CN115569640B - 一种煤化工废水中苯酚吸附处理剂的制备方法 - Google Patents
一种煤化工废水中苯酚吸附处理剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种煤化工废水中苯酚和氯离子的吸附处理剂制备方法，以苯酚为模板分子，丙烯酰胺（AM）为功能单体，乙二醇二甲基丙烯酸酯（EGDMA）为交联剂，偶氮二异丁腈为引发剂，引入改性聚乳酸（MPLA）及Zn/Al水滑石，用沉淀聚合法得到苯酚分子印迹聚合物微球（MIPs）。实验选择配方（质量比）为苯酚：AM：MPLA：EGDMA：AIBN：Zn/Al水滑石=（2~5）：（8~10）：（7~10）：（70~75）：（0.2~0.5）：（5~8），在60℃下聚合制备MIPs。吸附实验表明，MIPs对苯酚的吸附量为30.53 mg/g，在模拟煤化工废水中对苯酚的去除率可达99.92%。本发明制备的印迹聚合物微球在煤化工废水中可有效识别吸附苯酚污染物及痕量氯离子污染物。高分子吸附剂合成条件温和，产率高；吸附剂可循环使用减轻处理成本。
Description
技术领域
本发明属于煤化工水处理技术领域，特别提供煤化工废水预处理后苯酚及氯离子的吸附材料。
背景技术
煤化工废水中污染物种类繁多、浓度高且难降解，传统煤化工废水处理工艺的出水难以达到国家排放标准。在不同的煤化工废水中，氯离子含量高达100mg/L～1000mg/L，苯酚含量高达600mg/L～7500mg/L。苯酚是一种致癌物质，其毒性高、溶解性好、稳定性高且生物降解性低，已被宣布为最危险的水污染物之一，即使浓度很低，也会损伤人类和动物的皮肤及其他组织健康。如进入人体，还会损伤神经系统、造成肝脏及肾脏损伤、引起头痛等危害。氯离子是废水中常见的腐蚀性离子，对金属表面的氧化膜具有穿透性和破坏性，易对管道造成腐蚀伤害，如处理不干净排入水体，还会污染饮用水、造成土壤盐碱化、危害植物生长和人体健康。
煤化工废水经预处理后仍会存在苯酚及氯离子等污染物，这些污染物的存在会影响后续生化处理的效果。吸附法由于其高效的污染物吸附处理能力，已被广泛应用于煤化工废水中苯酚的吸附去除。吸附法对吸附剂的要求较高，尽管许多吸附剂具有吸附效果好或经济适用等优点，但具有吸附能力强且可再生的吸附材料通常价格比较昂贵，而价格较低的吸附材料容易对环境产生污染。王爱国发明一种负载微生物的多孔性海绵状复合材料，该材料可对苯酚进行吸附和降解，延长了使用寿命且避免了二次污染，但材料不可再生。因此寻找经济高效且具有再生性能的吸附剂用于吸附残余苯酚及氯离子污染物，使后续生化处理有效进行，对环境保护来说至关重要。本研究重点针对煤化工废水中的苯酚及氯离子污染物，制备一种吸附能力强、经济适用、可再生且能循环利用的绿色环保性吸附材料。
聚乳酸作为一种无毒、可再生的环境友好型可生物降解塑料，具有良好的生物相容性、生物降解性、无毒和可再生性，但也存在亲水性差等缺点，影响其在水处理领域的应用。为了改进PLA的亲水性能，先对其进行功能化改性，再针对煤化工废水制备吸附型功能微球，旨在开发环境友好型的多功能吸附微球材料。
发明内容
本发明的目的在于提供一种可综合吸附煤化工废水中苯酚及氯离子污染的绿色环保吸附材料。
为实现上述目的，本发明技术方案如下：
称取一定量的模板分子苯酚、MPLA和功能单体AM溶于乙腈溶液中，超声振荡使其完全溶解，5℃下预聚合10h。将上述溶液加入三口烧瓶中，并加入Zn/Al水滑石使其分散在溶液中，放入恒温磁力搅拌器中在50℃～80℃下搅拌并通氮除氧。将交联剂EGDMA和引发剂AIBN溶于乙腈溶液中，转移至恒压滴液漏斗后，在氮气保护下滴加溶解完全后密封三口烧瓶，在50℃～80℃恒温下搅拌引发聚合反应12h。聚合反应形成固体微球，将微球放入索氏提取器中，用甲醇和乙酸体积比为9：1的混合洗脱液在索氏提取器中除去模板分子，每隔4h换一次洗脱液，至洗脱液中检测不到苯酚，再用甲醇洗脱后，放入恒温干燥箱中烘干即获得苯酚分子印迹聚合物微球(MIPs)。
与现有技术相比，本发明具有下列特点和有益效果：
1.本发明中的MPLA是具有良好亲水性能及生物相容性能的绿色高分子聚酯，将其引入分子印迹聚合物微球中，可获得优异的综合性能。
2.本发明的MIPs对煤化工废水中的苯酚有良好的吸附去除效果，同时MIPs中含有Zn/Al水滑石，可同时吸附脱除预处理后煤化工废水中的苯酚及氯离子污染物。
3.本发明的MIPs对苯酚具有特异性识别及吸附作用，且作为可重复利用的吸附材料，在重复使用6次后，对苯酚仍有较好的吸附能力。
4.本发明的MIPs制备方法简单，高效且经济环保，在煤化工废水处理领域具有广阔的应用前景。
附图说明
图1为本发明的MIPs的反应方程式图；
图2为本发明的MIPs的红外光谱图；
图3为本发明的MIPs的扫描电镜图；
图4为本发明的MIPs的吸附再生实验图；
图5为本发明的Zn/Al水滑石用量对MIPs吸附影响效果图；
图6为本发明的MIPs对模拟废水中苯酚的吸附效果图。
图7为本发明的MIPs、NIPs的动力学吸附曲线。
具体实施方式
实施例1
实验选择配方为苯酚：AM：MPLA：EGDMA：AIBN：Zn/Al水滑石＝2：9：8.8：75：0.2：5，在50℃下聚合制备MIPs。考察该工艺制备MIPs对苯酚的吸附效果，称量6mg该MIPs，分别加入20mL浓度为30mg/L的苯酚水溶液中，超声混合均匀，放在振荡器上，在20℃的条件下振荡240min，取上清液测量其吸光度A，苯酚平衡吸附量(Q，mg/g)根据下公式计算得到：
式中：Q为MIPs对苯酚的吸附量(mg/g)；C0为溶液中苯酚初始质量浓度(mg/L)；Ce为吸附平衡时苯酚的质量浓度(mg/L)；V为苯酚溶液的体积(mL)；m为MIPs的质量(mg)。
通过该工艺制备的MIPs在苯酚水溶液中对苯酚的吸附量为28.26mg/g。
实施例2
实验选择配方为苯酚：AM：MPLA：EGDMA：AIBN：Zn/Al水滑石＝3：10：7：74.70：0.3：5，在80℃下聚合制备MIPs。使用实施例1的方法考察该工艺制备MIPs对苯酚的吸附效果，结果表明通过该工艺制备的MIPs在苯酚水溶液中对苯酚的吸附量为28.31mg/g。
实施例3
实验选择配方为苯酚：AM：MPLA：EGDMA：AIBN：Zn/Al水滑石＝5：9：7.5：70：0.5：8，在60℃下聚合制备MIPs。使用实施例1的方法考察该工艺制备MIPs对苯酚的吸附效果，结果表明通过该工艺制备的MIPs在苯酚水溶液中对苯酚的吸附量为30.53mg/g。
实施例4
模拟预处理后的煤化工废水，配制苯酚含量为300mg/L的水溶液。称取0.5g按照实施例3制备的MIPs，放入100mL模拟废水溶液中，在20℃条件下振荡吸附，分别测量在不同时间内，MIPs对废水中苯酚的吸附量。
吸附结果如图5所示，MIPs对苯酚的吸附量随着时间的增加而增加，在240min时，吸附量基本达到饱和，此时MIPs对苯酚的去除率为50.9％。由于废水中还存在大量苯酚，故将废水溶液中的MIPs取出，放入甲醇和乙酸体积比为9：1的混合洗脱液中，在索氏提取器中去除苯酚后，对模拟水溶液继续二次吸附处理，二次吸附中MIPs对苯酚的吸附量随着时间的增加而增加，在360min时，对苯酚的去除率达到99.92％，此时废水溶液中苯酚含量为0.24mg/L，低于国家规定的工业废水苯酚排放标准。故MIPs对煤化工废水中的苯酚具有量好的去除效果。
本发明未尽事宜为公知技术。
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。
Claims (8)
1.一种处理煤化工废水中苯酚和氯离子的吸附剂，其特征在于，所述吸附剂的制备方法，包括以下步骤：
(1)称取90～100mg的苯酚、0.3～0.4g改性聚乳酸MPLA、20～25g丙烯酰胺AM溶于乙腈溶液中，超声振荡使其完全溶解，3-7℃下预聚合8-10h；
(2)加入0.3～0.4gZn/Al水滑石使其分散在溶液中，放入恒温磁力搅拌器中在一定温度下搅拌，通入氮气除氧，恒温水浴；
(3)称取15～20mg引发剂偶氮二异丁腈和2.8～3.2g交联剂乙二醇二甲基丙烯酸酯溶解在乙腈中，30min内匀速滴加完成，高速搅拌至各组分混合均匀，继续通氮除氧，旋紧瓶塞，开始共聚反应；
(4)恒温反应10～12h，待反应结束，用甲醇和乙酸体积比9：1的混合洗脱液在索氏提取器中除去模板分子，每隔4h换一次洗脱液，至洗脱液中检测不到苯酚；
(5)再用甲醇洗脱后，放入真空干燥箱内烘干即获得苯酚分子印迹聚合物微球MIPs；
所述改性聚乳酸MPLA的制备方法为先对高分子PLA进行醇解处理，以获得反应活性高且带有双端羟基的PLA-diol，再使用马来酸酐MAH对PLA-diol进行接枝改性得到亲水性能良好的MPLA。
2.按照权利要求1所述的处理煤化工废水中苯酚和氯离子的吸附剂，其特征在于：所述改性聚乳酸MPLA醇解时间为1h，醇解产物分子量为7.3×103。
3.按照权利要求1所述的处理煤化工废水中苯酚和氯离子的吸附剂，其特征在于：苯酚、丙烯酰胺AM和改性聚乳酸MPLA溶于乙腈溶液中，其中苯酚占反应总单体质量分数为2～3％，AM占比为9～10％，MPLA为7～8％，超声振荡使其完全溶解，5℃下预聚合10h。
4.按照权利要求1所述的处理煤化工废水中苯酚和氯离子的吸附剂，其特征在于：交联剂乙二醇二甲基丙烯酸酯和引发剂偶氮二异丁腈溶解在乙腈溶液中，在氮气保护下用恒压滴液漏斗逐滴滴加。
5.按照权利要求1所述的处理煤化工废水中苯酚和氯离子的吸附剂，其特征在于：步骤(2)中恒温水浴温度为50℃～80℃。
6.按照权利要求1所述的处理煤化工废水中苯酚和氯离子的吸附剂，其特征在于：所述Zn/Al水滑石为采取共沉淀法制备的Zn：Al＝2：1的水滑石，占反应总单体质量分数为5％～6％。
7.按照权利要求1所述的处理煤化工废水中苯酚和氯离子的吸附剂，其特征在于：步骤(2)中加入的Zn/Al水滑石在温度为20℃下，Cl-浓度为100mg/L的环境中对Cl-的去除率可达到35％，在500mg/L的Cl-环境中对Cl-的去除率可达到20％。
8.按照权利要求1所述的处理煤化工废水中苯酚和氯离子的吸附剂，其特征在于：该MIPs在50min左右达到吸附平衡；MIPs对苯酚的吸附过程符合准二级动力学方程，印迹聚合物在重复使用6次后，对苯酚仍有较好的吸附能力。
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