CN104479208B - Ti-PO4-PEG阻燃剂及其复合阻燃材料和制备方法 - Google Patents

Ti-PO4-PEG阻燃剂及其复合阻燃材料和制备方法 Download PDF

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CN104479208B
CN104479208B CN201410821346.8A CN201410821346A CN104479208B CN 104479208 B CN104479208 B CN 104479208B CN 201410821346 A CN201410821346 A CN 201410821346A CN 104479208 B CN104479208 B CN 104479208B
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易浩然
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Abstract

本发明属于新材料技术领域，具体涉及一种Ti‑PO4‑PEG阻燃剂及其使用该阻燃剂的复合阻燃材料和制备方法；该阻燃剂由硫酸氧钛、硝酸、聚乙二醇、磷酸和水余量制备而得；本发明不仅制备工艺简单，所制得到的聚合物复合阻燃材料的阻燃性能、力学性能较好，同时还不影响聚合物的加工性能。

Description

Ti-PO4-PEG阻燃剂及其复合阻燃材料和制备方法
技术领域
本发明属于新材料技术领域，具体涉及一种Ti-PO4-PEG阻燃剂及其使用该阻燃剂的复合阻燃材料和制备方法。
背景技术
高分子化合物也叫高分子聚合物，它与低分子化合物相比较，分子量非常高。由于这一突出特点，使之显示出了特有的性能：高分子量、高弹性、高黏度、结晶度低、无气态。这些特点也赋予了高分子材料(如复合材料、橡胶等)具有高强度、高韧性、高弹性等优异的特点。使之被广泛应用于电气电子、结构建筑、建筑技术、车辆制造等领域。虽然它们具有良好的机械性能、可加工性和化学稳定性；但它们属于有机高分子材料，具有易燃性且燃烧速度快而难以扑灭的弊端。由此带来的火灾隐患已成为普遍关注的社会问题，如何改变高分子聚合物的易燃性已经成为科学研究的重点。
目前降低聚合物易燃性所采取的方法主要是在聚合物中添加阻燃剂。当前广泛使用的阻燃剂按其组成可分为含卤和无卤阻燃体系，其中含卤阻燃剂由于燃烧时释放大量的烟尘和有毒、有腐蚀性气体，造成大气污染和妨碍救生和逃生；而无卤阻燃剂中金属氢氧化物添加量大，从而影响材料的其他性能；另外阻燃齐聚物，阻燃效果好而且低烟低毒，但是合成工艺复杂，成本高。近年来由于环保意识的提高和可持续发展理念的推广，高效、低毒、低烟、机械和力学性能良好、具有火灾安全性、综合性能优化的新型阻燃材料成为阻燃领域发展的趋势。
发明内容
为了解决上述问题，本发明的目的在于提供一种与聚合物的之间具有较好相容性的Ti-PO4-PEG阻燃剂；相容性好，能很好起到阻燃效果的同时，对所得阻燃聚合物的物化性能进行综合调整优化。
本发明的目的之二是提供了所述Ti-PO4-PEG阻燃剂的制备方法，该方法简单易行。
本发明的目的之三是提供了所述含有Ti-PO4-PEG阻燃剂的复合阻燃材料，该复合阻燃材料不仅高效、低毒、低烟，而且机械和力学性能良好。
本发明的目的之四是提供了所述复合阻燃材料的制备方法；该方法简单易行。
本发明是通过以下技术方案来实现的：
Ti-PO4-PEG阻燃剂，所述Ti-PO4-PEG阻燃剂为层状或介孔状，并由以下方法制得：
(1)、先将TiOSO4和水溶液混合，并于50℃～70℃水浴加热；接着滴加氨水溶液调pH＝4～5，将反应所得浑浊液(当pH＞2.5时即开始产生沉淀，然后)抽滤、洗涤，直到滤饼中含有痕量的杂质离子；
(2)、将所得的沉淀物分散的硝酸溶液中，加热使之解胶和晶化，从而制得无色或淡蓝色透明的TiO2溶胶；
(3)、将TiO2溶胶加入到去离子水中，再加入所述量的PEG，搅拌0.5～2h；接着慢慢地滴加磷酸，最后加入氨水调pH值，搅拌20～35min；较佳地，所述PEG与TiO2溶胶的质量比问0.4：1。
(4)、将(淡蓝色的)清液在80～100℃回流20～25h，冷却到室温；接着充分洗涤至pH≥5，放入到真空干燥箱50～70℃真空干燥，制得所述Ti-PO4-PEG阻燃剂。
层状或介孔状，能很好的提高CaxAy-PO4-1,6-己二胺阻燃剂与聚合物之间的相容性。层状的无机盐经过插层处理，层间距增大，甚至呈一定程度的剥离状态，这有助于无机骨架酸性位与高分子基体充分作用，通过催化脱水，交联成炭，使膨胀碳层形成稳定的硅酸盐-炭阻隔层，从而阻隔燃烧过程中质和热的扩 散，因而改善体系的耐热氧化能力。介孔材料发展至今，大多集中在空旷骨架材料的经典(吸附、催化等)和非经典(药物控释、响应聚合物等功能组装体)性能的研究，骨架中稳定性较差的介观相(这类结构在膜板剂(完全)脱出后骨架塌陷，以无机骨架和有机膜板剂复合形式共存，且介观有序)的应用研究有待进一步的开展，而且这类材料层状无机骨架和有机膜板剂插层共存，无需进一步的插层改性，简化工艺流程。
一种含有TI-PO4-PEG阻燃剂的复合阻燃材料，由按质量比计算的如下原料制得：树脂90～99％和Ti-PO4-PEG阻燃剂1～10％。
其中，所述树脂为LDPE、PE、PP、PS、PVC、ABS、EVA中的一种或几种组合物。
较佳地，所述树脂为LDPE和EVA，更优选所述EVA占树脂重量比的20％。
制备所述复合阻燃材料的方法，具体为：
别称取树脂和Ti-PO4-PEG混合后，先用双锟混炼机上130～150℃混炼20～30min，剪切速度为15～25r/min，接着将混合物在平板硫化机130～160℃压5～10min即得到所述含有Ti-PO4-PEG阻燃剂的复合阻燃材料。
本发明通过有机-无机介观复合相实现了有机碳源(作为膜板剂/结构导向剂)和无机层状、网状骨架的协同复合。通过简单的制备，可以获得层状或者多孔结构的MP(有机-无机磷酸盐介观自组装体系)，层状的MP在结构和电荷匹配(膜板剂和无机骨架通过氢键、共价键作用达到电荷匹配)。在MP体系中，对顶角四面体连接的[AlPO6]与MMT(蒙脱土)中对顶角四面体连接的[Si2O6]具有等瓣关系，相对于层间，无机骨架层内作用力较强，因此，在剪切条件下，剥离的片层具有一定的完整性，剥离分散在高分子基体中。
总之，本发明与现有技术相比，本发明阻燃剂不仅制备工艺简单，而且能很好的与聚合物相容，使含有该阻燃剂的复合阻燃材料阻燃高效、低毒、低烟、机械和力学性能良好，同时还不影响聚合物的加工性能。
具体的实施方式
下面结合具体实施方式对本发明作进一步的详细说明，以助于本领域技术人员理解本发明。
实施例1
Ti-PO4-PEG阻燃剂，的如下方法制得：
(1)、先将TiOSO4和水溶液混合，并于60℃水浴加热；接着滴加氨水溶液调pH＝4.5，将反应所得浑浊液(当pH＞2.5时即开始产生沉淀，然后)抽滤、洗涤，直到滤饼中含有痕量的杂质离子；
(2)、将所得的沉淀物分散的硝酸溶液中，加热使之解胶和晶化，从而制得无色或淡蓝色透明的TiO2溶胶；
(3)、将TiO2溶胶加入到去离子水中，再加入所述量的PEG，搅拌1h；接着慢慢地滴加磷酸，最后加入氨水调pH值，搅拌30min；
(4)、将(淡蓝色的)清液在90℃回流24h，冷却到室温；接着充分洗涤至pH≥5，放入到真空干燥箱60℃真空干燥，制得所述Ti-PO4-PEG阻燃剂。
一种含有TI-PO4-PEG阻燃剂的复合阻燃材料，由按质量比计算的如下原料制得：树脂(LDPE和EVA20％)95％和Ti-PO4-PEG阻燃剂5％。
制备所述复合阻燃材料的方法，具体为：
别称取树脂和Ti-PO4-PEG混合后，先用双锟混炼机上140℃混炼25min，剪切速度为20r/min，接着将混合物在平板硫化机150℃压8min即得到所述含有Ti-PO4-PEG阻燃剂的复合阻燃材料。
实施例2
Ti-PO4-PEG阻燃剂，的如下方法制得：
(1)、先将TiOSO4和水溶液混合，并于50℃水浴加热；接着滴加氨水溶液调pH＝4，将反应所得浑浊液(当pH＞2.5时即开始产生沉淀，然后)抽滤、洗涤，直到滤饼中含有痕量的杂质离子；
(2)、将所得的沉淀物分散的硝酸溶液中，加热使之解胶和晶化，从而制得无色或淡蓝色透明的TiO2溶胶；
(3)、将TiO2溶胶加入到去离子水中，再加入所述量的PEG，搅拌0.5h；接着慢慢地滴加磷酸，最后加入氨水调pH值，搅拌20min；
(4)、将(淡蓝色的)清液在80℃回流20h，冷却到室温；接着充分洗涤至pH≥5，放入到真空干燥箱50℃真空干燥，制得所述Ti-PO4-PEG阻燃剂。
一种含有TI-PO4-PEG阻燃剂的复合阻燃材料，由按质量比计算的如下原料制得：树脂(LDPE和EVA20％)90％和Ti-PO4-PEG阻燃剂10％。
制备所述复合阻燃材料的方法，具体为：
别称取树脂和Ti-PO4-PEG混合后，先用双锟混炼机上130℃混炼20min，剪切速度为15r/min，接着将混合物在平板硫化机130℃压5min即得到所述含有Ti-PO4-PEG阻燃剂的复合阻燃材料。
实施例3
Ti-PO4-PEG阻燃剂，的如下方法制得：
(1)、先将TiOSO4和水溶液混合，并于70℃水浴加热；接着滴加氨水溶液调pH＝5，将反应所得浑浊液(当pH＞2.5时即开始产生沉淀，然后)抽滤、洗涤，直到滤饼中含有痕量的杂质离子；
(2)、将所得的沉淀物分散的硝酸溶液中，加热使之解胶和晶化，从而制得无色或淡蓝色透明的TiO2溶胶；
(3)、将TiO2溶胶加入到去离子水中，再加入所述量的PEG，搅拌2h；接着慢慢地滴加磷酸，最后加入氨水调pH值，搅拌35min；
(4)、将(淡蓝色的)清液在100℃回流25h，冷却到室温；接着充分洗涤至pH≥5，放入到真空干燥箱70℃真空干燥，制得所述Ti-PO4-PEG阻燃剂。
一种含有TI-PO4-PEG阻燃剂的复合阻燃材料，由按质量比计算的如下原料制得：树脂(LDPE)92％和Ti-PO4-PEG阻燃剂8％。
制备所述复合阻燃材料的方法，具体为：
别称取树脂和Ti-PO4-PEG混合后，先用双锟混炼机上150℃混炼30min，剪切速度为25r/min，接着将混合物在平板硫化机160℃压10min即得到所述含 有Ti-PO4-PEG阻燃剂的复合阻燃材料。
实施例4
Ti-PO4-PEG阻燃剂，的如下方法制得：
(1)、先将TiOSO4和水溶液混合，并于50℃水浴加热；接着滴加氨水溶液调pH＝5，将反应所得浑浊液(当pH＞2.5时即开始产生沉淀，然后)抽滤、洗涤，直到滤饼中含有痕量的杂质离子；
(2)、将所得的沉淀物分散的硝酸溶液中，加热使之解胶和晶化，从而制得无色或淡蓝色透明的TiO2溶胶；
(3)、将TiO2溶胶加入到去离子水中，再加入所述量的PEG，搅拌2h；接着慢慢地滴加磷酸，最后加入氨水调pH值，搅拌20min；
(4)、将(淡蓝色的)清液在80℃回流25h，冷却到室温；接着充分洗涤至pH≥5，放入到真空干燥箱70℃真空干燥，制得所述Ti-PO4-PEG阻燃剂。
一种含有TI-PO4-PEG阻燃剂的复合阻燃材料，由按质量比计算的如下原料制得：树脂(EVA)94％和Ti-PO4-PEG阻燃剂6％。
制备所述复合阻燃材料的方法，具体为：
别称取树脂和Ti-PO4-PEG混合后，先用双锟混炼机上150℃混炼20min，剪切速度为25r/min，接着将混合物在平板硫化机160℃压5min即得到所述含有Ti-PO4-PEG阻燃剂的复合阻燃材料。
本发明中阻燃剂也可以采用沉淀法、溶胶-凝胶法、回流法、固相反应法等方法进行制备。
上述实施例，只是本发明的较佳实施例，并非用来限制本发明实施范围，故凡以本发明权利要求所述的特征及原理所做的等效变化或修饰，均应包括在本发明权利要求范围之内。
测试结果表明，当Ti-PO4-PEG的含量在5％时，极限氧指数(LOI)最高，阻燃性能最好。

Claims (8)

1.Ti-PO4-PEG阻燃剂，其特征在于，所述Ti-PO4-PEG阻燃剂为层状或介孔状，并由以下方法制得：
(1)、先将TiOSO4和水溶液混合，并于50℃～70℃水浴加热；接着滴加氨水溶液调pH＝4～5，将反应所得浑浊液抽滤、洗涤，直到滤饼中含有痕量的杂质离子；
(2)、将所得的沉淀物分散的硝酸溶液中，加热使之解胶和晶化，从而制得无色或淡蓝色透明的TiO2溶胶；
(3)、将TiO2溶胶加入到去离子水中，再加入PEG，搅拌0.5～2h；接着慢慢地滴加磷酸，最后加入氨水调pH值，搅拌20～35min；
(4)、将清液在80～100℃回流20～25h，冷却到室温；接着充分洗涤至pH≥5，放入到真空干燥箱50～70℃真空干燥，制得所述Ti-PO4-PEG阻燃剂。
2.如权利要求1中所述制备TI-PO4-PEG阻燃剂的方法，其特征在于：所述PEG与TiO2溶胶的质量比为0.4︰1。
3.如权利要求1中所述制备TI-PO4-PEG阻燃剂的方法，其特征在于：步骤(2)中所述加热使之解胶和晶化的加热温度为70℃。
4.一种含有TI-PO4-PEG阻燃剂的复合阻燃材料，其特征在于，由按质量比计算的如下原料制得：树脂90～99％和Ti-PO4-PEG阻燃剂1～10％；所述Ti-PO4-PEG阻燃剂为权利要求1中所述的Ti-PO4-PEG阻燃剂。
5.如权利要求4所述复合阻燃材料，其特征在于，所述树脂为PE、PP、PS、PVC、ABS、EVA中的一种或几种组合物。
6.如权利要求5所述复合阻燃材料，其特征在于，所述树脂为LDPE和EVA。
7.如权利要求6所述复合阻燃材料，其特征在于，所述树脂为LDPE和EVA，所述EVA占树脂重量比的20％。
8.制备权利要求4－7中任意一项所述复合阻燃材料的方法，其特征在于，具体为：
分别称取树脂和Ti-PO4-PEG混合后，先用双锟混炼机上130～150℃混炼20～30min，剪切速度为15～25r/min，接着将混合物在平板硫化机130～160℃压5～10min即得到所述含有Ti-PO4-PEG阻燃剂的复合阻燃材料。
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