CN103756090A - 一种高比强度聚乙烯/碱木质素发泡材料的制备方法 - Google Patents

一种高比强度聚乙烯/碱木质素发泡材料的制备方法 Download PDF

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CN103756090A
CN103756090A CN201410006111.3A CN201410006111A CN103756090A CN 103756090 A CN103756090 A CN 103756090A CN 201410006111 A CN201410006111 A CN 201410006111A CN 103756090 A CN103756090 A CN 103756090A
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alkali lignin
foam material
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冯钠
李季
张桂霞
樊明帅
谷宇
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Abstract

本发明提供一种高比强度聚乙烯/碱木质素发泡材料的制备方法，在以低密度聚乙烯和烷基化改性碱木质素为原料，加入润滑剂、抗氧剂、交联剂、发泡剂和助发泡剂，经过塑炼和模压发泡过程制得所述发泡材料。本发明采用溴代或氯代烷烃对碱木质素进行烷基化改性，降低了碱木质素的分子极性，使二者相容性提高，引入的碱木质素可提高发泡材料的强度和热稳定性，且可在一定程度上解决碱木质素的废物处理问题，具有一定的环境效益。

Description

一种高比强度聚乙烯/碱木质素发泡材料的制备方法
技术领域
本发明涉及一种高比强度聚乙烯/碱木质素发泡材料的制备方法，属于高分子发泡材料技术领域。
背景技术
低密度聚乙烯泡沫塑料具有较低的密度、较大的比体积、良好的绝热性及柔韧性、优异的吸音性，因而广泛应用在建筑、化工和包装等领域。但目前低密度聚乙烯泡沫塑料存在一定的不足，如耐热性差，强度低，易燃烧等，因而对其进行改性具有现实意义。
木质素是一种可再生且来源广泛的有机资源，储量仅次于纤维素，是具有苯丙烷结构单元的三维高分子网状化合物。碱木质素是我国造纸工业中碱法制浆产生的副产品，这种工业碱木质素保留了木质素大分子骨架及功能基团，具有良好的阻燃性、高抗冲强度、热稳定性及耐溶剂性。迄今为止，仅有5%左右的木质素得到二次利用，其余均被燃烧、气化或降解，造成了资源浪费。
碱木质素具有的苯丙烷结构单元，使其显示出刚性材料的特征，促使发泡材料强度提高，紫丁香基苯环上甲氧基对羟基构成的受阻酚结构能够捕获热氧老化及光氧老化过程中产成的自由基，终止链反应，使材料的热稳定性有所提高。
将碱木质素引入到发泡材料中，不但可以提高发泡材料的强度及耐热性，而且为造纸厂排放废液带来的环境问题找到有效的解决办法。
发明内容
本发明为解决现有技术中的低密度聚乙烯泡沫材料强度低、耐热性差和易燃烧的问题，提供一种高比强度聚乙烯/碱木质素发泡材料的制备方法。本发明的发泡材料与普通低密度聚乙烯发泡材料相比，表观密度相当，但具有较高的拉伸强度、弯曲强度和氧指数，因此比强度高，且具有一定的阻燃效果。
本发明的技术目的通过以下技术方案实现：
一种高比强度聚乙烯/碱木质素发泡材料的制备方法，以低密度聚乙烯和烷基化改性碱木质素为原料，加入润滑剂、抗氧剂、交联剂、发泡剂和助发泡剂，经过塑炼和模压发泡过程制得所述发泡材料；
所述烷基化改性碱木质素是将C6～C12的溴代或氯代正烷烃与碱木质素反应进行的改性。
本发明所述溴代或氯代正烷烃优选为端基的一个H被溴或氯取代的直链烷烃。
本发明所述烷基化改性碱木质素还包括对碱木质素提纯的过程，然后对提纯的碱木质素进行烷基化改性，以提高分散效果及与低密度聚乙烯的相容性。
碱木质素提纯过程如下：将碱木质素溶解于氢氧化钠溶液，过滤除去不溶杂质，用盐酸调节溶液pH值至2，过滤，用蒸馏水将沉淀物充分洗涤至中性。
碱木质素烷基化过程如下：将提纯碱木质素溶于体积比为2:1的异丙醇-水混合溶剂中，以NaOH溶液调节pH为11～12，与溴代或氯代正烷烃于130-170℃反应2～4小时，碱木质素与溴代或氯代正烷烃的质量比为100:25～30，反应后的产物在盐酸溶液中沉淀、洗涤，用二氯乙烷洗去未反应的长链卤代烷，烘干备用。
以溴代烷烃为例，碱木质素烷基化改性反应如下式所示：
Lignin-OH+Br-CnH2n+1→Lignin-O-CnH2n+1+HBr
碱木质素结构中具有的羟基，使其容易形成分子内和分子间氢键，产生团聚现象，通过烷基化改性，减少了羟基含量，削弱团聚作用，引入的烷基链，降低了碱木质素的极性，提高了其与低密度聚乙烯的相容性。
本发明所述低密度聚乙烯密度在0.915～0.940g·cm-3范围。
本发明所述的制备方法，包括以下步骤：
①将低密度聚乙烯、烷基化改性碱木质素、润滑剂、抗氧剂、交联剂、发泡剂和助发泡剂以质量比为100:5-50:1:1:1-5:2-10:0.6-3比例混合均匀，于125℃-130℃塑炼5-10min；
②将步骤①塑炼后的混合物进行模压发泡，发泡温度为165℃-190℃，发泡压力为5MPa-15MPa，保压时间为10-20min。
本发明所述的制备方法，优选所述润滑剂为聚乙烯蜡；所述抗氧剂为酚类抗氧剂1010；所述交联剂为过氧化二异丙苯；所述发泡剂为吸-放热型复合发泡剂，优选为碳酸氢钠/偶氮二甲酰胺复合发泡剂，所述复合发泡剂优选碳酸氢钠与偶氮二甲酰胺的质量比为1:2；优选所述助发泡剂为柠檬酸和氧化锌的混合物，所述柠檬酸的加入量与碳酸氢钠的质量比为1:2，所述氧化锌的加入量与偶氮二甲酰胺的质量比为1:5。
本发明所述的制备方法，作为最优选的实施方式，低密度聚乙烯、烷基化改性碱木质素、聚乙烯蜡、抗氧剂1010、过氧化二异丙苯、碳酸氢钠/偶氮二甲酰胺、柠檬酸和氧化锌的质量比为100:20:1:1:2:6:1:0.8。
本发明的有益效果在于：
（1）采用溴代或氯代烷烃对碱木质素进行烷基化改性，降低了碱木质素的分子极性，提高其与低密度聚乙烯的相容性，有助于两者的复合，进而使泡沫塑料的力学性能有大幅度提高；
（2）采用适合于低密度聚乙烯/碱木质素体系的吸-放热复合发泡剂，使发泡材料的泡孔细腻均匀，发泡效果良好；
（3）将质轻且有增强效果的碱木质素引入到低密度聚乙烯发泡体系，碱木质素具有的苯丙烷结构单元，使其显示出刚性材料的特征，促使发泡材料强度提高，紫丁香基苯环上甲氧基对羟基构成的受阻酚结构能够捕获热氧老化及光氧老化过程中产成的自由基，终止链反应，使材料的热稳定性有所提高；
（4）为碱木质素的处理提供解决办法，例如可减少造纸厂因处理碱木质素排放的废液，具有一定的环境效益。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明，但不以任何方式限制本发明。
以下实施例中使用的高速混合机型号：GH-10，厂家：北京塑料机械厂；双辊开炼机型号：SK-160B，厂家：上海思南橡胶机械有限公司；平板硫化机型号：QLB-50D/Q，厂家：无锡市中凯橡塑机械有限公司；氧指数测试仪，型号：HC-2，厂家：北京市永丰机电技术公司。
以下实施例中所参照的标准分别为表观密度标准：GB/T6343-2009，拉伸强度标准：GB/T1040-2006，弯曲强度标准：GB/T9341-2008，氧指数测试标准：GB/T2406-1993。
实施例1
（1）碱木质素的提纯和烷基化改性
碱木质素的提取：将适量的碱木质素充分溶解于1mol/L的氢氧化钠溶液，过滤除去不溶杂质，然后用1mol/L的盐酸调节溶液pH值至2，过滤，用蒸馏水将沉淀物充分洗涤至中性。
烷基化改性：将上述提纯碱木质素充分溶于体积比为2:1的异丙醇-水混合溶剂，以NaOH调节pH为12，与溴代十二烷于140℃反应3小时，碱木质素与溴代十二烷质量比为10:3，产物在盐酸水溶液中沉淀、洗涤，用二氯乙烷洗去未反应的长链卤代烷，产物于100℃干燥12h备用。
（2）塑炼：
按以下质量份数准备原料：
Figure BDA0000453609510000031
Figure BDA0000453609510000041
依次将低密度聚乙烯、改性碱木质素、聚乙烯蜡、抗氧剂1010、过氧化二异丙苯、氧化锌、柠檬酸、偶氮二甲酰胺、碳酸氢钠放入高速混合机中混合均匀，后在双辊开炼机中于125℃塑炼。
（3）模压发泡：
将步骤（2）所得的均匀混合原料装入模具，再送入平板硫化机进行交联发泡，温度为175℃，压力为10MPa，保压时间为15min。实验结束后压力骤降，完成发泡过程，得到本发明的发泡材料。
实施例2
除了在步骤（2）中烷基化改性碱木质素的质量份数改为30份，其它按与实施例1相同的步骤进行。
实施例3
除了在步骤（2）中质量份数改为：烷基化改性碱木质素30份，偶氮二甲酰胺5份，碳酸氢钠2.5份，氧化锌1份，柠檬酸1.25份，其它按与实施例1相同的步骤进行。
实施例4
除了在步骤（3）在平板硫化机中发泡的压力改为8MPa，其它同实施例1。
本发明的各实施例材料性能检测数据与低密度聚乙烯发泡材料的性能对比如表1所示。
对比例1
除了在步骤（2）中不添加烷基化改性碱木质素，其他原料组成和操作步骤同实施例2，制备低密度聚乙烯发泡材料。
表1.本发明的发泡材料与低密度聚乙烯发泡材料的性能对比
Figure BDA0000453609510000042
Figure BDA0000453609510000051
与对比例1制备的低密度聚乙烯发泡材料相比，烷基化碱木质素的加入可以有效提高发泡材料的拉伸强度及弯曲强度，实施例2和对比例1的材料相比，表观密度略高，而拉伸强度由16.7MPa提高到23.4MPa，使材料具有较高的比强度，弯曲强度由27.9MPa提高到35.3MPa。从氧指数对比数据来看，实施例2较对比例1的发泡材料略有提高。以上数据说明：在低密度聚乙烯发泡材料中，烷基化碱木质素的加入，使材料的强度提高，且材料的热稳定性具有一定的提升。

Claims (8)

1.一种高比强度聚乙烯/碱木质素发泡材料的制备方法，其特征在于以低密度聚乙烯和烷基化改性碱木质素为原料，加入润滑剂、抗氧剂、交联剂、发泡剂和助发泡剂，经过塑炼和模压发泡过程制得所述发泡材料；
所述烷基化改性碱木质素是将C6～C12的溴代或氯代正烷烃与碱木质素反应进行的改性。
2.根据权利要求1所述的高比强度聚乙烯/碱木质素发泡材料的制备方法，其特征在于包括以下步骤：
①将低密度聚乙烯、烷基化改性碱木质素、润滑剂、抗氧剂、交联剂、发泡剂和助发泡剂以质量比为100:5-50:1:1:1-5:2-10:0.6-3比例混合均匀，于125℃-130℃塑炼5-10min；
②将步骤①塑炼后的混合物进行模压发泡，发泡温度为165℃-190℃，发泡压力为5MPa-15MPa，保压时间为10-20min。
3.根据权利要求1所述的高比强度聚乙烯/碱木质素发泡材料的制备方法，其特征在于所述润滑剂为聚乙烯蜡。
4.根据权利要求1所述的高比强度聚乙烯/碱木质素发泡材料的制备方法，其特征在于所述抗氧剂为抗氧剂1010。
5.根据权利要求1所述的高比强度聚乙烯/碱木质素发泡材料的制备方法，其特征在于所述交联剂为过氧化二异丙苯。
6.根据权利要求1所述的高比强度聚乙烯/碱木质素发泡材料的制备方法，其特征在于所述发泡剂为碳酸氢钠/偶氮二甲酰胺复合发泡剂。
7.根据权利要求6所述的高比强度聚乙烯/碱木质素发泡材料的制备方法，其特征在于所述复合发泡剂中碳酸氢钠与偶氮二甲酰胺的质量比为1:2。
8.根据权利要求1所述的高比强度聚乙烯/碱木质素发泡材料的制备方法，其特征在于所述助发泡剂为柠檬酸和氧化锌的混合物。
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