CN110655695A - 一种阻燃橡塑保温发泡材料及制备方法 - Google Patents
一种阻燃橡塑保温发泡材料及制备方法 Download PDFInfo
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Abstract
本发明涉及保温材料领域,公开了一种阻燃橡塑保温发泡材料及制备方法。包括如下制备过程:(1)以无机阻燃剂、无机微球和水玻璃为原料制备阻燃微球;(2)以CPE/CPVC树脂、阻燃微球、分散剂、偶联剂为原料制备橡塑阻燃母料;(3)以丁腈橡胶、PVC、橡塑阻燃母料、钙锌热稳定剂、热塑性弹性体、填充补强体系、增塑剂、AC发泡剂、硫化剂和硫化促进剂为原料制成胶条;(4)将胶条挤出成型后分段硫化发泡成型,制得橡塑保温发泡材料。本发明制得的橡塑保温发泡材料中,借助无机微球的高流动性和高润滑性,使得无机阻燃剂均匀分散,不影响橡塑发泡材料的强度,阻燃性能优异,拓宽了橡塑发泡材料的应用领域。
Description
技术领域
本发明涉及保温材料领域,公开了一种阻燃橡塑保温发泡材料及制备方法。
背景技术
随着我国科技的不断进步,近年来我国保温技术水平也有很大地提高,保温材料的生产能力也在不断扩大。其中,橡塑保温材料闭孔弹性材料,具有质轻、柔软、耐屈挠、耐寒、耐热、防水、导热系数低、减震、吸音等优异性能,被广泛应用于大型中央空调系统及热水管道、冷冻水管的保温。
目前的橡塑保温材料主要以聚氯乙烯和丁腈橡胶(PVC/NBR)为主要材料,添加各种优质辅助材料,经发泡而制成。但目前的橡塑发泡材料生产遵循胶硫化和发泡剂分解速率匹配性的原则,但是加工工序复杂,且容易产生大量烟雾,污染环境,因此需要改进。
无机阻燃母粒一般是由过量的无机阻燃剂粉体和颗粒状树脂载体经混合、塑化、挤出和造粒等工序制得的一种高浓缩型功能性颗粒。然而由于无机粉体与颗粒状树脂在比重、粒径、粒子形态以及粒子表面能方面存在很大的差距,在物料混合的过程中极易出现偏析现象,极大降低了混合物的均匀程度,从而影响发泡材料的阻燃稳定性和力学性能。
中国发明专利申请号201310268942.3公开了一种阻燃型NBR/CPVC橡塑发泡保温材料组合物,是由以下重量份的组分制成的:丁腈橡胶60~75份,CPVC树脂30~45份,Ca/Zn热稳定剂4~7份,阻燃性增塑剂20~50份,阻燃剂40~50份,偶氮二甲酰胺8~10份;硫磺2~4份;硫化促进剂4~7份,硫化活性剂7~9份,防老剂2~6份,补强剂25~40份,微晶蜡1.2~3份。
中国发明专利申请号201710873411.5公开了一种阻燃橡塑发泡保温材料的制备方法,将玻璃纤维和海泡石加入粉碎机中粉碎至颗粒状态;加入三元乙丙橡胶、氯丁橡胶和二乙二醇单丁醚,在温度140~150℃下快速搅拌反应20~30min;加入四溴双酚A、三异丙基亚磷酸酯,待温度降至100~120℃,静置反应30~40min;继续调整温度至80~100℃,加入偶氮二甲酰胺,边滴加边搅拌反应30~40min;随后冷却、烘干后即可得到阻燃橡塑发泡保温材料。
根据上述,现有方案中用于橡塑保温材料的无机阻燃剂在体系中难以均匀分散,存在阻燃稳定性和力学性能较差的缺陷,本发明提出了一种阻燃橡塑保温发泡材料及制备方法,可有效解决上述技术问题。
发明内容
目前应用较广的橡塑保温材料材料中,添加无机阻燃剂时,由于无机阻燃材料与树脂基体相容性差,致使无机阻燃剂在橡塑保温材料中分散性差,影响了材料的阻燃稳定性和力学性能。
本发明通过以下技术方案达到上述目的:
一种阻燃橡塑保温发泡材料的制备方法,制备的具体过程为:
(1)先配制水玻璃水溶液并加热,再将无机阻燃剂、无机微球分别浸渍在水玻璃水溶液中,一定时间后取出,采用流化床高速对撞干燥,制得组装的阻燃微球;
(2)以CPE/CPVC树脂作为载体树脂,加入步骤(1)制得的阻燃微球、分散剂、偶联剂混合,然后利用双螺杆挤出机挤出得到橡塑阻燃母料;
(3)先将丁腈橡胶、PVC、步骤(2)制得的橡塑阻燃母料、钙锌热稳定剂、热塑性弹性体、填充补强体系、增塑剂、AC发泡剂进行混炼,切割成胶片,再将所得胶片存放18~30h,加入硫化剂和硫化促进剂进行二次复炼,并加工成胶条;
(4)先将步骤(3)得到的胶条挤出成型,然后进行分段硫化发泡成型,制得橡塑保温发泡材料。
水玻璃是水溶性硅酸盐的水溶液,是一种矿物黏合剂,粘结力高,耐热性好,具有一定的阻燃能力,本发明通过水玻璃粘合无机阻燃剂和无机微球载体,制得组装的阻燃微球,不仅具有协同阻燃作用,提高了材料的阻燃性,而且无机微球的高流动性和高润滑性,使得阻燃微球可在树脂中均匀分散。作为本发明的优选,所述水玻璃水溶液是质量浓度为15%;所述无机阻燃剂为氢氧化铝、氢氧化镁、三氧化二锑中的至少一种;所述无机微球为玻璃微球、陶瓷微球、二氧化硅微球中的至少一种;所述各原料配比为,按质量百分数计,无机阻燃剂5~10%、无机微球20~30%、水玻璃水溶液60~75%。
氯化聚乙烯(CPE)为饱和高分子材料,是由高密度聚乙烯(HDPE)经氯化取代反应制得的高分子材料,具有优良的耐侯性、耐臭氧、耐化学药品及耐老化性能,具有良好的耐油性、阻燃性及着色性能。韧性良好(在-30℃仍有柔韧性),与其它高分子材料具有良好的相容性,除了可以单独使用以外,还可以与聚氯乙烯(PVC)、聚乙烯(PE)、聚丙烯(PP)、聚苯乙烯(PS)、ABS等树脂甚至聚氨酯(PU)共混使用。在橡胶工业中,CPE可作为高性能、高质量的特种橡胶,也可以与乙丙橡胶(EPR)、丁基橡胶(IIR)、丁腈橡胶(NBR)、氯磺化聚乙烯(CSM)等其它橡胶共混使用;CPVC 是一种应用前景广阔的新型工程塑料,由聚氯乙烯(PVC)树脂氯化改性制得,经过氯化后,分子键的不规则性增加,极性增加,使树脂的溶解性增大,化学稳定性增加,从而提高了材料的耐热性、耐酸、碱、盐、氧化剂等的腐蚀,提高了树脂的热变形温度的机械性能。通过CPE和CPVC共混得到CPE/CPVC树脂,进一步提高了树脂的机械性能和热学性能。本发明以CPE/CPVC树脂作为载体树脂,通过加入阻燃微球制备橡塑阻燃母料,不仅方法简单,而且可在保证无机阻燃剂良好分散性的同时,得到机械性能和热学性能优异的复合阻燃母料。作为本发明的优选,所述分散剂为亚甲基双萘磺酸钠、亚甲基双甲基萘磺酸钠、焦磷酸钠、硬脂酸钠中的至少一种;所述偶联剂为γ-氨丙基三乙氧基硅烷、γ-氨丙基三甲氧基硅烷、γ-巯丙基三甲氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷中的至少一种;所述各原料配比为,按质量百分数计,CPE树脂30~52%、CPVC树脂30~40%、阻燃微球15~25%、分散剂1~2%、偶联剂2~3%。
聚氯乙烯(PVC)具有较高的机械强度、良好的耐酸碱性能、介电性能和绝缘性能,同时和一般的橡胶相比,其还具有较好的耐磨性能及阻燃性能,氮气抗冲击性能、耐热、光稳定性较差,尤其是低温脆性就曲挠性能不好,而丁腈橡胶(NBR)在性能上基本能够弥补上述不足,而且PVC和 NBR都是极性聚合物,溶解度参数非常相近,相容性好,得到的PVC/NBR橡塑材料物理机械性能和阻燃性能较佳,进一步通过发泡成型,成为优质的橡塑保温发泡材料。由于橡塑阻燃母料中的无机阻燃剂的均匀分散,保证了材料的阻燃稳定性和机械强度。作为本发明的优选,所述热塑性弹性体为丁二烯-苯乙烯共聚物、异戊二烯-苯乙烯共聚物、热塑性聚氨酯中的一种;所述填充补强体系为纳米炭黑、白炭黑中的至少一种;所述增塑剂为邻苯二甲酸二仲辛酯、邻苯二甲酸二环己酯、邻苯二甲酸二丁酯、邻苯二甲酸二乙酯、邻苯二甲酸二正辛酯、邻苯二甲酸二甲酯中的至少一种;所述硫化剂为秋兰姆;所述各原料配比为,按质量百分数计,丁腈橡胶50-6-重量份、PVC 5~7重量份、橡塑阻燃母料55~72重量份、钙锌热稳定剂1~2重量份;热塑性弹性体4~6重量份、填充补强体系5~8重量份、增塑剂2~4重量份、AC发泡剂0.5~2重量份、硫化剂2~3重量份。
作为本发明的优选,步骤(1)所述加热温度为60℃,浸渍时间为1~2h。
作为本发明的优选,步骤(3)所述混炼温度为110-120℃,时间为10~15min。复炼温度为80℃。
采用分段硫化发泡成型的工艺,不仅能够使得硫化更彻底,而且可使发泡形成的泡孔更加均匀,提升发泡效果。作为本发明的优选,步骤(4)所述分段硫化发泡采用180℃条件下5-6min,130℃条件下8-10min。
由上述方法制备得到的一种阻燃橡塑保温发泡材料,无机阻燃剂在橡塑保温发泡材料分散均匀,其不但具有良好的阻燃稳定性,而且不影响橡塑发泡材料的强度。
本发明提供的一种阻燃橡塑保温发泡材料及制备方法,先配制水玻璃水溶液,再将无机阻燃剂、无机微球分别浸渍在水玻璃水溶液中,取出后用流化床高速对撞干燥,得到组装的阻燃微球,待用;以CPE/CPVC树脂作为载体树脂,加入阻燃微球,分散剂,偶联剂混合,利用双螺杆挤出机挤出得到橡塑阻燃母料;将丁腈橡胶、PVC、橡塑阻燃母料、钙锌热稳定剂、热塑性弹性体、填充补强体系、增塑剂、AC发泡剂进行混炼,切割成胶片,再将所得胶片存放一定时间后加入硫化剂,进行二次复炼,加工成胶条;最后将所得胶条挤出成型后,进行分段硫化发泡成型,即可。
本发明提供了一种阻燃橡塑保温发泡材料及制备方法,与现有技术相比,其突出的特点和优异的效果在于:
1、提出了采用水玻璃为粘结剂组装阻燃微球制备阻燃橡塑保温发泡材料的方法。
2、通过水玻璃粘合无机阻燃剂和微球载体,并制备成母料,接着进一步加入橡塑材料基体中混炼、分段硫化发泡成型得到橡塑保温发泡材料,处理手段简单易实现。
3、本发明制得的橡塑保温发泡材料中,借助阻燃微球中无机微球的高流动性和高润滑性,利于无机阻燃剂的均匀分散,不影响橡塑发泡材料的强度,并且具有优异的阻燃性能,拓宽了橡塑发泡材料的应用领域。
具体实施方式
以下通过具体实施方式对本发明作进一步的详细说明,但不应将此理解为本发明的范围仅限于以下的实例。在不脱离本发明上述方法思想的情况下,根据本领域普通技术知识和惯用手段做出的各种替换或变更,均应包含在本发明的范围内。
实施例1
(1)先配制水玻璃水溶液并加热,再将无机阻燃剂、无机微球分别浸渍在水玻璃水溶液中,一定时间后取出,采用流化床高速对撞干燥,制得组装的阻燃微球;水玻璃水溶液是质量浓度为15%;无机阻燃剂为氢氧化铝;无机微球为玻璃微球;加热温度为60℃,浸渍时间为2h;
原料配比为,按质量百分数计,无机阻燃剂10%、无机微球25%、水玻璃水溶液65%;
(2)以CPE/CPVC树脂作为载体树脂,加入阻燃微球、分散剂、偶联剂混合,然后利用双螺杆挤出机挤出得到橡塑阻燃母料;分散剂为亚甲基双萘磺酸钠;偶联剂为γ-氨丙基三乙氧基硅烷;
原料配比为,按质量百分数计,CPE树脂42%、CPVC树脂30%、阻燃微球25%、分散剂1%、偶联剂2%;
(3)先将丁腈橡胶、PVC、橡塑阻燃母料、钙锌热稳定剂、热塑性弹性体、填充补强体系、增塑剂、AC发泡剂进行混炼,切割成胶片,再将所得胶片存放18h,加入硫化剂进行二次复炼,并加工成胶条;热塑性弹性体为热塑性聚氨酯;填充补强体系为白炭黑;增塑剂为邻苯二甲酸二仲辛酯;硫化剂为秋兰姆;混炼温度为110℃,时间为15min;复炼温度为80℃。
原料配比为,按质量百分数计,丁腈橡胶50重量份、PVC 5重量份、橡塑阻燃母料60重量份、钙锌热稳定剂1重量份、热塑性弹性体6重量份、填充补强体系8重量份、增塑剂3重量份、AC发泡剂2重量份、硫化剂2重量份;
(4)先将所得胶条挤出成型,然后进行分段硫化发泡成型,制得橡塑保温发泡材;所述分段硫化发泡采用180℃条件下5min,130℃条件下8min。
实施例2
(1)先配制水玻璃水溶液并加热,再将无机阻燃剂、无机微球分别浸渍在水玻璃水溶液中,一定时间后取出,采用流化床高速对撞干燥,制得组装的阻燃微球;水玻璃水溶液是质量浓度为15%;无机阻燃剂为三氧化二锑;无机微球为陶瓷微球;加热温度为60℃,浸渍时间为1h;
原料配比为,按质量百分数计,无机阻燃剂8%、无机微球22%、水玻璃水溶液70%;
(2)以CPE/CPVC树脂作为载体树脂,加入阻燃微球、分散剂、偶联剂混合,然后利用双螺杆挤出机挤出得到橡塑阻燃母料;分散剂为亚甲基双萘磺酸钠;偶联剂为γ-氨丙基三甲氧基硅烷;
原料配比为,按质量百分数计,CPE树脂40%、CPVC树脂36%、阻燃微球20%、分散剂2%、偶联剂2%;
(3)先将丁腈橡胶、PVC、橡塑阻燃母料、钙锌热稳定剂、热塑性弹性体、填充补强体系、增塑剂、AC发泡剂进行混炼,切割成胶片,再将所得胶片存放20h,加入硫化剂进行二次复炼,并加工成胶条;热塑性弹性体为热塑性聚氨酯;填充补强体系为纳米炭黑;增塑剂为邻苯二甲酸二环己酯;硫化剂为秋兰姆;混炼温度为110℃,时间为15min;复炼温度80℃。
原料配比为,按质量百分数计,丁腈橡胶55重量份、PVC 6重量份、橡塑阻燃母料64重量份、钙锌热稳定剂1重量份、热塑性弹性体4重量份、填充补强体系8重量份、增塑剂4重量份、AC发泡剂1.5重量份、硫化剂2重量份;
(4)先将所得胶条挤出成型,然后进行分段硫化发泡成型,制得橡塑保温发泡材;所述分段硫化发泡采用180℃条件下6min,130℃条件下8min。
实施例3
(1)先配制水玻璃水溶液并加热,再将无机阻燃剂、无机微球分别浸渍在水玻璃水溶液中,一定时间后取出,采用流化床高速对撞干燥,制得组装的阻燃微球;水玻璃水溶液是质量浓度为15%;无机阻燃剂为氢氧化镁;无机微球为二氧化硅微球;加热温度为60℃,浸渍时间为1.5h;
原料配比为,按质量百分数计,无机阻燃剂7%、无机微球26%、水玻璃水溶液67%;
(2)以CPE/CPVC树脂作为载体树脂,加入阻燃微球、分散剂、偶联剂混合,然后利用双螺杆挤出机挤出得到橡塑阻燃母料;分散剂为焦磷酸钠;偶联剂为乙烯基三乙氧基硅烷;
原料配比为,按质量百分数计,CPE树脂42%、CPVC树脂36%、阻燃微球18%、分散剂1%、偶联剂3%;
(3)先将丁腈橡胶、PVC、橡塑阻燃母料、钙锌热稳定剂、热塑性弹性体、填充补强体系、增塑剂、AC发泡剂进行混炼,切割成胶片,再将所得胶片存放25h,加入硫化剂进行二次复炼,并加工成胶条;热塑性弹性体为异戊二烯-苯乙烯共聚物;填充补强体系为白炭黑;增塑剂为邻苯二甲酸二正辛酯;硫化剂为秋兰姆;混炼温度为110℃,时间为14min;复炼温度为80℃。
原料配比为,按质量百分数计,丁腈橡胶10重量份、PVC 5重量份、橡塑阻燃母料65重量份、钙锌热稳定剂2重量份、热塑性弹性体5重量份、填充补强体系7重量份、增塑剂3重量份、AC发泡剂1重量份、硫化剂2重量份;
(4)先将所得胶条挤出成型,然后进行分段硫化发泡成型,制得橡塑保温发泡材;所述分段硫化发泡采用180℃条件下5min,130℃条件下10min。
实施例4
(1)先配制水玻璃水溶液并加热,再将无机阻燃剂、无机微球分别浸渍在水玻璃水溶液中,一定时间后取出,采用流化床高速对撞干燥,制得组装的阻燃微球;水玻璃水溶液是质量浓度为15%;无机阻燃剂为三氧化二锑;无机微球为玻璃微球;加热温度为60℃,浸渍时间为2h;
原料配比为,按质量百分数计,无机阻燃剂10%、无机微球30%、水玻璃水溶液60%;
(2)以CPE/CPVC树脂作为载体树脂,加入阻燃微球、分散剂、偶联剂混合,然后利用双螺杆挤出机挤出得到橡塑阻燃母料;分散剂为亚甲基双甲基萘磺酸钠;偶联剂为乙烯基三乙氧基硅烷;
原料配比为,按质量百分数计,CPE树脂52%、CPVC树脂30%、阻燃微球15%、分散剂1%、偶联剂2%;
(3)先将丁腈橡胶、PVC、橡塑阻燃母料、钙锌热稳定剂、热塑性弹性体、填充补强体系、增塑剂、AC发泡剂进行混炼,切割成胶片,再将所得胶片存放30h,加入硫化剂进行二次复炼,并加工成胶条;热塑性弹性体为丁二烯-苯乙烯共聚物;填充补强体系为白炭黑;增塑剂为邻苯二甲酸二乙酯;硫化剂为秋兰姆;混炼温度为110℃,时间为12min;复炼温度为80℃。
原料配比为,按质量百分数计,丁腈橡胶8重量份、PVC 5重量份、橡塑阻燃母料72重量份、钙锌热稳定剂1重量份、热塑性弹性体4重量份、填充补强体系5重量份、增塑剂2重量份、AC发泡剂0.5重量份、硫化剂2重量份;
(4)先将所得胶条挤出成型,然后进行分段硫化发泡成型,制得橡塑保温发泡材;所述分段硫化发泡采用180℃条件下6min,130℃条件下8min。。
对比例1
对比例1没有采用水玻璃粘结无机阻燃剂、无机微球制备阻燃微球,而是直接添加无机阻燃剂,其他条件和实施例1相同,制得的橡塑保温发泡材料,其拉伸强度、撕裂强度、硬度及氧指数如表2所示。
上述性能指标的测试方法为:
拉伸强度:拉伸强度根据GB/T 6344-2008测定,试样裁刀尺寸为120mm×10mm,标点距离为25mm,拉伸速率为500mm/min;
氧指数:氧指数根据GB/T2406-2009进行测试,采用JF-3氧指数测试仪。
表1:
Claims (9)
1.一种阻燃橡塑保温发泡材料的制备方法,其特征在于,制备的具体过程为:
(1)先配制水玻璃水溶液并加热,再将无机阻燃剂、无机微球分别浸渍在水玻璃水溶液中,一定时间后取出,采用流化床高速对撞干燥,制得组装的阻燃微球;
(2)以CPE/CPVC树脂作为载体树脂,加入步骤(1)制得的阻燃微球、分散剂、偶联剂混合,然后利用双螺杆挤出机挤出得到橡塑阻燃母料;
(3)先将丁腈橡胶、PVC、步骤(2)制得的橡塑阻燃母料、钙锌热稳定剂、热塑性弹性体、填充补强体系、增塑剂、AC发泡剂进行混炼,切割成胶片,再将所得胶片存放18~30h,加入硫化剂进行二次复炼,并加工成胶条;
(4)先将步骤(3)得到的胶条挤出成型,然后进行分段硫化发泡成型,制得橡塑保温发泡材料。
2.根据权利要求1所述一种阻燃橡塑保温发泡材料的制备方法,其特征在于:
所述水玻璃水溶液是质量浓度为15%;
所述无机阻燃剂为氢氧化铝、氢氧化镁、三氧化二锑中的至少一种;
所述无机微球为玻璃微球、陶瓷微球、二氧化硅微球中的至少一种;
所述分散剂为亚甲基双萘磺酸钠、亚甲基双甲基萘磺酸钠、焦磷酸钠、硬脂酸钠中的至少一种;
所述偶联剂为γ-氨丙基三乙氧基硅烷、γ-氨丙基三甲氧基硅烷、γ-巯丙基三甲氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷中的至少一种;
所述热塑性弹性体为丁二烯-苯乙烯共聚物、异戊二烯-苯乙烯共聚物、热塑性聚氨酯中的一种;
所述填充补强体系为纳米炭黑、白炭黑中的至少一种;
所述增塑剂为邻苯二甲酸二仲辛酯、邻苯二甲酸二环己酯、邻苯二甲酸二丁酯、邻苯二甲酸二乙酯、邻苯二甲酸二正辛酯、邻苯二甲酸二甲酯中的至少一种;
所述硫化剂为秋兰姆。
3.根据权利要求1所述一种阻燃橡塑保温发泡材料的制备方法,其特征在于:步骤(1)所述各原料配比为,按质量百分数计,无机阻燃剂5~10%、无机微球20~30%、水玻璃水溶液60~75%。
4.根据权利要求1所述一种阻燃橡塑保温发泡材料的制备方法,其特征在于:步骤(2)所述各原料配比为,按质量百分数计,CPE树脂30~52%、CPVC树脂30~40%、阻燃微球15~25%、分散剂1~2%、偶联剂2~3%。
5.根据权利要求1所述一种阻燃橡塑保温发泡材料的制备方法,其特征在于:步骤(3)所述各原料配比为,按重量份计,丁腈橡胶50-60重量份、PVC 5~7重量份、橡塑阻燃母料55~72重量份、钙锌热稳定剂1~2重量份、热塑性弹性体4~6重量份、填充补强体系5~8重量份、增塑剂2~4重量份、AC发泡剂0.5~2重量份、硫化剂2~3重量份。
6.根据权利要求1所述一种阻燃橡塑保温发泡材料的制备方法,其特征在于:步骤(1)所述加热温度为60℃,浸渍时间为1~2h。
7.根据权利要求1所述一种阻燃橡塑保温发泡材料的制备方法,其特征在于:步骤(3)所述混炼温度为110-120℃,时间为10~15min,复炼温度为80℃。
8.根据权利要求1所述一种阻燃橡塑保温发泡材料的制备方法,其特征在于:步骤(4)所述分段硫化发泡采用180℃条件下5-6min,130℃条件下8-10min。
9.权利要求1~8任一项所述方法制备得到的一种阻燃橡塑保温发泡材料。
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