CN108479797A - 凹凸棒土/活性炭复合催化材料的制备方法 - Google Patents
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
本发明公开了凹凸棒土/活性炭复合非均相芬顿催化材料的制备方法,利用价廉易得的天然矿物材料——凹凸棒土和具有较强吸附能力的活性炭作为载体,与具有优越催化性能的铜、锰金属氧化物相结合。本发明由于活性炭的掺入,增加了凹凸棒土的吸附性能,锰的加入提高了样品的催化活性,该新型复合催化材料,可以有效催化过氧化氢处理污水,对有机染料废水、化工、CNC切削液废水等领域等难处理工业废水污染物具有良好的脱色和降解效果。
Description
技术领域
本发明涉及凹凸棒土/活性炭复合催化材料的制备方法,具体涉及一种高效催化降解难降解废水污染物的改性凹凸棒土/活性炭复合催化材料的制备方法,该材料可广泛应用在印染、化工、CNC切削液废水处理等领域。
背景技术
以强氧化性自由基·OH为基础的高级氧化技术对难降解有机污染物有显著的效果。传统Fenton技术主要利用Fe2+与H2O2反应生成·OH,由于其反应条件温和,设备简单,得到工业广泛应用。但是传统Fenton反应存在pH范围窄,产生大量的含铁污泥,H2O2利用率不高的缺点。近年来非均相芬顿反应成为研究热点,它是将过渡金属氧化物负载在固体介质的多相类芬顿体系上,其pH反应范围宽,催化剂可重复利用,利于回收。负载若干金属的载体可显著提高催化氧化效率,据此发展新型水处理技术以工艺简单、耗时较短且能有效提高废水的降解速率等优点成为研究热点。
凹凸棒土(ATP)作为催化剂载体的文献在近年来有所研究。凹凸棒石是一种具有特殊结构、形态、物理化学性质的层链状晶体结构和多孔的晶体形态的非金属矿资源,独特之处在于其微观形貌呈现直径约为30nm~40nm,长度可达数微米的纤维结构,具有很大的比表面积和类似分子筛的微孔结构,表现出很强的表面活性和吸附性能,是一种性能优异的天然纳米矿物材料。作为一种含有特殊通道,存在大量活化中心,比表面积较大的新型多孔材料,具有一定的可塑性及粘结力、优良的吸附和催化氧化性能、独特的分散、耐温、抗盐碱等胶体性质和较高的吸附脱色能力,已经作为催化剂广泛地用于提炼重油、作为一些金属或金属氧化物的担载物、用于选择吸附剂和离子交换剂等。凹凸棒土的催化性能表现为:当某种反应物质寄附于凹凸棒土晶体内部的大孔穴表面上时,其反应速度有所加快,且反应生成的新物质又可以从凹凸棒土粘土内部扩散释放出来,而凹凸棒土晶体格架不被破坏。因此凹凸棒土在用于催化剂方面有很大的潜力。活性炭是一种多孔物质,具有很大的比表面积以及较强的吸附性能,孔隙结构发达,耐热、耐酸碱,并具有一定的机械强度和耐磨性,因此广泛应用于气相或液相吸附剂以及催化剂的载体。
本发明采用活性炭和凹凸棒土复合作为载体能够提高催化剂的催化性能,载体原材料廉价易得,提高资源利用率,符合绿色环保材料要求,同时对于难降解工业废水的实践应用具有实际意义。
发明内容
发明目的:针对上述现有技术中的技术问题,本发明提供凹凸棒土/活性炭复合催化材料的制备方法,利用价廉易得的天然矿物和活性炭材料作为载体,与特殊金属结合形成复合材料,提供一种高效催化过氧化氢降解难降解废水污染物的改性凹凸棒土/活性炭新型催化剂材料。
技术方案:本发明所述的凹凸棒土/活性炭复合催化材料的制备方法,该凹凸棒土/活性炭复合催化材料的制备方法包括以下具体步骤:取一定比例ATP(凹凸棒土)、活性炭粉末,在搅拌下按照液固比3:1的比例加入1mol/L的盐酸溶液进行改性,并在室温下连续搅拌6h后,离心洗涤,至pH为5,将离心得到的固体在70℃下干燥12h后,对固体进行研磨。将研磨后的载体浸渍于一定含量的铜、锰浸渍液中,在25℃下搅拌6h,滤出固体,于烘箱中60℃烘6h后,研磨成粉末。在马弗炉中以300℃煅烧3h,冷却,所得即为非均相芬顿催化材料。
所述ATP(凹凸棒土)与活性炭以质量比2:1混合,所述铜、锰浸渍液为Cu(NO3)2与Mn(NO3)2的摩尔配比为1:2的溶液。。
所述ATP(凹凸棒土),其外观为白色粉末,白度为70.0%,粒度200目。PH约为8.0-9.8。化学成分为:SiO2为55.62%,Al2O3为9.71%,K2O为0.95%,Mg2O为9.92%,Fe2O3为1.99,H2O为0.8%。所述活性炭采用木质粉状活性炭,粒度200目。
有益效果:与现有技术相比,本发明的优点:
(1)本发明利用价廉易得的天然矿物材料——凹土和具有优良性能的活性炭作为载体,与具有优越的催化性能的铜、锰金属氧化物,形成一种新的复合催化材料,增强了复合载体的催化降解性能,负载若干金属的载体可显著提高催化氧化效率。
(2)本发明ATP(凹凸棒石)和活性炭采用盐酸进行改性,从而增加复合载体的比表面积,提高活性金属的负载能力,从而提高了样品的催化活性,对有机染料废水等工业废水具有良好的降解效果,可在染料废水处理实践中进行推广和应用,催化材料价廉易得,提高矿物资源的利用率。
附图说明
图1是凹凸棒土SEM图。
图2是如本发明实施例1所值得催化剂SEM图。
具体实施方式
下面结合具体实施例对本发明的技术解决方案作进一步说明,但是本发明的保护范围不局限于所述实施例,这些实施例不能理解为是对技术解决方案的限制。
实施例1:
取20g ATP(凹凸棒石),10g活性炭粉末,按照固液比3:1的比例加入1mol/L的盐酸溶液进行改性,并在室温下连续搅拌6h后,离心洗涤,至pH为5,将离心得到的固体在70℃下干燥12h后,对固体进行研磨备用。将研磨后的载体浸渍于20mL的1mol/L硝酸铜溶液,40mL的1mol/L硝酸锰溶液中,在25℃下搅拌6h,滤出固体,于烘箱中60℃烘6h后,在马弗炉中以300℃煅烧3h,冷却,所得载体备用。
实施例2:
制备好的ATP/活性炭复合催化材料为催化剂,H2O2为氧化剂,对印染废水生化处理后的出水进行降解处理,通过催化氧化对比实验,得到各种复合材料对印染废水生化处理后的出水的降解率顺序为ATP/活性炭>ATP>活性炭。
实施例3:
取COD为188mg/L,色度为100的印染废水生化处理后的出水溶液100mL,H2O2(浓度为30%)2.4mL,测定ATP/活性炭复合催化剂加入量对废水COD和色度降解率的影响,同时对催化剂进行五次重复利用实验。
结果表明对于100mLCOD浓度为188mg/L,色度为100的印染废水生化处理后的出水,H2O2(浓度为30%)2.4mL时,随着ATP/活性炭复合催化剂投加量的增多,COD的降解率先增后减,对于100mL印染废水生化处理后的出水,投加量1.5g时的COD降解率最大,最大降解率为93%,色度降解率为90%。该催化剂在重复使用5次后,对COD的降解率仍然达到80%,说明其重复使用率较好。
如上所述,尽管参照特定的优选实施例已经表示和表述了本发明,但其不得解释为对本发明自身的限制。在不脱离所附权利要求定义的本发明的精神和范围前提下,可对其在形式上和细节上作出各种变化。
Claims (6)
1.一种凹凸棒土/活性炭复合催化材料的制备方法,其特征在于:该复合催化材料的制备方法包括以下具体步骤:取一定比例ATP(凹凸棒土)、活性炭粉末,在搅拌下按照液固比3:1的比例加入1mol/L的盐酸溶液进行改性,并在室温下连续搅拌6h后,离心洗涤,至pH为5,将离心得到的固体在70℃下干燥12h后,对固体进行研磨。将研磨后的载体浸渍于一定含量的铜、锰浸渍液中,在25℃下搅拌6h,滤出固体,于烘箱中60℃烘6h后,在马弗炉中以300℃煅烧3h,冷却,即得。
2.根据权利要求1所述的凹凸棒土/活性炭复合催化材料的制备方法,其特征在于:所述ATP(凹凸棒土)与活性炭以质量比2:1混合,所述铜、锰浸渍液为含有Cu(NO3)2与Mn(NO3)2的摩尔配比为1:2的溶液。
3.根据权利要求1所述的凹凸棒土/活性炭复合催化材料的制备方法,其特征在于:所述ATP(凹凸棒土)其外观为白色粉末,白度为70.0%,粒度200目。PH约为8.0-9.8。化学成分为:SiO2为55.62%,Al2O3为9.71%,K2O为0.95%,Mg2O为9.92%,Fe2O3为1.99,H2O为0.8%。活性炭采用木质粉状活性炭,粒度200目。
4.一种红凹凸棒土/活性炭复合催化材料,其特征在于根据权利要求1所述的凹凸棒土/活性炭复合催化材料的制备方法所制得。
5.根据权利要求1所述方法所制得的凹凸棒土/活性炭复合催化材料的使用领域,其特征在于,所述领域为工业废水氧化领域。
6.根据权利要求5所述的使用领域,其特征在于,所述领域包括印染、化工、CNC切削液废水领域。
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