CN105347437B - 一种用于废水处理改性淀粉的制备方法 - Google Patents
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Abstract
本发明公开了一种用于废水处理改性淀粉的制备方法，属于淀粉领域。提供了一种改性淀粉作为天然高分子碳水化合物改性而得的水处理剂，本发明通过马铃薯淀粉用氢氧化钾/尿素的混合溶液、磷酸氧二钠‑柠檬酸缓冲液、交联剂、二硫化碳等对其进行改性制得改性淀粉，用二硫化碳作用于淀粉，易于沉淀，具有置换金属离子的效能，可用于除去工业废水中的铜、铬、锌以及其他许多重金属离子，既可回收重金属，又对环境无毒无害，不会对环境造成二次污染。
Description
技术领域
本发明公开了一种用于废水处理改性淀粉的制备方法，属于淀粉领域。
背景技术
皮革、电镀、采矿和冶金等行业都排放大量含重金属离子的废水，尤其是含铬离子的废水。含重金属的废水污染环境，破坏生态平衡，影响动植物生长，严重危害人类健康。随着工业的发展，从工业废水中流失的重金属越来越多，造成了资
源的极大浪费。另一方面，随着对重金属毒理学的深入研究及检测技术的发展，重金属废物的处理标准也日益趋向严格。因此，国内外学者都在积极探索和研究一种高效的重金属离子脱除方法。
人工合成的有机和无机水处理剂日益显出其致命弱点，它们大多数或呈微毒，会通过食物链进入人体，影响人体健康。或处理残渣会对环境造成二次污染。例如：聚丙烯酞胺可能会产生微毒致癌物，聚合氛化铝残留铝离子会致人衰老，而金属矿物水处理剂吸附重金属后其污泥即成为难以处理的二次污染源,继续进入生物链，危害健康。而改性淀粉作为天然高分子碳水化合物改性而得的水处理剂，在这方面显现出不可比拟的优点，它对环境无毒无害，且其处理残渣易被微生物降解。因此，不会对环境造成二次污染。被改性淀粉絮凝或吸附的污染物比较容易回收利用。在残渣无污染的前提下，可直接作农肥，或在堆肥的过程中自然降解。对有毒的如吸附重金属的沉渣，可通过高温碳化或化学方法减量。
改性淀粉是淀粉先经交联后再在碱性条件下进行黄原酸化而制得的一种淀粉衍生物，具有与多种重金属离子牢固结合的能力，是一种性能优良的离子交换絮凝剂。黄原酸酯法处理电镀废水具有药剂制备简单、成本低廉、脱除效果显著的特点，处理后的废水无色透明，符合国家工业废水排放标准，可作工业循环水利用，同时产生的污泥化学性质稳定，不会造成二次污染。
发明内容
本发明主要解决的技术问题：针对目前人工合成的有机和无机水处理剂它们大多数呈微毒，会通过食物链进入人体，影响人体健康，或处理残渣会对环境造成二次污染的问题，提供了一种改性淀粉作为天然高分子碳水化合物改性而得的水处理剂，本发明通过马铃薯淀粉用氢氧化钾/尿素的混合溶液、磷酸氧二钠-柠檬酸缓冲液、交联剂、二硫化碳等对其进行改性制得改性淀粉，用二硫化碳作用于淀粉，易于沉淀，具有置换金属离子的效能，可用于除去工业废水中的铜、铬、锌以及其他许多重金属离子，既可回收重金属，又对环境无毒无害，不会对环境造成二次污染。
为了解决上述技术问题，本发明所采用的技术方案是：
（1）在500mL的烧杯中加入60～70g氢氧化钾和40～50g尿素，向其中加入250～300mL的去离子水，搅拌至固体完全溶解，配制成氢氧化钾/尿素的混合溶液；
（2）称取100～150g的马铃薯粉末，向其中加入50～80mL去离子水，混合均匀制成淀粉乳，将其放入500mL的三口烧瓶中，放入60～70℃的水浴锅中，向瓶中加入上述制得的混合溶液，用磁力搅拌器用200～250r/min转速下搅拌，搅拌至均匀的淀粉糊，之后再向瓶中滴加质量分数6%的盐酸调节pH为7，继续搅拌20～30min后将反应物取出用蒸馏水清洗2～3次，清洗后再用无水乙醇洗涤2～3次，放置在50～60℃的烘箱中进行干燥1～2h；
（3）取60～80g上述干燥的固体于500mL的反应瓶中，向其中加入100～120mLpH值为6.0～6.5的磷酸氧二钠-柠檬酸缓冲液，放在50～55℃的水浴中搅拌20～30min，混合均匀后将其放入微波炉中，在200～300W微波功率下加热反应10～15min，每隔3min将产品拿出搅拌均匀，加热结束后冷却至室温，将反应物取出用质量分数85%的乙醇溶液进行冲洗2～3次，之后放在50～60℃烘箱中干燥50～60min；
（4）取上述40～50g烘干后固体加入到20～30mL质量分数30%的氢氧化钠溶液中，配成淀粉碱性乳液，将其放置在60～70℃的恒温水浴中加热，用注射器吸取4～5mL环氧氯丙烷逐渐滴入淀粉乳中，在3～5min内完成滴加，保持水浴温度搅拌30～40min，之后加入5～8mL二硫化碳，搅拌反应20～30min，再加入25～30mL质量浓度为0.3g/mL硫酸镁溶液，再继续反应10～15 min，反应结束后，将反应物取出，用蒸馏水冲洗2～3次，之后抽滤，将滤渣用丙酮洗涤2～3次，将滤饼放入50～60℃的干燥箱中干燥，取出粉碎、过筛得100～120目的粉末，即得改性淀粉。
本发明的应用方法：将本发明制备出的改性淀粉，对含铬重金属离子废水进行处理，取3～5g改性淀粉加入到2～3L的废水中，先测得废水中含铬量80～200mg/L为静置3～5min后，过滤，测得废水中的含铬量5～10mg/L，去除率为95%以上。
本发明的有益效果是：
（1)本发明通过马铃薯淀粉用氢氧化钾/尿素的混合溶液、磷酸氧二钠-柠檬酸缓冲液、交联剂、二硫化碳等对其进行改性制得改性淀粉，用二硫化碳作用于淀粉，易于沉淀，具有置换金属离子的效能；
（2)本发明制得的改性淀粉可用于除去工业废水中的铜、铬、锌以及其他许多重金属离子，既可回收重金属，又对环境无毒无害，不会对环境造成二次污染。
具体实施方式
首先在500mL的烧杯中加入60～70g氢氧化钾和40～50g尿素，向其中加入250～300mL的去离子水，搅拌至固体完全溶解，配制成氢氧化钾/尿素的混合溶液；称取100～150g的马铃薯粉末，向其中加入50～80mL去离子水，混合均匀制成淀粉乳，将其放入500mL的三口烧瓶中，放入60～70℃的水浴锅中，向瓶中加入上述制得的混合溶液，用磁力搅拌器用200～250r/min转速下搅拌，搅拌至均匀的淀粉糊，之后再向瓶中滴加质量分数6%的盐酸调节pH为7，继续搅拌20～30min后将反应物取出用蒸馏水清洗2～3次，清洗后再用无水乙醇洗涤2～3次，放置在50～60℃的烘箱中进行干燥1～2h；取60～80g干燥的固体于500mL的反应瓶中，向其中加入100～120mLpH值为6.0～6.5的磷酸氧二钠-柠檬酸缓冲液，放在50～55℃的水浴中搅拌20～30min，混合均匀后将其放入微波炉中，在200～300W微波功率下加热反应10～15min，每隔3min将产品拿出搅拌均匀，加热结束后冷却至室温，将反应物取出用质量分数85%的乙醇溶液进行冲洗2～3次，之后放在50～60℃烘箱中干燥50～60min；取40～50g烘干后固体加入到20～30mL质量分数30%的氢氧化钠溶液中，配成淀粉碱性乳液，将其放置在60～70℃的恒温水浴中加热，用注射器吸取4～5mL环氧氯丙烷逐渐滴入淀粉乳中，在3～5min内完成滴加，保持水浴温度搅拌30～40min，之后加入5～8mL二硫化碳，搅拌反应20～30min，再加入25～30mL质量浓度为0.3g/mL硫酸镁溶液，再继续反应10～15 min，反应结束后，将反应物取出，用蒸馏水冲洗2～3次，之后抽滤，将滤渣用丙酮洗涤2～3次，将滤饼放入50～60℃的干燥箱中干燥，取出粉碎、过筛得100～120目的粉末，即得改性淀粉。
实例1
首先在500mL的烧杯中加入60g氢氧化钾和40g尿素，向其中加入250mL的去离子水，搅拌至固体完全溶解，配制成氢氧化钾/尿素的混合溶液；称取100g的马铃薯粉末，向其中加入50mL去离子水，混合均匀制成淀粉乳，将其放入500mL的三口烧瓶中，放入60℃的水浴锅中，向瓶中加入上述制得的混合溶液，用磁力搅拌器用200r/min转速下搅拌，搅拌至均匀的淀粉糊，之后再向瓶中滴加质量分数6%的盐酸调节pH为7，继续搅拌20min后将反应物取出用蒸馏水清洗2次，清洗后再用无水乙醇洗涤2次，放置在50℃的烘箱中进行干燥1h；取60g干燥的固体于500mL的反应瓶中，向其中加入100mLpH值为6.0的磷酸氧二钠-柠檬酸缓冲液，放在50℃的水浴中搅拌20min，混合均匀后将其放入微波炉中，在200W微波功率下加热反应10min，每隔3min将产品拿出搅拌均匀，加热结束后冷却至室温，将反应物取出用质量分数85%的乙醇溶液进行冲洗2次，之后放在50℃烘箱中干燥50min；取40g烘干后固体加入到20mL质量分数30%的氢氧化钠溶液中，配成淀粉碱性乳液，将其放置在60℃的恒温水浴中加热，用注射器吸取4mL环氧氯丙烷逐渐滴入淀粉乳中，在3min内完成滴加，保持水浴温度搅拌30min，之后加入5mL二硫化碳，搅拌反应20min，再加入25mL质量浓度为0.3g/mL硫酸镁溶液，再继续反应10min，反应结束后，将反应物取出，用蒸馏水冲洗2次，之后抽滤，将滤渣用丙酮洗涤2次，将滤饼放入50℃的干燥箱中干燥，取出粉碎、过筛得100目的粉末，即得改性淀粉。
将本发明制备出的改性淀粉，对含铬重金属离子废水进行处理，取3g改性淀粉加入到2L的废水中，先测得废水中含铬量80mg/L为静置3min后，过滤，测得废水中的含铬量5mg/L，去除率为93.8%。
实例2
首先在500mL的烧杯中加入65g氢氧化钾和45g尿素，向其中加入275mL的去离子水，搅拌至固体完全溶解，配制成氢氧化钾/尿素的混合溶液；称取125g的马铃薯粉末，向其中加入75mL去离子水，混合均匀制成淀粉乳，将其放入500mL的三口烧瓶中，放入65℃的水浴锅中，向瓶中加入上述制得的混合溶液，用磁力搅拌器用225r/min转速下搅拌，搅拌至均匀的淀粉糊，之后再向瓶中滴加质量分数6%的盐酸调节pH为7，继续搅拌25min后将反应物取出用蒸馏水清洗2次，清洗后再用无水乙醇洗涤2次，放置在55℃的烘箱中进行干燥1.5h；取70g干燥的固体于500mL的反应瓶中，向其中加入110mLpH值为6.3的磷酸氧二钠-柠檬酸缓冲液，放在53℃的水浴中搅拌25min，混合均匀后将其放入微波炉中，在250W微波功率下加热反应13min，每隔3min将产品拿出搅拌均匀，加热结束后冷却至室温，将反应物取出用质量分数85%的乙醇溶液进行冲洗2次，之后放在55℃烘箱中干燥55min；取45g烘干后固体加入到25mL质量分数30%的氢氧化钠溶液中，配成淀粉碱性乳液，将其放置在65℃的恒温水浴中加热，用注射器吸取4.5mL环氧氯丙烷逐渐滴入淀粉乳中，在4min内完成滴加，保持水浴温度搅拌35min，之后加入5～8mL二硫化碳，搅拌反应25min，再加入27mL质量浓度为0.3g/mL硫酸镁溶液，再继续反应13min，反应结束后，将反应物取出，用蒸馏水冲洗2次，之后抽滤，将滤渣用丙酮洗涤2次，将滤饼放入55℃的干燥箱中干燥，取出粉碎、过筛得110目的粉末，即得改性淀粉。
将本发明制备出的改性淀粉，对含铬重金属离子废水进行处理，取4g改性淀粉加入到2.5L的废水中，先测得废水中含铬量150mg/L为静置4min后，过滤，测得废水中的含铬量8mg/L，去除率为94.7%。
实例3
首先在500mL的烧杯中加入70g氢氧化钾和50g尿素，向其中加入300mL的去离子水，搅拌至固体完全溶解，配制成氢氧化钾/尿素的混合溶液；称取150g的马铃薯粉末，向其中加入80mL去离子水，混合均匀制成淀粉乳，将其放入500mL的三口烧瓶中，放入70℃的水浴锅中，向瓶中加入上述制得的混合溶液，用磁力搅拌器用250r/min转速下搅拌，搅拌至均匀的淀粉糊，之后再向瓶中滴加质量分数6%的盐酸调节pH为7，继续搅拌30min后将反应物取出用蒸馏水清洗3次，清洗后再用无水乙醇洗涤3次，放置在60℃的烘箱中进行干燥2h；取80g干燥的固体于500mL的反应瓶中，向其中加入120mLpH值为6.5的磷酸氧二钠-柠檬酸缓冲液，放在55℃的水浴中搅拌30min，混合均匀后将其放入微波炉中，在300W微波功率下加热反应15min，每隔3min将产品拿出搅拌均匀，加热结束后冷却至室温，将反应物取出用质量分数85%的乙醇溶液进行冲洗3次，之后放在60℃烘箱中干燥60min；取50g烘干后固体加入到30mL质量分数30%的氢氧化钠溶液中，配成淀粉碱性乳液，将其放置在70℃的恒温水浴中加热，用注射器吸取5mL环氧氯丙烷逐渐滴入淀粉乳中，在5min内完成滴加，保持水浴温度搅拌40min，之后加入8mL二硫化碳，搅拌反应30min，再加入30mL质量浓度为0.3g/mL硫酸镁溶液，再继续反应15 min，反应结束后，将反应物取出，用蒸馏水冲洗3次，之后抽滤，将滤渣用丙酮洗涤3次，将滤饼放入60℃的干燥箱中干燥，取出粉碎、过筛得120目的粉末，即得改性淀粉。
将本发明制备出的改性淀粉，对含铬重金属离子废水进行处理，取5g改性淀粉加入到3L的废水中，先测得废水中含铬量200mg/L为静置35min后，过滤，测得废水中的含铬量10mg/L，去除率为95%。
Claims (1)
1.一种用于废水处理改性淀粉的制备方法，其特征在于改性淀粉具体制备步骤
为：
（1）在500mL的烧杯中加入60～70g氢氧化钾和40～50g尿素，向其中加入250～300mL的去离子水，搅拌至固体完全溶解，配制成氢氧化钾/尿素的混合溶液；
（2）称取100～150g的马铃薯粉末，向其中加入50～80mL去离子水，混合均匀制成淀粉乳，将其放入500mL的三口烧瓶中，放入60～70℃的水浴锅中，向瓶中加入上述制得的混合溶液，用磁力搅拌器用200～250r/min转速下搅拌，搅拌至均匀的淀粉糊，之后再向瓶中滴加质量分数6%的盐酸调节pH为7，继续搅拌20～30min后将反应物取出用蒸馏水清洗2～3次，清洗后再用无水乙醇洗涤2～3次，放置在50～60℃的烘箱中进行干燥1～2h；
（3）取60～80g上述干燥的固体于500mL的反应瓶中，向其中加入100～120mLpH值为6.0～6.5的磷酸氧二钠-柠檬酸缓冲液，放在50～55℃的水浴中搅拌20～30min，混合均匀后将其放入微波炉中，在200～300W微波功率下加热反应10～15min，每隔3min将产品拿出搅拌均匀，加热结束后冷却至室温，将反应物取出用质量分数85%的乙醇溶液进行冲洗2～3次，之后放在50～60℃烘箱中干燥50～60min；
（4）取上述40～50g烘干后固体加入到20～30mL质量分数30%的氢氧化钠溶液中，配成淀粉碱性乳液，将其放置在60～70℃的恒温水浴中加热，用注射器吸取4～5mL环氧氯丙烷逐渐滴入淀粉乳中，在3～5min内完成滴加，保持水浴温度搅拌30～40min，之后加入5～8mL二硫化碳，搅拌反应20～30min，再加入25～30mL质量浓度为0.3g/mL硫酸镁溶液，再继续反应10～15 min，反应结束后，将反应物取出，用蒸馏水冲洗2～3次，之后抽滤，将滤渣用丙酮洗涤2～3次，将滤饼放入50～60℃的干燥箱中干燥，取出粉碎、过筛得100～120目的粉末，即得改性淀粉。
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Effective date of registration: 20171110 Address after: Weiyi Chemical Industrial Park in Lianyungang city of Lianyungang province Jiangsu 222000 Applicant after: Lianyungang Shijie agrochemical Co. Ltd. Address before: 100086 Beijing city Haidian District North Sanhuan Road 43, Tsing Wun contemporary building 12A11 Applicant before: BEIJING ZHITAO SCIENCE & TECHNOLOGY CO., LTD. |
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Effective date of registration: 20190202 Address after: 750300 Bayin Aobao Industrial Park, Alxa League Economic and Technological Development Zone, Inner Mongolia Autonomous Region Patentee after: Inner Mongolia Shijie Chemical Co., Ltd. Address before: 222000 Weiyi Road, Lianyungang Chemical Industry Park, Lianyungang City, Jiangsu Province Patentee before: Lianyungang Shijie agrochemical Co. Ltd. |