CN113786838A - 一种核壳纳米复合材料及其制备方法和应用 - Google Patents
一种核壳纳米复合材料及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种核壳纳米复合材料及其制备方法,制备方法包括以下步骤:(1)采用溶胶‑凝胶法制备了Fe3O4@SiO2核壳微球;(2)采用化学沉淀法在Fe3O4@SiO2核壳微球表面沉积MgO的前驱层,在再惰性气氛下400‑600℃煅烧,煅烧后得到Fe3O4@SiO2@MgO核壳纳米复合材料。本发明还公开了Fe3O4@SiO2@MgO核壳纳米复合材料在催化臭氧氧化降解废水中的应用。本发明的Fe3O4@SiO2@MgO核壳纳米复合材料具有较好的臭氧催化活性,并且稳定性好,具有较好的磁响应性,易于分离。
Description
技术领域
本发明涉及废水处理领域,尤其涉及一种核壳纳米复合材料及其制备方法和应用。
背景技术
臭氧是一种环境友好、可高效降解难降解有机物的废水处理技术,但由于水中臭氧溶解度低,臭氧利用低,运行成本高,限制了该技术的广泛应用。
因此,有研究通过添加催化剂来提高臭氧的氧化效率,以克服这些限制。近年来,固体催化剂催化臭氧氧化废水中有机污染物表现出较高的降解效率。固体催化剂主要包括碳材料、金属氧化物和负载型金属氧化物。其中氧化镁具有表面活性高、反应活性高、水稳定性好、环境友好、毒性小等独特性能,是一种高效臭氧化催化剂。
公开号为CN107442095A的中国专利文献公开了一种纳米氧化镁臭氧催化剂的制备方法及用其催化氧化煤化工废水的深度处理方法。催化剂制备方法包括以下步骤:一、配制MgCl2溶液;二、加入分散剂;三、滴加NaOH溶液陈化;四、洗涤;五、烘干。
公开号为CN106861668A的中国专利文献公开了一种固体碱MgO/HC催化剂,该固体碱催化剂以蜂窝陶瓷作为载体,以MgO为活性组分。将MgO/HC固体碱催化剂用于催化臭氧化处理中性废水中有机物,发现过程中pH升高,对pH具有较好的缓冲作用。
然而,传统氧化镁催化剂通常存在金属离子的溶出导致活性组分流失、在pH为中性条件下效果不佳、pH适用范围小等缺点,并且在臭氧化过程中如何将氧化镁从水中有效分离或回收再利用仍然是一个难题。
在处理过程中采用磁选可简化生产和回收,而Fe3O4因其磁性强易与水溶液分离被大量用于水处理。
发明内容
本发明提供了一种Fe3O4@SiO2@MgO核壳纳米复合材料及其制备方法,该Fe3O4@SiO2@MgO核壳纳米复合材料具有良好的臭氧催化活性。
本发明的技术方案如下:
一种Fe3O4@SiO2@MgO核壳纳米复合材料的制备方法,包括以下步骤:
(1)采用溶胶-凝胶法制备了Fe3O4@SiO2核壳微球;
(2)采用化学沉淀法在Fe3O4@SiO2核壳微球表面沉积MgO的前驱层,在再惰性气氛下400-600℃煅烧,煅烧后得到Fe3O4@SiO2@MgO核壳纳米复合材料。
步骤(1)包括:
(1-1)将Fe3O4分散于柠檬酸钠溶液中,超声处理;分离并洗涤黑色沉淀,真空干燥;
(1-2)将烘干后的Fe3O4颗粒分散到盐酸水溶液中,超声处理;分离并洗涤黑色沉淀,之后将黑色沉淀分散于乙醇水溶液中;
(1-3)向步骤(1-2)的混合液中滴加正硅酸乙酯和浓缩氨水,30-50℃搅拌反应;
(1-4)反应结束后分离并洗涤、真空干燥,得到Fe3O4@SiO2核壳微球。
步骤(1-1)中采用柠檬酸钠对Fe3O4进行处理的目的是增强其分散性,优选的,柠檬酸钠溶液的质量浓度为5-15wt%。
步骤(1-2)中采用盐酸水溶液对Fe3O4颗粒表面进行酸处理,目的是让其更好地包覆二氧化硅,优选的,盐酸水溶液的浓度为0.05-0.2mol/L。
步骤(1-3)包括,向步骤(1-2)的混合液中滴加3-5ml正硅酸乙酯和3-5ml浓度为25-30wt%的浓缩氨水,反应3-5h;
再向反应后的混合液中滴加1-3ml正硅酸乙酯和1-3ml浓度为25-30wt%的浓缩氨水,30-50℃搅拌反应5-15h;
步骤(1-2)的混合液为2-2.5g步骤(1-2)处理得到的黑色沉淀分散于200-220ml的乙醇水溶液中得到。
步骤(2)包括:
(2-1)向Fe3O4@SiO2核壳微球中滴加镁盐溶液,超声反应0.1-1h后,再滴加碱溶液,40-60℃下搅拌反应;
(2-2)反应结束后,分离并洗涤沉淀,真空干燥;
(2-3)将干燥后的粉末在惰性气氛下400-600℃煅烧1-3h,得到Fe3O4@SiO2@MgO核壳纳米复合材料。
步骤(2-1)中,Fe3O4@SiO2核壳微球、镁盐、碱的比例为1kg:6-7mol:25-30mol。
优选的,步骤(2-1)中,所述的镁盐溶液为硝酸镁溶液;所述的碱溶液为氢氧化钠溶液。
步骤(2-3)中,煅烧过程包括:以5℃/min的升温速度从常温煅烧至400-600℃,在400-600℃下保温煅烧1-3h;
煅烧过程中使用惰性气体作为保护气体,保护气体的流速为0.5-1L/min。
本发明还提供了一种通过上述制备方法制备的Fe3O4@SiO2@MgO核壳纳米复合材料。
在Fe3O4表面引入SiO2,使得与Fe3O4相比,制得的Fe3O4@SiO2@MgO核壳纳米复合材料的比表面积和总孔容得到大大提高,这样可以为催化剂提供更多的反应位点,提高催化剂在氧化降解反应中的催化性能。另一方面,SiO2与MgO相互协同作用,进一步提高了Fe3O4@SiO2@MgO核壳纳米复合材料的催化性能。
本发明制备的Fe3O4@SiO2@MgO核壳纳米复合材料在外磁场下易于从水溶液中分离,具有良好的磁响应性和可分散性,可以避免催化剂对环境的有害分布和二次污染,具有实际应用前景。
本发明还提供了上述Fe3O4@SiO2@MgO核壳纳米复合材料在废水处理中的应用,包括:
向待处理废水中投加Fe3O4@SiO2@MgO核壳纳米复合材料,通入臭氧,进行臭氧催化氧化降解反应。
优选的,所述的废水的pH值为4-10;进一步优先的,所述的废水的pH值为6-8。
本发明制备的Fe3O4@SiO2@MgO核壳纳米复合材料稳定性强、易回收,可多次重复回收使用。
与现有技术相比,本发明的有益效果为:
(1)本发明制备的Fe3O4@SiO2@MgO核壳纳米复合材料稳定性强,活性组分不易流失,可重复使用;
(2)本发明制备的Fe3O4@SiO2@MgO核壳纳米复合材料的催化活性较高,在催化臭氧氧化中,pH适用范围广;
(3)本发明制备的Fe3O4@SiO2@MgO核壳纳米复合材料具有良好的磁响应性和可分散性,易与水溶液分离,在废水处理过程中可采用磁性回收,可简化生产和回收,可被大量用于废水处理。
附图说明
图1为MgO、Fe3O4、实施例1步骤(7)得到的Fe3O4@SiO2、实施例1步骤(10)得到的Fe3O4@SiO2@MgO的XRD图;
图2为实施例1步骤(7)得到的Fe3O4@SiO2、实施例1步骤(10)得到的Fe3O4@SiO2@MgO的TEM图;其中,(a)为Fe3O4@SiO2的标尺为200nm的TEM图,(b)为(a)的局部放大图;(c)为Fe3O4@SiO2@MgO的标尺为200nm的TEM图,(d)为(c)的局部放大图;
图3为Fe3O4、实施例1步骤(7)得到的Fe3O4@SiO2、实施例1步骤(10)得到的Fe3O4@SiO2@MgO的VSM图;
图4为应用例1的水样处理效果图;
图5为Fe3O4@SiO2@MgO的稳定性实验结果图;
图6为不同废水初始pH对水处理效果的影响图;
图7为不同臭氧投加量对水处理效果的影响图;
图8为不同催化剂投加量对水处理效果的影响图;
图9为不同DMAC的初始浓度对水处理效果的影响图。
具体实施方式
实施例1
Fe3O4@SiO2@MgO的制备方法,包括如下步骤:
(1)称取2.32g Fe3O4放置于烧杯中,溶于100ml柠檬酸钠溶液(10%wt),超声处理30min,目的是增加磁铁的分散性;
(2)然后步骤(1)得到的磁颗粒经永磁体分离后用无水乙醇和去离子水洗涤黑色沉淀数次,在65℃真空干燥12小时;
(3)将烘干后的Fe3O4颗粒加入150mL浓度为0.1mol/L的HCl水溶液,超声振荡10min,目的是对其表面进行酸处理,让其更好包覆二氧化硅;
(4)颗粒经永磁体分离后经去离子水洗涤后均匀分散于乙醇(180ml)和去离子水(30ml)的混合溶液中;
(5)将4.0mL的正硅酸乙酯(TEOS)和4.0mL浓缩氨水溶液(28%wt)滴入上述混合溶液中;
(6)4h后再向混合溶液中加入2ml浓缩氨水溶液(28%wt)和2.0mL的正硅酸乙酯(TEOS),45℃下机械搅拌10h;
(7)然后磁颗粒经永磁体分离得到Fe3O4@SiO2微球,用蒸馏水和乙醇交替洗涤数次,在65℃下真空干燥12小时;
(8)向Fe3O4@SiO2颗粒(1.16g)中缓慢滴加100ml 0.075mol/L的Mg(NO3)2溶液,先超声30min,然后在三口烧瓶中逐滴加入60mL 0.5mol/LNaOH,控制温度在50℃连续机械搅拌2小时,然后冷却至室温得到目标产品;
(9)磁铁分离后用无水乙醇和去离子水洗涤沉淀数次,在65℃下真空干燥12小时;
(10)干燥后的粉末在管式炉中以5℃/min的升温速度从常温煅烧至500℃,并在该温度下保温2h。煅烧过程中使用氮气作为保护气体,流速为0.6L/min。煅烧后得到Fe3O4@SiO2@MgO纳米颗粒。
图1为MgO、Fe3O4、步骤(7)得到的Fe3O4@SiO2、步骤(10)得到的Fe3O4@SiO2@MgO的XRD图。
从图1可知Fe3O4@SiO2的XRD谱图与Fe3O4的XRD谱图相似,由于Fe3O4负载的SiO2是无定形的,所以没有检测到SiO2对应的特征衍射峰,相应的Fe3O4纳米颗粒(hkl)值(111)、(220)、(311)、(222)、(400)、(422)、(511)和(440)在2θ=18.3°、30.1°、35.4°、37.0°、43.0°、53.4°、56.9°、62.5°,与Fe3O4(JCPDS卡片号72-2303)一致。相应的MgO纳米颗粒(hkl)值(111)、(200)、(220)、(311)和(222)在2θ=36.9°、42.8°、62.2°、74.5°、78.4°,与MgO(JCPDS卡片号74-1225)一致。合成的Fe3O4@SiO2@MgO的衍射峰尖锐清晰,所有特征衍射峰排除Fe3O4特征衍射峰外,都归属于MgO的纯相。MgO具有明显的(200)和(220)峰,表明合成的复合材料结晶度较高。
图2为实施例1步骤(7)得到的Fe3O4@SiO2、实施例1步骤(10)得到的Fe3O4@SiO2@MgO的TEM图;其中,(a)为Fe3O4@SiO2的标尺为200nm的TEM图,(b)为(a)的局部放大图;(c)为Fe3O4@SiO2@MgO的标尺为200nm的TEM图,(d)为(c)的局部放大图。
在图2的(a)、(b)中,Fe3O4@SiO2透射电镜图像上的暗区可能与Fe3O4粒子的高电子密度有关,而亮区和低暗区可能与SiO2有关。Fe3O4@SiO2纳米粒子表现为明显的核壳结构,可以清楚观察到Fe3O4纳米粒子上包裹了一层致密的SiO2,SiO2层的尺寸约为30~60nm。在图2的(c)、(d)中,与Fe3O4@SiO2相比,Fe3O4@SiO2@MgO的外表面比原始Fe3O4粗糙得多,多孔性更强,可以为催化剂提供更多的反应位点,提高催化剂在氧化降解反应中的催化性能,这一特性有助于提高所合成纳米催化剂的表面催化活性。结果表明Fe3O4微球表面均匀沉积了SiO2和MgO层。
对实施例1步骤(7)得到的Fe3O4@SiO2、实施例1步骤(10)得到的Fe3O4@SiO2@MgO进行EDX光谱检测,结果分别如表1和表2所示:
表1
元素 | 重量百分数(%) | 原子百分数(%) |
O(K) | 42.5 | 63.87 |
Mg(K) | 0.04 | 0.04 |
Si(K) | 26.66 | 22.82 |
Fe(K) | 30.78 | 13.25 |
表2
元素 | 重量百分数(%) | 原子百分数(%) |
O(K) | 43.44 | 56.13 |
Mg(K) | 40.94 | 34.81 |
Si(K) | 8.94 | 6.57 |
Fe(K) | 6.66 | 2.46 |
由表1可知,Fe3O4@SiO2是由O、Si和Fe三种元素组成,元素的wt%分别为42.5%、26.66%和30.78%;由表2可知,Fe3O4@SiO2@MgO纳米颗粒是由O、Mg、Si和Fe四种元素组成,元素的wt%分别为43.44%、40.94%、8.94%和6.66%,Fe信号较弱,说明Fe存在于催化剂内层。
图3为Fe3O4、实施例1步骤(7)得到的Fe3O4@SiO2、实施例1步骤(10)得到的Fe3O4@SiO2@MgO的VSM图。
由图3可知,Fe3O4、Fe3O4@SiO2、Fe3O4@SiO2@MgO的饱和磁化性能分别为93.6emu g-1、76.6emu g-1、56.9emu g-1。Fe3O4纳米颗粒外层无定形SiO2的存在可能使Fe3O4@SiO2复合材料的饱和磁化强度值略低于Fe3O4。因此,无定形SiO2中间层和非磁性MgO最外层使得Fe3O4@SiO2@MgO复合材料的饱和磁化强度值远低于Fe3O4和Fe3O4@SiO2。合成的Fe3O4@SiO2@MgO复合材料在外磁场下易于从水溶液中分离,具有良好的磁响应性和可分散性,可以避免催化剂对环境的有害分布和二次污染,具有实际应用前景。
Fe3O4、Fe3O4@SiO2和Fe3O4@SiO2@MgO的比表面积分别为1.1597m2·g-1、2.1740m2·g-1和2.1421m2·g-1。Fe3O4、Fe3O4@SiO2和Fe3O4@SiO2@MgO的总孔隙体积分别为0.00391cm3·g-1、0.00612cm3·g-1和0.00620cm3·g-1。Fe3O4@SiO2和Fe3O4@SiO2@MgO的比表面积和总孔容的增加可能是由于SiO2具有较高的比表面积和一定的孔容的特点,因此SiO2在Fe3O4表面的分散造成的。
应用例1
配置250mL含有20mg/L的DMAC溶液,并调节pH至7。
评价了不同系统对DMAC的降解效果,不同的实验包括(a)O3系统,(b)Fe3O4/O3系统,(c)Fe3O4@SiO2/O3系统,(d)Fe3O4@SiO2@MgO/O3系统,(e)Fe3O4@SiO2@MgO/O2系统。
催化剂的投加量为0.5g/L,臭氧的投加量为10mg/min。实验开始,反应12min后取样检测。
检测方法:DMAC采用ThermoFisher Dionex Ultimate3000高效液相色谱法。
水样处理12min后效果如图4所示。
图4-9的纵坐标表示DMAC的剩余率,DMAC的去除率=100%-剩余率。
由图4可知,加入Fe3O4@SiO2@MgO和Fe3O4@SiO2均能不同程度地提高DMAC的去除效率。Fe3O4@SiO2@MgO的催化活性最高,12min内DMAC的去除率为99.9%。远优于Fe3O4@SiO2(32.04%),Fe3O4(25.61%)和单独臭氧(23.11%)。表明合成的Fe3O4@SiO2@MgO纳米颗粒对DMAC的臭氧氧化具有显著的催化性能。
应用例2
配置250mL含有20mg/L的DMAC溶液,并调节pH至7,再加入催化剂,催化剂的投加量为0.5g/L,然后加入到臭氧反应器中,并且通入臭氧进行反应。
臭氧的投加量为10mg/min。实验开始,反应12min后取样检测。
检测方法:DMAC采用ThermoFisher Dionex Ultimate3000高效液相色谱法。
水样处理12min后效果如表3所示:
表3
催化剂种类 | DMAC去除率 |
Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@MgO | 99.90% |
Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@CeO<sub>2</sub> | 43.53% |
Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@MnO<sub>2</sub> | 50.30% |
Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@CuO | 48.52% |
Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>@ZnO | 58.92% |
单独臭氧 | 23.11% |
水样处理12min后效果如表1所示。加入表中各类催化剂均能不同程度地提高DMAC的去除效率。Fe3O4@SiO2@MgO的催化活性最高,12min内DMAC的去除率为99.6%。远优于Fe3O4@SiO2@CeO2(43.53%),Fe3O4@SiO2@MnO2(50.30%),Fe3O4@SiO2@CuO(48.52%),Fe3O4@SiO2@ZnO(58.92%)和单独臭氧(23.11%)。表明合成的Fe3O4@SiO2@MgO纳米颗粒对DMAC的臭氧氧化具有显著的催化性能。
应用例3
配置250mL含有20mg/L的DMAC溶液,并调节pH至7,再加入催化剂,催化剂的投加量为0.5g/L,然后加入到臭氧反应器中,并且通入臭氧。
臭氧的投加量为10mg/min。实验开始,反应12min后取样检测。
检测方法:DMAC采用ThermoFisher Dionex Ultimate3000高效液相色谱法。
水样处理12min后效果如表4所示:
表4
水样处理12min后效果如表4所示。加入表中各类催化剂均能不同程度地提高DMAC的去除效率。Fe3O4@SiO2@MgO的催化活性最高,12min内DMAC的去除率为99.9%。远优于CH@MgO(78.6%),GF@MgO(85.9%)和单独臭氧(23.11%)。表明合成的Fe3O4@SiO2@MgO纳米颗粒对DMAC的臭氧氧化具有显著的催化性能。
应用例4
为确定Fe3O4@SiO2@MgO催化剂的稳定性,配置250mL含有20mg/L的DMAC溶液,并调节pH至7,催化剂的投加量为0.5g/L,臭氧的投加量为10mg/min。实验开始,反应12min后取样检测,进行5次连续循环催化臭氧化DMAC。在每个循环后通过磁性分离和65℃干燥回收的情况下重复使用。
实验结果如图5所示,从图5可以看出,经过5次循环后,Fe3O4@SiO2@MgO/O3工艺对DMAC的去除率只有轻微下降。
可能原因为:(1)反应中间体在每个循环后对孔隙和活性位点的阻塞是催化剂失活的因素之一;(2)由于连续洗涤和干燥过程,催化剂的活性位点减少。结果表明,在可循环性试验中,Fe3O4@SiO2@MgO保持了较高的催化活性,对长期实际应用具有重要意义。因此,Fe3O4@SiO2@MgO具有良好的可重复使用性能,是去除DMAC的一种经济有效的催化剂。
应用例5
配置250mL含有20mg/L的乙酸溶液,并调节pH至7,再加入催化剂,催化剂的投加量为0.5g/L,然后加入到臭氧反应器中,并且通入臭氧。
臭氧的投加量为10mg/min。实验开始,反应12min后取样检测。
检测方法:乙酸采用ThermoFisher Dionex Ultimate3000高效液相色谱法。
水样处理12min后,Fe3O4@SiO2@MgO/O3对乙酸的降解效率为72.20%。乙酸是大多数有机污染物臭氧化的最终产物之一,Fe3O4@SiO2@MgO/O3对乙酸具有较好的降解效果,表明Fe3O4@SiO2@MgO/O3体系对有机污染物的降解具有普遍的催化活性。
应用例6
配置250mL含有20mg/L的DMAC溶液,并调节pH分别至4、6、7、8、10,再加入催化剂,催化剂的投加量为0.5g/L,然后加入到臭氧反应器中,并且通入臭氧。
臭氧的投加量为10mg/min。实验开始,反应12min后取样检测。
检测方法:DMAC采用ThermoFisher Dionex Ultimate3000高效液相色谱法。
水样处理12min后效果如图6所示。DMAC的去除率在pH=4~10的范围内均较高,DMAC的去除率随初始pH的增加而有所增加,当初始pH为7.0时,DMAC的去除率已达到99.96%。
应用例7
与应用例3相比,将臭氧投加量分别调整为0、5、15、20mg/min,其它同应用例3。
水样处理12min后效果如图7所示。
应用例8
与应用例3相比,将催化剂投加量分别调整为0、0.25、0.5、1.0g/L,其它同应用例3。
水样处理12min后效果如图8所示。
应用例9
与应用例3相比,将DMAC的初始浓度分别调整为10、20、50、100、200mg/L,其它同应用例3。
水样处理12min后效果如图9所示。
以上所述的实施例对本发明的技术方案和有益效果进行了详细说明,应理解的是以上所述仅为本发明的具体实施例,并不用于限制本发明,凡在本发明的原则范围内所做的任何修改、补充和等同替换等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种Fe3O4@SiO2@MgO核壳纳米复合材料的制备方法,其特征在于,包括以下步骤:
(1)采用溶胶-凝胶法制备了Fe3O4@SiO2核壳微球;
(2)采用化学沉淀法在Fe3O4@SiO2核壳微球表面沉积MgO的前驱层,在再惰性气氛下400-600℃煅烧,煅烧后得到Fe3O4@SiO2@MgO核壳纳米复合材料。
2.根据权利要求1所示的Fe3O4@SiO2@MgO核壳纳米复合材料的制备方法,其特征在于,步骤(1)包括:
(1-1)将Fe3O4分散于柠檬酸钠溶液中,超声处理;分离并洗涤黑色沉淀,真空干燥;
(1-2)将烘干后的Fe3O4颗粒分散到盐酸水溶液中,超声处理;分离并洗涤黑色沉淀,之后将黑色沉淀分散于乙醇水溶液中;
(1-3)向步骤(1-2)的混合液中滴加正硅酸乙酯和浓缩氨水,30-50℃搅拌反应;
(1-4)反应结束后分离并洗涤、真空干燥,得到Fe3O4@SiO2核壳微球。
3.根据权利要求2所示的Fe3O4@SiO2@MgO核壳纳米复合材料的制备方法,其特征在于,步骤(1-3)包括,向步骤(1-2)的混合液中滴加3-5ml正硅酸乙酯和3-5ml浓度为25-30wt%的浓缩氨水,反应3-5h;
再向反应后的混合液中滴加1-3ml正硅酸乙酯和1-3ml浓度为25-30wt%的浓缩氨水,30-50℃搅拌反应5-15h;
步骤(1-2)的混合液为2-2.5g步骤(1-2)处理得到的黑色沉淀分散于200-220ml的乙醇水溶液中得到。
4.根据权利要求1所示的Fe3O4@SiO2@MgO核壳纳米复合材料的制备方法,其特征在于,步骤(2)包括:
(2-1)向Fe3O4@SiO2核壳微球中滴加镁盐溶液,超声反应0.1-1h后,再滴加碱溶液,40-60℃下搅拌反应;
(2-2)反应结束后,分离并洗涤沉淀,真空干燥;
(2-3)将干燥后的粉末在惰性气氛下400-600℃煅烧1-3h,得到Fe3O4@SiO2@MgO核壳纳米复合材料。
5.根据权利要求4所示的Fe3O4@SiO2@MgO核壳纳米复合材料的制备方法,其特征在于,步骤(2-1)中,Fe3O4@SiO2核壳微球、镁盐、碱的比例为1kg:6-7mol:25-30mol。
6.根据权利要求4所示的Fe3O4@SiO2@MgO核壳纳米复合材料的制备方法,其特征在于,步骤(2-3)中,煅烧过程包括:以5℃/min的升温速度从常温煅烧至400-600℃,在400-600℃下保温煅烧1-3h;
煅烧过程中使用惰性气体作为保护气体,保护气体的流速为0.5-1L/min。
7.一种Fe3O4@SiO2@MgO核壳纳米复合材料,其特征在于,采用如权利要求1-6所示的制备方法制备得到。
8.一种如权利要求7所示的Fe3O4@SiO2@MgO核壳纳米复合材料在废水处理中的应用,包括:
向待处理废水中投加Fe3O4@SiO2@MgO核壳纳米复合材料,通入臭氧,进行臭氧催化氧化降解反应。
9.根据权利要求8所示的应用,其特征在于,所述的废水的pH值为4-10。
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