CN103331149A - 一种海绵状高分子吸附材料 - Google Patents

一种海绵状高分子吸附材料 Download PDF

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CN103331149A
CN103331149A CN2013102775490A CN201310277549A CN103331149A CN 103331149 A CN103331149 A CN 103331149A CN 2013102775490 A CN2013102775490 A CN 2013102775490A CN 201310277549 A CN201310277549 A CN 201310277549A CN 103331149 A CN103331149 A CN 103331149A
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路建美
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Suzhou Shuilan Environmental Protection Technology Co., Ltd
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Abstract

本发明公开了一种海绵状高分子吸附材料，其厚度为15～20mm，密度为600～720g/L；其由纤维状高分子吸附材料编织得到，具体为先将分子量为1.5～2万的线性聚合物经过熔喷纺丝的方法制备成聚合物丝；然后将丝通过交联剂以及致孔剂溶液，于130～150℃下，经过25～35秒得到纤维状高分子吸附材料；最后经过编织获得海绵状高分子吸附材料。本发明公开的海绵状高分子吸附材料，厚度和密度可控，具有大吸附容量、快速吸附以及强度好的特点，能够满足突发事故处置，特别是油品泄露污染处理，需要快速响应、快速处置的要求；并不会对环境造成破坏，适合工业化应用。

Description

一种海绵状高分子吸附材料
技术领域
本发明涉及一种吸附材料，具体涉及一种海绵状高分子吸附材料，属于高分子材料领域。
背景技术
随着工业化的发展，全球环境污染问题日趋严重，其中，各种有机物以及因各种事故泄漏的机油、原油，造成的河流、海洋等水资源污染的突发性事故频发的问题亟待遏制和解决。突发性水域污染具有污染面积大、处理对象不稳定的特点。
目前对油品泄漏目前国际上普遍采用加消油剂的方法。消油剂又名溢油分散剂，由多种表面活性剂和强渗透性溶剂组成，其作用机理是将水面浮油乳化，形成细小粒子分散在水中，并不能真正的消油；并且由于其增大了油与水的接触界面，使油更容易在水域扩散，造成了更大面积的污染，同时组成消油剂的化学物质会给水域生态环境带来二次污染。
吸附技术是通过吸附材料捕集排入环境中的有害物达到处理的目的，可避免对环境的破坏，其核心在于吸附材料，以活性炭为代表的传统吸附材料以及相关吸附技术在吸附效果和工艺操作方面存在的缺陷，无法达到工业化的治理要求，尤其是颗粒状活性炭用于突发性水污染事故处置时，由于在大面积流动的水域操作困难，根本无法实现对水面漂浮有毒有机污染物的清理回收，因此需要开发新的吸附材料以有效的处置突发水域污染事故。
发明内容
本发明的目的是提供一种海绵状高分子吸附材料，该吸附材料具有吸附速度快、吸附容量大、强度好和可重复使用的特点。 
为达到上述发明目的，本发明采用的技术方案是：
一种海绵状高分子吸附材料，所述海绵状高分子吸附材料由纤维状高分子吸附材料编织得到；所述海绵状高分子吸附材料的厚度为15～20mm，密度为600～720g/L；
所述纤维状高分子吸附材料通过以下步骤制备得到：首先将分子量为1.5-2万的线性聚合物经过熔喷纺丝的方法制备成丝；然后将丝通过装有交联剂以及致孔剂的槽；最后经过低温交联致孔得到直径为4～6微米的纤维状高分子吸附材料；其中，交联剂的用量为聚合物质量的1.5%；致孔剂的用量为聚合物质量的1%；所述低温交联致孔时的温度为130～150℃，时间为25～35秒；
所述交联剂为二丙烯酸酯类化合物，其结构式如J1、J2或者J3所示：
Figure 886586DEST_PATH_IMAGE001
；
所述致孔剂为改性石蜡，由固体石蜡通过以下步骤制备得到：将固体石蜡和浓度为1～100mg/ml的分散剂水溶液混合，于60～100℃下搅拌均匀后滴加丙烯酸酯单体和过氧化苯甲酰，进行聚合反应2.5～4小时，最后快速倒入水中，得到固体颗粒即为改性石蜡；
所述分散剂为明胶和羟乙基纤维素，其中明胶和羟乙基纤维素的质量比例为1∶2；所述过氧化苯甲酰为丙烯酸酯单体质量的1%～3%。
上述技术方案中，线性聚合物为甲基丙烯酸长链酯、甲基丙烯酸烷基酯、9-(12-((4-乙烯基苄基)氧)十二烷基)稠环芳烃或12-(稠环芳烃-9-基)十二烷基乙酸酯中的一种；所述甲基丙烯酸长链酯中，长链为C6-C18的直链烷基；甲基丙烯酸烷基酯中烷基为C1-C6的直链烃；所述稠环芳烃为苯、萘、蒽或蔥。
优选的技术方案，上述聚合物的熔点为150℃。
上述技术方案中，交联剂为液体，致孔剂在热处理温度下直接能融化；熔喷纺丝亦为常规技术。
本发明中J1、J2、J3交联剂可以通过以下方式制备：将4,4’-联苯二酚、萘四甲酸二酐和苝四甲酸二酐分别与1-氯乙醇、2-氨基乙醇和2-氨基乙醇反应得到三种2-位取代的乙醇中间体，再与丙烯酰氯在吡啶溶液中缩合分别得到交联剂J1、J2和J3。
上述方案中的交联工艺和致孔工艺很重要。本发明中制备纤维状高分子吸附材料的时候先纺丝后交联技术既保证了聚合物能满足纺丝的要求，又保证了最终得到的纤维具有一定的强度；通过致孔剂可以使纤维具有多孔结构，有效增加比表面积，亲油基团不仅存在于纤维表面，也大量存在微孔中，加快纤维吸附速度并进一步提高吸附容量。
本发明中，海绵状高分子吸附材料的厚度与密度对实际应用很重要。太薄，吸附材料强度差，在实际应用时不能耐受水流的冲击，更无法承受配套装备的机械力，不能满足处置突发事故的要求；吸附材料太厚，则影响吸附性能，不能实现快速吸附和大容量吸附，同样不能满足突发性事故快速处置的要求；密度过小的吸附材料保油性不佳，而密度过大会影响其吸附速度，通过孔径和纤维堆积紧密程度的综合调节可以得到不同密度的产品，满足不同应用需求，比如密度大的吸附材料用于低粘度有机物、密度小的吸附材料用于成品油及原油。
本发明的整体工艺步骤为：聚合物→计量泵→熔喷模头喷丝孔挤出→熔体细流拉伸与冷却→浸渍→交联和致孔→收集纤维→编织。
由于上述技术方案运用，本发明与现有技术相比具有下列优点：
本发明公开的海绵状高分子吸附材料，厚度和密度可控，具有大吸附容量、快速吸附以及强度好的特点，能够满足突发事故处置，特别是油品泄露污染处理，需要快速响应、快速处置的要求；并不会对环境造成破坏，适合工业化应用。
具体实施方式
下面结合实施例对本发明作进一步描述：
实施例一 纤维状高分子吸附材料的制备
以常规合成方法合成线性聚合物，通过工艺调节控制分子量为1.5～2万、熔点为150℃，以满足纺丝要求，将聚合物采用熔喷纺丝方法成丝，并使其通过装有聚合物质量1.5%的交联剂和聚合物质量1%的致孔剂的槽，最后使纤维在较低温下（140℃）快速（35秒）交联，使纤维表面形成交联层并致孔，最终得到直径在4～6微米的纤维状高分子吸附材料，其吸附速度快，达到饱和时间远远低于目前国际上普遍的4～6小时。
所述线性聚合物为聚{甲基丙烯酸十八酯-甲基丙烯酸己酯-[9-(12-((4-乙烯基苄基)氧)十二烷基)蒽]}；上述交联剂为二丙烯酸酯类化合物J1，结构式为：
Figure 439053DEST_PATH_IMAGE002
。
交联剂（J1）制备：
将4,4’-联苯二酚（20 mmol）和1-氯乙醇（40 mmol）的2N氢氧化钠溶液（1.6 g，10 mL水）加热回流2 h后，室温搅拌10小时。以二氯甲烷萃取（3 × 30 mL）、10%的氢氧化钠（50 mL）和水（3 × 30 mL）洗涤，无水硫酸镁干燥，蒸除溶剂得中间体产品；
在0 ℃下，将丙烯酰氯（10 mmol）缓慢滴加到上述中间体（10 mmol）的吡啶（30 mL）溶液中，搅拌2 h后，室温搅拌10小时后倾入冰水中，以乙醚（3× 60 mL）萃取、5%盐酸（60 mL）和水（3 × 60 mL）洗涤，无水硫酸镁干燥，蒸除溶剂并以二氯甲烷/石油醚柱层析即得产品交联剂J1。
实施例二 海绵状高分子吸附材料的制备
以实施例一中的纤维状高分子吸附材料为原料，控制编织速度为5-10m/min，调节编织厚度密度，得到系列化产品，可用于不同污染物造成的突发事故的应急处置。采用无纺布拉力测试机测试强度；表一为不同厚度产品的强度，密度为650 g/L；表二为产品密度与吸附性能、强度之间的关系，吸附对象为甲苯，产品厚度为18mm。
表一  产品强度与厚度的关系
表二  产品密度与吸附性能、强度之间的关系
Figure 607046DEST_PATH_IMAGE004
。

Claims (3)

1.一种海绵状高分子吸附材料，其特征在于，所述海绵状高分子吸附材料由纤维状高分子吸附材料编织得到；所述海绵状高分子吸附材料的厚度为15～20mm，密度为600～720g/L；
所述纤维状高分子吸附材料通过以下步骤制备得到：首先将分子量为1.5～2万的线性聚合物经过熔喷纺丝的方法制备成聚合物丝；然后将丝通过装有交联剂以及致孔剂的槽；经过低温交联致孔得到直径为4～6微米的纤维状高分子吸附材料；其中，交联剂的用量为聚合物质量的1.5%；致孔剂的用量为聚合物质量的1%；所述低温交联致孔时的温度为130～150℃，时间为25～35秒； 
所述交联剂为二丙烯酸酯类化合物，其结构式如J1、J2或者J3所示：
Figure 2013102775490100001DEST_PATH_IMAGE001
；
所述致孔剂为改性石蜡，由固体石蜡通过以下步骤制备得到：将固体石蜡和浓度为1～100mg/ml的分散剂水溶液混合，于60～100℃下搅拌均匀后滴加丙烯酸酯单体和过氧化苯甲酰，进行聚合反应2.5～4小时，最后快速倒入水中，得到固体颗粒即为改性石蜡；
所述分散剂为明胶和羟乙基纤维素，其中明胶和羟乙基纤维素的质量比例为1∶2；所述过氧化苯甲酰为丙烯酸酯单体质量的1%～3%。
2.根据权利要求1所述的海绵状高分子吸附材料，其特征在于：所述线性聚合物为甲基丙烯酸长链酯、甲基丙烯酸烷基酯、9-(12-((4-乙烯基苄基)氧)十二烷基)稠环芳烃或12-(稠环芳烃-9-基)十二烷基乙酸酯中的一种；
所述甲基丙烯酸长链酯中，长链为C6-C18的直链烷基；甲基丙烯酸烷基酯中烷基为C1-C6的直链烃；
所述稠环芳烃为苯、萘、蒽或蔥。
3.根据权利要求1所述的海绵状高分子吸附材料，其特征在于：所述线性聚合物的熔点为150℃。
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