CN107286365A - 一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法 - Google Patents
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Abstract
本发明公开了一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,首先通过利用苄基三苯基氯化膦对蒙脱土进行有机改性,其次,利用偶氮二甲酰胺对改性后的蒙脱土进行插层,通过一系列的工艺条件控制,实现了偶氮二甲酰胺在蒙脱土层板之间的均匀分散,最后配合适量氧化锌与碳酸氢钠的添加,进一步降低了发泡剂的分解温度,添加到聚氯乙烯中,能够避免聚氯乙烯产生糊料的现象。本发明工艺生产的产品合成工艺便于工业控制,降低了生产成本,发泡温度适中,非常适合用于聚氯乙烯的发泡工艺,在发泡过程中不分解,不糊料,用此发泡剂形成的发泡材料质量稳定,泡孔细密均匀,保温效果优异,且具有一定的阻燃效果。
Description
技术领域
本发明涉及发泡聚氯乙烯技术领域,尤其涉及一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法。
背景技术
近年来,国内外泡沫塑料行业的发张迅速,其应用范围也越来越广泛,特别是在包装、建筑、运输、电缆材料等行业,泡沫塑料已经成为了不可替代的材料。聚氯乙烯发泡材料具有优越的韧性和保温性能,同时材料成本低,阻燃性能优异,在泡沫塑料领域中具有不可替代的地位。聚氯乙烯发泡工艺一般采用化学发泡,其中大部分采用偶氮二甲酰胺,俗称AC发泡剂,或者OBSH发泡剂( 4,4-氧代双苯磺酰肼。但是两种发泡剂均存在两种问题:(1)分解温度较高,AC分解温度在190-220℃ 之间,OBSH分解温度在 150-160℃ 范围内。在使用AC、OBSH 作为发泡剂加入基体材料中进行发泡时,会出现分解温度过高与聚氯乙烯软化温度不吻合、发泡材料容易老化、变黄等问题;(2)容易吸收空气中的水分出现团聚现象,使得发泡材料出现局部发泡剂含量过高、集中发泡、泡孔破裂、并泡等现象。聚氯乙烯材料受热非常容易分解,容易糊料,不稳定,固不能简单的使用这两种常用的化学发泡剂。这就需要研发一种分解温度低,且在聚氯乙烯中分散均匀的发泡剂。
发明内容
本发明目的就是为了弥补已有技术的缺陷,提供一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法。
本发明是通过以下技术方案实现的:
一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,包括以下具体步骤:
(1)将蒙脱土加入30-35倍量的去离子水中,搅拌均匀形成悬浮液,加热至70-75℃,搅拌5-6小时,再加入适量的苄基三苯基氯化膦溶液,继续恒温搅拌4-5小时后冷却至室温,将反应物抽滤,将沉淀物用去离子水清洗2-3次后再用乙醇溶液清洗1次,将洗净的改性蒙脱土在烘箱中以100-110℃烘干,研磨,过300目筛;
(2)将步骤(1)得到的改性蒙脱土分散于15-16倍量的去离子水中,加热至50-55℃,以1000-1200转/分的速度搅拌30-40分钟,调节体系pH为9待用;将偶氮二甲酰胺溶于25-28倍量二甲基亚砜中形成溶液,然后将其缓慢加入上述改性蒙脱土分散体系中,加热至55-60℃,剧烈搅拌10-12小时,反应结束后对体系进行离心,将滤饼分别用二甲基亚砜洗涤2-3次后放入真空干燥箱中,以60-70℃干燥20-24小时,得到偶氮二甲酰胺插层改性蒙脱石;
(3)将步骤(2)产物与适量的氧化锌、碳酸氢钠混合均匀即可。
一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,步骤(1)中所述的苄基三苯基氯化膦溶液是指质量浓度为10%的苄基三苯基氯化膦水溶液,且添加量为蒙脱土与苄基三苯基氯化膦的质量比为50:1。
一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,步骤(1)中所述的乙醇溶液为体积浓度为50%的乙醇溶液。
一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,步骤(2)中所述的调节体系pH使用的是1mol/L的氢氧化钠溶液。
一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,步骤(2)中所述的偶氮二甲酰胺与步骤(1)产物的质量配比为1:1。
一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,步骤(3)中所述的氧化锌与碳酸氢钠的质量比为2:1,且总添加量为步骤(2)产物质量的3-6%。
本发明的优点是:本发明首先通过利用苄基三苯基氯化膦对蒙脱土进行有机改性,不仅能够降低蒙脱土与聚合物聚氯乙烯基体之间的相容性,还提高了蒙脱土的表面以及层间结合位点,便于后续步骤的进行;其次,利用偶氮二甲酰胺对改性后的蒙脱土进行插层,通过一系列的工艺条件控制,实现了偶氮二甲酰胺在蒙脱土层板之间的均匀分散,改善了蒙脱土的团状结构,使蒙脱土无序度增加,结构更加蓬松,表面呈现松散的独立片层状,这不仅能够降低发泡剂的分解温度、局部发泡剂量,而且能够提高蒙脱土在基体聚氯乙烯中的分散程度;配合适量氧化锌与碳酸氢钠的添加,进一步降低了发泡剂的分解温度,添加到聚氯乙烯中,能够避免聚氯乙烯产生糊料的现象。本发明工艺生产的产品合成工艺便于工业控制,降低了生产成本,发泡温度适中,非常适合用于聚氯乙烯的发泡工艺,在发泡过程中不分解,不糊料,用此发泡剂形成的发泡材料质量稳定,泡孔细密均匀,保温效果优异,且具有一定的阻燃效果。
具体实施方式
一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,包括以下具体步骤:
(1)将80g蒙脱土加入30倍量的去离子水中,搅拌均匀形成悬浮液,加热至70℃,搅拌5小时,再将16g苄基三苯基氯化膦溶于160g去离子水中形成溶液加入上述分散液中,继续恒温搅拌4小时后冷却至室温,将反应物抽滤,将沉淀物用去离子水清洗2次后再用体积浓度为50%的乙醇溶液清洗1次,将洗净的改性蒙脱土在烘箱中以100℃烘干,研磨,过300目筛;
(2)将步骤(1)得到的改性蒙脱土分散于15倍量的去离子水中,加热至50℃,以1000转/分的速度搅拌30分钟,用1mol/L的氢氧化钠溶液调节体系pH为9待用;将于改性蒙脱土等量的偶氮二甲酰胺溶于25倍量二甲基亚砜中形成溶液,然后将其缓慢加入上述改性蒙脱土分散体系中,加热至55℃,剧烈搅拌10小时,反应结束后对体系进行离心,将沉淀物分别用二甲基亚砜洗涤2次后放入真空干燥箱中,以60℃干燥20小时,得到偶氮二甲酰胺插层改性蒙脱石;
(3)将步骤(2)产物与3.4g氧化锌、1.7g碳酸氢钠混合均匀即可。
Claims (6)
1.一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,其特征在于,包括以下具体步骤:
(1)将蒙脱土加入30-35倍量的去离子水中,搅拌均匀形成悬浮液,加热至70-75℃,搅拌5-6小时,再加入适量的苄基三苯基氯化膦溶液,继续恒温搅拌4-5小时后冷却至室温,将反应物抽滤,将沉淀物用去离子水清洗2-3次后再用乙醇溶液清洗1次,将洗净的改性蒙脱土在烘箱中以100-110℃烘干,研磨,过300目筛;
(2)将步骤(1)得到的改性蒙脱土分散于15-16倍量的去离子水中,加热至50-55℃,以1000-1200转/分的速度搅拌30-40分钟,调节体系pH为9待用;将偶氮二甲酰胺溶于25-28倍量二甲基亚砜中形成溶液,然后将其缓慢加入上述改性蒙脱土分散体系中,加热至55-60℃,剧烈搅拌10-12小时,反应结束后对体系进行离心,将滤饼分别用二甲基亚砜洗涤2-3次后放入真空干燥箱中,以60-70℃干燥20-24小时,得到偶氮二甲酰胺插层改性蒙脱石;
(3)将步骤(2)产物与适量的氧化锌、碳酸氢钠混合均匀即可。
2.根据权利要求1所述的一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,其特征在于,步骤(1)中所述的苄基三苯基氯化膦溶液是指质量浓度为10%的苄基三苯基氯化膦水溶液,且添加量为蒙脱土与苄基三苯基氯化膦的质量比为50:1。
3.根据权利要求1所述的一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,其特征在于,步骤(1)中所述的乙醇溶液为体积浓度为50%的乙醇溶液。
4.根据权利要求1所述的一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,其特征在于,步骤(2)中所述的调节体系pH使用的是1mol/L的氢氧化钠溶液。
5.根据权利要求1所述的一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,其特征在于,步骤(2)中所述的偶氮二甲酰胺与步骤(1)产物的质量配比为1:1。
6.根据权利要求1所述的一种用于聚氯乙烯的插层改性有机蒙脱土复合发泡剂的制备方法,其特征在于,步骤(3)中所述的氧化锌与碳酸氢钠的质量比为2:1,且总添加量为步骤(2)产物质量的3-6%。
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CN115108776A (zh) * | 2022-05-31 | 2022-09-27 | 江苏泰林建设有限公司 | 一种高强度再生混凝土 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101899166A (zh) * | 2009-05-25 | 2010-12-01 | 北京化工大学 | 一种插层型纳米复合发泡剂的制备方法 |
CN102504618A (zh) * | 2011-11-22 | 2012-06-20 | 华南理工大学 | 蒙脱土的改性方法及纳米复合微发泡材料的制备方法 |
CN104592553A (zh) * | 2014-12-31 | 2015-05-06 | 贵州省材料产业技术研究院 | 复合阻燃剂及其制备方法 |
GB2527731A (en) * | 2014-04-10 | 2016-01-06 | Thermoseal Group Ltd | Glazing spacer bar |
-
2017
- 2017-06-06 CN CN201710419669.8A patent/CN107286365A/zh active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101899166A (zh) * | 2009-05-25 | 2010-12-01 | 北京化工大学 | 一种插层型纳米复合发泡剂的制备方法 |
CN102504618A (zh) * | 2011-11-22 | 2012-06-20 | 华南理工大学 | 蒙脱土的改性方法及纳米复合微发泡材料的制备方法 |
GB2527731A (en) * | 2014-04-10 | 2016-01-06 | Thermoseal Group Ltd | Glazing spacer bar |
CN104592553A (zh) * | 2014-12-31 | 2015-05-06 | 贵州省材料产业技术研究院 | 复合阻燃剂及其制备方法 |
Cited By (1)
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CN115108776A (zh) * | 2022-05-31 | 2022-09-27 | 江苏泰林建设有限公司 | 一种高强度再生混凝土 |
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