CN104289197A - 一种胺化增强改性秸秆基复合材料及其制备方法 - Google Patents
一种胺化增强改性秸秆基复合材料及其制备方法 Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本发明涉及一种胺化增强改性秸秆基复合材料及其制备方法，以重量计，将80-90份的胺化增强改性秸秆、1-10份的氧化石墨烯、1-10份的海藻酸盐缓慢加入到浴比1:10-20的去离子水中，超声处理1-24h，再经钙离子交联、冷冻干燥制得胺化增强改性秸秆/氧化石墨烯/海藻酸盐复合材料。本发明以胺化增强改性秸秆为载体负载氧化石墨烯和海藻酸盐，经钙离子交联、冷冻干燥制得胺化增强改性秸秆/氧化石墨烯/海藻酸盐复合材料。该复合材料具备绿色环保、机械性能好、组织结构规整、孔隙率高、吸附量大、吸附速度快、适用范围广、易于解吸，可重复利用等优点。
Description
技术领域
本发明属于功能材料技术领域，特别涉及一种胺化增强改性秸秆基复合材料及其制备方法。
背景技术
我国的农作物秸秆资源拥有量居世界首位。我国粮食的播种面积约为1.13亿hm2，粮食总产量4.9亿t，玉米、小麦等谷物秸秆总产量为5亿t，加上其他作物的秸秆，每年生产秸秆6亿t以上。虽然2.5亿t用于造肥还田；0.48亿t用于工业原料；1.8亿t用于农民生活燃料，但尚有1.2亿t秸秆剩余，成为生活垃圾或白白烧掉。农作物秸秆是地球上第一大可再生资源，是农作物的重要副产品，焚烧造成了资源的巨大浪费、并且向空气中放出大量的二氧化硫、苯丙吡等有害物质。充分挖掘秸秆的潜在价值，是近年来秸秆利用的主要发展方向。
随着我国经济、社会的快速发展，人口数量的不断增长，工业化和城镇化的加快推进，涉及水污染的行业正保持着强劲的增长势头，水污染事件频发，给环境和人们的健康带来了严重的损害，治理水污染已经成为一项刻不容缓的任务。
治理水污染的方法很多，传统的有化学沉淀法、氧化还原法、铁氧体法、电解法、蒸发浓缩法、离子交换树脂法等，但这些方法大多存在投资大、运行成本高、操作管理麻烦、并且会产生二次污染和不能很好地解决水资源再利用等问题。而生物质吸附剂具有吸附量大、吸附速度快、成本低、操作简单、不产生二次污染等优点，越来越受到人们的青睐。作为一种富含纤维素和木质素的天然高分子材料，秸秆来源十分广泛，将秸秆材料应用于水处理中，制备高效环保的水处理剂无疑极具经济和社会价值。
本公司于2013年9月2日申请了一项发明专利CN201310391613.8，依次通过秸秆原材料发酵预处理、阳离子型改性处理、阴离子型改性处理、碱化和交联制备等工艺步骤的特殊设计和相关参数的特殊优化，制备了一种吸附量大、吸附速度快、工艺流程成本低、工艺操作简单、适合工业化生产且不产生二次污染的胺化增强改性秸秆吸附材料。
发明内容
本发明在此基础上，结合氧化石墨烯和海藻酸盐，制备了一种复合吸附材料，提供一种胺化增强改性秸秆基复合材料及其制备方法。
本发明通过下述技术方案予以实现：以重量计，将80-90份的胺化增强改性秸秆、1-10份的氧化石墨烯、1-10份的海藻酸盐缓慢加入到浴比1:10-20的去离子水中，超声处理1-24h，再经钙离子交联、冷冻干燥制得胺化增强改性秸秆/氧化石墨烯/海藻酸盐复合材料。
作为优选方案，所述的胺化增强改性秸秆为秸秆原材料依次经过阳离子改性、阴离子改性、碱化和交联处理制备得到。详细制备方法参见中国发明专利CN201310391613.8。
作为优选方案，所述的海藻酸盐为海藻酸钠、海藻酸钙、海藻酸钾、海藻酸铵中的一种或多种。
作为优选方案，钙离子交联的步骤为：向共混溶液中加入浓度为1-5wt%的氯化钙溶液，混合搅拌后，向复合溶液中滴加1mol/L醋酸溶液，醋酸溶液与混合溶液的体积比为1:1-1:10，搅拌30-120min后，转入模具静置交联1-48h，用蒸馏水反复清洗，所述的氯化钙为海藻酸盐质量的10%-20%。
作为优选方案，冷冻干燥工艺条件为：在-50℃～-20℃的温度条件下以速度为1℃/min升温至室温，再干燥处理1-24h。
本发明的原理为：秸秆的纤维素和半纤维素被木质素包裹，且高分子链间通过氢键作用紧密结合，结晶程度较高，因此秸秆材料通常具有水溶性差，反应活性差等不足之处。将秸秆纤维素经阳离子改性、阴离子改性、碱化和交联处理后，可以破坏原有的有序结构，引进了阴离子基团、阳离子基团和氨基，提高了反应性。氧化石墨烯是石墨烯的派生物，与石墨烯的结构大体相同，其基面及边缘含有大量羟基、羧基、羰基等功能性基团。海藻酸盐是一种多糖化合物，表面富含活性基团。因而三者可以通过共价键、静电引力、氢键等相互作用力产生紧密结合，形成复合材料。对水体中的杂质、印染废水、带有正电荷或负电荷的污染物、重金属离子等均具有良好的吸附效果，污水处理适用范围广。
本发明具有如下有益效果：（1）本发明所用材料均为天然物质，来源丰富、价格低廉、绿色环保。（2）复合材料具有机械性能好、组织结构规整、孔隙率高、吸附量大、吸附速度快、适用范围广等优点，同时易于解吸，可重复利用。（3）制备的复合材料的吸附稳定性、耐热性、耐热水性、均匀性和持久性都有很大的提高。
具体实施方式
下面结合具体实施方式，进一步阐述本发明。
实施例1：
将0.85g胺化增强改性秸秆、0.05g氧化石墨烯、0.1g的海藻酸钠缓慢加入到10ml的去离子水中，超声处理1h，加入0.2ml的5wt%的氯化钙溶液，混合搅拌后，向复合溶液中滴加5ml的1mmol/ml醋酸溶液，搅拌30min后，转入模具静置交联12h，用蒸馏水反复清洗。在-50℃的温度条件下以速度为1℃/min升温至室温，再干燥处理12h制得胺化增强改性秸秆/氧化石墨烯/环糊精复合材料
实施例2：
将0.9g胺化增强改性秸秆、0.05g氧化石墨烯、0.05g的海藻酸钙缓慢加入到浴比20ml的去离子水中，超声处理24h，加入0.5ml的2wt%的氯化钙溶液，混合搅拌后，向复合溶液中滴加10ml的1mmol/ml醋酸溶液，搅拌60min后，转入模具静置交联24h，用蒸馏水反复清洗。在-30℃的温度条件下以速度为1℃/min升温至室温，再干燥处理10h制得胺化增强改性秸秆/氧化石墨烯/环糊精复合材料。
实施例3：
将0.8g胺化增强改性秸秆、0.1g氧化石墨烯、0.1g的海藻酸钾缓慢加入到浴比15ml的去离子水中，超声处理4h，加入2ml的1wt%的氯化钙溶液，混合搅拌后，向复合溶液中滴加8ml的1mmol/ml醋酸溶液，搅拌120min后，转入模具静置交联48h，用蒸馏水反复清洗。在-20℃的温度条件下以速度为1℃/min升温至室温，再干燥处理24h制得胺化增强改性秸秆/氧化石墨烯/环糊精复合材料。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无法对所有的实施方式予以穷举。凡是属于本发明的技术方案所引申出的显而易见的变化或变动仍处于本发明的保护范围之列。
Claims (7)
1. 一种胺化增强改性秸秆基复合材料及其制备方法，其特征在于，以重量计，将80-90份的胺化增强改性秸秆、1-10份的氧化石墨烯、1-10份的海藻酸盐缓慢加入到浴比1:10-20的去离子水中，超声处理一段时间，再经钙离子交联、冷冻干燥制得胺化增强改性秸秆/氧化石墨烯/海藻酸盐复合材料。
2.根据权利要求1所述的一种胺化增强改性秸秆基复合材料及其制备方法，其特征在于，所述的胺化增强改性秸秆为秸秆原材料依次经过阳离子改性、阴离子改性、碱化和交联处理制备得到。
3.根据权利要求1所述的一种胺化增强改性秸秆基复合材料及其制备方法，其特征在于，所述的海藻酸盐为海藻酸钠、海藻酸钙、海藻酸钾、海藻酸铵中的一种或多种。
4.根据权利要求1所述的一种胺化增强改性秸秆基复合材料及其制备方法，其特征在于，超声处理的时间为1-24h。
5.根据权利要求1所述的一种胺化增强改性秸秆基复合材料及其制备方法，其特征在于，钙离子交联的步骤为：向共混溶液中加入浓度为1-5wt%的氯化钙溶液，混合搅拌后，向复合溶液中滴加1mol/L醋酸溶液，酸溶液与混合溶液的体积比为1:1-1:10，搅拌30-120min后，转入模具静置交联1-48h，用蒸馏水反复清洗。
6.根据权利要求1或5所述的一种胺化增强改性秸秆基复合材料及其制备方法，其特征在于，所述的氯化钙为海藻酸盐质量的10%-20%。
7.根据权利要求1所述的一种胺化增强改性秸秆基复合材料及其制备方法，其特征在于，冷冻干燥工艺条件为：在-50℃～-20℃的温度条件下以速度为1℃/min升温至室温，再干燥处理1-24h。
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