CN108192145A - 一种二维纳米填料协效阻燃剂及其制备方法、应用 - Google Patents
一种二维纳米填料协效阻燃剂及其制备方法、应用 Download PDFInfo
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- CN108192145A CN108192145A CN201810024903.1A CN201810024903A CN108192145A CN 108192145 A CN108192145 A CN 108192145A CN 201810024903 A CN201810024903 A CN 201810024903A CN 108192145 A CN108192145 A CN 108192145A
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Abstract
本发明属于聚合物阻燃剂技术领域，具体涉及一种二维纳米填料协效阻燃剂及其制备方法、应用，所述协效阻燃剂的组成是：阻燃剂100质量份，二维纳米填料2～500质量份，植物多酚5～500质量份，多价金属盐1～100质量份。该协效阻燃剂的制备方法是：先利用植物多酚和多价金属离子的多配位络合反应分别对阻燃剂和二维纳米填料进行包覆，然后再利用该络合反应将阻燃剂负载到二维纳米填料表面；其原料配比科学合理，制备工艺简单，操作方便，成本低，制备的协效阻燃剂分散性好，阻燃效率高，将其通过溶液共混、乳液共混或熔融共混的方法添加到聚合物基体中，能够制备出兼具优异阻燃和力学等性能的高性能阻燃聚合物复合材料，应用广泛。
Description
技术领域：
本发明属于聚合物阻燃剂技术领域，具体涉及一种二维纳米填料协效阻燃剂及其制备方法、应用。
背景技术：
聚合物的易燃性给人类的生产生活带来了严重的安全隐患，因此，阻燃聚合物材料的开发具有重要的现实意义和紧迫性。聚合物的阻燃机理包括气相阻燃、凝聚相阻燃和协效阻燃，其中气相阻燃机理主要是通过捕捉燃烧的链支化反应所需的自由基或产生不可燃性气体稀释可燃气体来实现；凝聚相阻燃机理最主要的是成炭阻燃机理，即通过炭层阻隔气相和凝聚相间热量和物质的交换实现的，相比于气相阻燃机理，凝聚相成炭阻燃机理更常见；协效阻燃是指通过不同阻燃机理的多种阻燃剂的合理复配发挥出比单一阻燃剂更高的阻燃效果，因此，协效阻燃是阻燃领域的研究热点【Polymer Degradation andStability,2016,130,194】。
传统的阻燃剂有卤系阻燃剂、磷系阻燃剂、膨胀型阻燃剂、硅系阻燃剂和无机阻燃剂，但是由于绝大多数阻燃剂都是极性的，导致其与聚合物基体的相容性较差，使用过程中会发生分散不均匀、表面迁移等问题；而且绝大多数阻燃剂要想发挥有效的阻燃效果，填充量往往较大，导致聚合物的力学、老化等性能严重下降。通过阻燃剂的包覆改性提高阻燃剂与基体的相容性是解决上述问题的有效途径【Polymer Degradation and Stability,2015,113,96；Journal of Thermal Analysis and Calorimetry,2014,118,349；Journalof Thermal Analysis and Calorimetry,2016,123,1239】。此外，为了构建协效阻燃体系，炭层补强是一个关键切入点，具有二维片层结构的纳米填料，不仅能够发挥聚合物补强、炭层补强的作用，而且具有优异的阻隔作用，能够进一步提高炭层阻隔作用而提高阻燃效率【Progress in Polymer Science,2017,69,22；Journal of Macromolecular Science,Part B:Physics,2015,54,1282】。近年来引起了科学家们的广泛关注。
综上，阻燃剂的包覆改性和二维纳米填料的炭层补强是构建高效协效阻燃体系的两个关键切入点，通过两者的技术融合有望开发出新型高效的阻燃剂体系，为制备兼具优异阻燃、力学等性能的聚合物复合材料提供一种新思路。
发明内容
本发明的目的在于克服现有技术存在的缺点，设计提供一种二维纳米填料协效阻燃剂及其制备方法、应用，先利用植物多酚和多价金属离子的多配位络合反应分别对阻燃剂和二维纳米填料进行包覆，然后再利用该络合反应将阻燃剂负载到二维纳米填料表面，从而制备出兼具优异阻燃、力学等性能的高性能阻燃聚合物复合材料。
为了实现上述目的，本发明所述二维纳米填料协效阻燃剂的组成是：阻燃剂100质量份，二维纳米填料2～500质量份，植物多酚5～500质量份，多价金属盐1～100质量份。
本发明所述阻燃剂为卤系阻燃剂、磷系阻燃剂、膨胀型阻燃剂、硅系阻燃剂和无机阻燃剂中的一种或两种以上的混合物，其中硅系阻燃剂包括多溴二苯醚、溴代苯酚、四溴邻苯二甲酸酐、四溴邻苯二甲酸酯、四溴双酚A、溴代苯乙烯及其聚合物、十溴二苯醚、2，4，6-三溴苯酚、得克隆、氯化石蜡、氯化聚乙烯、四氯双酚A、四氯邻苯二甲酸酐、海特酸酐、六氯环戊二烯、全氯五环癸烷，磷系阻燃剂包括磷酸酯、膦酸酯、亚磷酸酯、次膦酸盐、氧化膦、鏻盐，膨胀型阻燃剂包括聚磷酸铵、三聚氰胺、硼酸三聚氰胺、聚磷酸三聚氰胺、焦磷酸三聚氰胺、氰尿酸三聚氰胺、正磷酸三聚氰胺、磷酸脲、双氰胺及其衍生物、胍及胍盐、焦磷酸铵、磷酸锌、磷腈、三嗪衍生物，硅系阻燃剂包括陶瓷前体聚合物、低熔点玻璃粉、低熔点陶瓷粉，无机阻燃剂包括三氧化二锑、五氧化二锑、锑酸钠、氢氧化镁、氢氧化铝、红磷、磷石膏、硼酸锌、硼酸、硼砂、三氧化钼、八钼酸铵、八钼酸密铵。
本发明所述二维纳米填料为层数≤20层的黏土、石墨及其衍生物、氮化硼、黑磷、片层金属化合物中的一种或两种以上的混合物。
本发明所述植物多酚为水解单宁、缩合单宁或复杂多酚中的一种或多种的混合物，或为以植物多酚为主要成份的天然产物，其中复杂多酚的分子结构中同时具有水解单宁和缩合单宁的结构特征。
本发明所述多价金属盐为含有价态≥2金属离子的金属盐。
本发明所述二维纳米填料协效阻燃剂的具体制备过程为：
(1)阻燃剂的包覆：将100质量份的阻燃剂分散在pH＝8～12的碱性水溶液中，加入2.5～250质量份的植物多酚和0.25～25质量份的多价金属盐后搅拌反应1～30min，水洗至中性得到包覆后的阻燃剂；
(2)二维纳米填料的包覆：将2～500质量份的二维纳米填料分散在2.5～250质量份的植物多酚水溶液中，加入0.25～25质量份的多价金属盐后，调整pH＝8～12，搅拌反应1～30min，水洗至中性得到包覆后的二维纳米填料；
(3)协效阻燃剂的制备：以500～2500质量份水为介质，将包覆后的阻燃剂和二维纳米填料混合均匀，加入0.5～50质量份的多价金属盐后，调整pH＝8～12，搅拌反应1～30min，水洗至中性，制备得到二位纳米填料协效阻燃剂。
本发明制备的二维纳米填料协效阻燃剂用于制备兼具优异阻燃、力学等性能的高性能阻燃聚合物复合材料。
本发明与现有技术相比，解决了传统阻燃剂在聚合物基体中分散性差、阻燃效率低的问题，其原料配比科学合理，制备工艺简单，操作方便，成本低，制备的协效阻燃剂分散性好，阻燃效率高，将其通过溶液共混、乳液共混或熔融共混的方法添加到聚合物基体中，能够制备出兼具优异阻燃和力学等性能的高性能阻燃聚合物复合材料，应用广泛。
附图说明：
图1为本发明实施例1中聚磷酸铵(A)和包覆聚磷酸铵(B)的光学照片。
图2为本发明实施例1中聚磷酸铵(A)、水浸泡7天的聚磷酸铵(B)、包覆聚磷酸铵(C)和水浸泡7天的包覆聚磷酸铵(D)的透射电镜照片。
图3为本发明实施例1制备的聚磷酸铵-氧化石墨烯协效阻燃剂的透射电镜照片。
图4为本发明实施例1制备的天然橡胶复合材料的扫描电镜照片，其中A为天然橡胶/协效阻燃剂复合材料，B为对照组。
图5为本发明实施例2制备的红磷-黏土协效阻燃剂的透射电镜照片。
具体实施方式：
下面通过实施例并结合附图对本发明做进一步详细说明。
实施例1：
本实施例所述二维纳米填料协效阻燃剂的组成是聚磷酸铵(膨胀型阻燃剂，山东昶盛，CS FR APP 232)100质量份、氧化石墨烯(1～5层，先锋纳米，XF224)10质量份、单宁酸(水解单宁，国药)20质量份、三氯化铁(国药)10质量份，该协效阻燃剂采用如下步骤制备：
(1)将100质量份的聚磷酸铵分散在pH＝10的碱性水溶液中，加入10质量份的单宁酸和2.5质量份的三氯化铁后搅拌反应10min，水洗至中性，得到包覆后的聚磷酸铵，图1为包覆前后聚磷酸铵的颜色对比，包覆后聚磷酸铵的颜色由白色变成深棕色，直观地证明包覆反应成功进行；图2是聚磷酸铵和包覆聚磷酸铵浸泡7天前后的透射电镜照片，通过对比发现，纯聚磷酸铵浸泡7天后有明显的溶胀变形和溶并现象，而包覆后的聚磷酸铵浸泡7天后仍然是规则的球形，其耐水性明显提高；
(2)将10质量份的氧化石墨烯分散在10质量份单宁酸的水溶液中，加入2.5质量份的三氯化铁后，调整pH＝10，搅拌反应10min，水洗至中性，得到包覆后氧化石墨烯；
(3)以500质量份水为介质，将包覆后的聚磷酸铵和氧化石墨烯混合均匀，加入5质量份的三氯化铁后，调整pH＝10，搅拌反应10min，水洗至中性，制备得到聚磷酸铵-氧化石墨烯协效阻燃剂，其透射电镜照片如图3所示，从图中可以看出，聚磷酸铵均匀负载在氧化石墨烯表面。
本实施例将制备的聚磷酸铵-氧化石墨烯协效阻燃剂与天然胶乳(天然橡胶含量60wt％，海胶集团，166.7质量份)混合均匀，加5质量份氯化钠破乳、水洗、干燥后，在开炼机上混入其它橡胶助剂，最后硫化成型得到天然橡胶/协效阻燃剂复合材料，并测试复合材料的阻燃性能和力学性能；制备的天然橡胶/协效阻燃剂复合材料的组成是：天然橡胶100质量份，协效阻燃剂30质量份，炭黑35质量份，氧化锌5质量份，硬脂酸4质量份，硫磺2质量份，促进剂CZ 0.8质量份，促进剂TMTD 0.35质量份，防老剂4010 1质量份，液体石蜡1质量份；对照组用30质量份聚磷酸铵取代协效阻燃剂，制备工艺相同，从表1天然橡胶/协效阻燃剂复合材料和对照组的性能对比发现，协效阻燃剂能够明显提高天然橡胶的阻燃和力学性能；图4为天然橡胶/协效阻燃剂复合材料的扫描电镜照片，与对照组相比(图4A)，协效阻燃剂在天然橡胶中的分散更加均匀，无明显团聚现象(图4B)。
表1：天然橡胶/协效阻燃剂复合材料和对照组的性能对比
实施例2：
本实施例所述二维纳米填料协效阻燃剂的组成是红磷(无机阻燃剂，川磷化工)100质量份、有机黏土(1～10层，NANOCOR，I.31PS)100质量份、茶单宁(缩合单宁，丰泰生物)100质量份、硫酸钴(阿拉丁)50质量份，该协效阻燃剂采用如下步骤制备：
(1)将100质量份的红磷分散在pH＝8的碱性水溶液中，加入50质量份的茶单宁和12.5质量份的硫酸钴后搅拌反应30min，水洗至中性，得到包覆后的红磷；
(2)将100质量份的有机黏土分散在50质量份茶单宁的水溶液中，加入12.5质量份的硫酸钴后，调整pH＝8，搅拌反应30min，水洗至中性，得到包覆后的有机黏土；
(3)以1000质量份水为介质，将包覆后的红磷和有机黏土混合均匀，加入25质量份的硫酸钴后，调整pH＝8，搅拌反应30min，水洗至中性，制备得到红磷-黏土协效阻燃剂，其透射电镜照片如图5所示，从图中可以看出，红磷均匀负载在黏土表面。
本实施例将制备的红磷-黏土协效阻燃剂加入到1000质量份浓度为10wt％，聚苯乙烯(DENKA，MF-21-301)的甲苯溶液中混合均匀，加入1000质量份甲醇沉淀、干燥后，模压成型制备得到聚苯乙烯/协效阻燃剂复合材料，并测试其阻燃性能和力学性能；聚苯乙烯/协效阻燃剂复合材料的组成是：聚苯乙烯100质量份，协效阻燃剂30质量份，对照组用30质量份红磷取代该协效阻燃剂，制备工艺相同，从表2聚苯乙烯/协效阻燃剂复合材料和对照组的性能对比发现，协效阻燃剂能够明显提高聚苯乙烯的阻燃和力学性能。
表2：聚苯乙烯/协效阻燃剂复合材料和对照组的性能对比
实施例3：
本实施例所述二维纳米填料协效阻燃剂的组成是十溴二苯醚(卤系阻燃剂，郑州智逸)100质量份、黑磷纳米片(1～10层，先锋纳米，XF207)2质量份、狭叶栎单宁(复杂多酚，青岛泰联)5质量份、氯化锆(阿拉丁)1质量份，该协效阻燃剂采用如下步骤制备：
(1)将100质量份的十溴二苯醚分散在pH＝12的碱性水溶液中，加入2.5质量份的狭叶栎单宁和0.25质量份的氯化锆后搅拌反应1min，水洗至中性，得到包覆后的十溴二苯醚；
(2)将2质量份的黑磷纳米片分散在2.5质量份狭叶栎单宁的水溶液中，加入0.25质量份的氯化锆后，调整pH＝12，搅拌反应1min，水洗至中性，得到包覆后的黑磷纳米片；
(3)以500质量份水为介质，将包覆后的十溴二苯醚和黑磷纳米片混合均匀，加入0.5质量份的氯化锆后，调整pH＝12，搅拌反应1min，水洗至中性，制备得到协效阻燃剂。
本实施例利用哈克流变仪将制备的协效阻燃剂与低密度聚乙烯(燕山石化，112A)熔融共混，模压成型得到低密度聚乙烯/协效阻燃剂复合材料，并测试低密度聚乙烯/协效阻燃剂复合材料的阻燃性能和力学性能，低密度聚乙烯/协效阻燃剂复合材料的组成是：低密度聚乙烯100质量份，协效阻燃剂20质量份；对照组用20质量份十溴二苯醚取代该协效阻燃剂，制备工艺相同，从表3低密度聚乙烯/协效阻燃剂复合材料和对照组的性能对比发现，协效阻燃剂能够明显提高低密度聚乙烯的阻燃和力学性能。
表3：低密度聚乙烯/协效阻燃剂复合材料和对照组的性能对比
实施例4：
本实施例所述二维纳米填料协效阻燃剂的组成是磷酸三(β-氯乙基)酯(磷系阻燃剂，雅瑞化工)100质量份、氮化硼(1～20层，天元化研所)500质量份、橡椀栲胶(植物多酚为主要成份，百色栲胶厂)500质量份、氯化钼(阿拉丁)100质量份，该协效阻燃剂采用如下步骤制备：
(1)将100质量份的磷酸三(β-氯乙基)酯分散在pH＝9的碱性水溶液中，加入250质量份的橡椀栲胶和25质量份的氯化钼后搅拌反应5min，水洗至中性，得到包覆后的磷酸三(β-氯乙基)酯；
(2)将500质量份的氮化硼分散在250质量份橡椀栲胶的水溶液中，加入25质量份的氯化钼后，调整pH＝9，搅拌反应5min，水洗至中性，得到包覆后的氮化硼；
(3)以2500质量份水为介质，将包覆后的磷酸三(β-氯乙基)酯和氮化硼混合均匀，加入50质量份的氯化钼后，调整pH＝9，搅拌反应5min，水洗至中性，制备得到协效阻燃剂；
本实施例将制备的协效阻燃剂加入到环氧树脂(Struers，Epofix)的丙酮溶液(50wt％)中混合均匀，浇筑到模具中，抽真空除气泡和溶剂后，固化成型得到环氧树脂/协效阻燃剂复合材料，并测试其阻燃性能和力学性能；环氧树脂/协效阻燃剂复合材料的组成是：环氧树脂100质量份，协效阻燃剂20质量份；对照组用20质量份磷酸三(β-氯乙基)酯取代该协效阻燃剂，制备工艺相同，从表4环氧树脂/协效阻燃剂复合材料和对照组的性能对比发现，协效阻燃剂能够明显提高环氧树脂的阻燃和力学性能。
表4：环氧树脂/协效阻燃剂复合材料和对照组的性能对比
实施例5：
本实施例所述二维纳米填料协效阻燃剂的组成是四溴双酚A(卤系阻燃剂，振日化工)50质量份、低熔点玻璃粉(硅系阻燃剂，安米微纳)50质量份、二硫化钼(1～10层，先锋纳米，XF209)50质量份、落叶松树皮栲胶(植物多酚为主要成份，百色栲胶厂)80质量份、氯化锑(阿拉丁)40质量份，该协效阻燃剂采用如下步骤制备：
(1)将50质量份的四溴双酚A和50质量份的低熔点玻璃粉分散在pH＝10的碱性水溶液中，加入40质量份的落叶松树皮栲胶和10质量份的氯化锑后搅拌反应5min，水洗至中性，得到包覆后的四溴双酚A、低熔点玻璃粉；
(2)将50质量份的二硫化钼分散在40质量份落叶松树皮栲胶的水溶液中，加入10质量份的氯化锑后，调整pH＝10，搅拌反应5min，水洗至中性，得到包覆后的二硫化钼；
(3)以1000质量份水为介质，将包覆后的四溴双酚A、低熔点玻璃粉、二硫化钼混合均匀，加入20质量份的氯化锑后，调整pH＝10，搅拌反应5min，水洗至中性制备得到协效阻燃剂。
本实施例将制备的协效阻燃剂与丁苯胶乳(丁苯橡胶含量52wt％，上海强盛，SQS-5601，192.3质量份)混合均匀，加5质量份氯化钠破乳、水洗、干燥后，在开炼机上混入其它橡胶助剂，最后硫化成型得到丁苯橡胶/协效阻燃剂复合材料，测试复合材料的阻燃性能和力学性能；丁苯橡胶/协效阻燃剂复合材料的组成是：丁苯橡胶100质量份，协效阻燃剂30质量份，白炭黑40质量份，氧化锌5质量份，硬脂酸2质量份，硫磺2.8质量份，促进剂NOBS 1.5质量份，防老剂4010NA 1质量份；对照组用15质量份四溴双酚A和15质量份低熔点玻璃粉取代协效阻燃剂，制备工艺相同，从表5丁苯橡胶/协效阻燃剂复合材料和对照组的性能对比发现，协效阻燃剂能够明显提高丁苯橡胶的阻燃和力学性能。
表5丁苯橡胶/协效阻燃剂复合材料和对照组的性能对比
Claims (7)
1.一种二维纳米填料协效阻燃剂，其特征在于其组成是：阻燃剂100质量份，二维纳米填料2～500质量份，植物多酚5～500质量份，多价金属盐1～100质量份。
2.根据权利要求1所述二维纳米填料协效阻燃剂，其特征在于所述阻燃剂为卤系阻燃剂、磷系阻燃剂、膨胀型阻燃剂、硅系阻燃剂和无机阻燃剂中的一种或两种以上的混合物，其中硅系阻燃剂包括多溴二苯醚、溴代苯酚、四溴邻苯二甲酸酐、四溴邻苯二甲酸酯、四溴双酚A、溴代苯乙烯及其聚合物、十溴二苯醚、2，4，6-三溴苯酚、得克隆、氯化石蜡、氯化聚乙烯、四氯双酚A、四氯邻苯二甲酸酐、海特酸酐、六氯环戊二烯、全氯五环癸烷，磷系阻燃剂包括磷酸酯、膦酸酯、亚磷酸酯、次膦酸盐、氧化膦、鏻盐，膨胀型阻燃剂包括聚磷酸铵、三聚氰胺、硼酸三聚氰胺、聚磷酸三聚氰胺、焦磷酸三聚氰胺、氰尿酸三聚氰胺、正磷酸三聚氰胺、磷酸脲、双氰胺及其衍生物、胍及胍盐、焦磷酸铵、磷酸锌、磷腈、三嗪衍生物，硅系阻燃剂包括陶瓷前体聚合物、低熔点玻璃粉、低熔点陶瓷粉，无机阻燃剂包括三氧化二锑、五氧化二锑、锑酸钠、氢氧化镁、氢氧化铝、红磷、磷石膏、硼酸锌、硼酸、硼砂、三氧化钼、八钼酸铵、八钼酸密铵。
3.根据权利要求2所述二维纳米填料协效阻燃剂，其特征在于所述二维纳米填料协效阻燃剂，其特征在于所述二维纳米填料为层数≤20层的黏土、石墨及其衍生物、氮化硼、黑磷、片层金属化合物中的一种或两种以上的混合物。
4.根据权利要求3所述二维纳米填料协效阻燃剂，其特征在于所述植物多酚为水解单宁、缩合单宁或复杂多酚中的一种或多种的混合物，或为以植物多酚为主要成份的天然产物，其中复杂多酚的分子结构中同时具有水解单宁和缩合单宁的结构特征。
5.根据权利要求4所述二维纳米填料协效阻燃剂，其特征在于所述多价金属盐为含有价态≥2金属离子的金属盐。
6.一种如权利要求5所述二维纳米填料协效阻燃剂的制备方法，其特征在于具体制备过程为：
(1)阻燃剂的包覆：将100质量份的阻燃剂分散在pH＝8～12的碱性水溶液中，加入2.5～250质量份的植物多酚和0.25～25质量份的多价金属盐后搅拌反应1～30min，水洗至中性得到包覆后的阻燃剂；
(2)二维纳米填料的包覆：将2～500质量份的二维纳米填料分散在2.5～250质量份的植物多酚水溶液中，加入0.25～25质量份的多价金属盐后，调整pH＝8～12，搅拌反应1～30min，水洗至中性得到包覆后的二维纳米填料；
(3)协效阻燃剂的制备：以500～2500质量份水为介质，将包覆后的阻燃剂和二维纳米填料混合均匀，加入0.5～50质量份的多价金属盐后，调整pH＝8～12，搅拌反应1～30min，水洗至中性，制备得到二位纳米填料协效阻燃剂。
7.一种权利要求6制备的二维纳米填料协效阻燃剂的应用，其特征在于用于制备阻燃聚合物复合材料。
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| CN110194851A (zh) * | 2019-04-18 | 2019-09-03 | 昆明理工大学 | 一种复合磷烯阻燃剂、阻燃高分子复合材料及其制备方法 |
| CN110194851B (zh) * | 2019-04-18 | 2021-09-03 | 昆明理工大学 | 一种复合磷烯阻燃剂、阻燃高分子复合材料及其制备方法 |
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| CN110240739A (zh) * | 2019-06-21 | 2019-09-17 | 青岛科技大学 | 一种反应诱导三维填料网络构筑技术制备轻质高性能聚合物复合材料的方法 |
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| CN111363289A (zh) * | 2020-04-13 | 2020-07-03 | 汕头市华麟塑化有限公司 | 一种聚苯乙烯复合材料及其制备方法 |
| KR20220097729A (ko) * | 2020-12-31 | 2022-07-08 | 양세욱 | 나노 세라믹 입자가 포함된 난연제 조성물 및 그 제조방법 |
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