CN114102960A - 一种阻燃pet泡沫板材的连续挤出制备方法 - Google Patents
一种阻燃pet泡沫板材的连续挤出制备方法 Download PDFInfo
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Abstract
本发明涉及一种阻燃PET泡沫板材的连续挤出制备方法，包括如下步骤：以重量计，将PET发泡原料树脂100份，扩链剂0.3～1份，成核剂0.1～10份，热稳定剂0.1～10份，阻燃剂5～15份，协效剂0.1～5份加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头形成稳定固化的泡孔结构；将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。本发明配方可制备发泡材料；由连续法取代了间歇法生产，提高了生产效率；在挤出发泡区设置集气罩对尾气进行收集与处理，满足环保要求。
Description
技术领域
本发明涉及PET泡沫板材技术领域，尤其涉及一种阻燃PET泡沫板材的连续挤出制备方法。
背景技术
目前对阻燃PET研究较多，王良等利用合成的2-丙酸钠苯基次磷酸钠(CEPP–Na)与PET共混，当CEPP–Na的质量分数为15％时，PET的阻燃性能提高了，但由于阻燃剂含量高，无法用于制备发泡材料；阻燃PET泡沫涉及配方设计、生产设备、生产工艺等因素，实现连续生产存在较高难度。
华东理工大学高亮研究了阻燃改性PET及其挤出发泡材料，刘君玉采用超临界CO2发泡PET聚合物的研究，两者均采用间歇法；间歇法生产效率低，产品质量无法控制。
综上所述，现有技术具有如下技术缺陷：
1)阻燃PET因阻燃剂含量高，无法制备发泡材料；
2)基本采用间歇法进行阻燃PET泡沫的生产，未能实现连续化生产；
3)尾气的收集与处理，对环境的影响。
发明内容
本发明的目的是提供一种阻燃PET泡沫板材的连续挤出制备方法，以解决上述技术问题。
本发明提供了一种阻燃PET泡沫板材的连续挤出制备方法，采用阻燃PET泡沫板材制备系统连续性挤出生产阻燃PET泡沫材料，所述阻燃PET泡沫板材制备系统包括依次连接的高扭矩双螺杆挤出机、单螺杆挤出机、熔体冷却器、静态混合器、条刨模头；
所述连续挤出制备方法包括如下步骤：
1)以重量计，将PET发泡原料树脂100份，扩链剂0.3～1份，成核剂0.1～10份，热稳定剂0.1～10份，阻燃剂5～15份，协效剂0.1～5份加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；
2)混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头内的高压与周围环境之间较高的压降速率诱发体系的热力学不稳定性，从而形成气泡核，随着气泡的生长和熔体的冷却，当泡孔生长的内外压力达到平衡时，发泡材料逐步形成稳定固化的泡孔结构；
3)将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。
进一步地，所述高扭矩双螺杆挤出机温度为一区210～265℃，二区255～275℃，三区260～280℃，四区260～280℃，五区260～280℃，六区260～275℃；所述单螺杆挤出机温度为一区250～270℃，二区260～275℃，三区260～280℃，四区260～280℃，五区255～275℃，六区250～270℃，主机转速300r/min；进料口转速为15～25r/min。
进一步地，所述PET为瓶级PET树脂，所述扩链剂为均苯四甲酸酐，所述成核剂为滑石粉、碳酸钙、二氧化硅、二氧化钛、改性蒙脱石中的一种或几种，所述热稳定剂为磷酸三苯酯、磷酰基乙酸三乙酯、酚类抗氧剂中的一种或几种)，，所述阻燃剂为有机磷酸系，如磷酸酯、亚磷酸酯、有机磷酸盐、磷杂环化合物及聚合物磷酸酯中的一种或几种，所述协效剂为nano-CaCO3或nano-Al2O3。
进一步地，所述阻燃PET泡沫板材制备系统还包括设于挤出发泡区用于收集尾气的集气罩。
借由上述方案，通过阻燃PET泡沫板材的连续挤出制备方法，具有如下技术效果：
针对PET中阻燃剂含量增多，无法制备发泡材料问题，本发明的配方能达到相同阻燃效果，其中金属化合物纳米颗粒(协效剂)与阻燃剂磷酸盐有明显的协效作用，能够促进PET在燃烧的过程中形成稳定的炭层，阻燃剂体系更容易产生较为明显的磷酸盐并附着在聚合物表面，并与燃烧产生的炭层很好的结合在泡沫表面，抑制炭层坍塌，从而提高磷酸盐的阻燃效率，同时由于纳米粒子的协效作用，可减少阻燃剂的添加量从而使阻燃剂能够更好地分散在聚合物内部，进而减缓PET熔体强度的下降，提高其熔体发泡性。通过该方法制备的PET泡沫板材密度在60～400kg/m3，闭孔率达95％以上，泡沫均一，阻燃性能达b2级，氧指数>＝28.5。
2)本发明由连续法取代了间歇法生产，提高了生产效率。
3)本发明挤出发泡区设置集气罩(收集效率达90％)，废气经UV光氧催化和二级活性碳吸附处理后由排气筒高空排放，对尾气进行收集与处理，满足环保要求。
上述说明仅是本发明技术方案的概述，为了能够更清楚了解本发明的技术手段，并可依照说明书的内容予以实施，以下以本发明的较佳实施例并配合附图详细说明如后。
附图说明
图1是本发明阻燃PET泡沫板材的连续挤出制备方法的流程图。
具体实施方式
下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。
本实施例提供了一种阻燃PET泡沫板材的连续挤出制备方法，采用阻燃PET泡沫板材制备系统连续性挤出生产阻燃PET泡沫材料，所述阻燃PET泡沫板材制备系统包括依次连接的高扭矩双螺杆挤出机、单螺杆挤出机、熔体冷却器、静态混合器、条刨模头；
所述连续挤出制备方法包括如下步骤：
1)以重量计(失重称计量)，将PET发泡原料树脂100份(预混料，改性的聚合物颗粒，粒料在高温下对水比较敏感，水份含量不超过0.02％)，扩链剂0.3～1份，成核剂0.1～10份，热稳定剂0.1～10份，阻燃剂5～15份，协效剂0.1～5份等助剂加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成聚合物熔体，定量定压将CO2或环戊烷(发泡剂)注入到机筒内与聚合物熔体混合，通过与螺杆结构的相互匹配，建立高背压、防止气体向后溢出，保证两相体系的正常输送；其次，通过螺杆在高转速下的强剪切混合作用，将大气泡分散成大量的小气泡，通过气体对聚合物的扩散溶解特性形成聚合物和气体的均相共混体系；
2)混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头内的高压与周围环境之间较高的压降速率诱发体系的热力学不稳定性，从而形成气泡核，随着气泡的生长和熔体的冷却，当泡孔生长的内外压力达到平衡时，发泡材料逐步形成稳定固化的泡孔结构；
3)将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。
在本实施例中，所述高扭矩双螺杆挤出机温度为一区210～265℃，二区255～275℃，三区260～280℃，四区260～280℃，五区260～280℃，六区260～275℃；所述单螺杆挤出机温度为一区250～270℃，二区260～275℃，三区260～280℃，四区260～280℃，五区255～275℃，六区250～270℃，主机转速300r/min；进料口转速为15～25r/min。
在本实施例中，所述PET为瓶级PET树脂，所述扩链剂为均苯四甲酸酐，所述成核剂为滑石粉、碳酸钙、二氧化硅、二氧化钛、改性蒙脱石中的一种或几种，所述热稳定剂为磷酸三苯酯、磷酰基乙酸三乙酯、酚类抗氧剂，所述阻燃剂为有机磷酸系，如磷酸酯、亚磷酸酯、有机磷酸盐、磷杂环化合物及聚合物磷酸酯中的一种或几种，所述协效剂为nano-CaCO3或nano-Al2O3。
在本实施例中，所述阻燃PET泡沫板材制备系统还包括设于挤出发泡区用于收集尾气的集气罩，废气经UV光氧催化和二级活性碳吸附处理后由排气筒高空排放，满足环保要求。
实施例1
将PET发泡原料树脂100kg，均苯四甲酸酐400g，滑石粉200g，磷酸三苯酯6g，有机磷酸盐5kg，加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头形成稳定固化的泡孔结构；将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。其中高扭矩双螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区270℃，五区265℃，六区260℃；所述单螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区265℃，五区260℃，六区250℃，主机转速300r/min；进料口转速为20r/min。静态混合器230℃，机头温度228℃。而PET发泡材料表观密度为77kg/m3，LOI值为23.4。
实施例2
将PET发泡原料树脂100kg，均苯四甲酸酐400g，滑石粉200g，磷酸三苯酯6g，有机磷酸盐5kg，nano-Al2O31kg，加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头形成稳定固化的泡孔结构；将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。其中高扭矩双螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区270℃，五区265℃，六区260℃；所述单螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区265℃，五区260℃，六区250℃，主机转速300r/min；进料口转速为20r/min。而PET发泡材料表观密度为83kg/m3，LOI值为26.9。
实施例3
将PET发泡原料树脂100kg，均苯四甲酸酐400g，改性蒙脱石200g，抗氧剂1010 6g，有机磷酸盐6.5kg，nano-Al2O31kg，加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头形成稳定固化的泡孔结构；将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。其中挤出温度如下：第一区温度255℃，第二区温度275℃，第三区温度260℃，第四区温度250℃，静态混合器230℃，机头温度228℃。而PET发泡材料表观密度为80kg/m3，LOI值为27.9。
实施例4
将PET发泡原料树脂100kg，均苯四甲酸酐400g，滑石粉200g，磷酸三苯酯6g，有机磷酸盐7.5kg，加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头形成稳定固化的泡孔结构；将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。其中高扭矩双螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区270℃，五区265℃，六区260℃；所述单螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区265℃，五区260℃，六区250℃，主机转速300r/min；进料口转速为20r/min。而PET发泡材料表观密度为79kg/m3，LOI值为27.6。
实施例5
将PET发泡原料树脂100kg，均苯四甲酸酐400g，滑石粉200g，磷酸三苯酯6g，有机磷酸盐7.5kg，nano-Al2O31kg，加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头形成稳定固化的泡孔结构；将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。其中高扭矩双螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区270℃，五区265℃，六区260℃；所述单螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区265℃，五区260℃，六区250℃，主机转速300r/min；进料口转速为20r/min。而PET发泡材料表观密度为78kg/m3，LOI值为28.6。
实施例6
将PET发泡原料树脂100kg，均苯四甲酸酐400g，滑石粉200g，磷酸三苯酯6g，有机磷酸盐10kg，nano-Al2O31kg，加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头形成稳定固化的泡孔结构；将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。其中高扭矩双螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区270℃，五区265℃，六区260℃；所述单螺杆挤出机温度为一区255℃，二区270℃，三区275℃，四区265℃，五区260℃，六区250℃，主机转速300r/min；进料口转速为20r/min。而PET发泡材料表观密度为101kg/m3，LOI值为32.3。
该阻燃PET泡沫板材的连续挤出制备方法，具有如下技术效果：
1)针对PET中阻燃剂含量增多，无法制备发泡材料问题，本发明的配方能达到相同阻燃效果，其中金属化合物纳米颗粒(协效剂)与阻燃剂磷酸盐有明显的协效作用，能够促进PET在燃烧的过程中形成稳定的炭层，阻燃剂体系更容易产生较为明显的磷酸盐并附着在聚合物表面，并与燃烧产生的炭层很好的结合在泡沫表面，抑制炭层坍塌，从而提高磷酸盐的阻燃效率，同时由于纳米粒子的协效作用，可减少阻燃剂的添加量从而使阻燃剂能够更好地分散在聚合物内部，进而减缓PET熔体强度的下降，提高其熔体发泡性。通过该方法制备的PET泡沫板材密度在60～400kg/m3，闭孔率达95％以上，泡沫均一，阻燃性能达b2级，氧指数>＝28.5。
2)本发明由连续法取代了间歇法生产，提高了生产效率。
3)本发明挤出发泡区设置集气罩(收集效率达90％)，废气经UV光氧催化和二级活性碳吸附处理后由排气筒高空排放，对尾气进行收集与处理，满足环保要求。
以上所述仅是本发明的优选实施方式，并不用于限制本发明，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变型，这些改进和变型也应视为本发明的保护范围。
Claims (4)
1.一种阻燃PET泡沫板材的连续挤出制备方法，其特征在于，采用阻燃PET泡沫板材制备系统连续性挤出生产阻燃PET泡沫材料，所述阻燃PET泡沫板材制备系统包括依次连接的高扭矩双螺杆挤出机、单螺杆挤出机、熔体冷却器、静态混合器、条刨模头；
所述连续挤出制备方法包括如下步骤：
1)以重量计，将PET发泡原料树脂100份，扩链剂0.3～1份，成核剂0.1～10份，热稳定剂0.1～10份，阻燃剂5～15份，协效剂0.1～5份加入到高扭矩双螺杆挤出机中，在高扭矩双螺杆挤出机机筒内完全熔融混合形成熔体，定量定压将CO2或环戊烷注入到机筒内与熔体混合；
2)混合后的熔体经高扭矩双螺杆挤出机和单螺杆挤出机挤出，熔体冷却器冷却，静态混合器混合后，通过条泡模头内的高压与周围环境之间较高的压降速率诱发体系的热力学不稳定性，从而形成气泡核，随着气泡的生长和熔体的冷却，当泡孔生长的内外压力达到平衡时，发泡材料逐步形成稳定固化的泡孔结构；
3)将固化的泡孔结构随辅机牵引、降温、定型、切边、裁切成标准板材。
2.根据权利要求1所述的阻燃PET泡沫板材的连续挤出制备方法，其特征在于，所述高扭矩双螺杆挤出机温度为一区210～265℃，二区255～275℃，三区260～280℃，四区260～280℃，五区260～280℃，六区260～275℃；所述单螺杆挤出机温度为一区250～270℃，二区260～275℃，三区260～280℃，四区260～280℃，五区255～275℃，六区250～270℃，主机转速300r/min；进料口转速为15～25r/min。
3.根据权利要求1所述的阻燃PET泡沫板材的连续挤出制备方法，其特征在于，所述PET为瓶级PET树脂，所述扩链剂为均苯四甲酸酐，所述成核剂为滑石粉、碳酸钙、二氧化硅、二氧化钛、改性蒙脱石中的一种或几种，所述热稳定剂为磷酸三苯酯、磷酰基乙酸三乙酯、酚类抗氧剂中的一种或几种，所述阻燃剂为有机磷酸系，如磷酸酯、亚磷酸酯、有机磷酸盐、磷杂环化合物及聚合物磷酸酯中的一种或几种，所述协效剂为nano-CaCO3或nano-Al2O3。
4.根据权利要求1所述的阻燃PET泡沫板材的连续挤出制备方法，其特征在于，所述阻燃PET泡沫板材制备系统还包括设于挤出发泡区用于收集尾气的集气罩。
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| CN114851459A (zh) * | 2022-04-21 | 2022-08-05 | 巩义市泛锐熠辉复合材料有限公司 | 一种泡沫夹心蜂窝板的生产设备及其制备方法 |
| CN115011087A (zh) * | 2022-07-18 | 2022-09-06 | 华润化学材料科技股份有限公司 | 一种阻燃聚酯泡沫板及其制备方法 |
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| CN114851459A (zh) * | 2022-04-21 | 2022-08-05 | 巩义市泛锐熠辉复合材料有限公司 | 一种泡沫夹心蜂窝板的生产设备及其制备方法 |
| CN114851459B (zh) * | 2022-04-21 | 2023-06-06 | 巩义市泛锐熠辉复合材料有限公司 | 一种泡沫夹心蜂窝板的生产设备及其制备方法 |
| CN115011087A (zh) * | 2022-07-18 | 2022-09-06 | 华润化学材料科技股份有限公司 | 一种阻燃聚酯泡沫板及其制备方法 |
| CN115011087B (zh) * | 2022-07-18 | 2024-05-17 | 华润化学材料科技股份有限公司 | 一种阻燃聚酯泡沫板及其制备方法 |
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