CN110539543A - 一种高强度绝热毡的制备方法 - Google Patents
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Abstract
本发明涉及一种高强度绝热毡的制备方法,属于吸附材料技术领域。本发明将顺丁橡胶和三元乙丙橡胶混合,通过静电纺丝技术制备橡胶纤维,通过溅射成膜技术在橡胶纤维表面镀一层铝膜,在橡胶纤维的表面包覆一层铝膜,将经过阳极氧化法处理后的铝箔和改性橡胶纤维复合,极大的阻止了热量的传递,形成了“热阻”效应,使得制备的绝热毡具有良好的绝热性和机械强度;本发明通过荷能粒子轰击靶材,使靶材表面原子或原子团逸出的现象,逸出的原子在基体表面形成与靶材表面成分相同的薄膜,该薄膜组织致密、无针孔、无气泡、厚度均匀,能有效增强橡胶纤维的强度,使得制备的绝热毡具有良好的机械性能。
Description
技术领域
本发明涉及一种高强度绝热毡的制备方法,属于绝热材料技术领域。
背景技术
超级绝热材料(Superinsulation)的概念是美国人HuntAJ等人在1992年的国际材料工程大会上提出的,是指在特定的使用条件下,导热系数低于“静止空气”导热系数的绝热材料。二氧化硅气凝胶材料的结构中具有大量的纳米孔隙,且85%以上的孔隙直径小于50nm,空气中的氧气、氮气分子的平均自由程约为70nm,当孔隙直径小于气体的平均自由程时,空气分子可以被视为“静止”,有效消除了气体的对流传热,同时超高气孔率又使得二氧化硅气凝胶材料的固相传热受到限制。由于二氧化硅气凝胶这种独特结构,使其具有优异的隔热保温性能,但其多孔的骨架同时也导致气凝胶材料的强度低、韧性小、力学性能差、结构不稳定,从而限制了其实际应用,因此,在维持二氧化硅气凝胶超级隔热性能的前提下,改善其力学性能能成为促进气凝胶材料发展和应用的重要途径。
目前较为有效的方法是采用纤维等材料作为增强体制备气凝胶复合材料,增强气凝胶的韧性和强度,解决其力学强度弱等问题。通常是以纳米级的二氧化硅粉末为主要组分加上纤维和其他助剂进行压制,再采用烧结或利用粘结剂成型,由于纳米孔绝热材料的绝热功能集中体现在其超细微的纳米级孔隙结构上,因而在加工制品时为了防止孔隙结构的破坏,添加烧结助剂或粘结助剂的用量都比较少,从而最终制备得到纳米孔绝热材料的整体机械强度都比较低、不耐撞击,而且上述纳米孔绝热材料在安装使用过程中,存在表面浮尘量大,极易产生可吸入的纤维及粉体,对人体、环境造成危害,易吸潮和不防水等缺点。
绝热毡是工业设备常用的保温材料,通常用于工业管道、储罐、工业炉体、电厂、注塑机、金属、玻璃等领域的保温隔热,如制成可拆卸式保温套等。
目前,气凝胶纤维毡是较为普遍的绝热毡,气凝胶纤维毡是将二氧化硅气凝胶复合于纤维毡中制得的保温材料,其中,纤维毡(常为玻璃纤维毡)提供了优异的强度和韧性,二氧化硅气凝胶提供了纳米孔洞、降低材料的对流传热,提高纤维毡的绝热效果。二者复合,充分结合了两种材料的优势,使绝热毡既具有良好的绝热保温效果,也具有优异的强度、韧性等机械性能,满足实际施工和使用需求。
以往,制备该类绝热毡的工艺包括超临界工艺和非超临界工艺。超临界工艺制得的气凝胶复合玻璃纤维毡具有更低的导热系数,但其生产成本极高,且存在较高危险性,难以实现市场化生产。相比之下,非临界工艺安全性提高,但产品性能如绝热性有所降低,且往往也要经过陈化、老化等工艺,生产周期较长,成本较高。
为克服上述问题,现有技术提出一些改进的制备方法,如公开号为CN105599396A的专利申请公开了一种喷压式气凝胶毡及其制备方法,所述喷压式气凝胶毡包括绝热布表层和绝热布底层,所述绝热布表层与绝热布底层之间设有至少一个复合绝热层,所述复合绝热层由玻璃纤维层以及气凝胶粉层复合在一起,产生隔热保温协同效应,解决了传统的气凝胶毡在运输、施工和使用过程中气凝胶微小颗粒、粉尘易脱落的现象,提高了气凝胶毡的使用寿命,且具有防潮、防火、耐腐蚀等优点。公开号为CN105209248A的专利申请公开了一种制造无纺湿法气凝胶毡的方法,所得气凝胶毡可呈现改善的导热率、较低的腐蚀性、较低的灰尘产生和均匀的结构。有别于传统超临界和非超临界工艺,上述制备方法相对简单易操作,为工业化生产提供了便利。
但是,上述方法仍存在一定缺陷,CN105599396A提供的方法仅将纤维毡和气凝胶粉料层叠在一起,无任何粘结剂,虽然上下层设有绝热布,能够抑制粉料脱落,但其绝热效果仍欠佳,且层间强度差,易剥落,尤其是在运输和施工过程中,纤维毡会受到不同程度振动,导致气凝胶粉料沿着纤维交织的孔洞迁移至上下表层,使气凝胶粉分布不均,更加影响绝热效果,且其憎水效果差。CN105209248A通过湿法制浆工艺制备气凝胶毡,虽可保证气凝胶粉料在坯体中均匀分布,但为保证毡体的强度和韧性,需引入大量有机结合剂,影响其导热性能,且该类气凝胶毡子在高温环镜下,有机结合剂会燃烧,导致毡体强度衰减严重,并挥发出大量刺激性烟气,严重影响使用效果,并对环境造成危害。因此,绝热毡的绝热性及强度韧性等机械性能往往难以兼顾,且尤其是经运输施工后,更易导致绝热性或强度明显下降。而如何获得绝热性、强度性能优异、环保,且性能保持性好的绝热毡已成为亟待解决的问题。
发明内容
本发明所要解决的技术问题:针对现有技术中绝热毡的绝热性及强度韧性等机械性能往往难以兼顾的问题,提供了一种高强度绝热毡的制备方法。
为解决上述技术问题,本发明采用的技术方案是:
(1)将顺丁橡胶和三元乙丙橡胶混合置于混炼机中,混炼处理,即得混炼胶,将混炼胶和二氯甲烷混合,高速搅拌处理,即得纺丝液,将纺丝液静电纺丝处理,即得橡胶纤维;
(2)将橡胶纤维进行溅射成膜处理,即得改性橡胶纤维;
(3)将铝箔进行脱脂处理,即得脱脂铝箔,按体积比1∶4将次氯酸和无水乙醇混合均匀,即得抛光液,将脱脂铝箔抛光处理,即得抛光铝箔;将抛光铝箔进行阳极氧化处理,即得预处理铝箔;
(4)将改性橡胶纤维置于纤维解离器中,以水为介质,解离3~5min,即得悬浮液,将聚氧化乙烯、丁苯乳液、阳离子聚丙烯酰胺和悬浮液混合,搅拌处理,即得前驱体溶液,将前驱体溶液进行抄取,即得湿纤维网,将湿纤维网置于温度为50~60℃的烘箱中,干燥至恒重,冷却至室温,即得纤维网;
(5)将卡夫特k-609粘结剂均匀涂抹在铝箔表面上,将纤维网覆盖在涂有粘结剂的铝箔表面上,并置于热压机中,热压处理,冷却至室温,即得高强度绝热毡。
步骤(1)所述的混炼处理步骤为:按质量比1∶1将顺丁橡胶和三元乙丙橡胶混合置于混炼机中,在温度为40~50℃下混炼20~30min。
步骤(1)所述的高速搅拌处理步骤为:按质量比1∶3将混炼胶和二氯甲烷混合,在搅拌速度为800~1000r/min,常温下高速搅拌8~12h。
步骤(1)所述的静电纺丝处理步骤为:将纺丝液置于注射器中,铝箔作为接收装置,在纺丝电压为20~25kV,接收距离为8~12cm下静电纺丝。
步骤(2)所述的溅射成膜处理步骤为:将橡胶纤维进行溅射成膜处理,溅射靶材为Φ60mm×3mm的高纯Al靶,纯度为99.999%,溅射气体为99.99%的氩气,反应气体为99.99%的氧气,真空室真空度为9.9×10-4Pa,靶基距60mm,溅射靶功率密度为5~15W/cm2。
步骤(3)所述的脱脂处理步骤为:将铝箔浸泡在质量分数为5%氢氧化钠溶液中10~15min后取出,用去离子水冲洗3~5次。
步骤(3)所述的抛光处理步骤为:将脱脂铝箔在电压为16~18V,温度为10~15℃下抛光3~5min后,用去离子水冲洗2~4次。
步骤(3)所述的阳极氧化处理步骤为:将抛光铝箔在质量分数为10%硫酸溶液中进行阳极氧化处理,电压为15~20kV,温度为20~25℃,时间为1~2h。
步骤(4)所述的搅拌处理步骤为:按质量比1∶1∶2∶10将聚氧化乙烯、丁苯乳液、阳离子聚丙烯酰胺和悬浮液混合,在搅拌速度为100~120r/min下搅拌3~5min。
步骤(5)所述的热压处理步骤为:在温度为480~190℃下热压50~60s。
本发明与其他方法相比,有益技术效果是:
(1)本发明将顺丁橡胶和三元乙丙橡胶混合,通过静电纺丝技术制备橡胶纤维,通过溅射成膜技术在橡胶纤维表面镀一层铝膜,在橡胶纤维的表面包覆一层铝膜,将经过阳极氧化法处理后的铝箔和改性橡胶纤维复合,热量在相邻纤维之间传递时会先经过铝膜,极大的阻止了热量的传递,形成了“热阻”效应,使得制备的绝热毡具有良好的绝热性和机械强度,铝膜在空气中能自我钝化形成微密的氧化膜而具有抗腐蚀性能;
(2)本发明中三元乙丙橡胶是乙烯、丙烯和少量的非共轭二烯烃的共聚物,是乙丙橡胶的一种,因其主链是由化学稳定的饱和烃组成,只在侧链中含有不饱和双键,故其耐臭氧、耐热、耐候等耐老化性能优异;顺丁橡胶是由丁二烯聚合而成的结构规整的合成橡胶,硫化后其耐寒性、耐磨性和弹性特别优异,动负荷下发热少,耐老化性尚好,将顺丁橡胶和三元乙丙橡胶混合,通过静电纺丝技术制备的橡胶纤维具有良好的耐热性、耐磨性和弹性;
(3)本发明通过荷能粒子轰击靶材,使靶材表面原子或原子团逸出的现象,逸出的原子在基体表面形成与靶材表面成分相同的薄膜,该薄膜组织致密、无针孔、无气泡、厚度均匀,能有效增强橡胶纤维的强度,使得制备的绝热毡具有良好的机械性能;
(4)本发明利用阳极氧化法预处理铝箔,具有清洁环保,能耗低等优势,将铝箔作为阳极,选择酸性电解液,酸性电解液主要是磷酸、铬酸、硫酸、硼酸、草酸等,在酸性电解液中,铝作为阳极被氧化成Al3+,Al3+与电解液中的O2-反应,生成Al2O3氧化膜;由于酸性电解液可将生成的Al2O3氧化膜溶解,使铝和铝制品表面形成的氧化膜产生孔隙,形成疏松多孔的Al2O3氧化膜,该膜不仅可以提高铝箔的耐腐蚀性,还可以提高其力学性能,如粘结强度和抗拉强度等,使得制备的绝热毡的物理机械性能得到提高;阳极氧化法预处理铝箔,可以使铝箔表面形成增强粘结界面积的疏松多孔氧化膜,从而提高橡胶纤维与铝箔的粘结性能,提高绝热毡的撕裂强度。
具体实施方式
按质量比1∶1将顺丁橡胶和三元乙丙橡胶混合置于混炼机中,在温度为40~50℃下混炼20~30min,即得混炼胶,按质量比1∶3将混炼胶和二氯甲烷混合,在搅拌速度为800~1000r/min,常温下高速搅拌8~12h,即得纺丝液,将纺丝液置于注射器中,铝箔作为接收装置,在纺丝电压为20~25kV,接收距离为8~12cm下静电纺丝,即得橡胶纤维;将橡胶纤维进行溅射成膜处理,溅射靶材为Φ60mm×3mm的高纯Al靶,纯度为99.999%,溅射气体为99.99%的氩气,反应气体为99.99%的氧气,真空室真空度为9.9×10-4Pa,靶基距60mm,溅射靶功率密度为5~15W/cm2,即得改性橡胶纤维;将铝箔浸泡在质量分数为5%氢氧化钠溶液中10~15min后取出,用去离子水冲洗3~5次,即得脱脂铝箔,按体积比1∶4将次氯酸和无水乙醇混合均匀,即得抛光液,将脱脂铝箔在电压为16~18V,温度为10~15℃下抛光3~5min后,用去离子水冲洗2~4次,即得抛光铝箔;将抛光铝箔在质量分数为10%硫酸溶液中进行阳极氧化处理,电压为15~20kV,温度为20~25℃,时间为1~2h,即得预处理铝箔;将改性橡胶纤维置于纤维解离器中,以水为介质,解离3~5min,即得悬浮液,按质量比1∶1∶2∶10将聚氧化乙烯、丁苯乳液、阳离子聚丙烯酰胺和悬浮液混合,在搅拌速度为100~120r/min下搅拌3~5min,即得前驱体溶液,将前驱体溶液进行抄取,即得湿纤维网,将湿纤维网置于温度为50~60℃的烘箱中,干燥至恒重,冷却至室温,即得纤维网;将卡夫特k-609粘结剂均匀涂抹在铝箔表面上,将纤维网覆盖在涂有粘结剂的铝箔表面上,并置于热压机中,在温度为180~190℃下热压50~60s,冷却至室温,即得高强度绝热毡。
实施例1
按质量比1∶1将顺丁橡胶和三元乙丙橡胶混合置于混炼机中,在温度为40℃下混炼20min,即得混炼胶,按质量比1∶3将混炼胶和二氯甲烷混合,在搅拌速度为800r/min,常温下高速搅拌8h,即得纺丝液,将纺丝液置于注射器中,铝箔作为接收装置,在纺丝电压为20kV,接收距离为8cm下静电纺丝,即得橡胶纤维;将橡胶纤维进行溅射成膜处理,溅射靶材为Φ60mm×3mm的高纯Al靶,纯度为99.999%,溅射气体为99.99%的氩气,反应气体为99.99%的氧气,真空室真空度为9.9×10-4Pa,靶基距60mm,溅射靶功率密度为5W/cm2,即得改性橡胶纤维;将铝箔浸泡在质量分数为5%氢氧化钠溶液中10min后取出,用去离子水冲洗3次,即得脱脂铝箔,按体积比1∶4将次氯酸和无水乙醇混合均匀,即得抛光液,将脱脂铝箔在电压为16V,温度为10℃下抛光3min后,用去离子水冲洗2次,即得抛光铝箔;将抛光铝箔在质量分数为10%硫酸溶液中进行阳极氧化处理,电压为15kV,温度为20℃,时间为1h,即得预处理铝箔;将改性橡胶纤维置于纤维解离器中,以水为介质,解离3min,即得悬浮液,按质量比1∶1∶2∶10将聚氧化乙烯、丁苯乳液、阳离子聚丙烯酰胺和悬浮液混合,在搅拌速度为100r/min下搅拌3min,即得前驱体溶液,将前驱体溶液进行抄取,即得湿纤维网,将湿纤维网置于温度为50℃的烘箱中,干燥至恒重,冷却至室温,即得纤维网;将卡夫特k-609粘结剂均匀涂抹在铝箔表面上,将纤维网覆盖在涂有粘结剂的铝箔表面上,并置于热压机中,在温度为180℃下热压50s,冷却至室温,即得高强度绝热毡。
实施例2
按质量比1∶1将顺丁橡胶和三元乙丙橡胶混合置于混炼机中,在温度为45℃下混炼25min,即得混炼胶,按质量比1∶3将混炼胶和二氯甲烷混合,在搅拌速度为900r/min,常温下高速搅拌10h,即得纺丝液,将纺丝液置于注射器中,铝箔作为接收装置,在纺丝电压为23kV,接收距离为10cm下静电纺丝,即得橡胶纤维;将橡胶纤维进行溅射成膜处理,溅射靶材为Φ60mm×3mm的高纯Al靶,纯度为99.999%,溅射气体为99.99%的氩气,反应气体为99.99%的氧气,真空室真空度为9.9×10-4Pa,靶基距60mm,溅射靶功率密度为10W/cm2,即得改性橡胶纤维;将铝箔浸泡在质量分数为5%氢氧化钠溶液中13min后取出,用去离子水冲洗4次,即得脱脂铝箔,按体积比1∶4将次氯酸和无水乙醇混合均匀,即得抛光液,将脱脂铝箔在电压为17V,温度为13℃下抛光45min后,用去离子水冲洗3次,即得抛光铝箔;将抛光铝箔在质量分数为10%硫酸溶液中进行阳极氧化处理,电压为17kV,温度为23℃,时间为1.5h,即得预处理铝箔;将改性橡胶纤维置于纤维解离器中,以水为介质,解离4min,即得悬浮液,按质量比1∶1∶2∶10将聚氧化乙烯、丁苯乳液、阳离子聚丙烯酰胺和悬浮液混合,在搅拌速度为110r/min下搅拌4min,即得前驱体溶液,将前驱体溶液进行抄取,即得湿纤维网,将湿纤维网置于温度为55℃的烘箱中,干燥至恒重,冷却至室温,即得纤维网;将卡夫特k-609粘结剂均匀涂抹在铝箔表面上,将纤维网覆盖在涂有粘结剂的铝箔表面上,并置于热压机中,在温度为185℃下热压55s,冷却至室温,即得高强度绝热毡。
实施例3
按质量比1∶1将顺丁橡胶和三元乙丙橡胶混合置于混炼机中,在温度为50℃下混炼30min,即得混炼胶,按质量比1∶3将混炼胶和二氯甲烷混合,在搅拌速度为1000r/min,常温下高速搅拌12h,即得纺丝液,将纺丝液置于注射器中,铝箔作为接收装置,在纺丝电压为25kV,接收距离为12cm下静电纺丝,即得橡胶纤维;将橡胶纤维进行溅射成膜处理,溅射靶材为Φ60mm×3mm的高纯Al靶,纯度为99.999%,溅射气体为99.99%的氩气,反应气体为99.99%的氧气,真空室真空度为9.9×10-4Pa,靶基距60mm,溅射靶功率密度为15W/cm2,即得改性橡胶纤维;将铝箔浸泡在质量分数为5%氢氧化钠溶液中15min后取出,用去离子水冲洗5次,即得脱脂铝箔,按体积比1∶4将次氯酸和无水乙醇混合均匀,即得抛光液,将脱脂铝箔在电压为18V,温度为15℃下抛光5min后,用去离子水冲洗4次,即得抛光铝箔;将抛光铝箔在质量分数为10%硫酸溶液中进行阳极氧化处理,电压为20kV,温度为25℃,时间为2h,即得预处理铝箔;将改性橡胶纤维置于纤维解离器中,以水为介质,解离5min,即得悬浮液,按质量比1∶1∶2∶10将聚氧化乙烯、丁苯乳液、阳离子聚丙烯酰胺和悬浮液混合,在搅拌速度为120r/min下搅拌5min,即得前驱体溶液,将前驱体溶液进行抄取,即得湿纤维网,将湿纤维网置于温度为60℃的烘箱中,干燥至恒重,冷却至室温,即得纤维网;将卡夫特k-609粘结剂均匀涂抹在铝箔表面上,将纤维网覆盖在涂有粘结剂的铝箔表面上,并置于热压机中,在温度为190℃下热压60s,冷却至室温,即得高强度绝热毡。
将本发明制备的高强度绝热毡及市售绝热毡进行检测,具体检测结果如下表表1:
测试方法:
进行GB/T3001-2007抗折强度、 GB/T10294-2008导热系数、GB/T5988-2007加热线变化测试。
表1高强度绝热毡性能表征
由表1可知本发明制备的高强度绝热毡,抗折强度大,导热系数小,在600℃维持24小时后其加热永久线变化低于0.5%,表现出较好的柔韧性和隔热保温性能。
Claims (10)
1.一种高强度绝热毡的制备方法,其特征在于具体制备步骤为:
(1)将顺丁橡胶和三元乙丙橡胶混合置于混炼机中,混炼处理,即得混炼胶,将混炼胶和二氯甲烷混合,高速搅拌处理,即得纺丝液,将纺丝液静电纺丝处理,即得橡胶纤维;
(2)将橡胶纤维进行溅射成膜处理,即得改性橡胶纤维;
(3)将铝箔进行脱脂处理,即得脱脂铝箔,按体积比1∶4将次氯酸和无水乙醇混合均匀,即得抛光液,将脱脂铝箔抛光处理,即得抛光铝箔;将抛光铝箔进行阳极氧化处理,即得预处理铝箔;
(4)将改性橡胶纤维置于纤维解离器中,以水为介质,解离3~5min,即得悬浮液,将聚氧化乙烯、丁苯乳液、阳离子聚丙烯酰胺和悬浮液混合,搅拌处理,即得前驱体溶液,将前驱体溶液进行抄取,即得湿纤维网,将湿纤维网置于温度为50~60℃的烘箱中,干燥至恒重,冷却至室温,即得纤维网;
(5)将卡夫特k-609粘结剂均匀涂抹在铝箔表面上,将纤维网覆盖在涂有粘结剂的铝箔表面上,并置于热压机中,热压处理,冷却至室温,即得高强度绝热毡。
2.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(1)所述的混炼处理步骤为:按质量比1∶1将顺丁橡胶和三元乙丙橡胶混合置于混炼机中,在温度为40~50℃下混炼20~30min。
3.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(1)所述的高速搅拌处理步骤为:按质量比1∶3将混炼胶和二氯甲烷混合,在搅拌速度为800~1000r/min,常温下高速搅拌8~12h。
4.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(1)所述的静电纺丝处理步骤为:将纺丝液置于注射器中,铝箔作为接收装置,在纺丝电压为20~25kV,接收距离为8~12cm下静电纺丝。
5.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(2)所述的溅射成膜处理步骤为:将橡胶纤维进行溅射成膜处理,溅射靶材为Φ60mm×3mm的高纯Al靶,纯度为99.999%,溅射气体为99.99%的氩气,反应气体为99.99%的氧气,真空室真空度为9.9×10-4Pa,靶基距60mm,溅射靶功率密度为5~15W/cm2。
6.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(3)所述的脱脂处理步骤为:将铝箔浸泡在质量分数为5%氢氧化钠溶液中10~15min后取出,用去离子水冲洗3~5次。
7.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(3)所述的抛光处理步骤为:将脱脂铝箔在电压为16~18V,温度为10~15℃下抛光3~5min后,用去离子水冲洗2~4次。
8.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(3)所述的阳极氧化处理步骤为:将抛光铝箔在质量分数为10%硫酸溶液中进行阳极氧化处理,电压为15~20kV,温度为20~25℃,时间为1~2h。
9.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(4)所述的搅拌处理步骤为:按质量比1∶1∶2∶10将聚氧化乙烯、丁苯乳液、阳离子聚丙烯酰胺和悬浮液混合,在搅拌速度为100~120r/min下搅拌3~5min。
10.根据权利要求1所述的一种高强度绝热毡的制备方法,其特征在于:步骤(5)所述的热压处理步骤为:在温度为480~190℃下热压50~60s。
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