CN112745854B - 一种土壤修复剂 - Google Patents
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Abstract
本发明涉及一种土壤修复剂，其制备方法包括如下步骤：称取SnCl2·2H2O与Na2WO4·2H2O、Nd盐溶解于去离子水中，搅拌至溶解完全，滴入柠檬酸钠溶液，将该反应液置于80‑120℃下的水浴中反应1‑5h，反应结束后将产物抽滤、洗涤、冷冻干燥；将六水合氯化铁和四水合氯化亚铁加水配制成混合溶液，滴加氨水和聚乙二醇水溶液在130‑200℃水浴条件反应，反应过程中持续施加超声，结束后用去离子水和乙醇清洗多次，干燥，该复合材料可实现对污染土壤的高效修复。
Description
技术领域
本发明涉及土壤的原位修复，具体的说是一种用于有机物(如农药)污染和重金属污染土壤修复的磁性微球的制备方法。
背景技术
随着工业化进程的不断加快，土壤重金属污染和有机物污染日趋严重，对土壤的生态系统造成了严重的危害，同时还会通过食物链进入人体，从而对人体的身心健康造成危害。目前，土壤修复技术已取得了显著地进展，常用且有效的修复技术有3大类：化学修复法、物理修复法、生物修复法、工程修复法。在这些的修复方法中，化学固化/稳定修复技术是比较有效且经济的土壤污染修复技术。
专利号为CN 103056155的专利公开了一种低温等离子体协同光催化处理污染土壤的反应器及其处理方法，污染土壤在低温等离子体反应段先进行放电反应，进行一次降解，将从土壤中挥发出的剩余有机物引入光催化反应段进行光催化反应，缩短了土壤中有机污染物的降解时间，提高了其降解效果，但是存在异位修复土壤预处理复杂、设备成本高、耗电过多的缺点。专利CN111360059 A公开了一种有机物污染土壤原位修复方法，首先将有机物污染土壤进行简单预处理，然后将增溶剂/TiO2/CdS膨润土磁性水凝胶微球洒在土壤表层，太阳光照射下进行光催化降解有机污染物，所用的增溶剂/TiO2/CdS膨润土磁性水凝胶微球，制备简单，在外加磁场作用下即可分离回收。该土壤修复技术材料活性较低，修复效率低下。
发明内容
本发明提供了一种对环境友好的土壤修复材料及其应用。该修复材料是由Fe3O4和掺Nb的SnWO4复合，可实现对重金属以及有机污染物污染土壤的高效修复。
一种土壤修复剂，其制备方法包括如下步骤：
(1)称取SnCl2·2H2O与Na2WO4·2H2O、Nd盐溶解于去离子水中，搅拌至溶解完全，滴入柠檬酸钠溶液，将该反应液置于80-120℃下的水浴中反应1-5h，反应结束后将产物抽滤、洗涤、冷冻干燥；
(2)将六水合氯化铁和四水合氯化亚铁加水配制成混合溶液，滴加氨水和聚乙二醇，在130-200℃水浴条件反应，反应过程中持续施加超声，结束后用去离子水和乙醇清洗多次，干燥。
优选的，所述SnCl2·2H2O与Na2WO4·2H2O、Nd盐比例为1:1：(0.02-0.1)。
优选的，所述步骤(2)中的超声功率为20-100w。
优选的，所述Nd盐为Nd(NO3)3、NdCl3中的至少一种。
优选的，步骤(2)中的反应时间为1-8h。
技术效果：本申请在柠檬酸的辅助作用下，生成三维花瓣状的SnWO4，在与Fe3O4复合过程中、持续施加超声，在反应液中生成大量气泡作为模板，从而生成多孔纳米的Fe3O4；多孔纳米的Fe3O4均匀的分散于SnWO4花瓣之间，该复合材料具有较高的比表面积，能提高对土壤中污染物的吸附能力，通过对SnWO 4进行Nb掺杂，有效的提高了其光催化效率。
附图说明
图1为本申请的复合材料的SEM图；
图2为本申请的复合材料的TEM图；
具体实施方式
实施例1
称取摩尔比为1:1:0.1的SnCl2·2H2O与Na2WO4·2H2O、NdCl3溶解于100ml去离子水中，搅拌至溶解完全，滴入50mg的柠檬酸钠溶液，将该反应液置于120℃下的水浴中反应3h，反应结束后将产物抽滤、洗涤、-50℃下冷冻干燥24h；
将摩尔比为1:1.1的六水合氯化铁和四水合氯化亚铁加水配制成混合溶液，滴加氨水和聚乙二醇，在130℃水浴条件反应3h，反应过程中持续施加超声，超声功率为90w，结束后用去离子水和乙醇清洗多次，干燥。
实施例2
称取摩尔比为1:1:0.08的SnCl2·2H2O与Na2WO4·2H2O、NdCl3溶解于100ml去离子水中，搅拌至溶解完全，滴入20mg的柠檬酸钠溶液，将该反应液置于100℃下的水浴中反应5h，反应结束后将产物抽滤、洗涤、-60℃下冷冻干燥24h；
将摩尔比为1:1.05的六水合氯化铁和四水合氯化亚铁加水配制成混合溶液，滴加氨水和聚乙二醇，在130℃水浴条件反应3h，反应过程中持续施加超声，超声功率为100w，结束后用去离子水和乙醇清洗多次，干燥。
实施例3
称取摩尔比为1:1:0.08的SnCl2·2H2O与Na2WO4·2H2O、NdCl3溶解于100ml去离子水中，搅拌至溶解完全，滴入20mg的柠檬酸钠溶液，将该反应液置于100℃下的水浴中反应5h，反应结束后将产物抽滤、洗涤、-60℃下冷冻干燥24h；
将摩尔比为1:1.05的六水合氯化铁和四水合氯化亚铁加水配制成混合溶液，滴加氨水和聚乙二醇，在140℃水浴条件反应3h，反应过程中持续施加超声，超声功率为95w，结束后用去离子水和乙醇清洗多次，干燥。
检测实施例1-3材料对土壤中重金属离子的修复效果：取3份1.0kg土壤样品(Pb5mg/kg；Cd 3mg/kg)，分别加入实施例1-3的复合材料50g，混合均匀，每天翻土一次，三周后，检测土壤部分重金属含量并计算去除率。
| Pb | Cd | |
| 实施例1 | 75％ | 73％ |
| 实施例2 | 69％ | 65％ |
| 实施例3 | 71％ | 68％ |
检测实施例1-3材料对土壤中有机物的修复效果：各取3份1kg土壤(阿特拉津和多氯联苯PCB77含量均为100mg/kg)，向各3份样品中分别加入实施例1-3的复合材料20g，混合均匀，每天翻土一次，三周以后，检测土壤中农药的含量并计算去除率。
| 阿特拉津 | 多氯联苯PCB77 | |
| 实施例1 | 67％ | 72％ |
| 实施例2 | 65％ | 63％ |
| 实施例3 | 73％ | 79％ |
从以上检测来看，本申请制备的复合材料具有优异的重金属/有机污染物去除率，是一种非常有前景的土壤修复剂。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。
Claims (1)
1.一种土壤修复剂，其制备方法包括如下步骤：
(1)称取SnCl2·2H2O与Na2WO4·2H2O、Nd盐溶解于去离子水中，搅拌至溶解完全，滴入柠檬酸钠溶液，将该反应液置于80-120℃下的水浴中反应1-5h，反应结束后将产物抽滤、洗涤、冷冻干燥；
(2)将六水合氯化铁和四水合氯化亚铁加水配制成混合溶液，滴加氨水和聚乙二醇，在130-180℃水浴条件反应，反应过程中持续施加超声，结束后用去离子水和乙醇清洗多次，干燥；在柠檬酸钠的辅助作用下，生成三维花瓣状的SnWO4，在与Fe3O4 复合过程中、持续施加超声，在反应液中生成大量气泡作为模板，从而生成多孔纳米的 Fe3O4；得到复合材料为多孔纳米的Fe3O4均匀的分散于掺Nd的SnWO4三维花瓣之间；SnCl2·2H2O与Na2WO4·2H2O、Nd盐比例为1:1：(0.02-0.1)；步骤(2)中的超声功率为20-100w，所述Nd盐为Nd(NO3)3、NdCl3中的至少一种，步骤(2)中的反应时间为1-8h，步骤(1)中的冷冻干燥时间为24-48h。
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690891A (zh) * | 2009-09-25 | 2010-04-07 | 南京大学 | 一种可见光催化剂SnWO4的合成方法 |
| CN101745381A (zh) * | 2009-10-27 | 2010-06-23 | 南京大学 | 水热法合成可见光催化剂SnWO4的方法 |
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| CN109530418A (zh) * | 2018-12-31 | 2019-03-29 | 南京格洛特环境工程股份有限公司 | 重金属污染土壤修复方法 |
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| CN101690891A (zh) * | 2009-09-25 | 2010-04-07 | 南京大学 | 一种可见光催化剂SnWO4的合成方法 |
| CN101745381A (zh) * | 2009-10-27 | 2010-06-23 | 南京大学 | 水热法合成可见光催化剂SnWO4的方法 |
| CN102533716B (zh) * | 2012-01-20 | 2013-06-12 | 安徽农业大学 | 一种用于有机氯污染土壤修复的磁性纳米生物微球制备方法 |
| CN105140018A (zh) * | 2015-08-21 | 2015-12-09 | 浙江大学 | 一种磁性高分子纳米球的制备方法 |
| CN107737942A (zh) * | 2017-10-23 | 2018-02-27 | 南京工程学院 | 一种零价铁／花状氧化锌纳米复合材料及其制备方法 |
| CN109530418A (zh) * | 2018-12-31 | 2019-03-29 | 南京格洛特环境工程股份有限公司 | 重金属污染土壤修复方法 |
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