CN112745549B - 一种无卤膨胀型的陶瓷化聚烯烃组合物及其制备方法和应用 - Google Patents
一种无卤膨胀型的陶瓷化聚烯烃组合物及其制备方法和应用 Download PDFInfo
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- CN112745549B CN112745549B CN202011482695.3A CN202011482695A CN112745549B CN 112745549 B CN112745549 B CN 112745549B CN 202011482695 A CN202011482695 A CN 202011482695A CN 112745549 B CN112745549 B CN 112745549B
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Abstract
本发明公开了一种无卤膨胀型的陶瓷化聚烯烃组合物及其制备方法和应用。该无卤膨胀型的陶瓷化聚烯烃组合物，包括如下组分：聚烯烃树脂，成瓷填料，磷氮类阻燃剂，成炭剂，发泡剂，微米助溶剂，纳米助溶剂，其他助剂；所述发泡剂为碳酸钠、碳酸镁或碳酸钾中的一种或几种；所述纳米助溶剂为海泡石、蒙脱土、改性蒙脱土中的一种或几种；所述微米助溶剂为低熔点玻璃粉和/或硼酸锌。本发明通过微米助溶剂、纳米助溶剂和发泡剂的复配协效作用，制得了一种无卤膨胀型的陶瓷化聚烯烃组合物。该陶瓷化聚烯烃组合物能够在较低温度下迅速陶瓷化，且陶瓷化聚烯烃组合物经烧结成瓷后，膨胀率高、强度大，陶瓷层坚固且隔热性能优异。
Description
技术领域
本发明涉及高分子材料领域，更具体的，涉及一种种无卤膨胀型的陶瓷化聚烯烃材料及其制备方法和应用。
背景技术
可瓷化高分子复合材料作为一种新型的阻燃防火材料，在被动防火领域已获广泛应用，有望取代传统的防火材料。这种材料在火焰烧蚀条件下，低烟、无毒、无熔融滴落,可转变为坚硬的陶瓷体，保持原有的形状和尺寸不改变。结构完整的自支撑陶瓷体能有效的阻碍物质对流和热量传输，抑制材料内部物质挥发损耗的同时，阻隔外界热量向材料内部扩散，阻隔火焰的蔓延。加强可瓷化高分子复合材料的应用研究对推动防火材料的发展，提高技术水平有积极作用。
陶瓷化聚烯烃材料主要集中在EVA、PE以及其共聚物中，应用领域大多为防火线缆，而随着人们对材料防火性能的逐渐重视，对常用电子电器壳体材料的阻燃性能要求越来越高，尤其是对于电器设备的易燃的电控盒等高风险部件。此外，随着行业对绿色电子的要求越来越高，最新颁布的RoHS法令中，已明确十八种必须排除的有害物质，其中第一类群组即为溴系阻燃剂，包括六环溴十二烷与印刷电路板中最常用的四溴丙二酚等。自此，许多国际大公司如ASUS、Dell、HP、Apple等均声明开始导入无卤材料。
传统陶瓷化聚烯烃材料存在陶瓷化速率慢、陶瓷化温度高，并且形成的陶瓷层隔热效果不佳等一系列问题。并且传统的陶瓷化聚烯烃通常应用在绝缘性电缆料中。中国专利申请CN 110818995 A公开了一种成瓷性低烟无卤材料，制备原料包括乙烯-醋酸乙烯共聚物、聚乙烯、马来酸酐接枝物、成瓷剂、成瓷助剂，该成瓷性低烟无卤材料在800℃以上条件下能烧结成瓷，陶瓷化温度高、速率慢。
因此，需要开发出一种能够在较低温度下快速陶瓷化的聚烯烃组合物。
发明内容
本发明为克服上述现有技术所述的陶瓷化温度高、速率慢的缺陷，提供一种无卤膨胀型的陶瓷化聚烯烃组合物，该陶瓷化聚烯烃组合物能够在较低温度下快速陶瓷化。
本发明的另一目的在于提供上述无卤膨胀型的陶瓷化聚烯烃组合物的制备方法。
本发明的另一目的在于提供上述无卤膨胀型的陶瓷化聚烯烃组合物的应用。
为解决上述技术问题，本发明采用的技术方案是：
一种无卤膨胀型的陶瓷化聚烯烃组合物，包括如下重量份的组分：
聚烯烃树脂30～40份，
成瓷填料20～30份，
磷氮类阻燃剂20～30份，
成炭剂3～5份，
发泡剂1～3份，
微米助溶剂1～5份，
纳米助溶剂1～5份，
其他助剂0～2份；
所述发泡剂为碳酸钠、碳酸镁或碳酸钾中的一种或几种；
所述纳米助溶剂为海泡石、蒙脱土、改性蒙脱土中的一种或几种；
所述微米助溶剂为低熔点玻璃粉和/或硼酸锌。
本发明的陶瓷化聚烯烃组合物采用微米助溶+纳米助溶体系，所述微米助溶剂能在300～400℃的条件下迅速转变为液态，从而降低成瓷填料的烧结温度。但若仅有微米助溶剂则存在经烧结后陶瓷体强度不足的问题。通过引入所述纳米助溶剂，纳米助溶剂能够在烧结过程中充分富集于成瓷填料片层结构的周边，在烧结中作为桥梁作用使得成瓷填料的边缘迅速熔化并互相粘结成自支撑体结构。
磷氮类阻燃剂在受热时经分解释放出大量无毒且能抑制火焰蔓延的气体，同时发生膨胀形成海绵状泡沫结构的化合物，并在成炭剂的作用下形成多孔膨胀炭层。多孔炭层结构被固定在成瓷填料形成的陶瓷层中，形成多孔的陶瓷层，从而能够隔绝火焰的蔓延，并具有良好的隔热性能。
所述发泡剂为碳酸钠、碳酸镁或碳酸钾中的一种或几种，发泡剂在燃烧过程中经分解产生金属氧化物(氧化钠、氧化镁或氧化钾)和二氧化碳气体。发泡剂分解产生金属氧化物一方面可以起到一定程度的助溶作用，进一步改善聚烯烃组合物的成瓷效果，另一方面可提供游离氧，使得硅酸盐结构中O/Si的比例增加，起到断链的作用，降低高温下陶瓷的黏度，使得陶瓷更易熔化粘结；二氧化碳气体为多孔的陶瓷层制造更多的微孔结构，以达到更优的隔热效果。
而其他种类的碳酸金属盐，一方面分解温度过高，无法在燃烧过程中迅速产生二氧化碳气体，另一方面，分解产生的金属氧化物无法起到助溶作用。
发明人研究发现，通过特定种类的微米助溶剂、纳米助溶剂和发泡剂的复配协效作用，结合磷氮类阻燃剂、成炭剂和成瓷填料，能够大大降低聚烯烃组合物的陶瓷化温度、提高陶瓷化速率。并且，所述陶瓷化聚烯烃组合物经烧结成瓷后，膨胀率高、强度大，陶瓷层坚固且隔热性能优异。
优选地，所述发泡剂的平均粒径为10～100μm。
所述改性蒙脱土的制备方法为：在搅拌釜中将表面改性剂和蒙脱土原粉反应1～2h后，经过过滤后得到所述改性蒙脱土。
优选地，所述表面改性剂为硅烷偶联剂或硬脂酸盐。
所述纳米助溶剂的平均粒径为50nm～1500nm；所述微米助溶剂的平均粒径为5μm～300μm。
平均粒径较低的纳米助溶剂更能充分富集于成瓷填料片层结构的周边，使得成瓷填料的边缘熔化更迅速。
所述低熔点玻璃粉的熔点为360～650℃。
优选地，所述低熔点玻璃粉优选为氧化铅玻璃粉、硅酸盐类玻璃粉、磷酸盐玻璃粉或硼酸盐玻璃粉。
优选地，所述微米助溶剂为低熔点玻璃粉。
优选地，所述纳米助溶剂为海泡石。
优选地，所述聚烯烃树脂优选为聚乙烯、聚丙烯、乙烯-醋酸乙酯烯酯共聚物、乙烯-辛烯共聚物中的一种或几种。
所述磷氮类阻燃剂可以是聚烯烃中常用的磷氮类阻燃剂。
优选地，所述磷氮类阻燃剂优选为聚磷酸铵、改性聚磷酸铵、次磷酸铵、磷酸三苯酯、三聚氰胺聚磷酸盐、三聚氰胺磷酸盐、三聚氰胺焦磷酸盐、三聚氰胺氰尿酸盐、三聚氰胺次磷酸盐、三聚氰胺焦磷酸盐和焦磷酸哌嗪的复合物、聚磷酸哌嗪、次磷酸哌嗪中的一种或几种。
所述成炭剂可以是陶瓷化聚烯烃中常用的成炭剂。
优选地，所述成炭剂优选为酚醛树脂、聚酰胺、山梨醇、丁四醇、环己六醇、葡萄糖、麦芽糖、阿拉伯糖、间苯二酚、淀粉、季戊四醇中的一种或几种。
优选地，所述成瓷填料为高岭土、水镁石、滑石粉、云母中的一种或几种。
高岭土、水镁石、滑石粉、云母具有片层结构，使得烧结过程中纳米助溶剂能够充分富集于成瓷填料片层结构的周边。
可选的，所述成瓷填料还包括玻璃纤维和/或二氧化硅。
发明人研究发现，当成瓷填料还包括玻璃纤维或二氧化硅时，陶瓷化聚烯烃组合物成瓷后具有更优异的弯曲强度。
优选地，所述其他助剂为抗氧剂和/或加工助剂。
更优选地，所述抗氧剂优选为酚类抗氧剂、亚磷酸酯类抗氧剂、二价硫类抗氧剂或受阻胺类抗氧剂中的一种或几种。
可选地，所述酚类抗氧剂为抗氧剂264、抗氧剂1010、抗氧剂1076、防老剂SP、抗氧剂2246、抗氧剂CA、抗氧剂330、Irganox1890、抗氧剂3114；所述亚磷酸酯类抗氧剂为抗氧剂TNP、抗氧剂ODP、抗氧剂168、Irganox1093或Irganox1222；所述二价硫类抗氧剂为二月桂酸硫代二丙酸酯(DLTP)、二硬脂酸硫代二丙酸酯(DSTP)；所述受阻胺类抗氧剂为LS-744、LS-770、GW-540或Flamstab NOR116。
优选地，所述加工助剂优选为低分子脂类、金属皂类、硬脂酸复合酯类或酰胺类中的一种或几种。
可选地，所述低分子脂类为固体石蜡、液体石蜡或低分子聚烯烃蜡；所述金属皂类为硬脂酸钙、硬脂酸镁、硬脂酸锌或硬脂酸钡；所述硬脂酸复合酯类为硬脂酸乙二醇酯、硬脂酸甘油酯或硬脂酸季戊四醇酯；所述酰胺类为芥酸酰胺、甲撑双硬脂酸酰胺或N，N-乙撑双硬脂酸酰胺。
本发明还保护上述无卤膨胀型的陶瓷化聚烯烃组合物的制备方法，包括如下步骤：
将聚烯烃树脂、成瓷填料、磷氮类阻燃剂、成炭剂、发泡剂、微米助溶剂、纳米助溶剂和其他助剂混合后加入挤出机，经熔融挤出造粒，得到无卤膨胀型的陶瓷化聚烯烃组合物。
优选地，所述挤出机为双螺杆挤出机，螺杆温度为180～200℃。
本发明还保护上述无卤膨胀型的陶瓷化聚烯烃组合物在制备电线电缆或电子电器壳体中的应用。
与现有技术相比，本发明的有益效果是：
本发明通过特定种类的微米助溶剂、纳米助溶剂和发泡剂的复配协效作用，结合磷氮类阻燃剂、成炭剂和成瓷填料，制得了一种无卤膨胀型的陶瓷化聚烯烃组合物。该陶瓷化聚烯烃组合物能够在较低温度下迅速陶瓷化，且陶瓷化聚烯烃组合物经烧结成瓷后，膨胀率高、强度大，陶瓷层坚固且隔热性能优异。
具体实施方式
下面结合具体实施方式对本发明作进一步的说明。
实施例及对比例中的原料均可通过市售得到；
除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
实施例1～19
实施例1～19提供一种陶瓷化聚烯烃组合物，陶瓷化聚烯烃组合物各组分的含量如表1所示。
表1实施例1～19中各组分含量(重量份)
实施例1～19的陶瓷化聚烯烃组合物的制备方法均为：
将聚烯烃树脂、成瓷填料、磷氮类阻燃剂、成炭剂、发泡剂、微米助溶剂、纳米助溶剂和其他助剂混合后加入挤出机，经熔融挤出造粒，得到无卤膨胀型的陶瓷化聚烯烃组合物。
其中挤出机为双螺杆挤出机，螺杆温度为180～200℃。
对比例1～7
对比例1～7提供一种陶瓷化聚烯烃组合物，陶瓷化聚烯烃组合物各组分的含量如表2所示。
表2对比例1～7中各组分含量(重量份)
性能测试
对上述实施例及对比例制备的陶瓷化聚烯烃组合物进行性能测试。
检测方法具体如下：
燃烧后样条形貌：按照UL94-2016标准，进行垂直燃烧测试，测试样条厚度为1.6mm；
受火面背火面温度差：采用甲烷气作为燃料的本色灯，调整火焰高度为125mm，内焰高度为40mm，对3.0mm厚度样品进行施焰，受火面温度为火焰温度，背火面温度采用非接触式红外测温仪进行测量，受火面背火面温度差＝受火面温度-背火面温度，单位为℃；
弯曲强度：根据GB/T 6569-2006《精细陶瓷弯曲强度测试》，检测陶瓷化聚烯烃组合物成瓷后的弯曲强度，单位为MPa；
膨胀率：将样品放在氧化铝坩埚中，将坩埚至于800℃马弗炉中，烧蚀样品，测定烧结后样品体积与烧结前样品体系的百分比，单位为％；
成瓷速率：采用锥形量热分析按照ASTM E-1354-2002进行测试，热辐射功率为50Kw/m2，样板厚度为2.0mm，面积为100mm*100mm，水平放置，成瓷速率采用测试过程中样品质量下降速率MLS<0.05g/s所对应的测试时间，单位为s。
实施例1～19的测试结果见表3，对比例1～7的测试结果见表4。
表3实施例1～19的性能测试结果
根据表3的测试结果，本发明各实施例的陶瓷化聚烯烃组合物经过烧结，均形成了隔热性良好、膨胀率高、弯曲强度高的陶瓷层，且成瓷速率快。
由实施例1、3～5，成瓷填料为滑石粉时，陶瓷层的隔热性能更优，受火面背火面温度差达到520℃，且陶瓷层的膨胀率更高、弯曲强度更大，成瓷速率越快。
由实施例1、实施例6～7，碳酸钠作为发泡剂，陶瓷化聚烯烃组合物成瓷后的隔热性、成瓷速率、膨胀率综合效果最优，碳酸钾作为发泡剂的陶瓷体强度稍低，碳酸镁作为发泡剂的成瓷速率稍慢。
由实施例1、实施例8～10，海泡石作为纳米助溶剂、低熔点玻璃粉作为微米助溶剂，制得的陶瓷化聚烯烃组合物，在燃烧后陶瓷体的弯曲强度更优。由实施例16～18，当纳米助溶剂、微米助溶剂或发泡剂添加量较少时，陶瓷化聚烯烃组合物经燃烧样条形貌完好，会出现微裂纹，隔热性稍差，但仍能满足实际的陶瓷体自支撑性及隔热需求。
表4对比例1～7的性能测试结果
根据表4的测试结果，对比例1中未添加发泡剂、对比例2中未添加纳米助溶剂、对比例3中未添加微米助溶剂，制得的陶瓷化聚烯烃组合物成瓷速率较慢，燃烧后膨胀率非常低，分别仅为22％、15％、25％，从而影响了陶瓷化聚烯烃组合物成瓷后的隔热性，且对比例3的陶瓷化聚烯烃组合物样条燃烧后还出现了裂纹。对比例4中成瓷填料添加量过多，样条燃烧后有裂纹且不完整，弯曲强度较低。对比例5～7分别为发泡剂、纳米助溶剂、微米助溶剂添加量过多，陶瓷化聚烯烃组合物燃烧后陶瓷体均有裂纹。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明权利要求的保护范围之内。
Claims (9)
1.一种无卤膨胀型的陶瓷化聚烯烃组合物，其特征在于，包括如下重量份的组分：
聚烯烃树脂30～40份，成瓷填料20～30份，磷氮类阻燃剂20～30份，成炭剂3～5份，发泡剂1～3份，微米助熔剂1～5份，纳米助熔剂1～5份，其他助剂0～2份；
所述发泡剂为碳酸钠、碳酸镁或碳酸钾中的一种或几种；
所述纳米助熔剂为海泡石、蒙脱土、改性蒙脱土中的一种或几种；
所述微米助熔剂为低熔点玻璃粉和/或硼酸锌；
所述纳米助熔剂的平均粒径为50nm～1500nm；所述微米助熔剂的平均粒径为5μm～300μm。
2.根据权利要求1所述陶瓷化聚烯烃组合物，其特征在于，所述发泡剂为碳酸钠。
3.根据权利要求1所述陶瓷化聚烯烃组合物，其特征在于，所述微米助熔剂为低熔点玻璃粉。
4.根据权利要求1所述陶瓷化聚烯烃组合物，其特征在于，所述纳米助熔剂为海泡石。
5.根据权利要求1所述陶瓷化聚烯烃组合物，其特征在于，所述成瓷填料为高岭土、水镁石、滑石粉、云母中的一种或几种。
6.根据权利要求5所述陶瓷化聚烯烃组合物，其特征在于，所述成瓷填料还包括玻璃纤维和/或二氧化硅。
7.根据权利要求1所述陶瓷化聚烯烃组合物，其特征在于，所述聚烯烃树脂为聚乙烯、聚丙烯、乙烯-醋酸乙酯烯酯共聚物、乙烯-辛烯共聚物中的一种或几种。
8.权利要求1～7所述陶瓷化聚烯烃组合物的制备方法，其特征在于，包括如下步骤：
将聚烯烃树脂、成瓷填料、磷氮类阻燃剂、成炭剂、发泡剂、微米助熔剂、纳米助熔剂和其他助剂混合后加入挤出机，经熔融挤出造粒，得到无卤膨胀型的陶瓷化聚烯烃组合物。
9.权利要求1～7所述陶瓷化聚烯烃组合物在制备电线电缆或电子电器壳体中的应用。
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Effective date of registration: 20240530 Address after: 510663 Guangzhou science and Technology Development Zone, Guangdong, China, 33 Patentee after: KINGFA SCI. & TECH. Co.,Ltd. Country or region after: China Patentee after: TIANJIN KINGFA MATERIAL Co.,Ltd. Address before: 510663 No.33 Kefeng Road, Science City, high tech Industrial Development Zone, Huangpu District, Guangzhou City, Guangdong Province Patentee before: KINGFA SCI. & TECH. Co.,Ltd. Country or region before: China |