CN112264094A - 一种可再生的非均相类芬顿催化材料制备方法 - Google Patents
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002808 molecular sieve Substances 0.000 claims abstract description 21
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0213—Preparation of the impregnating solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
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Abstract
本发明公开了一种可再生的非均相类芬顿催化材料制备方法,在催化剂材料的体系设计上,采用介孔分子筛为载体,通过氯代磺酸类有机分子与分子筛表面硅铝羟基的接枝反应对分子筛表面进行磺酸化修饰,利用磺酸基团与Fe形成紧密结合的化学键,增强活性组分在载体上的分散性和结合力,也调节活性组分的化学价态,进而提高芬顿反应的催化效率。在催化剂材料的体系设计上,采用商用沸石作为载体,用聚乙烯亚胺等高分子对载体进行修饰,本发明不仅增强了活性组分在载体上的分散性,也调节了活性组分的化学价态,进而能有效提高芬顿反应的催化效率。
Description
技术领域
本发明涉及环境功能材料领域,具体涉及一种可再生的非均相类芬顿催化材料制备方法。
背景技术
非均相类芬顿催化剂通常将各种价态的铁固定在催化剂或者载体上,如粘土、氧化铝、硅沸石和碳材料。非均相类芬顿反应一般发生在固液界面上,铁作为矿物或吸附离子基本上保持在固相中。其中,碳材料作为催化剂载体固定铁用于非均相类芬顿反应已有诸多应用,其中包括活性炭,碳纳米管、介孔碳和碳气凝胶等。。
芬顿体系在使用过程中具有试剂无毒性,均相体系没有传输阻碍,操作简单,投资相对较小等优点,所以一直广泛用于有毒有害废水的处理中。但传统芬顿法仍存在缺点,如H2O2利用率低,反应所需pH较低,产生的Fe2+和Fe3+影响出水色度等。因此类芬顿体系逐渐受到人们的关注,如通过引入光照(可见光、紫外光)、电流等诱导HO·产生;研究应用于芬顿体系的新型催化剂,提高芬顿体系处理能力并尽量消除其负面影响。
芬顿催化剂早期研究主要集中在均相方面,具有催化反应迅速,无传质阻力,反应条件更温和等优点,常用催化剂为过渡金属,如Co、Fe、Mn、Cu、Ni等盐类,研究表明硫酸铜[宋天顺等,水处理技术,2007,33,22]、硫酸铁[Ramirez J.H.,et.al.,CatalysisToday2005,107,68]催化染料废水的效果均非常显著。随着芬顿体系中催化剂研究的深入,均相催化剂存在适用pH范围较窄、催化剂难以回收利用、化学污泥产量大且难处理等问题,因此,非均相催化剂逐渐成为芬顿体系的研究重点。非均相催化剂与废水的分离较简便,处理流程大大简化,常用非均相催化剂主要分为三类:贵金属(如Pd、Pt、Au、Ag等)、过渡金属(主要为Fe和Co)及稀土金属等。大量研究表明,贵金属和稀土金属具有较高的催化活性和催化稳定性,过渡金属虽然活性相对一般,但价格较低,在非均相芬顿体系催化剂开发上具有显著的发展优势和潜在的发展前景。
发明内容
(一)要解决的技术问题
为了克服现有技术不足,现提出一种可再生的非均相类芬顿催化材料制备方法,以解决上述背景技术中提出的问题。
(二)技术方案
本发明通过如下技术方案实现:本发明提出了一种可再生的非均相类芬顿催化材料制备方法,包括如下步骤:
S1:将介孔分子筛分散到一定量的三氯甲烷中,加入氯磺酸和乙二胺,氮气保护下加热回流4h,冷至室温、过滤,三氯甲烷和丙酮洗涤至无氯离子,150℃真空干燥12h,得到载体;
S2:将高分子聚合物溶于一定量甲醇溶液,再将作为载体的商用沸石分子筛浸渍于上述溶液中;室温下搅拌1-12h,用旋转蒸发仪去除溶剂,30-100℃干燥1-12h,然后高温(120℃)活化;
S3:将活性组分Fe或Co的前驱体配置成前驱体盐溶液;
S4:将活性组分的前驱体盐溶液采用常压浸渍到沸石载体上,浸渍温度为10-25℃,浸渍时间0.5h~12h,以金属元素计,控制催化剂中最终活性组分负载量为5~25wt.%;
S5:将浸渍后的固体在25~120℃下干燥1~5h,然后置于马弗炉中300~700℃下焙烧2~7h,即得到所需的沸石负载型催化剂。
进一步而言,步骤1中,介孔分子筛为MCM-41、SBA-15等介孔分子筛。
进一步而言,步骤2中,高分子聚合物为聚醚酰亚胺或聚乙烯亚胺伙聚甲亚胺,载体为商用Y型沸石、β沸石、丝光沸石、镁碱沸石或ZSM-5沸石,其硅铝比为2-∞,晶粒尺寸为0.1~2μm。
进一步而言,步骤3中,活性组分Fe的前驱体为硝酸铁、硫酸铁、硫酸亚铁、氯化铁等。
进一步而言,步骤4中,前驱体盐溶液浓度为0.18-0.9mol/L。
(三)有益效果
本发明相对于现有技术,具有以下有益效果:
本发明提到的一种可再生的非均相类芬顿催化材料制备方法,在催化剂材料的体系设计上,采用介孔分子筛为载体,通过氯代磺酸类有机分子与分子筛表面硅铝羟基的接枝反应对分子筛表面进行磺酸化修饰,利用磺酸基团与Fe形成紧密结合的化学键,增强活性组分在载体上的分散性和结合力,也调节活性组分的化学价态,进而提高芬顿反应的催化效率。在催化剂材料的体系设计上,采用商用沸石作为载体,用聚乙烯亚胺等高分子对载体进行修饰,不仅增强了活性组分在载体上的分散性,也调节了活性组分的化学价态,进而能有效提高芬顿反应的催化效率。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
本发明提出了一种可再生的非均相类芬顿催化材料制备方法,包括如下步骤:
S1:将介孔分子筛分散到一定量的三氯甲烷中,加入氯磺酸和乙二胺,氮气保护下加热回流4h,冷至室温、过滤,三氯甲烷和丙酮洗涤至无氯离子,150℃真空干燥12h,得到载体;
S2:将高分子聚合物溶于一定量甲醇溶液,再将作为载体的商用沸石分子筛浸渍于上述溶液中;室温下搅拌1-12h,用旋转蒸发仪去除溶剂,30-100℃干燥1-12h,然后高温(120℃)活化;
S3:将活性组分Fe或Co的前驱体配置成前驱体盐溶液;
S4:将活性组分的前驱体盐溶液采用常压浸渍到沸石载体上,浸渍温度为10-25℃,浸渍时间0.5h~12h,以金属元素计,控制催化剂中最终活性组分负载量为5~25wt.%;
S5:将浸渍后的固体在25~120℃下干燥1~5h,然后置于马弗炉中300~700℃下焙烧2~7h,即得到所需的沸石负载型催化剂。
进一步而言,步骤1中,介孔分子筛为MCM-41、SBA-15等介孔分子筛。
进一步而言,步骤2中,高分子聚合物为聚醚酰亚胺或聚乙烯亚胺伙聚甲亚胺,载体为商用Y型沸石、β沸石、丝光沸石、镁碱沸石或ZSM-5沸石,其硅铝比为2-∞,晶粒尺寸为0.1~2μm。
进一步而言,步骤3中,活性组分Fe的前驱体为硝酸铁、硫酸铁、硫酸亚铁、氯化铁等。
进一步而言,步骤4中,前驱体盐溶液浓度为0.18-0.9mol/L。
本发明提到的一种可再生的非均相类芬顿催化材料制备方法,在催化剂材料的体系设计上,采用介孔分子筛为载体,通过氯代磺酸类有机分子与分子筛表面硅铝羟基的接枝反应对分子筛表面进行磺酸化修饰,利用磺酸基团与Fe形成紧密结合的化学键,增强活性组分在载体上的分散性和结合力,也调节活性组分的化学价态,进而提高芬顿反应的催化效率。在催化剂材料的体系设计上,采用商用沸石作为载体,用聚乙烯亚胺等高分子对载体进行修饰,不仅增强了活性组分在载体上的分散性,也调节了活性组分的化学价态,进而能有效提高芬顿反应的催化效率。
上面所述的实施例仅仅是对本发明的优选实施方式进行描述,并非对本发明的构思和范围进行限定。在不脱离本发明设计构思的前提下,本领域普通人员对本发明的技术方案做出的各种变型和改进,均应落入到本发明的保护范围,本发明请求保护的技术内容,已经全部记载在权利要求书中。
Claims (5)
1.一种可再生的非均相类芬顿催化材料制备方法,其特征在于:包括如下步骤:
S1:将介孔分子筛分散到一定量的三氯甲烷中,加入氯磺酸和乙二胺,氮气保护下加热回流4h,冷至室温、过滤,三氯甲烷和丙酮洗涤至无氯离子,150℃真空干燥12h,得到载体;
S2:将高分子聚合物溶于一定量甲醇溶液,再将作为载体的商用沸石分子筛浸渍于上述溶液中;室温下搅拌1-12h,用旋转蒸发仪去除溶剂,30-100℃干燥1-12h,然后高温(120℃)活化;
S3:将活性组分Fe或Co的前驱体配置成前驱体盐溶液;
S4:将活性组分的前驱体盐溶液采用常压浸渍到沸石载体上,浸渍温度为10-25℃,浸渍时间0.5h~12h,以金属元素计,控制催化剂中最终活性组分负载量为5~25wt.%;
S5:将浸渍后的固体在25~120℃下干燥1~5h,然后置于马弗炉中300~700℃下焙烧2~7h,即得到所需的沸石负载型催化剂。
2.根据权利要求1所述的可再生的非均相类芬顿催化材料制备方法,其特征在于:步骤1中,介孔分子筛为MCM-41、SBA-15等介孔分子筛。
3.根据权利要求1所述的可再生的非均相类芬顿催化材料制备方法,其特征在于:步骤2中,高分子聚合物为聚醚酰亚胺或聚乙烯亚胺伙聚甲亚胺,载体为商用Y型沸石、β沸石、丝光沸石、镁碱沸石或ZSM-5沸石,其硅铝比为2-∞,晶粒尺寸为0.1~2μm。
4.根据权利要求1所述的可再生的非均相类芬顿催化材料制备方法,其特征在于:步骤3中,活性组分Fe的前驱体为硝酸铁、硫酸铁、硫酸亚铁、氯化铁等。
5.根据权利要求1所述的可再生的非均相类芬顿催化材料制备方法,其特征在于:步骤4中,前驱体盐溶液浓度为0.18-0.9mol/L。
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