CN114797749A - 一种重金属吸附剂及其制备方法和应用 - Google Patents
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Abstract
本发明属于固体废弃物再生利用领域，特别是涉及一种重金属吸附剂及其制备方法和应用。本发明提供了一种重金属吸附剂，通过不同条件处理煤基胡敏素废渣使之克服了活性官能团少，对重金属的吸附能力较低的缺陷，使煤基胡敏素废渣具有了吸附重金属的能力。本发明提供的重金属吸附剂能够有效吸附废水中的镉离子，去除率高达86.43％。当本发明提供的重金属吸附剂应用于镉污染土壤时，不仅可以去除土壤中的镉还能够有效促进作物的生长，同时还能够降低作物的重金属镉的富集系数。
Description
技术领域
本发明属于固体废弃物再生利用领域，特别是涉及一种重金属吸附剂及其制备方法和应用。
背景技术
土壤重金属镉污染问题逐渐引起了人们的广泛关注，镉即使在相对较低的浓度下也具有很高的毒性和致畸致癌性，且由于重金属镉的持久性，很难通过食物链被降解，最终对人类健康构成威胁。如何缓解重金属镉污染，减轻对人类健康的影响，是目前研究工作者的难点问题。现阶段针对重金属镉污染修复方法较多，包括物理、化学和生物等，但在实际应用中，农田和矿山土壤重金属镉污染多采取化学吸附钝化的方法，但相关材料具有价格高昂的缺陷。
风化煤根据酸碱溶解性的不同分为棕腐酸、富里酸和胡敏素。从风化煤和褐煤中提取棕腐酸和黄腐酸的过程中产生大量腐植酸废渣(富含胡敏素)，腐植酸废渣由于官能团少、活性低等缺陷难以被利用，因此腐植酸废渣不仅造成环境污染，也会造成资源的大量浪费。如何对这部分资源进行无害化处理，实现废弃资源的利用，是现阶段的研究重点。
发明内容
为了解决上述问题，本发明提供了一种重金属吸附剂及其制备方法和应用。本发明通过不同条件处理煤基胡敏素废渣使之克服了活性官能团少，对重金属的吸附能力较低的缺陷，使之具有了吸附重金属的能力。
为了实现上述目的，本发明提供了如下技术方案：
本发明提供了一种重金属吸附剂，所述重金属吸附剂由以下原料制备得到：煤基胡敏素废渣和氢氧化钙。
优选的，所述煤基胡敏素废渣为风化煤提取棕腐酸和黄腐酸产品后所剩的废渣。
本发明还提供了上述重金属吸附剂的制备方法，所述制备方法包括以下步骤：
将煤基胡敏素废渣、氢氧化钙和水混合后进行超声处理，得到悬浮液；对悬浮液进行水热反应得到水热反应产物；过滤洗涤水热反应产物直至洗涤液为中性得到待处理产物；烘干待处理产物得到重金属吸附剂。
优选的，所述煤基胡敏素废渣和氢氧化钙的质量比为3：(1～3)。
优选的，所述超声的时间为1～3h。
优选的，所述水热反应的温度为25～85℃。
本发明还提供了上述重金属吸附剂或上述制备方法制备得到的重金属吸附剂在处理含重金属离子废水和/镉污染土壤中的应用。
优选的，所述重金属吸附剂在处理含重金属离子废水时，使用方法为：将含重金属离子废水的pH值调节为5，每30mL含重金属离子废水的重金属吸附剂投放量为为0.05g；
所述含重金属离子废水中镉离子的含量为100mg/L。
优选的，所述重金属吸附剂在处理镉污染土壤时，使用方法为：向镉污染土壤中投放镉污染土壤质量1％的重金属吸附剂；
所述镉污染土壤中镉的含量为6mg/kg。
本发明的提供的技术方案是以风化煤提取棕腐酸和黄腐酸后所剩的煤基胡敏素废渣为原料的重金属吸附剂。本发明采用超声辅助钙化水热法对煤基胡敏素废渣进行改性，以提高其吸附重金属的能力，从而制备得到一种重金属镉的环境钝化材料，从而实现煤基胡敏素废渣的“生态回归”。
本发明提供的重金属吸附剂的制备方法，是通过增加材料(即煤基胡敏素废渣)表面活性官能团的含量，进而提高其对重金属镉的吸附能力(表面络合)；同时，由于氢氧化钙(Ca(OH)2)是一种强碱，具有腐蚀性，对煤基胡敏素废渣有侵蚀溶解作用，这种作用使材料的含氧官能团的化学键断裂，使Ca2+能够成功的负载到材料表面，然后通过同晶替代的方式使Cd2+吸附到材料表面；另外，本发明提供的制备方法中使用的氢氧化钙能够水解产生OH-1，能够与Cd2+形成氢氧化物沉淀，从而达到吸附Cd2+目的。
由实施例可知，本发明提供的重金属吸附剂能够有效吸附废水中的镉离子，去除率高达86.43％。当本发明提供的重金属吸附剂应用于镉污染土壤中时，不仅可以去除土壤中的镉(土壤有效态镉降低了4.07％)还能够有效促进作物的生长(作物地上部鲜重增加16.08％，地下部鲜重增加27.37％)，同时还能够降低作物的重金属富集系数(作物地上部镉含量降低20.39％，作物地上部富集系数降低22.85％)。
附图说明
图1为不同条件下钙化改性对镉去除率的影响。
具体实施方式
下文中涉及使用的试剂或器械未注明具体技术或条件者，则按照常规试验条件进行，未明确说明有试剂公司说明书的，则按照说明书所建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规产品。
实施例1
1、重金属吸附剂的制备
将山西风化煤提取棕腐酸和黄腐酸产品后所剩的废渣(即本发明所述煤基胡敏素废渣)与氢氧化钙以3:(1～3)的质量比混合得到混合物，向混合物中加入去离子水(煤基胡敏素废渣：水＝1:20)混合后进行超声处理，得到悬浮液。超声处理的时间为1～5h，超声频率为40KHZ。
对悬浮液进行水热反应得到水热反应产物。水热反应的温度为25℃～85℃，水热反应的处理时间为10h。
过滤洗涤水热反应产物直至洗涤液为中性得到待处理产物，以35℃烘干待处理产物得到重金属吸附剂。
2、重金属吸附剂的优化
通过三因素三水平正交试验，确定煤基胡敏素废渣在钙化改性过程中的最佳投加量、水热处理的温度和超声时间。试验三因素分别为煤基胡敏素废渣与Ca(OH)2的投加比例、水热处理的温度(℃)和超声时间(h)，共10组处理，每组处理设置3个重复，具体方法如下。
CK：煤基胡敏素废渣；
处理1：煤基胡敏素废渣与Ca(OH)2的投加比例为3:1，水热温度为25℃，超声时间为1h；
处理2：煤基胡敏素废渣与Ca(OH)2的投加比例为3:1，水热温度为55℃，超声时间为3h；
处理3：煤基胡敏素废渣与Ca(OH)2的投加比例为3:1，水热温度85℃，超声时间为5h；
处理4：煤基胡敏素废渣与Ca(OH)2的投加比例为3:2，水热温度为25℃，超声时间为3h；
处理5：煤基胡敏素废渣与Ca(OH)2的投加比例为3:2，水热温度为55℃，超声时间为5h；
处理6：煤基胡敏素废渣与Ca(OH)2的投加比例为3:2，水热温度为85℃，超声时间为1h；
处理7：煤基胡敏素废渣与Ca(OH)2的投加比例为3:3，水热温度为25℃，超声时间为5h；
处理8：煤基胡敏素废渣与Ca(OH)2的投加比例为3:3，水热温度为55℃，超声时间为1h；
处理9：煤基胡敏素废渣与Ca(OH)2的投加比例为3:3，水热温度为85℃，超声时间为3h。
不同条件下钙化改性煤基胡敏素对镉吸附量的影响和极差分析如表1所示。
表1不同条件下钙化改性煤基煤基胡敏素废渣对镉吸附量的极差分析
由表1可知，通过钙基化后，处理1～9制备获得的产物对镉的吸附量均有所提高，且差异显著，可见通过Ca(OH)2改性能显著提高材料对镉的吸附能力，但不同条件下制备的材料对镉的吸附量是有差异的。通过对正交试验结果进行极差分析能够确定不同制备条件下对镉吸附的最佳配比组合。根据材料对镉吸附量的对比，由极差分析，优水平为A3B3C2，即材料和Ca(OH)2的投加配比为1:1，水热温度为85℃，超声时间为3h时，材料对镉的吸附量最强。同时由分析可知，三因素对材料吸附镉能力影响由主到次以此为：投加量>水热温度>超声时间。
3、具体试验
具体试验的环境条件为pH＝5，各组材料的投加量为0.05g，加30mL Cd浓度为100mg/L的溶液，反应时间为24h，试验进行时的环境温度为25℃，测试结果如图1所示。
由图1可知，CK对Cd的去除率为70.79％，经过上述处理钙基化后，9个处理对Cd的去除率显著提高。与CK相比，第9组处理(即材料和Ca(OH)2的投加配比为1:1，水热温度为85℃，超声时间为3h时)对镉的去除率最好，达到86.43％。
实施例2
试验于2021年8月27日至10月11日在中国矿业大学(北京)逸夫楼进行种植，盆栽土壤为制备得到的镉含量为6mg/kg的镉污染土壤。本试验共设3个处理：CK、SHM(煤基胡敏素)和Ca-SHM(钙性煤基胡敏素，即本发明实施例1处理9提供的重金属吸附剂)，按等量化(SHM和Ca-SHM分别占风干土壤质量的1％)投入原则设计试验。每个处理中氮、磷、钾肥按照尿素和磷酸二氢钾施用量分别为0.2g·kg-1和0.36g·kg-1土壤的计量折算添加，每个处理重复3次，随机区组排列。
小白菜种子于2021年9月4日播种于花盆中，出苗后一周，每盆保留长势一致的健壮苗6株。生长期间根据实际情况进行合理浇水，始终保持土壤湿润，其他日常管理按农户操作习惯进行，试验于2021年10月11日收获，小白菜收获后一次性带回实验室，用自来水冲洗干净，再用蒸馏水冲洗，后用吸水纸擦干称重，测定相关指标。检测结果如表2和表3所示。
表2钙化改性煤基胡敏素对小白菜鲜重和土壤有效态镉含量的影响
由表2可知，施用SHM能明显提高小白菜产量，与CK相比，SHM和Ca-SHM的处理中小白菜地上部鲜重分别增加了11.03％和16.08％，地下部鲜重分别增加了5.21％和27.37％，表明在镉胁迫条件下，添加钙基改性胡敏素能够促进小白菜的生长，缓解镉对小白菜生长的毒害作用。CK处理的土壤有效态镉为4.37mg/kg，与CK相比，SHM和Ca-SHM处理的土壤有效态镉分别降低了2.86％和4.07％，表明本发明提供的重金属吸附剂能够降低土壤有效态镉含量，对重金属镉的钝化起到良好的作用。
表3钙化改性煤基胡敏素对小白菜地上部镉含量、地上部镉富集系数、转运系数和抗性系数的影响
由表3可知，添加煤基胡敏素后，小白菜地上部含量显著降低(P<0.05)，与CK相比，SHM和Ca-SHM处理的小白菜地上部镉含量分别降低了9.55％和20.39％，小白菜地上部富集系数分别降低了12.55％和22.85％。钙基化处理后，Ca-SHM处理对重金属镉的转运系数为0.86小于1，可能是由于钙基化煤基胡敏素施入土壤后，对小白菜产生了影响，进而通过自身的排斥机制减少了镉的毒害。与SHM相比，钙基化后的Ca-SHM处理对Cd的抗性系数增加了8.35％，表明钙基化后，Ca-SHM处理会促进小白菜的生长。
以上所述仅是本发明的优选实施方式，应当指出，对于本发明的发明人来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (9)
1.一种重金属吸附剂，其特征在于，所述重金属吸附剂由以下原料制备得到：煤基胡敏素废渣和氢氧化钙。
2.根据权利要求1所述的重金属吸附剂，其特征在于，所述煤基胡敏素废渣为风化煤提取棕腐酸和黄腐酸产品后所剩的废渣。
3.权利要求1或2所述的重金属吸附剂的制备方法，其特征在于，所述制备方法包括以下步骤：
将煤基胡敏素废渣、氢氧化钙和水混合后进行超声处理，得到悬浮液；对悬浮液进行水热反应得到水热反应产物；过滤洗涤水热反应产物直至洗涤液为中性得到待处理产物；烘干待处理产物得到重金属吸附剂。
4.根据权利要求3所述的制备方法，其特征在于，所述煤基胡敏素废渣和氢氧化钙的质量比为3：(1～3)。
5.根据权利要求3所述的制备方法，其特征在于，所述超声的时间为1～3h。
6.根据权利要求3所述的制备方法，其特征在于，所述水热反应的温度为25～85℃。
7.权利要求1或2所述重金属吸附剂或权利要求3～6任一项所述制备方法制备得到的重金属吸附剂在处理含重金属离子废水和/或镉污染土壤中的应用。
8.根据权利要求7所述的应用，其特征在于，所述重金属吸附剂在处理含重金属离子废水时，使用方法为：将含重金属离子废水的pH值调节为5，每30mL含重金属离子废水的重金属吸附剂投放量为为0.05g；
所述含重金属离子废水中镉离子的含量为100mg/L。
9.根据权利要求7所述的应用，其特征在于，所述重金属吸附剂在处理镉污染土壤时，使用方法为：向镉污染土壤中投放镉污染土壤质量1％的重金属吸附剂；
所述镉污染土壤中镉的含量为6mg/kg。
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