CN114395396B - 一种土壤修复改良剂的制备及其应用 - Google Patents
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Abstract
本发明涉及一种土壤改良剂，其制备工艺如下：将镍盐、铁盐溶于乙二醇中，随后加入四丁基溴化铵和乙酸钠，超声混合均匀，在180‑200摄氏度条件下溶剂热反应10‑20h，得到花状的NiFe2O4；将花状的NiFe2O4采用去离子水和乙醇洗涤多次，随后将其加入去离子水中，随后加入氯化铁、聚乙二醇以及柠檬酸钠，将其混合均匀后，置于高压反应釜中，180‑200摄氏度下水热反应，得到多孔花状的NiFe2O4负载纳米Fe3O4纳米粒子的复合材料，多孔花状的NiFe2O4作为载体负载纳米Fe3O4，二者易形成异质结，促进光生电子和空穴的转移，增强材料的催化性能；本发明可用于去除土壤中的有机污染物以及重金属离子等多种物质，使用范围广。
Description
技术领域
本发明属于生态污染治理技术领域，特别涉及土壤改良剂在土壤污染治理中的应用。
背景技术
随着工业化以及农业的发展，工业化产生的重金属以及农业产生的有机污染物(如农药、抗生素)直接或间接排放到自然环境中，造成大面积环境污染，通过食物链影响动物和人类的健康。《全国土壤污染状况调查公报》显示，全国土壤环境状况总体不容乐观，部分地区土壤污染较重，土壤环境质量堪忧，工矿业废弃地土壤环境问题突出。近年来，光催化技术在土壤治理方面取得了良好的效果，而光催化技术的核心在于光催化材料，因此，开发一种高效的土壤改良光催化剂对于修复土壤具有十分重要的现实意义。
CN112238136A提供了一种重金属离子吸附材料及其在土壤污染治理中的应用，包括第一多孔衬底以及设于所述第一多孔衬底至少一个表面上的静电纺丝纤维膜，所述静电纺丝纤维膜中包含壳聚糖和/或非水溶性壳聚糖衍生物。利用壳聚糖或非水溶性壳聚糖衍生物的静电纺丝纤维膜来实现对重金属离子的吸附，同时解决吸附后的材料回收和再利用问题。
CN109499546A提供一种Fe3O4@细菌纤维素/氧化石墨烯复合气凝胶及其制备方法与应用。制备方法包括：细菌纤维素用水洗涤，氢氧化钠碱液浸泡、脱糖处理；将经榨碎处理的细菌纤维素浆体，加入经超声分散的氧化石墨烯混合液，搅拌均匀，然后超声震动混合，静置放置一段时间；加入适量的FeSO4·7H2O，FeCl3·6H2O，聚乙二醇4000和无水乙醇的混合液，在高温搅拌下，滴加适量的氨水，反应一段时间，冷冻干燥后得到Fe3O4@细菌纤维素/氧化石墨烯复合气凝胶材料；该材料用于处理污水和污染土壤中的Pb、Cd、Cu、Cr和Mn等重金属吸附脱除，不仅提升了细菌纤维素的吸附性能，还增强了材料的分离效果，避免二次污染问题。
发明内容
本发明所要解决的技术问题是提供一种土壤改良剂的制备方法，制备工艺简单、成本低，环保、且便于回收，具有较好的催化降解效果。
一种土壤改良剂，其制备工艺如下：将镍盐、铁盐溶于乙二醇中，随后加入四丁基溴化铵和乙酸钠，超声混合均匀，在180-200摄氏度条件下溶剂热反应10-20h，得到多孔花状的NiFe2O4；
将花状的NiFe2O4采用去离子水和乙醇洗涤多次，随后将其加入去离子水中，随后加入氯化铁、聚乙二醇以及柠檬酸钠，将其混合均匀后，置于高压反应釜中，180-200摄氏度下水热反应10-20h，得到多孔花状的NiFe2O4负载纳米Fe3O4纳米粒子的复合材料。
优选的，镍盐为硝酸镍，铁盐为硝酸铁；
优选的，硝酸镍和硝酸铁、四丁基溴化铵和乙酸钠的摩尔比为1：2：(1-2)：(1-2)；
优选的，氯化铁、聚乙二醇以及柠檬酸钠的比例为(5-10)mmol：(20-30)mg：(2-3)mmol；
技术效果：
本申请通过在溶剂热过程中加入四丁基溴化铵和乙酸钠，通过对原料和反应条件的精确调控得到尺寸均一稳定的多孔花状结构的NiFe2O4，此外，花状结构的双金属氧化物NiFe2O4具有较高的比表面积和较大的孔隙率，增大了与污染物的接触面积，从而提升光催化性能；值得注意的是，原料组分以及配比关系为一个有机的整体，替换任何一种原料组分以及反应条件均不能得到预期的花状结构；将多孔花状的NiFe2O4作为载体负载纳米Fe3O4，聚乙二醇和柠檬酸钠保证了纳米颗粒的形成，二者易形成异质结，促进光生电子和空穴的转移，增强材料的催化性能；本发明可用于去除土壤中的有机污染物以及重金属离子等多种物质，使用范围广。
附图说明
附图1为本申请实施例1制备的复合材料的SEM图。
具体实施方式
实施例1
将30mmol的硝酸铁和15mmol的硝酸镍溶于80ml乙二醇中，随后加入15mmol四丁基溴化铵和15mmol乙酸钠，超声混合均匀，在180摄氏度条件下溶剂热反应10h，得到花状的NiFe2O4；
将花状的NiFe2O4采用去离子水和乙醇洗涤多次，随后将其加入50ml去离子水中，随后加入8mmol氯化铁、20mg聚乙二醇以及2mmol柠檬酸钠，将其混合均匀后，置于高压反应釜中，200摄氏度下水热反应12h，得到花状的NiFe2O4负载纳米Fe3O4纳米粒子的复合材料。
实施例2
将30mmol的硝酸铁和15mmol的硝酸镍溶于80ml乙二醇中，随后加入15mmol四丁基溴化铵和15mmol乙酸钠，超声混合均匀，在200摄氏度条件下溶剂热反应12h，得到花状的NiFe2O4；
将花状的NiFe2O4采用去离子水和乙醇洗涤多次，随后将其加入50ml去离子水中，随后加入10mmol氯化铁、20mg聚乙二醇以及2mmol柠檬酸钠，将其混合均匀后，置于高压反应釜中，200摄氏度下水热反应12h，得到花状的NiFe2O4负载纳米Fe3O4纳米粒子的复合材料。
对比例1
将30mmol的硝酸铁和15mmol的硝酸镍溶于80ml乙二醇中，随后加入15mmol四丁基溴化铵和15mmol乙酸钠，超声混合均匀，在180摄氏度条件下溶剂热反应10h，得到花状的NiFe2O4。
对比例2
在50ml去离子水中加入8mmol氯化铁、20mg聚乙二醇以及2mmol柠檬酸钠，将其混合均匀后，置于高压反应釜中，200摄氏度下水热反应，得到Fe3O4。
将本发明实施例1-2和对比例1-2所制得的复合材料进行光降解性能测试，具体测试条件如下：在室温下分别把苯酚以及Pb2+加入土壤样品中混合均匀分别得到浓度为100mg/kg苯酚污染土壤样品以及50mmol/kg的重金属土壤样品。将催化剂和土样以质量比为1：80混合均匀，在100w的高压汞灯照射24h，测试苯酚以及重金属的降解率。
| 苯酚降解率 | Pb降解率 | |
| 实施例1 | 95.7％ | 93.8％ |
| 实施例2 | 98.6％ | 94.9％ |
| 对比例1 | 78.5％ | 71.9％ |
| 对比例2 | 73.0％ | 82.7％ |
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)
1.一种土壤改良剂，其制备工艺如下：将镍盐、铁盐溶于乙二醇中，随后加入四丁基溴化铵和乙酸钠，超声混合均匀，在180-200摄氏度条件下溶剂热反应10-20h，得到多孔花状的NiFe2O4，镍盐为硝酸镍，铁盐为硝酸铁；
将花状的NiFe2O4采用去离子水和乙醇洗涤多次，随后将其加入去离子水中，随后加入氯化铁、聚乙二醇以及柠檬酸钠，将其混合均匀后，置于高压反应釜中，180-200摄氏度下水热反应10-20h，得到多孔花状NiFe2O4负载纳米Fe3O4纳米粒子的复合材料，该复合材料粒径为1-1.2微米；硝酸镍和硝酸铁、四丁基溴化铵和乙酸钠的摩尔比为1：2：(1-2)：(1-2)；氯化铁、聚乙二醇以及柠檬酸钠的比例为(5-10)mmol：(20-30)mg：(2-3)mmol。
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