结构上,可以使光线、热量在微孔腔体内反复反射,从而起到阻隔热量的作用,提高保温性能,使改性石墨烯EPS模塑聚苯板具有更优异的综合力学性能展现。本发明通过同时提高EPS的强度与保温性能,达到同样的使用效果只需原来一半左右的材料,大大简化了施工工艺与节约了材料。
附图说明
图1为本发明提供的一种改性石墨烯的工艺流程示意图;
图2是本发明提供的改性石墨烯加入到EPS发泡打板制成的聚苯板与国家标准GB/T 29906-2013的抗拉强度对比图;
图3是本发明提供的改性石墨烯加入到EPS发泡打板制成的聚苯板与国家标准GB/T 29906-2013的导热系数对比图。
具体实施方式
下面结合附图和实施例,对本发明进行具体描述。
实施例1
(1)预分散:将氧化还原石墨烯粉末50g、十二烷基苯磺酸钠2.5g在1000g去离子水中进行超声预分散。
(2)石墨烯的改性:然后加入2.5g硅烷偶联剂KH550、5g活性磷酸钙、0.5g聚乙二醇400(400为分子量,下同)进行石墨烯的改性分散,搅拌剪切分散2h,先8000r/min高速剪切搅拌1.5h,然后5000r/min中速搅拌分散0.5h。
(3)过滤干燥:改性结束后进行过滤,然后微波干燥得改性石墨烯粉末。
(4)将此改性石墨烯粉末加入到白料EPS中进行聚合,聚合体系中按石墨烯相对苯乙烯为0.5%wt,悬浮聚合过程11h,纯水:苯乙烯重量比为4:1,聚合体系组成:苯乙烯20wt%,纯水80wt%,BPO 0.04wt%,活性磷酸钙0.1wt%,石墨烯0.1wt%,戊烷1.4wt%,然后发泡打板,模塑聚苯板的密度为16kg/m3,测试抗拉强度与导热系数,测试为抗拉强度0.255MPa,导热系数0.0285W/(m·K)
实施例2
(1)预分散:将氧化还原石墨烯粉末50g、十二烷基苯磺酸钠0.25g、十六烷基苯磺酸钠0.25g在500g乙醇中进行超声预分散。
(2)石墨烯的改性:然后加入2g硅烷偶联剂KH560、2.5g活性磷酸钙、0.2g聚乙二醇800、0.1g聚乙二醇1000进行石墨烯的改性分散,搅拌剪切分散2h,先7500r/min高速剪切搅拌1.5h,然后4000r/min中速搅拌分散0.5h。
(3)过滤干燥:改性结束后进行过滤,然后真空干燥得改性石墨烯粉末。
(4)将此改性石墨烯粉末加入到白料EPS中进行聚合聚合体系中按石墨烯相对苯乙烯为0.5%wt,悬浮聚合过程10h,纯水:苯乙烯重量比为3:1,聚合体系组成:苯乙烯25wt%,纯水75wt%,BPO 0.075wt%,活性磷酸钙0.175wt%,石墨烯0.125wt%,戊烷2.0wt%,然后发泡打板,模塑聚苯板的密度为16kg/m3,测试抗拉强度与导热系数,测试为抗拉强度0.261MPa,导热系数0.0286W/(m·K)
实施例3
(1)预分散:将氧化还原石墨烯粉末50g、十八烷基苯磺酸钠1.5g在350g乙二醇中进行超声预分散。
(2)石墨烯的改性:然后加入0.2g硅烷偶联剂KH560、0.3g钛酸酯偶联剂101、1g活性磷酸钙、0.5g活性碳酸钙、0.25g聚乙二醇10000进行石墨烯的改性分散,搅拌剪切分散2h,先7000r/min高速剪切搅拌1.5h,然后4000r/min中速搅拌分散0.5h。
(3)过滤干燥:改性结束后进行过滤,然后常压鼓风干燥得改性石墨烯粉末。
(4)将此改性石墨烯粉末加入到白料EPS中进行聚合,悬浮聚合过程12h,纯水:苯乙烯重量比为2:1,聚合体系组成:苯乙烯33wt%,纯水66wt%,BPO0.132wt%,活性磷酸钙0.265wt%,石墨烯0.165wt%,戊烷2.97wt%,然后发泡打板,模塑聚苯板的密度为16kg/m3,测试抗拉强度与导热系数,测试为抗拉强度0.253MPa,导热系数0.0284W/(m·K)
实施例4
(1)预分散:将氧化还原石墨烯粉末50g、十二烷基苯磺酸钠1g、十八烷基苯磺酸钠1g在250g正丁醇中进行超声预分散。
(2)石墨烯的改性:然后加入0.5g铝酸酯偶联剂DL-411、1g铝锆偶联剂TL-4、4g活性磷酸钙、0.2g聚乙二醇400、0.2g聚乙二醇6000进行石墨烯的改性分散,搅拌剪切分散2h,先7500r/min高速剪切搅拌1.5h,然后4000r/min中速搅拌分散0.5h。
(3)过滤干燥:改性结束后进行过滤,然后红外干燥得改性石墨烯粉末。
(4)将此改性石墨烯粉末加入到白料EPS中进行聚合,聚合体系中按石墨烯相对苯乙烯为0.5%wt,悬浮聚合过程11.5h,纯水:苯乙烯重量比为1:1,聚合体系组成:苯乙烯50wt%,纯水50wt%,BPO 0.25wt%,活性磷酸钙0.5wt%,石墨烯0.25wt%,戊烷5wt%,然后发泡打板,模塑聚苯板的密度为16kg/m3,测试抗拉强度与导热系数,测试为抗拉强度0.258MPa,导热系数0.0283W/(m·K)
测试例:
1、将本发明制备得到的改性石墨烯加入到EPS发泡打板制成的模塑聚苯板与国家标准GBT 29906-2013进行性能对比,结果如表1所示。
表1
2、本发明提供的改性石墨烯制备得到的EPS发泡模塑聚苯板经常用于建筑领域,在实际施工使用中,虽然最外面有保护层来保证模塑板外保温系统的机械强度和耐久性,但还是会经常接触潮湿、高温和低温交替等环境,因此需测试本发明制备的EPS模塑聚苯板在这些严苛的环境中的耐受性。
(1)耐湿性
将实施例3制备得到的EPS发泡模塑聚苯板放置于40℃、空气湿度为85%的密闭空间内,放置一段时间以后测试其强度和导热系数的变化,结果如表2所示。
表2
实施例3 | 抗拉强度MPa | 导热系数W/(m·K) |
30天 | 0.253 | 0.0284 |
60天 | 0.253 | 0.0284 |
90天 | 0.250 | 0.0285 |
120天 | 0.236 | 0.0289 |
(2)耐高低温循环性
将实施例3制备得到的EPS发泡板进行高低温循环处理,即现在50℃温度、湿度50%的环境中放置8h,再在-20℃温度的环境中放置16h,这样处理称为一个循环;处理若干个循环后测试其强度和导热系数的变化,结果如表3所示。
表3
实施例3 | 抗拉强度MPa | 导热系数W/(m·K) |
5个循环 | 0.253 | 0.0284 |
10个循环 | 0.253 | 0.0284 |
30个循环 | 0.251 | 0.0284 |
60个循环 | 0.243 | 0.0290 |
Claims (5)
1.一种用于EPS的改性石墨烯的制备方法,其特征在于包括以下步骤:
(1)预分散:将氧化还原石墨烯粉末、活化剂在去离子水或有机溶剂中进行预分散;
(2)氧化还原石墨烯的改性:然后加入改性剂、活性分散剂、助分散剂进行氧化还原石墨烯的改性分散;
(3)过滤干燥:改性结束后进行过滤干燥得到所述改性石墨烯粉末;
上述各原料的用量为:氧化还原石墨烯为去离子水或有机溶剂的5~20wt%、活化剂为氧化还原石墨烯的1~5wt%、改性剂为氧化还原石墨烯的1~5wt%、活性分散剂为氧化还原石墨烯的3~10wt%、助分散剂为氧化还原石墨烯的0.5-1wt%;
所述氧化还原石墨烯为各种氧化还原法生产的石墨烯,石墨烯层数在10层以下;所述活化剂为烷基苯磺酸钠;
所述改性剂为硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂中的一种或多种;
所述活性分散剂为活性磷酸钙、活性碳酸钙中的一种或多种。
2.根据权利要求1所述的制备方法,其特征在于,所述活化剂为十二烷基苯磺酸钠、十六烷基苯磺酸钠、十八烷基苯磺酸钠中的一种或多种。
3.根据权利要求1所述的制备方法,其特征在于,所述有机溶剂为乙醇、丁醇、丙醇、甘油,或乙二醇中的一种。
4.根据权利要求1所述的制备方法,其特征在于,所述助分散剂为各种分子量的聚乙二醇中的一种或多种。
5.一种权利要求1~4任一项所述的改性石墨烯的应用,其特征在于,将改性石墨烯加入到白料EPS体系中进行悬浮聚合,所述白料EPS聚合体系包括纯水、苯乙烯、引发剂BPO、分散剂活性磷酸钙、发泡剂戊烷;其中纯水与苯乙烯的重量比为1~4:1,石墨烯为苯乙烯的0.5%wt,引发剂为苯乙烯的0.2~0.5wt%、分散剂为苯乙烯的0.5~1wt%、发泡剂戊烷为苯乙烯的7~10wt%;然后发泡打板,制备得到可发性聚苯乙烯模塑聚苯乙烯板。
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