CN108676327A - 一种环氧树脂用高导热填料的制备方法 - Google Patents
一种环氧树脂用高导热填料的制备方法 Download PDFInfo
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Abstract
本发明涉及一种环氧树脂用高导热填料的制备方法,属于导热填料制备技术领域。本发明首先以亚麻纤维为原料,利用茶籽油浸渍亚麻纤维后放在高温高湿的条件下静置酸败,再将酸败纤维密封后短时间发酵,使得亚麻纤维微腐,在亚麻纤维表面产生微孔,炭化后再用高锰酸钾氧化,将氧化后的亚麻碳纤维依次和硝酸铜溶液以及葡萄糖溶液混合反应,再经电弧防电处理,制得导热材料粗品,最后将导热材料粗品和猪油以及沼液共混发酵改性,最终制得高导热填料,本发明制得的高导热材料具有极佳的导热效率,稳定性高,增韧抗冲击性能好,具有广阔的应用前景。
Description
技术领域
本发明涉及一种环氧树脂用高导热填料的制备方法,属于导热填料制备技术领域。
背景技术
环氧树脂由于其优良的力学性能和介电性能,在电器封装、变压器浇注体、线路板以及其他领域得到了广泛的应用。但由于环氧树脂热导率低(小于0.2W/m·K),容易在器件运行过程中产生热量积聚,使内应力增加,导致制品开裂等一系列问题。因此,在对导热性能要求较高的领域,需要环氧复合材料具有高导热、良好的加工性及高性价比等优越的综合性能。为有效地提高热导率,在环氧体系中添加高导热性能填料是一种通用的方法。此类填充型环氧树脂基复合材料导热性能的提升主要是通过导热填料在树脂基体中相互搭接形成导热网络,提升体系对声子或电子的传导能力,使导热性能提高。
金属粉末是最常用的环氧树脂导热填料,金属粉末表面由于具有众多悬空键和未饱和键,比表面积大,表面能高,因而具有很强的化学活性,对温度、湿度、气氛、光照、电磁场等所处环境特别敏感,易与气体或液体分子交互作用发生氧化反应,从而导致其稳定性变差,发生团聚,并且与环氧树脂的界面相容性差,从而严重影响环氧树脂的抗冲击韧性,导致环氧树脂容易开裂,导热性下降。
因此,发明一种稳定性好,导热性强,能增加环氧树脂抗冲击性能,并且防止开裂的新型高导热填料具有积极的意义。
发明内容
本发明所要解决的技术问题,针对目前常见的环氧树脂热导率低,而最常见的金属导热填料容易氧化,稳定性差,会在环氧树脂中团聚,并且与环氧树脂的界面相容性差,从而严重影响环氧树脂的抗冲击韧性,导致环氧树脂容易开裂,导热性下降的缺陷,提供了一种环氧树脂用高导热填料的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
一种环氧树脂用高导热填料的制备方法,其特征在于具体制备步骤为:
(1)称取亚麻秸秆用石磙反复碾压3~5遍,碾压后人工抽取亚麻纤维,将抽取的亚麻纤维用茶籽油浸泡20~30min后取出,平铺在竹筛中,再将竹筛移入处理室中,静置酸败4~5天;
(2)待上述酸败结束后,得到酸败产物,将酸败产物放入发酵罐中,密封发酵,发酵结束后,过滤分离得到发酵滤渣,将发酵滤渣移入炭化炉中,在氮气保护作用下炭化,得到多孔亚麻碳纤维;
(3)将上述多孔亚麻碳纤维和质量分数为30%的高锰酸钾混合后装入水浴锅中,搅拌反应后过滤,分离得到反应滤渣;
(4)将上述反应滤渣和质量分数为40%的硝酸铜溶液混合后放入超声振荡仪中,超声振荡反应,反应结束后过滤分离得到滤渣,再将滤渣和质量分数为50%的葡萄糖溶液混合后装入烧瓶中,搅拌反应;
(5)待上述搅拌反应结束后,过滤分离得到反应滤饼,将得到的反应滤饼作为阳极材料平铺在电弧放电系统的样品台上,再将石墨棒作为阴极材料固定在顶部电极杆上,调节石墨阴极材料与底部样品台阳极材料之间的距离为2~3mm,在氩气保护状态下以150~160A的电流放电反应5~10min,反应结束后取出反应后的阳极材料,即为高导热填料粗品;
(6)将上述高导热填料粗品和猪油以及沼液混合后装入发酵罐中,密封罐口后,静置发酵,发酵结束后过滤分离得到发酵滤饼,将发酵滤饼分别用无水乙醇和去离子水冲洗3~5遍后放入烘箱,干燥,出料即得高导热填料。
步骤(1)中所述的处理室的温度为25~35℃,空气相对湿度为60~70%。
步骤(2)中所述的密封发酵的温度为25~35℃,密封发酵的时间为1~2天,炭化温度为300~400℃,炭化时间为1~2h。
步骤(3)中所述的多孔亚麻碳纤维和质量分数为30%的高锰酸钾的质量比为1:10,搅拌反应的温度为70~80℃,搅拌反应的时间为30~40min。
步骤(4)中所述的反应滤渣和质量分数为40%的硝酸铜溶液的质量比为1:8,超声振荡反应的频率为30~50kHz,超声振荡反应的时间为1~2h,滤渣和质量分数为50%的葡萄糖溶液的质量比为1:5,搅拌反应的温度为120~130℃,搅拌反应的时间为1~2h。
步骤(6)中所述的高导热填料粗品和猪油以及沼液的质量比为2:1:1,静置发酵的温度为25~35℃,静置发酵的时间为7~9天,干燥的温度为105~110℃,干燥的时间为1~2h。
本发明的有益效果是:
(1)本发明首先以亚麻纤维为原料,利用茶籽油浸渍亚麻纤维后放在高温高湿的条件下静置酸败,再将酸败纤维密封后短时间发酵,使得亚麻纤维微腐,在亚麻纤维表面产生微孔,炭化后再用高锰酸钾氧化,将氧化后的亚麻碳纤维依次和硝酸铜溶液以及葡萄糖溶液混合反应,再经电弧防电处理,制得导热材料粗品,最后将导热材料粗品和猪油以及沼液共混发酵改性,最终制得高导热填料,本发明制得的高导热填料首先以亚麻纤维为原料,利用油脂浸泡后在适合微生物生长的高温高湿条件下酸败处理,油脂酸败时产生的羧酸类物质会向亚麻纤维表面引入羧基,同时在微生物的作用下亚麻纤维会被微腐,从而在纤维表面产生微孔,得到多孔亚麻纤维,将多孔亚麻纤维炭化后,再用高锰酸钾将多孔亚麻纤维碳表面的羟基氧化成羧基,得到表面以及孔隙中带有羧基的多孔碳纤维,接着将碳纤维和硝酸铜溶液超声振荡反应,利用多孔碳纤维孔隙内部以及表面的羧基螯合固着铜离子,再用葡萄糖溶液在高温条件下将铜离子还原成铜单质,从而得到负载铜单质的碳纤维,接着通过电弧沉积的方法再在多孔载铜碳纤维表面沉积一层炭层,将碳纤维孔隙中的铜单质覆盖包覆,得到以铜为内核,碳质为壳的复合导热材料,铜和炭材料结为导热性良好的物质,并且用高稳定性的炭质材料将铜单质包覆后,可以起到保护作用,避免单质铜被氧化,提高铜粉的稳定性,而且本发明制得的导热填料是纤维状的物质,当其分布在环氧树脂基体中时会以无序状进行排列,形成物理状的网状结构,这层网状结构可以作为环氧树脂基体受到外力冲击时的应力传递路径,起到分散应力的作用,因此还提高了环氧树脂的抗冲击韧性,导热填料形成的物理网状结构大大提高了环氧树脂的热量传递效率,增大热量传递的范围,显著提高了环氧树脂的导热性能;
(2)本发明最后还对导热填料粗品进行了发酵改性,通过富含微生物的沼液向发酵体系中引入微生物,再利用微生物将生物油脂降解产生大量的游离性酯基基团,并在发酵的过程中将这些游离酯基基团引入到导热填料表面,而酯基作为疏水性基团,它的引入降低了导热填料粗品表面的表面能,使其在环氧树脂基团中更容易分散润湿,提高了导热填料和环氧树脂基体间的界面相容性,避免了由于界面相容性差导致的环氧树脂开裂以及导热性下降的缺陷,具有广阔的应用前景。
具体实施方式
称取亚麻秸秆用石磙反复碾压3~5遍,碾压后人工抽取亚麻纤维,将抽取的亚麻纤维用茶籽油浸泡20~30min后取出,平铺在竹筛中,再将竹筛移入温度为25~35℃,空气相对湿度为60~70%的处理室中,静置酸败4~5天;待酸败结束后,得到酸败产物,将酸败产物放入发酵罐中,密封罐口,在25~35℃下密封发酵1~2天,发酵结束后,过滤分离得到发酵滤渣,将发酵滤渣移入炭化炉中,在氮气保护作用下加热升温至300~400℃,炭化1~2h,得到多孔亚麻碳纤维;将多孔亚麻碳纤维和质量分数为30%的高锰酸钾按质量比为1:10混合后装入水浴锅中,加热升温至70~80℃,搅拌反应30~40min后过滤,分离得到反应滤渣;将反应滤渣和质量分数为40%的硝酸铜溶液按质量比为1:8混合后放入超声振荡仪中,以30~50kHz的频率振荡反应1~2h,反应结束后过滤分离得到滤渣,再将滤渣和质量分数为50%的葡萄糖溶液按质量比为1:5混合后装入烧瓶中,加热升温至120~130℃,搅拌反应1~2h;待搅拌反应结束后,过滤分离得到反应滤饼,将得到的反应滤饼作为阳极材料平铺在电弧放电系统的样品台上,再将石墨棒作为阴极材料固定在顶部电极杆上,调节石墨阴极材料与底部样品台阳极材料之间的距离为2~3mm,在氩气保护状态下以150~160A的电流放电反应5~10min,反应结束后取出反应后的阳极材料,即为高导热填料粗品;将高导热填料粗品和猪油以及沼液混合后装入发酵罐中,密封罐口后放在温度为25~35℃的条件下,静置发酵7~9天,发酵结束后过滤分离得到发酵滤饼,将发酵滤饼分别用无水乙醇和去离子水冲洗3~5遍后放入烘箱,在105~110℃下干燥1~2h,出料即得高导热填料。
称取亚麻秸秆用石磙反复碾压3遍,碾压后人工抽取亚麻纤维,将抽取的亚麻纤维用茶籽油浸泡20min后取出,平铺在竹筛中,再将竹筛移入温度为25℃,空气相对湿度为60%的处理室中,静置酸败4天;待酸败结束后,得到酸败产物,将酸败产物放入发酵罐中,密封罐口,在25℃下密封发酵1天,发酵结束后,过滤分离得到发酵滤渣,将发酵滤渣移入炭化炉中,在氮气保护作用下加热升温至300℃,炭化1h,得到多孔亚麻碳纤维;将多孔亚麻碳纤维和质量分数为30%的高锰酸钾按质量比为1:10混合后装入水浴锅中,加热升温至70℃,搅拌反应30min后过滤,分离得到反应滤渣;将反应滤渣和质量分数为40%的硝酸铜溶液按质量比为1:8混合后放入超声振荡仪中,以30kHz的频率振荡反应1h,反应结束后过滤分离得到滤渣,再将滤渣和质量分数为50%的葡萄糖溶液按质量比为1:5混合后装入烧瓶中,加热升温至120℃,搅拌反应1h;待搅拌反应结束后,过滤分离得到反应滤饼,将得到的反应滤饼作为阳极材料平铺在电弧放电系统的样品台上,再将石墨棒作为阴极材料固定在顶部电极杆上,调节石墨阴极材料与底部样品台阳极材料之间的距离为2mm,在氩气保护状态下以150A的电流放电反应5min,反应结束后取出反应后的阳极材料,即为高导热填料粗品;将高导热填料粗品和猪油以及沼液混合后装入发酵罐中,密封罐口后放在温度为25℃的条件下,静置发酵7天,发酵结束后过滤分离得到发酵滤饼,将发酵滤饼分别用无水乙醇和去离子水冲洗3遍后放入烘箱,在105℃下干燥1h,出料即得高导热填料。
称取亚麻秸秆用石磙反复碾压4遍,碾压后人工抽取亚麻纤维,将抽取的亚麻纤维用茶籽油浸泡25min后取出,平铺在竹筛中,再将竹筛移入温度为30℃,空气相对湿度为65%的处理室中,静置酸败4天;待酸败结束后,得到酸败产物,将酸败产物放入发酵罐中,密封罐口,在30℃下密封发酵2天,发酵结束后,过滤分离得到发酵滤渣,将发酵滤渣移入炭化炉中,在氮气保护作用下加热升温至350℃,炭化2h,得到多孔亚麻碳纤维;将多孔亚麻碳纤维和质量分数为30%的高锰酸钾按质量比为1:10混合后装入水浴锅中,加热升温至75℃,搅拌反应35min后过滤,分离得到反应滤渣;将反应滤渣和质量分数为40%的硝酸铜溶液按质量比为1:8混合后放入超声振荡仪中,以40kHz的频率振荡反应2h,反应结束后过滤分离得到滤渣,再将滤渣和质量分数为50%的葡萄糖溶液按质量比为1:5混合后装入烧瓶中,加热升温至125℃,搅拌反应2h;待搅拌反应结束后,过滤分离得到反应滤饼,将得到的反应滤饼作为阳极材料平铺在电弧放电系统的样品台上,再将石墨棒作为阴极材料固定在顶部电极杆上,调节石墨阴极材料与底部样品台阳极材料之间的距离为3mm,在氩气保护状态下以155A的电流放电反应8min,反应结束后取出反应后的阳极材料,即为高导热填料粗品;将高导热填料粗品和猪油以及沼液混合后装入发酵罐中,密封罐口后放在温度为30℃的条件下,静置发酵8天,发酵结束后过滤分离得到发酵滤饼,将发酵滤饼分别用无水乙醇和去离子水冲洗4遍后放入烘箱,在108℃下干燥2h,出料即得高导热填料。
称取亚麻秸秆用石磙反复碾压5遍,碾压后人工抽取亚麻纤维,将抽取的亚麻纤维用茶籽油浸泡30min后取出,平铺在竹筛中,再将竹筛移入温度为35℃,空气相对湿度为70%的处理室中,静置酸败5天;待酸败结束后,得到酸败产物,将酸败产物放入发酵罐中,密封罐口,在35℃下密封发酵2天,发酵结束后,过滤分离得到发酵滤渣,将发酵滤渣移入炭化炉中,在氮气保护作用下加热升温至400℃,炭化2h,得到多孔亚麻碳纤维;将多孔亚麻碳纤维和质量分数为30%的高锰酸钾按质量比为1:10混合后装入水浴锅中,加热升温至80℃,搅拌反应40min后过滤,分离得到反应滤渣;将反应滤渣和质量分数为40%的硝酸铜溶液按质量比为1:8混合后放入超声振荡仪中,以50kHz的频率振荡反应2h,反应结束后过滤分离得到滤渣,再将滤渣和质量分数为50%的葡萄糖溶液按质量比为1:5混合后装入烧瓶中,加热升温至130℃,搅拌反应2h;待搅拌反应结束后,过滤分离得到反应滤饼,将得到的反应滤饼作为阳极材料平铺在电弧放电系统的样品台上,再将石墨棒作为阴极材料固定在顶部电极杆上,调节石墨阴极材料与底部样品台阳极材料之间的距离为3mm,在氩气保护状态下以160A的电流放电反应10min,反应结束后取出反应后的阳极材料,即为高导热填料粗品;将高导热填料粗品和猪油以及沼液混合后装入发酵罐中,密封罐口后放在温度为35℃的条件下,静置发酵9天,发酵结束后过滤分离得到发酵滤饼,将发酵滤饼分别用无水乙醇和去离子水冲洗5遍后放入烘箱,在110℃下干燥2h,出料即得高导热填料。
对照例以广东省某公司生产的炭包铜导热材料作为对照例
对本发明制得的高导热材料和对照例中的导热材料进行性能检测,检测结果如表1所示:
表1 性能检测结果
由上表中检测数据可以看出,本发明制得的高导热材料具有极佳的导热效率,稳定性高,增韧抗冲击性能好,具有广阔的应用前景。
Claims (6)
1.一种环氧树脂用高导热填料的制备方法,其特征在于具体制备步骤为:
(1)称取亚麻秸秆用石磙反复碾压3~5遍,碾压后人工抽取亚麻纤维,将抽取的亚麻纤维用茶籽油浸泡20~30min后取出,平铺在竹筛中,再将竹筛移入处理室中,静置酸败4~5天;
(2)待上述酸败结束后,得到酸败产物,将酸败产物放入发酵罐中,密封发酵,发酵结束后,过滤分离得到发酵滤渣,将发酵滤渣移入炭化炉中,在氮气保护作用下炭化,得到多孔亚麻碳纤维;
(3)将上述多孔亚麻碳纤维和质量分数为30%的高锰酸钾混合后装入水浴锅中,搅拌反应后过滤,分离得到反应滤渣;
(4)将上述反应滤渣和质量分数为40%的硝酸铜溶液混合后放入超声振荡仪中,超声振荡反应,反应结束后过滤分离得到滤渣,再将滤渣和质量分数为50%的葡萄糖溶液混合后装入烧瓶中,搅拌反应;
(5)待上述搅拌反应结束后,过滤分离得到反应滤饼,将得到的反应滤饼作为阳极材料平铺在电弧放电系统的样品台上,再将石墨棒作为阴极材料固定在顶部电极杆上,调节石墨阴极材料与底部样品台阳极材料之间的距离为2~3mm,在氩气保护状态下以150~160A的电流放电反应5~10min,反应结束后取出反应后的阳极材料,即为高导热填料粗品;
(6)将上述高导热填料粗品和猪油以及沼液混合后装入发酵罐中,密封罐口后,静置发酵,发酵结束后过滤分离得到发酵滤饼,将发酵滤饼分别用无水乙醇和去离子水冲洗3~5遍后放入烘箱,干燥,出料即得高导热填料。
2.根据权利要求1所述的一种环氧树脂用高导热填料的制备方法,其特征在于:步骤(1)中所述的处理室的温度为25~35℃,空气相对湿度为60~70%。
3.根据权利要求1所述的一种环氧树脂用高导热填料的制备方法,其特征在于:步骤(2)中所述的密封发酵的温度为25~35℃,密封发酵的时间为1~2天,炭化温度为300~400℃,炭化时间为1~2h。
4.根据权利要求1所述的一种环氧树脂用高导热填料的制备方法,其特征在于:步骤(3)中所述的多孔亚麻碳纤维和质量分数为30%的高锰酸钾的质量比为1:10,搅拌反应的温度为70~80℃,搅拌反应的时间为30~40min。
5.根据权利要求1所述的一种环氧树脂用高导热填料的制备方法,其特征在于:步骤(4)中所述的反应滤渣和质量分数为40%的硝酸铜溶液的质量比为1:8,超声振荡反应的频率为30~50kHz,超声振荡反应的时间为1~2h,滤渣和质量分数为50%的葡萄糖溶液的质量比为1:5,搅拌反应的温度为120~130℃,搅拌反应的时间为1~2h。
6.根据权利要求1所述的一种环氧树脂用高导热填料的制备方法,其特征在于:步骤(6)中所述的高导热填料粗品和猪油以及沼液的质量比为2:1:1,静置发酵的温度为25~35℃,静置发酵的时间为7~9天,干燥的温度为105~110℃,干燥的时间为1~2h。
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CN109535855A (zh) * | 2018-10-29 | 2019-03-29 | 刘凡领 | 一种高效电热膜的制备方法 |
CN110527493A (zh) * | 2019-07-04 | 2019-12-03 | 浙江海洋大学 | 一种定形相变材料的制备方法 |
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CN109535855A (zh) * | 2018-10-29 | 2019-03-29 | 刘凡领 | 一种高效电热膜的制备方法 |
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