CN111514899A - 一种处理有机废水的催化剂及其制备方法 - Google Patents
一种处理有机废水的催化剂及其制备方法 Download PDFInfo
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- CN111514899A CN111514899A CN202010391509.9A CN202010391509A CN111514899A CN 111514899 A CN111514899 A CN 111514899A CN 202010391509 A CN202010391509 A CN 202010391509A CN 111514899 A CN111514899 A CN 111514899A
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- catalyst
- hydrotalcite
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- organic wastewater
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- Chemical Kinetics & Catalysis (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
本发明公开了一种处理有机废水的催化剂及其制备方法,涉及有机废水处理领域,包括以下步骤:步骤一:向类水滑石水溶液中加入载体,不断搅拌进行负载;步骤二:向步骤一中的负载好的类水滑石,进行水浴陈化,得到一级催化剂;步骤三:步骤二得到的一级催化剂用去离子水进行抽滤,抽滤至滤液呈中性,得到二级催化剂;步骤四:将步骤三得到的二级催化剂进行干燥,得到成品催化剂。本发明将类水滑石与载体用共沉淀方法制备类水滑石催化剂,类水滑石中的活性成分能够均匀的镶嵌在水滑石载体中结构里不发生团聚,同时也不会被掩盖,增大了类水滑石的表面活性物质的接触面积,进一步提高了最大限度的利用催化剂的活性成分的催化性能。
Description
技术领域
本发明涉及有机废水处理领域,尤其是一种处理有机废水的催化剂及其制备方法。
背景技术
LDHs是一种层状双羟基金属氧化物,又称为层状阴离子型化合物。LDHs是由带正电荷的主板和层间阴离子通过非共价键的相互作用组装成的化合水滑石类材料特殊的组成结构包括主板化学组成的多元性、金属阳离子比例的可调性和层间阴离子种类的丰富性,带正电荷的主板主要由二价和三价金属阳离子构成。常见的二价金属阳离子主要有Zn2 +,Mg2+,Cu2+,Ca2+等,三价金属阳离子主要有Al3+,Fe3+,Cr3+。水滑石的层状结构和离子水滑石类材料特殊的组成结构包括主板化学组成的多元性,金属阳离子比例的可调性和层间阴离子种类的丰富性,使其具有特殊的多样性能,在催化剂、吸附剂、离子交换载体、生物医药、阻燃剂和高分子聚合物纳米材料等方面得到了广泛的应用。在自然界中人们发现水滑石较少,而且自然界中的水滑石通常含很多杂质,所以在应用上存在着缺陷。自然界中水滑石的种类较少,大多数都是镁铝水滑石选择性较少。类水滑石在催化剂等领域具有重要很好的应用前景。
类水滑石是一类在废水处理中研究非常广泛的材料。许多的研究发现水滑石对水体的阴离子,金属离子以及有机物都具有优秀的吸附效果。根据在废水中的处理不同应用可以将类水滑石分为四大类:水滑石作为吸附剂处理废水,水滑石作为载体负载活性成分处理废水,水滑石当做催化剂处理废水,水滑石作为前驱体处理废水。
在现有技术中,大多是简单的共沉淀法制备催化剂,通过改变催化剂的先驱化合物成分改变催化剂的组成,然后煅烧。如CN1579622A中公开了一种经层状插层前体制备高分散铜基氧化催化剂及其组装方法。发明利用水滑石LDHs结构的可设计性,层板组成的可调变性和层间离子的可交换性特点,先在层板定量引入Fe、Cu、Ni、Mn、Zn、Al、Cr或稀土元素Ce、La、Y等不同种类和数量的催化活性组份,再经插层组装在层间引入少量的Cu、Mn、Fe、Pd、Ru、Pt等络合阴离子,制备得到插层化合物前体,通过焙烧插层前体可制备出高分散、高活性、铜基氧化催化剂,这种催化剂主要用于双氧水氧化苯酚,该发明中仅介绍了苯酚的转化率,没有提及COD的去除率。
CN1358567A公开了一种用于催化湿式氧化处理工业废水的铜基催化剂的制备及应用。催化剂的主要成分为铜、锌、镍、镁、铝、铬、铁和一部分稀土金属的氧化物,其中以氧化物的含量来计算:CuO为20-55%;nO、NiO或MgO为20-55%;Cr2O3、Al2O3或Fe2O3为10-40%;稀土金属氧化物为0-10%。该催化剂由含有各种金属的盐共沉淀得到类水滑石结构的催化剂前驱体,并焙烧所得。该催化剂能有效处理含酚、磺基水杨酸、H-酸和表面活性剂等有毒难降解的工业有机废水,不仅有较高的催化活性,并且活性组分的流失得到了控制,其中铜离子的流失文献报道相比较降低一个数量级以上,但在150℃温度下,其活性小于80%。
发明内容
本发明的发明目的在于:针对上述存在的问题,提供一种处理有机废水的催化剂及其制备新方,通过引入载体解决。
本发明采用的技术方案如下:
一种处理有机废水的催化剂,其特征在于,包括类水滑石和载体。
本发明的创新点在于,将类水滑石与载体共沉淀方法制备催化剂,类水滑石中的能够均匀的镶嵌在载体中结构里不发生团聚,同时也不会被掩盖,增大了类水滑石的表面活性物质的接触面积,进一步提高了催化性能。同时申请人发现,载体不同比例和不同种类,会形成不同类型的类水滑石,包括包裹型,分散型,以及反包型。
传统水滑石催化剂处理废水残留物主要是小分子酸(乙酸,已二酸),这些小分子酸在CWO比较难降解,但是通过生物法可以很好的降解。从检测结果的谱图中可知,本发明制备的类水滑石催化剂的催化下残留的有机物主要是苯乙醚,1.5-二异丁基苯醌和3-甲基-1.5-二异丁基苯酚此类大分子,表明本发明制备的催化剂对小分子酸具有很好的氧化作用。
进一步的,所述载体为二氧化钛、γ-Al2O3、活性炭、碳化硅、硅藻土、堇青石中的一种。
二氧化钛、γ-Al2O3、活性炭等均具有高稳定性和高分散性,同时二氧化钛还可以助催化,活性炭丰富孔结构可以增加催化剂比表面积。
一种处理有机废水的催化剂的制备方法,其特征在于,包括以下步骤:
步骤一:类水滑石与载体进行负载;
步骤二:向步骤一中的负载好的类水滑石,在水浴中进行陈化,得到一级催化剂;
步骤三:步骤二得到的一级催化剂用去离子水进行抽滤,抽滤至滤液呈中性,得到二级催化剂;
步骤四:将步骤三得到的二级催化剂进行干燥,得到成品催化剂。
进一步的,还包括以下步骤:步骤五:将催化剂浸渍在硝酸铈或硝酸钌溶液中1~2h,然后用去离子水洗涤、烘干。
铈和钌都是极好的催化剂,将制备得到的类水滑石催化剂浸泡在硝酸铈或硝酸钌溶液,然后将其进行干燥,硝酸铈或硝酸钌溶液可以沉淀在类水滑石表面及层隙中,铈具有储氧的能力,钌是氧化活性中心并可以对氨进行分解,可以提高催化效率。
进一步的,将步骤四或五烘干后的催化剂,在200~400℃条件下煅烧。
干燥得到的类水滑石具有较高的活性,但是其内的金属离子容易流失,所以需要对催化剂进行煅烧。如果煅烧温度高于700℃,类水滑石就转变为尖晶石结构,会对极大影湿式催化氧化的催化活性;但是如果低温(小于400℃)进行煅烧,煅烧后的类水滑石中金属离子的仍容易溶出。本发明通过引入载体,使类水滑石在其表面进行生长,其高度分散性及类水滑石与外核的通过氧-金属键的强相互作用,不仅可以提高了催化性能,而且在经烘干或者低温煅烧后,其仍能保持稳定的层状结构,可以大大减少了活性金属离子的溶出,解决现有技术中低温煅烧会导致金属离子溶出的问题。而在低温煅烧过程中硝酸盐可以进行分解,不留杂质离子。
进一步的,所述类水滑石的制备方法,包括以下步骤:
(1)原料的制备:包括硝酸盐溶液和碱溶液;
(2)混合沉淀:将步骤(1)中制备好的碱溶液和硝酸盐溶液混合,反应形成水滑石沉淀,不断搅拌直至不再有沉淀产生;
(3)陈化:将步骤(2)制备得到的水滑石在水浴中陈化;
(4)抽滤:用去离子水对步骤(3)陈化后的水滑石不断进行洗涤抽滤,直至抽滤的滤液呈中性为止;
(5)干燥:将步骤(4)得到的水滑石干燥即得到成品催化剂。
进一步的,所述步骤一,具体包括:将所述步骤(2)制备得到的类水滑石水溶液与载体水溶液,不断搅拌进行负载。
进一步的,所述步骤一,具体包括:将步骤(1)中硝酸盐溶液、碱性溶液与载体混合,不断搅拌进行负载。
进一步的,所述步骤(1)中硝酸盐中的金属阳离子总浓度为1mol/L。
进一步的,所述步骤(1)中碱溶液中的阳离子浓度为硝酸盐中硝酸根离子浓度相等。
综上所述,由于采用了上述技术方案,本发明的有益效果是:
1、本发明通过将类水滑石与载体共沉淀方法制备得到的催化剂,类水滑石中的能够均匀的镶嵌在载体中,使类水滑石不发生团聚,增大了类水滑石的表面活性物质的接触面积,提高了催化性能,提高了降低废水COD的能力。
2、本发明通过引入载体制备的催化剂在低温煅烧过程后,仍能保持稳定的层状结构,同时由于其高度分散性及类水滑石与外核的通过氧-金属键的强相互作用,可以大大减少了活性金属离子的溶出率,其中Cu2+离子的溶出降低了99%,Zn2+离子的溶出降低了99.9%,Fe3+离子的溶出降低了90%。
附图说明
本发明将通过例子并参照附图的方式说明,其中:
附图说明:
图1为传统类水滑石催化剂的SEM图;
图2为Cu1Zn2Fe0.3Al0.7/γ-Al2O3类水滑石SEM图
图3为Cu1Zn2Fe0.3Al0.7/γ-Al2O3类水滑石催化能力再现效果图;
图4为类水滑石催化苯酚降解后的产物。
具体实施方式
本说明书中公开的所有特征,或公开的所有方法或过程中的步骤,除了互相排斥的特征和/或步骤以外,均可以以任何方式组合。
本说明书(包括任何附加权利要求、摘要)中公开的任一特征,除非特别叙述,均可被其他等效或具有类似目的的替代特征加以替换。即,除非特别叙述,每个特征只是一系列等效或类似特征中的一个例子而已。
一种通过共沉淀方法制备类水滑石的方法(类水滑石的制备对本领域技术人员是已知的,在其他实施例中本领域技术人员可以采用其他试剂和条件取得相同化学转化),包括以下步骤:
(1)原料的制备:包括硝酸盐溶液和碱溶液,
硝酸盐溶液:不同实施例可以选择不同种的阳离子,加水配置成阳离子重量为1mol的硝酸盐混合溶液,,
碱溶液:将3.5mol/L的NaOH溶液和0.25mol/L的Na2CO3水溶液混合;
(2)混合沉淀:按照体积比1:1向70℃离子水中同步加入碱溶液和硝酸盐溶液,混合反应形成水滑石沉淀,不断搅拌直至不再有沉淀产生;
(3)陈化:将步骤(2)制备得到的水滑石在80℃水浴中陈化4h;
(4)抽滤:用去离子水对步骤(3)陈化后的水滑石不断进行洗涤抽滤,直至抽滤的滤液呈中性为止;
(5)干燥:将步骤(4)得到的水滑石干燥即得到成品类水滑石。
一种处理有机废水的催化剂的制备方法,包括以下步骤:
步骤一:按照质量比1:1,将制备得到类水滑石与载体过混合(在其他实施例中可以为向步骤(1)中硝酸盐溶液和碱性溶液加入到载体中),不断搅拌进行负载,其中;
步骤二:向步骤一中的负载好的类水滑石,在80℃水浴陈化12h,得到一级催化剂;
步骤三:步骤二得到的一级催化剂用去离子水进行抽滤,抽滤至滤液呈中性,得到二级催化剂;
步骤四:将步骤三得到的二级催化剂进行干燥,得到第三级催化剂;
步骤五:将第三级催化剂浸渍在浸渍在10g/L硝酸钌溶液或20g/L硝酸铈的混合溶液中1~2h,然后用去离子水洗涤、烘干;
步骤六:将步骤五烘干后的催化剂在400℃条件下煅烧2小时。
表1:实施例1~12制备的催化剂的配方特征
表2:实施例1~12制备得到的催化剂的性能
如图3所示,为实施例5制备得到的催化剂在循环利用5次后催化剂对COD的降解率,由图3可知,实施例5制备得到的催化剂,在循环5次之后对苯酚废水COD的降解率都保持在90%以上。
由表2所示,实施例3制备的催化剂的Cu2+离子的溶出降比实施例1低了63.4%,Zn2 +离子的溶出降低了90%,Fe3+离子的溶出降低了92.2%。
实施例5的Cu2+离子的溶出比实施例2降低了37.5%,Zn2+离子的溶出降低了95.5%,Fe3+离子的溶出降低了84.5%。
实施例4对减少金属溶出效果不大,活性基本不变。用COD 20000mg/L的模拟苯酚废水COD的除去率91.5%。
实施例11的Cu2+离子的溶出比实施例1降低了99%,Zn2+离子的溶出降低了99.9%,Fe3+离子的溶出降低了90%。用COD 20000mg/L的模拟苯酚废水COD的除去率98.5%。
实施例12的Cu2+离子的溶出比实施例2降低了99%,Zn2+离子的溶出降低了99.9%,Fe3+离子的溶出降低了91%。用COD 20000mg/L的模拟苯酚废水COD的除去率93.5%。
如图4所示,传统水滑石催化剂处理废水残留物主要是小分子酸(乙酸,已二酸),这些小分子酸在CWO比较难降解,但是通过生物法可以很好的降解。从检测结果的谱图中可知,本发明制备的类水滑石催化剂的催化下残留的有机物主要是苯乙醚,1.5-二异丁基苯醌和3-甲基-1.5-二异丁基苯酚此类大分子,表明实验制备的催化剂对小分子酸具有很好的氧化作用。
本发明并不局限于前述的具体实施方式。本发明扩展到任何在本说明书中披露的新特征或任何新的组合,以及披露的任一新的方法或过程的步骤或任何新的组合。
Claims (10)
1.一种处理有机废水的催化剂,其特征在于,包括类水滑石和载体。
2.根据权利要求1所述的有机废水的催化剂,其特征在于,所述载体为二氧化钛、γ-Al2O3、活性炭、碳化硅、硅藻土、堇青石中的一种或几种的组合。
3.根据权利要求1或2所述的处理有机废水的催化剂的制备方法,其特征在于,包括以下步骤:
步骤一:类水滑石与载体进行负载;
步骤二:向步骤一中的负载好的类水滑石进行水浴陈化,得到一级催化剂;
步骤三:步骤二得到的一级催化剂用去离子水进行抽滤,抽滤至滤液呈中性,得到二级催化剂;
步骤四:将步骤三得到的二级催化剂进行干燥,得到成品催化剂。
4.根据权利要求3所述的有机废水的催化剂的制备方法,其特征在于,还包括以下步骤:
步骤五:将所述步骤四得到的催化剂浸渍在硝酸铈或硝酸钌溶液中1~2h,然后用去离子水洗涤、烘干。
5.根据权利要求4所述的有机废水的催化剂的制备方法,其特征在于,还包括以下步骤:
将步骤四或五烘干后的催化剂,在200~400℃条件下煅烧。
6.根据权利要求3所述的有机废水的催化剂的制备方法,其特征在于,所述类水滑石的制备方法,包括以下步骤:
(1)原料的制备:包括硝酸盐溶液和碱溶液;
(2)混合沉淀:将步骤(1)中制备好的碱溶液和硝酸盐溶液混合,反应形成水滑石沉淀,不断搅拌直至不再有沉淀产生;
(3)陈化:将步骤(2)制备得到的水滑石进行水浴中陈化;
(4)抽滤:用去离子水对步骤(3)陈化后的水滑石不断进行洗涤抽滤,直至抽滤的滤液呈中性为止;
(5)干燥:将步骤(4)得到的水滑石干燥即得到成品类水滑石。
7.根据权利要求6所述的有机废水的催化剂的制备方法,其特征在于,所述步骤一,具体包括:将所述步骤(2)制备得到的类水滑石水溶液与载体水溶液,不断搅拌进行负载。
8.根据权利要求6所述的有机废水的催化剂的制备方法,其特征在于,所述步骤一,具体包括:将步骤(1)中硝酸盐溶液、碱性溶液加入到与载体混合,不断搅拌进行负载。
9.根据权利要求6所述的处理有机废水的催化剂制备方法,其特征在于,所述步骤(1)中硝酸盐中的金属阳离子总浓度为1mol/L。
10.根据权利要求6所述的有机废水的催化剂的制备方法,其特征在于,所述步骤(1)中碱溶液中的阳离子浓度与硝酸盐中硝酸根离子浓度相等。
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