CN113663639A - 掺镧层状双氧化物的制备方法、其产物及应用 - Google Patents
掺镧层状双氧化物的制备方法、其产物及应用 Download PDFInfo
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Abstract
本发明公开了一种掺镧层状双氧化物的制备方法、其产物及应用,所述方法包括以下步骤1:制备金属硝酸盐溶液和氢氧化钠溶液;S2:将所述金属硝酸盐溶液和氢氧化钠溶液以相同的速度加入水中混合,以保持PH为恒定值,便于形成层状双氢氧化物沉淀;S3:取S1所得沉淀依次陈化、过滤、烘干、研磨、煅烧。本发明还涉及由此方法制得的掺镧层状双氧化物及其应用。
Description
技术领域
本发明涉及层状双氧化物技术领域,具体是一种掺镧层状双氧化物的制备方法、其产物及应用。
背景技术
磷是水生生物的主要营养源之一,但过量磷将导致水体富营养化和水质恶化。随着人类生活生产活动的日益频繁产生了大量的含磷工业废水、农业废水及生活污水,这些含磷废水经污水处理厂处理后仍含有低浓度的磷,排入到江河湖泊等天然水体中,使水体中磷物质的含量超过水体可承受的浓度水平,水体中以磷作为营养物质的微生物、藻类及其他水生植物快速生长繁殖,水体溶解氧含量下降,破坏水体生态系统平衡,引发水体富营养化的发生。在自然界中,磷通常以PO4 3-的形式存在,水体中的水生植物如藻类也主要吸收PO4 3-作为磷营养物质进行繁殖和生命活动,因此,如何去除水体中的PO4 3-解决水体富营养化问题成为人们关注的重点。到目前为止,人们已经提出了各种方法来去除水中的磷酸盐,主要包括生物吸收、化学沉淀、离子交换和吸附。与其他传统技术相比,吸附法因其经济、操作简单、效率高的优点而被广泛用于除磷。
层状双氢氧化物(LDHs),也称水滑石(hydrotalcite)、类水滑石(hydrotalcite-like)或阴离子粘土(anion clays),是一种阴离子型黏土,其具有典型的层状结构,已显示出在许多方面的应用潜力。LDHs具有对各种化学组分(污染物)包容性、化学成分多变性、易于结晶和合成、结构正电荷密度大等特性。LDH的一般公式为[MII1-xMIIIx(OH)2]x+[An- x/n-yH2O]x-,其中M(II)和M(III)分别为二价和三价金属阳离子,An-是n价阴离子。LDHs的煅烧衍生物,被称为层状双氧化物(LDO),通常由混合金属氧化物或尖晶石构成。有趣的是,LDO往往表现出一种"记忆效应",即混合氧化物浸泡在阴离子溶液中时,会重建类似氢氧化铝的结构,同时具有较高的阴离子交换能力,是理想的污染物赋存载体和阴离子交换吸附材料,因此如何制备一种针对水体中的PO4 3-具有高效吸附作用的LDO以解决水体富营养化问题,成为了如今研究的热点。
发明内容
本发明的目的之一在于克服现有技术的不足,提供一种掺镧层状双氧化物的制备方法、产品及应用,该方法原料易得、操作简便、成本低、绿色无污染、易于工业化,所述双氧化物用于去除废水中的磷酸盐,具有高效、吸附性好的特点,且吸附磷酸盐后的双氧化物还可以作为磷肥,对植物生长提供养分,无废弃产生。
本发明的目的是通过以下技术方案来实现的:
一种掺镧层状双氧化物的制备方法,包括以下步骤:
S1:制备同时含有2价和3价金属硝酸盐的溶液和氢氧化钠溶液;
S2::在60℃-70℃的温度下,将所述金属硝酸盐溶液和氢氧化钠溶液匀速缓慢加入超纯水中进行共沉淀,沉淀过程中保持pH恒定为10.8-11.2;氢氧化钠浓度和用量以能维持反应体系pH一直恒定为准;
S3:将S2所得物料进行陈化和过滤,然后烘干并研磨;
S4:对研磨所得物料进行煅烧,得到掺镧层状双氧化物。
本发明所述方法全程控制pH恒定,这是为了保证阳离子同时沉淀,因此步骤S2须将配置好的硝酸盐溶液和饱和氢氧化钠溶液同时缓慢的滴加到超纯水中,以保持金属盐共沉淀所需的pH值。
进一步的,步骤S1中,所述金属硝酸盐包括硝酸镧、硝酸铁和硝酸镁。
进一步的,步骤S1中所述硝酸盐溶液中,La3+:Fe3+:Mg2+的摩尔比为1:9:30。
进一步的,步骤S2中,整个过程在氮气氛围中进行。
在氮气氛围中进行是为了避免空气中的二氧化碳进入层状结构中,取代硝酸根离子形成碳酸根夹层。一般来说,对于带正电的金属氢氧化物层板而言,高价阴离子比低价阴离子具有更大的结合强度,因而NO3 -与层板的结合强度略强于CO3 2–,相应的LDHs在制备过程中可能得到更大的插层量,因此如果形成碳酸根插层会降低材料的吸附性能。
进一步的,步骤S3中,所述陈化为将步骤S2所得的物料在60℃-70℃的温度下,静置至少16h-24h。
进一步的,所述煅烧的温度为300℃-400℃、煅烧时间为2h-4h,煅烧时按5-10℃/分钟进行升温。
其中,煅烧温度不宜过高,过高的温度会改变材料的性质,导致层状结构坍塌。
本发明的目的之二在于提供一种由该方法制得的层状双氧化物,具体结构如附图所示。
本发明的目的之三在于提供一种所述层状双氧化物在吸附磷酸盐方面的应用,也就是将所述层状双氧化物用于吸附磷酸盐,而吸附磷酸盐后,还可作为肥料用于作物栽培,无废弃排放。
本发明的有益效果是:
1、本发明提供的掺镧层状双氧化物的制备方法,具有原料易得、操作简便、绿色无污染、易于工业化、成本低的优点。
2、采用本发明方法制备的掺镧层状双氧化物,该层状双氧化物对PO4 3-有极佳的的吸附能力,可用于净化含磷废水,防治水体富营养化,有良好的的市场前景。
附图说明
图1为不同煅烧温度下掺镧层状双氧化物的X射线衍射图;
图2为不同煅烧温度下掺镧层状双氧化物的磷酸盐吸附量柱状图;
图3为所述掺镧层状双氧化物的TGA曲线图;
图4为不同La/(La+Fe)比例下掺镧层状双氧化物的X射线衍射图;
图5为不同La/(La+Fe)比例下掺镧层状双氧化物的磷酸盐吸附量柱状图。
图6为吸附磷酸盐后的MFL-1/10-350的XRD图谱(C)
具体实施方式
下面结合附图进一步详细描述本发明的技术方案,但本发明的保护范围不局限于以下所述。
(一)制备掺镧层状双氧化物
1、制备过程:
S1:制备同时含有2价和3价金属硝酸盐的溶液(其金属总浓度为1mol/L,因表格字数问题,以下简称A溶液)和氢氧化钠溶液(以下简称B溶液);
S2:在65℃的温度和氮气保护下,将所述金属硝酸盐溶液和氢氧化钠溶液匀速缓慢加入超纯水中进行共沉淀,共沉淀过程中保持pH恒定;
S3:将S2经共沉淀后所得物料与65℃水浴条件进行陈化和过滤,超纯水洗涤后,烘干并研磨成100nm粒度的颗粒;
S4:对研磨所得物料进行煅烧,得到掺镧层状双氧化物。
2、各实施例工艺条件见下表,其中氢氧化钠溶液浓度控制在2mol/L,用量以维持反应体系pH恒定为准。
(二)制备不同煅烧温度和时间下的掺镧层状双氧化物,并进行吸附磷酸盐的性能测试,制备方法如第(一)部分记载,制备掺镧层状双氧化物工艺条件如实施例2-5:
即,分别以250℃、350℃、450℃、550℃煅烧3小时,剩余的1组不进行煅烧处理,所得5份产物的XRD图如图1所示。
取上述5份产物分别加入等浓度的磷酸盐溶液中,然后于恒温振荡箱中振荡吸附24h,检测溶液中剩余磷酸盐浓度并计算吸附量,结果如图2所示。
(三)取实施例1样品于热重分析仪中测定0-1000℃的TGA曲线,热重分析曲线结果如图3所示。
(四)制备不同La、Fe、Mg比例下的掺镧层状双氧化物,并测试吸附磷酸盐的性能,制备方法如第(一)部分所述,制备所用工艺条件如实施例6-9:
比较实施例1和实施例6-9所得5份产物的XRD图,如图4所示。
(五)取第(四)部分获得的5份产物分别加入等浓度的磷酸盐溶液中,然后于恒温振荡箱中振荡吸附24h,检测溶液中剩余磷酸盐浓度并计算吸附量,结果如图5所示。
(六)本发明材料的结构重建特性测试,以实施例1样品为对象
如图6所示,材料(以MFL-1/10-350表示)吸附磷酸盐之前与之后的特征衍射峰没有明显变化。然而,在吸附了20mg/L的磷酸盐后,材料又出现了层状的双氢氧化物结构,说明材料特有的“记忆效应”并造成结构重建。在较低的磷酸盐浓度下,主要的吸附机制是重建过程,而在较高的磷酸盐浓度下,是表面沉淀。
以上所述仅是本发明的优选实施方式,应当理解本发明并非局限于本文所披露的形式,不应看作是对其他实施例的排除,而可用于各种其他组合、修改和环境,并能够在本文所述构想范围内,通过上述教导或相关领域的技术或知识进行改动。而本领域人员所进行的改动和变化不脱离本发明的精神和范围,则都应在本发明所附权利要求的保护范围内。
Claims (9)
1.一种掺镧层状双氧化物的制备方法,其特征在于,包括以下步骤:
S1:制备同时含有2价和3价金属硝酸盐的溶液和氢氧化钠溶液;
S2:在60℃-70℃温度下,将所述金属硝酸盐溶液和氢氧化钠溶液匀速缓慢加入至超纯水中进行共沉淀,共沉淀过程中保持pH恒定为10.8-11.2;
S3:对S2所得物料进行陈化和过滤,然后烘干并研磨;
S4:对研磨所得物料进行煅烧,得到掺镧层状双氧化物。
2.根据权利要求1所述的制备方法,其特征在于:步骤S1中,所述金属硝酸盐包括硝酸镧、硝酸铁和硝酸镁。
3.根据权利要求2所述的制备方法,其特征在于:步骤S1所述硝酸盐溶液中,La3+:Fe3+:Mg2+的摩尔比为1:9:30。
4.根据权利要求1-3任一项权利要求所述的制备方法,其特征在于:步骤S2是在氮气保护下进行。
5.根据权利要求1所述的制备方法,其特征在于:步骤S3中,所述陈化是将步骤S2所得物料在60℃-70℃静置至少16h-24h。
6.根据权利要求1所述的制备方法,其特征在于:所述煅烧的温度为300℃-400℃、煅烧时间为2h-4h,煅烧时按5-10℃/分钟进行升温。
7.按照权利要求1-6任一项权利要求所述方法制得的层状双氧化物。
8.权利要求7所述的层状双氧化物的应用,其特征在于:是将所述层状双氧化物用于吸附磷酸盐。
9.根据权利要求8所述的层状双氧化物的应用,其特征在于:将吸附磷酸盐的层状双氧化物作为磷肥。
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