CN112058308A - 有机-无机复合甲醛催化组合物及制备方法、空气净化滤芯 - Google Patents
有机-无机复合甲醛催化组合物及制备方法、空气净化滤芯 Download PDFInfo
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- CN112058308A CN112058308A CN202011246260.9A CN202011246260A CN112058308A CN 112058308 A CN112058308 A CN 112058308A CN 202011246260 A CN202011246260 A CN 202011246260A CN 112058308 A CN112058308 A CN 112058308A
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Classifications
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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
- 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
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/869—Multiple step processes
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/894—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
本发明提出有机‑无机复合甲醛催化组合物及制备方法、空气净化滤芯,其重量份组成为:改性催化剂10‑50份,改性膨润土30‑50份,高分子有机聚合物40‑100份。通过稀土元素改性载体搭载贵金属掺杂的复合光催化剂,稀土金属固态离子在催化剂表面形成微环境不仅可有效避免反应过程中水气对催化活性的抑制,还可强化两种光催化剂与Pt之间的协同效应,从而在室温下将甲醛完全催化转化为二氧化碳和水,显著降低贵金属的添加量,而不降低其室温内催化氧化甲醛的性能。通过引入有机聚合物和改性膨润土,表面羟基和网状结构牢牢锁定甲醛分子,将甲醛捕获集中,提升对浓度较低时甲醛分子的分解效率,有效提升对于甲醛去除率不高的问题。
Description
技术领域
本发明涉及一种净化空气中甲醛、PM2.5颗粒物以及有害细菌的组合物,具体涉及一种具有网状结构的高分子有机复合甲醛催化剂的组合物及其制备方法,属于空气净化技术领域。
背景技术
甲醛是危害室内空气污染的主要来源之一。目前,90%的室内污染物超标是由室内装修产生的甲醛所引起。甲醛容易从建筑和家具材料中释放出,释放期可长达15年。长期接触甲醛可能会对人类健康造成严重影响,如过敏反应、皮炎、鼻咽癌和白血病。2006年,甲醛被世界卫生组织列为致癌和致畸物质。鉴于甲醛对人体的危害,世界各国对室内甲醛浓度有严格的规定。因此,从室内空气中有效去除甲醛对改善室内空气质量和保证人体健康至关重要。由此,甲醛清除剂应运而生。
室内净化主要为空气净化器和新风系统。空气净化器又称空气清洁器、空气清新机等,是指能够过滤、吸附、分解或转化各种空气污染物(粉尘、异味、甲醛之类的装修污染、细菌、过敏源等),能有效提高空气清洁度的家电产品,主要分为家用、商用、工业等。目前市场上空气净化器应用领域广泛,使用的技术也各式各样。其中主流技术有活性炭吸附技术、负离子技术、臭氧灭菌技术、光触媒技术、HEPA过滤技术几种。
室内空气净化方法按其原理可分为机械、物理和化学方法三种。机械方法是指利用活性炭吸附、过滤、膜分离等技术实现颗粒物分离;物理方法是指利用负离子或静电技术使微小颗粒物互相吸附,聚合成大颗粒物,从而净化空气的方法;化学方法是通过各种化学反应去除空气中有害物质,主要包括光催化净化、等离子体净化、臭氧氧化净化、化学去除剂净化等技术。不同于另两种方法只改变物质的形态(或相态),化学方法能产生新物质,将有害物质彻底消除。因此,化学净化技术成为室内空气净化领域的研究热点,也是清除甲醛最主要的途径。
其中化学清除剂是靠化学反应来去除污染物,在一定条件下与甲醛发生化学反应,按其活性成分可分为强氧化剂、亲核试剂、催化剂和生物甲醛捕捉剂等四类。研究中应注意化学清除剂安全性和环境相容性。由于室内污染物组成复杂,单一的净化技术难以满足同时去除多种污染物的要求,因此,人们将各种净化技术进行有效组合,并研究其净化效果。
CN110523267A公开了一种甲醛分解催化剂、甲醛催化分解毡及它们的制造方法,该发明的甲醛分解催化剂,主要由δ晶型的MnO2形成的亚微米-微米级花瓣状颗粒所构成。甲醛催化分解毡,包含透气支撑物和附着在透气支撑物上的上述甲醛分解催化剂。上述甲醛分解催化剂涉及特定晶型、微观形貌、直径大小以及直径分布的MnO2颗粒,该MnO2颗粒基于申请人开发的一种规模化生产工艺所得到,该工艺不仅大大提高了甲醛分解催化剂的生产效率,同时,得到的产品即上述甲醛分解催化剂除甲醛效果也突破预期,相比于其他现有甲醛分解催化剂具有理想的除甲醛效率。该发明的甲醛分解催化剂主要是通过特有晶型的强氧化剂来实现,主要解决了催化剂生产成本的问题,其分解方式较为单一,分解效果并不理想。
CN111644052A公开了一种新型高效催化甲醛材料及其制备的数显甲醛净化器,此新型高效催化甲醛材料,包括载体以及载体上涂覆的催化甲醛涂层,所述载体包括固定在一起的无纺布层和复合面料层,所述催化甲醛涂层由如下原料组成:高孔隙率氧化锰纤维微球、甲基甘氨酸脯氨酸、粘接剂、纳米二氧化钛、高锰酸盐、蒸馏水、消泡剂和分散剂;高孔隙率氧化锰纤维微球的制备方法为:通过宽度1.5m、内部纤维杂乱分布的氧化锰纤维膜加捻聚拢成氧化锰纤维束条,然后经切断后挤压成多孔结构纳米纤维微球。由于涂层内的高孔隙率氧化锰纤维微球表面及内部存在大量的微孔。该发明主要通过在无纺布层搭载TiO2涂层,通过物理吸附和光催化剂起到催化分解甲醛,对于常温下捕获和分解甲醛的分解效果并不理想。
CN107096320A公开了一种空气净化方法及空气净化滤芯,采用空气净化方法制作的空气净化滤芯包括初级颗粒过滤层、催化氧化及杀菌层、有机气体吸附层、高效过滤层和臭氧降解催化层;初级颗粒过滤层的孔径大于或等于2.5微米;催化氧化及杀菌层负载有甲醛氧化催化剂和T型管,T型管内放置有二氧化氯缓释片,有机气体吸附层包括用于吸附有机气体的吸附剂颗粒;高效过滤层的过滤孔径小于2.5微米;臭氧降解催化层包括用于将臭氧常温分解为氧气的纳米氧化物催化剂。本发明通过二氧化氯抑制空气净化装置内部致病菌的滋生,且可进一步提高室内空气质量;二氧化氯结合甲醛氧化催化剂,达到了降低甲醛含量和杀菌的双重功能,可以消除室内臭氧污染。该发明的复合净化滤芯主要通过复合本领域常规的二氧化氯缓释片抑制剂以及甲醛氧化催化剂达到分解甲醛的作用,对于常温的甲醛分解效果并不理想,而且二氧化氯缓释片的缓释效果不佳,容易造成二次污染。
现有技术中,对于室内甲醛的分解效果,特别是常温下对于甲醛的捕获和化学分解或光分解效果和分解效率差强人意,没有综合体现。
发明内容
本发明的目的是针对现有技术中存在的技术问题,提供一种具有有机-无机复合结构的空气净化组合物、复合滤芯层及其制备方法。对于甲醛催化剂的选择是甲醛催化氧化技术的关键,本发明通过引入吸附剂、表面修饰的甲醛光催化剂、氧化剂,从而通过高效的催化氧化将甲醛捕获和常温下分解,同时通过高分子的网状结构和缓释功能,提高甲醛的消除效果,使其具有高效分解甲醛、杀菌和降低PM2.5的多重功能,有效改善现有空气净化装置无法有效净化甲醛的性能。
本发明的一方面,提供一种有机-无机复合甲醛催化组合物,其组成如下(重量份):
其中,所述改性催化剂以经稀土金属改性的氧化铝为载体,载体表面负载Pt/光催化剂,其中,光催化剂选自钼酸铁、氧化镍、氧化锌、四氧化三钴、氧化锡、氧化钨中的一种与二氧化钛混合组成,二者的重量比例范围为1:(1-3),所述光催化剂含量占所述改性催化剂总重量的10wt%-13wt%,Pt的含量占所述光催化剂总重量的0.8wt%-1.5wt%,所述稀土金属选自镧、铈、钪的一种或多种,所述稀土金属含量占所述载体总重量的1.5wt%-2.5wt%,所述改性催化剂为纳米级或微米级;
所述改性膨润土采用经过季胺盐复合有机改性剂改性后的有机膨润土;
所述高分子有机聚合物选自聚N-异丙基丙烯酰胺、聚羧乙基纤维素/N-异丙基丙烯酰胺、Nafion树脂中的一种。
可选的,所述改性催化剂负载为Pt/Ni-Ti光催化剂,其中Pt的含量占所述光催化剂总重量的0.8wt%,Ni/Ti的重量比为1:1。
可选的,所述改性催化剂负载为Pt/ Fe-Mo-Ti光催化剂,其中Pt的含量占所述光催化剂总重量的1wt%,Fe-Mo /Ti的重量比为1:2。
可选的,所述稀土金属选自铈和钪,其中氧化铈含量占所述载体总重量的1.5wt%-2wt%,氧化钪含量占所述载体总重量的2wt%-2.5wt%。
可选的,所述季胺盐复合有机改性剂为十二烷基三甲基溴化铵或十四烷基三甲基溴化铵;
可选的,所述高分子有机聚合物为聚羧乙基纤维素/N-异丙基丙烯酰胺。
可选的,所述高分子有机聚合物为Nafion树脂。
本发明的另一方面,提供一种前文记载的甲醛催化组合物的制备方法,具体步骤包括:
(1)制备改性催化剂:
(a)用含稀土金属的溶液浸渍氧化铝载体后,经干燥、焙烧获得经稀土金属改性的氧化铝载体;
(b)将乙二醇碱性溶液与氯铂酸的水溶液超声混合形成Pt前驱体溶液,按照预设比重将所述Pt前驱体溶液加入到光催化剂氧化物的盐溶液充分混合,形成负载Pt/光催化剂前驱体溶液;
(c)将所述经稀土金属改性的氧化铝载体在Pt/光催化剂前驱体溶液中浸渍后,经干燥、焙烧、研磨获得所述改性催化剂;其中,所述改性催化剂为纳米级或微米级;
(2)制备改性膨润土:
(a)准备钠基膨润土水悬浮液;
(b)将季胺盐复合有机改性剂按照1:100-150的重量比混溶于溶剂中,搅拌溶解,形成均一体系,所述季铵盐复合有机改性剂为十二烷基三甲基溴化铵和十四烷基三甲基溴化铵,所述溶剂为DMF或氮甲基吡咯烷酮;
(c)按照所述季胺盐复合有机改性剂加入量是钠基膨润土阳离子交换能力的50%-70%摩尔当量,将所述季胺盐复合有机改性剂加入到上述钠基膨润土悬浮液中,经搅拌、加热回流、洗涤、干燥,研磨后得到所述改性膨润土;
(3)制备有机-无机复合催化剂
(a)常温下,将高分子有机聚合物单体加入去离子水, 在氮气保护下搅拌至均匀;
(b)依次加入所述改性催化剂、所述改性膨润土和二茂铁,形成溶胶液体;
(c)依次加入有机聚合物单体、交联剂、引发剂,用氢氧化钠碱溶液将pH值调至8-11后,加速搅拌,使其交联聚合充分反应,得到有机-无机复合型聚合物凝胶;
(d)将所述有机-无机复合型聚合物凝胶配制成浓度为15%-30%的水溶液,用丙酮对聚合物进行沉淀分离后,在真空干燥箱中进行干燥,干燥温度50-80℃,得到所述甲醛催化组合物。
可选的,所述高分子有机聚合物为N-异丙基丙烯酰胺或Nafion树脂溶液时,所述制备有机-无机复合催化剂,包括:
(a)常温下,将N-异丙基丙烯酰胺单体或Nafion树脂溶液加入去离子水, 在氮气保护下搅拌至均匀;
(b)依次加入所述改性催化剂、所述改性膨润土和二茂铁,形成溶胶液体;
(c)将所述凝胶配制成浓度为15%-30%的水溶液,用丙酮对聚合物进行沉淀分离后,在真空干燥箱中进行干燥,干燥温度50-80℃,得到所述甲醛催化组合物。
本发明的另一方面,提供一种有机-无机复合空气净化滤芯,所述滤芯复合层从空气进入的方向分为三层结构,分别是甲醛催化氧化层、甲醛光催化分解层、甲醛深度分解层;其中,
所述甲醛催化氧化层为,以直径范围为0.5-50nm,长度范围为100nm-50μm的Pt/Ag基碳纳米纤维为载体负载MnO2,Pt/Ag担载量为碳纳米纤维的0.1wt%,MnO2活性组分担载量为载体的10wt%-35wt%;
所述甲醛光催化分解层为由本发明所提出的有机-无机复合甲醛催化组合物形成;
所述甲醛深度分解层为,以石墨烯为载体负载TiO2,活性组分负载量为载体的5wt%-25wt%。
可选的,所述三层结构可以多层重复交替组合,或者所述三层结构与二氧化氯缓释片层、活性炭吸附层组合。
本发明创造性地引入了通过稀土元素改性载体搭载贵金属掺杂的复合光催化剂,稀土金属固态离子在催化剂表面形成的独特微环境不仅可以有效避免反应过程中水气对催化活性的抑制,而且还可以强化两种光催化剂与Pt之间的协同效应,从而在室温下将甲醛完全催化转化为二氧化碳和水,显著降低贵金属的添加量,而不降低其室温内催化氧化甲醛的性能,同时为了解决现有技术甲醛浓度低时分解效果欠佳的问题,通过引入有机聚合物和改性膨润土,表面羟基和网状结构,牢牢锁定甲醛分子,将甲醛捕获集中,提升对浓度较低时,甲醛分子的分解效率。通过吸附剂将甲醛气体吸附到催化剂上,再在其表面进行催化反应,这样可以缩短气体扩散到催化剂表面的时间,并使得表面甲醛气体浓度增大,进而加快反应速率,从而达到强化脱除效果。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案,下面结合具体实施方式对本发明作进一步详细描述。
本发明的一方面,提供以下技术方案,一种有机-无机复合甲醛催化组合物,其组成如下(重量份):
其中,本实施例的其一组份改性催化剂,是以经稀土金属改性的氧化铝为载体,载体表面负载Pt/光催化剂,其中,光催化剂选自钼酸铁、氧化镍、氧化锌、四氧化三钴、氧化锡、氧化钨中的一种与二氧化钛混合组成,二者的重量比例范围为1:(1-3),光催化剂含量占催化剂总重量的10wt%-13wt%,Pt的含量占光催化剂总重量的0.8wt%-1.5wt%,所述的稀土金属选自镧、铈、钪的一种或多种,含量占载体总重量的1.5wt%-2.5wt%,所述改性催化剂为纳米级或微米级。
优选的,在一些实施例中,改性催化剂负载为Pt/Ni-Ti光催化剂,其中Pt的含量占光催化剂总重量的0.8wt%,Ni/Ti的重量比为1:1。
优选的,在另一些实施例中,改性催化剂负载为Pt/ Fe-Mo-Ti光催化剂,其中Pt的含量占光催化剂总重量的1wt%,Fe-Mo /Ti的重量比为1:2。
优选的,上述改性催化剂中的稀土金属选自铈和钪,其中氧化铈含量占载体总重量的1.5wt%-2wt%,氧化钪含量占载体总重量的2wt%-2.5wt%。
本实施例的改性催化剂改变了现有光催化剂单一来源和单一改性的手段,采用经稀土金属改性的氧化铝为载体,稀土金属因具有独特的电子排布结构,独特的价态配置、氧空位为催化性能的提升大有助益。优选稀土铈,不同价态铈离子的转变过程中,伴随着O2的存储和释放,释放的同时形成氧空位可直接参与反应,故而表现出氧化还原性能,同时铈元素的掺杂能够有效的降低光催化剂的光生电子-空穴复合率,所以铈元素掺杂能够显著的提升其光催化性能。其次,氧化铝具有大比表面积和多孔性,可以更为分散均匀地负载光催化剂和起到吸附捕获甲醛的作用。
进一步的,光催化剂的选择具有更好的光催化性能和更温和的催化条件,即在常温或低温下更好地去催化分解甲醛,贵金属以其优良的催化活性常作为催化氧化有机物的催化剂,通过贵金属活性组分与载体的匹配来设计氧化催化剂,可以实现室温条件完全催化氧化甲醛的目的。钼酸铁具有响应紫外可见光、比表面能高、可选择性、外露活性强等优异性能。更值得人们所关注的是,在钼酸铁中钼酸本身就具有催化性能,而且铁也具有催化性能,因此,二者之间可达到协同催化的效果,使得钼酸铁的催化性能更强。NiO、SnO2、ZnO、WO3 都是属于广谱气敏材料,它们对甲醛具有强烈的气敏响应和催化性能。其中NiO作为P型半导体,对甲醛催化和响应尤为突出,通过掺杂贵金属可有效提升对甲醛的选择性和催化氧化性。Co3O4因其具有尖晶石结构,可有效用于甲醛催化氧化。本发明将具有高效光催化性能的钼酸铁、氧化镍、氧化锌、四氧化三钴、氧化锡、氧化钨中的一种与二氧化钛混合组成,通过引入第二种光催化剂,形成复合光催化活性组分,弥补了二氧化钛催化的单一催化性能,通过相互关联作用能常温下能显著提升其对甲醛的催化氧化性能,在保持高活性的条件下,达到降低贵金属的负载量的作用。
其次,本实施例的另一组份改性膨润土,为经过季胺盐复合有机改性剂改性后的有机膨润土;
优选的,在一些实施例中,季胺盐复合有机改性剂为十二烷基三甲基溴化铵或十四烷基三甲基溴化铵,对此不作具体限定。
需要说明的是,本实施例的膨润土是以蒙脱石为主的含水粘土矿,它具有特殊的性质:膨润性、催化性以及阳离子交换性等, 因蒙脱石具有层状结构,其层间可交换的阳离子用有机阳离子取代,晶层之间氧层的联系力很小,所以甲醛分子容易进入层间。经改性后表面硅氧结构具有丰富的表面羟基,能够提升捕获甲醛的能力,经改性后的膨润土,层间距扩大,捕获甲醛性能更好。
另外,本实施例的另一组份高分子有机聚合物,选自聚N-异丙基丙烯酰胺、聚羧乙基纤维素/N-异丙基丙烯酰胺、Nafion树脂中的一种,对此不作具体限定。
优选的,在一些实施例中,所述高分子有机聚合物为聚羧乙基纤维素/N-异丙基丙烯酰胺。当然,在另一些实施例中,还可以选择述高分子有机聚合物为Nafion树脂。
本实施例根据羧甲基纤维素具有丰富的羟基,将树脂单体N-异丙基丙烯酰胺引入链中发生聚合、交联、接枝,形成网状结构,使得甲醛分子易于与网状链接触、渗透入网隙,形成凝胶状物而捕获,将改性催化剂包覆羧甲基纤维素高分子复合作用机理,聚合物分子间的交联度会形成网状结构,通过表面富含的羟基通过物理吸附和化学吸附甲醛,结合改性膨润土,可以牢牢锁住甲醛,然后通过改性催化剂将其催化分解。
本发明还意外发现Nafion树脂引入改性催化剂,同样可以显著提升甲醛的捕获和催化氧化性能,但是考虑到其价格较为昂贵,在考虑成本的情况下优先选择使用其他富含羟基的且具有网状结构的聚合物。
本发明的另一方面,提供一种有机-无机复合甲醛催化组合物的制备方法,具体步骤包括:
(1)制备改性催化剂:
(a)用含稀土金属的溶液浸渍氧化铝载体后,经干燥、焙烧获得经稀土金属改性的改性氧化铝载体;
(b)将乙二醇碱性溶液与氯铂酸的水溶液超声混合形成Pt前驱体溶液,按照比重将前驱体溶液加入到光催化剂氧化物的盐溶液充分混合形成负载Pt/光催化剂前驱体溶液;
(c)将经稀土金属改性的氧化铝载体在Pt/光催化剂前驱体溶液中浸渍后,经干燥、焙烧、研磨获得所述改性催化剂;所述改性催化剂为纳米级或微米级。
(2)制备改性膨润土
(a)准备钠基膨润土水悬浮液;
(b)将季胺盐复合有机改性剂按照1:100-150的重量比混溶于溶剂中,搅拌溶解,形成均一体系,所述的复合有机改性剂为十二烷基三甲基溴化铵和十四烷基三甲基溴化铵,所述溶剂为DMF或氮甲基吡咯烷酮;
(c)按照季胺盐复合有机改性剂加入量是钠基膨润土阳离子交换能力的50%-70%摩尔当量,将季胺盐复合有机改性剂加入到上述钠基膨润土悬浮液中,经搅拌、加热回流、洗涤、干燥,研磨后得到改性有机膨润土;
(3)制备有机-无机复合催化剂
(a)常温下,将高分子有机聚合物单体加入去离子水, 在氮气保护下搅拌至均匀;
(b)依次加入改性催化剂、改性膨润土和二茂铁,形成溶胶液体;
(c)依次加入另外有机聚合物单体、交联剂、引发剂,用氢氧化钠碱溶液将pH值调至8-11后,加速搅拌,使其交联聚合充分反应,得到有机-无机复合型聚合物凝胶;
(d)将凝胶配制成浓度为15%-30%的水溶液,用丙酮对聚合物进行沉淀分离后,在真空干燥箱中进行干燥,干燥温度50-80℃,得到组合物。
需要说明的是,当步骤(3a)中的高分子有机聚合物为N-异丙基丙烯酰胺或Nafion树脂溶液时,制备有机-无机复合催化剂包括以下步骤:
(a)常温下,将N-异丙基丙烯酰胺单体或Nafion树脂溶液加入去离子水, 在氮气保护下搅拌至均匀;
(b)依次加入步骤(1)中形成的改性催化剂、步骤(2)中形成的改性膨润土,以及二茂铁,形成溶胶液体;
(c)将凝胶配制成浓度为15%-30%的水溶液,用丙酮对聚合物进行沉淀分离后,在真空干燥箱中进行干燥,干燥温度50-80℃,得到有机-无机复合甲醛催化组合物。
本发明的另一方面,提供一种有机-无机复合空气净化滤芯,所述滤芯复合层从空气进入的方向分为三层结构(即从外向内包括有三层),分别是甲醛催化氧化层、甲醛光催化分解层、甲醛深度分解层;其中,最外层的甲醛催化氧化层为,以直径为0.5-50nm,长度为100nm-50μm的Pt/Ag基碳纳米纤维为载体负载MnO2,Pt/Ag担载量为碳纳米纤维的0.1wt%,MnO2活性组分担载量为载体的10wt%-35wt%。中间层的甲醛光催化分解层由前文记载的所述有机-无机复合甲醛催化组合物形成。最内层的甲醛深度分解层为,以石墨烯为载体负载TiO2,活性组分负载量为载体的5wt%-25wt%。
需要说明的是,上述三层结构可以多层重复交替组合,或者上述三层结构还可以与二氧化氯缓释片层、活性炭吸附层组合,以达到更好的空气净化效果。
采用本发明的催化剂组合物对甲醛的CADR平均值为300m3 /h以上,对TVOC 的CADR平均值为290 m3 /h以上,显著高于现有技术的平均值。
为了更好地提升甲醛去除性能,根据作用机理,本发明还设计了三层分解层,包括在碳纳米纤维负载强氧化剂二氧化锰,并担载少量Pt/Ag,通过碳纳米纤维高比表面积,强化初步的甲醛氧化效果。第二层通过本发明核心的光催化层,基本上可以实现将浓度较低没有经过强氧化的甲醛捕获收集和分解,第三层通过大比表面积石墨烯负载光催化剂二氧化钛,将没有经过分解的少量甲醛吸附和分解。通过本发明的三层结构基本上可以将甲醛的去除率达到95%以上。
与现有技术相比,本发明具有的有益效果如下:本发明创造性地引入了通过稀土元素改性载体搭载贵金属掺杂的复合光催化剂,稀土金属固态离子在催化剂表面形成的独特微环境不仅可以有效避免反应过程中水气对催化活性的抑制,而且还可以强化两种光催化剂与Pt之间的协同效应,从而在室温下将甲醛完全催化转化为二氧化碳和水,显著降低贵金属的添加量,而不降低其室温内催化氧化甲醛的性能,同时为了解决现有技术甲醛浓度低时分解效果欠佳的问题,通过引入有机聚合物和改性膨润土,表面羟基和网状结构,牢牢锁定甲醛分子,将甲醛捕获集中,提升对浓度较低时,甲醛分子的分解效率。通过吸附剂将甲醛气体吸附到催化剂上,再在其表面进行催化反应,这样可以缩短气体扩散到催化剂表面的时间,并使得表面甲醛气体浓度增大,进而加快反应速率,从而达到强化脱除效果。本发明基于室内甲醛浓度低、释放周期长等特点,改变了传统吸附技术和催化氧化技术,更有利于实现甲醛完全去除,从而实现室内空气质量良性循环,有效提升了现有技术中对于甲醛去除率不高的问题。
下面将结合几个具体实施例进一步说明甲醛催化剂组合物的制备方法:
实施例1
常温下,按担载量为1.5wt%的比例将硝酸铈的乙醇溶液浸渍氧化铝载体后,经干燥、焙烧获得经氧化铈改性的氧化铝载体;将乙二醇和氢氧化钠碱性溶液与氯铂酸的水溶液超声混合形成Pt前驱体溶液,按照Pt负载量为0.8wt%光催化剂的比重将前驱体溶液加入到六水合硝酸镍溶液和TiOSO4溶液充分混合形成负载Pt/NiO-TiO2前驱体溶液,NiO:TiO2比重为1:1;将氧化铈/氧化铝载体在Pt/光催化剂前驱体溶液中浸渍后,光催化剂占载体比重为15wt%,经干燥、焙烧、研磨获得改性催化剂,准备钠基膨润土水悬浮液,将十四烷基三甲基溴化铵按照1:120的重量比混溶于DMF溶剂中,搅拌溶解,形成均一体系,按照十四烷基三甲基溴化铵加入量是钠基膨润土阳离子交换能力的50%摩尔当量,将十四烷基三甲基溴化铵加入到上述钠基膨润土悬浮液中,经搅拌、加热回流、洗涤、干燥,研磨后得到改性有机膨润土;常温下,将20份羧甲基纤维素单体加入去离子水, 在氮气保护下搅拌至均匀,依次加入10份改性催化剂、10份改性膨润土和少量二茂铁、比如1份二茂铁,形成溶胶液体,依次加入20份N-异丙基丙烯酰胺单体、交联剂、引发剂,用氢氧化钠碱溶液将pH值调至8-11后,加速搅拌,使其交联聚合充分反应,得到有机-无机复合型聚合物凝胶;将凝胶配制成浓度为15%的水溶液,用丙酮对聚合物进行沉淀分离后,在真空干燥箱中进行干燥,干燥温度60℃,得到甲醛催化剂组合物。
实施例2
常温下,按担载量为2wt%的比例将氯化镧溶液浸渍氧化铝载体后,经干燥、焙烧获得经氧化镧改性的氧化铝载体;将乙二醇和氢氧化钠碱性溶液与氯铂酸的水溶液超声混合形成Pt前驱体溶液,按照Pt负载量为1wt%光催化剂的比重将前驱体溶液加入到钼酸铁溶液和TiOSO4 溶液充分混合形成负载Pt/Fe-Mo-Ti前驱体溶液,Fe-Mo:Ti比重为1:2;将氧化镧/氧化铝载体在Pt/光催化剂前驱体溶液中浸渍后,光催化剂占载体比重为25wt%,经干燥、焙烧、研磨获得改性催化剂,准备钠基膨润土水悬浮液,将十四烷基三甲基溴化铵按照1:150的重量比混溶于DMF溶剂中,搅拌溶解,形成均一体系,按照十二烷基三甲基溴化铵加入量是钠基膨润土阳离子交换能力的60%摩尔当量,将十二烷基三甲基溴化铵加入到上述钠基膨润土悬浮液中,经搅拌、加热回流、洗涤、干燥,研磨后得到改性有机膨润土;常温下,将40份杜邦公司的Nafion树脂溶液与去离子水在氮气保护下搅拌至均匀,依次加入10份改性催化剂、30份改性膨润土和少量二茂铁、比如1份二茂铁,形成溶胶液体,加速搅拌,使其交联聚合充分反应,得到有机-无机复合型聚合物凝胶;将凝胶配制成浓度为20%的水溶液,用丙酮对聚合物进行沉淀分离后,在真空干燥箱中进行干燥,干燥温度75℃,得到甲醛催化剂组合物。
在上述形成甲醛催化剂组合物的基础上,下面将结合具体实施例进一步说明复合甲醛过滤滤芯制备方法:
实施例3
选择直径为10nm,长度为100nm的碳纳米纤维经酸化、高温去胶后,用水热合成法搭载0.1wt%Ag和30wt%的MnO2,高温煅烧后制备得到甲醛氧化材料,组装过滤第一层分解网,将实施例2制备得到甲醛催化剂组合组有机-无机复合甲醛催化组合物组装成第二层分解网,将石墨烯为载体负载25wt%TiO2材料,组装成第三层分解网,压实形成三层结构的过滤组件,形成复合甲醛过滤滤芯。
可以理解的是,以上实施方式仅仅是为了说明本发明的原理而采用的示例性实施方式,然而本发明并不局限于此。对于本领域内的普通技术人员而言,在不脱离本发明的精神和实质的情况下,可以做出各种变型和改进,这些变型和改进也视为本发明的保护范围。
Claims (11)
1.一种有机-无机复合甲醛催化组合物,其特征在于,其重量份组成如下:
改性催化剂 10-50;
改性膨润土 30-50;
高分子有机聚合物 40-100;
其中,所述改性催化剂以经稀土金属改性的氧化铝为载体,载体表面负载Pt/光催化剂,其中,光催化剂选自钼酸铁、氧化镍、氧化锌、四氧化三钴、氧化锡、氧化钨中的一种与二氧化钛混合组成,二者的重量比例范围为1:(1-3),所述光催化剂含量占所述改性催化剂总重量的10wt%-13wt%,Pt的含量占所述光催化剂总重量的0.8wt%-1.5wt%,所述稀土金属选自镧、铈、钪的一种或多种,所述稀土金属含量占所述载体总重量的1.5wt%-2.5wt%,所述改性催化剂为纳米级或微米级;
所述改性膨润土采用经过季铵盐复合有机改性剂改性后的有机膨润土;
所述高分子有机聚合物选自聚N-异丙基丙烯酰胺、聚羧乙基纤维素/N-异丙基丙烯酰胺、Nafion树脂中的一种。
2.根据权利要求1所述的甲醛催化组合物,其特征在于:所述改性催化剂负载为Pt/Ni-Ti光催化剂,其中Pt的含量占所述光催化剂总重量的0.8wt%,Ni/Ti的重量比为1:1。
3.根据权利要求1所述的甲醛催化组合物,其特征在于:所述改性催化剂负载为Pt/Fe-Mo-Ti光催化剂,其中Pt的含量占所述光催化剂总重量的1wt%,Fe-Mo /Ti的重量比为1:2。
4.根据权利要求1所述的甲醛催化组合物,其特征在于:所述稀土金属选自铈和钪,其中氧化铈含量占所述载体总重量的1.5wt%-2wt%,氧化钪含量占所述载体总重量的2wt%-2.5wt%。
5.根据权利要求1所述的甲醛催化组合物,其特征在于:所述季铵盐复合有机改性剂为十二烷基三甲基溴化铵或十四烷基三甲基溴化铵。
6.根据权利要求1所述的甲醛催化组合物,其特征在于:所述高分子有机聚合物为聚羧乙基纤维素/N-异丙基丙烯酰胺。
7.根据权利要求1所述的甲醛催化组合物,其特征在于:所述高分子有机聚合物为Nafion树脂。
8.一种如权利要求1至7任一项所述的甲醛催化组合物的制备方法,其特征在于:具体步骤包括:
(1)制备改性催化剂:
(a)用含稀土金属的溶液浸渍氧化铝载体后,经干燥、焙烧获得经稀土金属改性的氧化铝载体;
(b)将乙二醇碱性溶液与氯铂酸的水溶液超声混合形成Pt前驱体溶液,按照预设比重将所述Pt前驱体溶液加入到光催化剂氧化物的盐溶液充分混合,形成负载Pt/光催化剂前驱体溶液;
(c)将所述经稀土金属改性的氧化铝载体在Pt/光催化剂前驱体溶液中浸渍后,经干燥、焙烧、研磨获得所述改性催化剂;其中,所述改性催化剂为纳米级或微米级;
(2)制备改性膨润土:
(a)准备钠基膨润土水悬浮液;
(b)将季铵盐复合有机改性剂按照1:100-150的重量比混溶于溶剂中,搅拌溶解,形成均一体系,所述季铵盐复合有机改性剂为十二烷基三甲基溴化铵或十四烷基三甲基溴化铵,所述溶剂为DMF或氮甲基吡咯烷酮;
(c)按照所述季铵盐复合有机改性剂加入量是钠基膨润土阳离子交换能力的50%-70%摩尔当量,将所述季铵盐复合有机改性剂加入到上述钠基膨润土悬浮液中,经搅拌、加热回流、洗涤、干燥,研磨后得到所述改性膨润土;
(3)制备有机-无机复合催化剂
(a)常温下,将高分子有机聚合物单体加入去离子水, 在氮气保护下搅拌至均匀;
(b)依次加入所述改性催化剂、所述改性膨润土和二茂铁,形成溶胶液体;
(c)依次加入高分子有机聚合物单体、交联剂、引发剂,用氢氧化钠碱溶液将pH值调至8-11后,加速搅拌,使其交联聚合充分反应,得到有机-无机复合型聚合物凝胶;
(d)将所述有机-无机复合型聚合物凝胶配制成浓度为15%-30%的水溶液,用丙酮对上述水溶液进行沉淀分离后,在真空干燥箱中进行干燥,干燥温度50-80℃,得到所述甲醛催化组合物。
9.根据权利要求8所述的甲醛催化组合物的制备方法,其特征在于:所述高分子有机聚合物为N-异丙基丙烯酰胺或Nafion树脂溶液时,所述制备有机-无机复合催化剂,包括:
(a)常温下,将N-异丙基丙烯酰胺单体或Nafion树脂溶液加入去离子水, 在氮气保护下搅拌至均匀;
(b)依次加入所述改性催化剂、所述改性膨润土和二茂铁,形成溶胶液体;
(c)将所述凝胶配制成浓度为15%-30%的水溶液,用丙酮对上述水溶液进行沉淀分离后,在真空干燥箱中进行干燥,干燥温度50-80℃,得到所述甲醛催化组合物。
10.一种有机-无机复合空气净化滤芯,其特征在于:
所述滤芯复合层从空气进入的方向分为三层结构,分别是甲醛催化氧化层、甲醛光催化分解层、甲醛深度分解层;其中,
所述甲醛催化氧化层为,以直径范围为0.5nm-50nm,长度范围为100nm-50μm的Pt/Ag基碳纳米纤维为载体负载MnO2,Pt/Ag担载量为碳纳米纤维的0.1wt%,MnO2活性组分担载量为载体的10wt%-35wt%;
所述甲醛光催化分解层由权利要求1至7任一项所述的有机-无机复合甲醛催化组合物形成;
所述甲醛深度分解层为,以石墨烯为载体负载TiO2,活性组分负载量为载体的5wt%-25wt%。
11.根据权利要求10所述的有机-无机复合空气净化滤芯,其特征在于:所述三层结构可以多层重复交替组合,或者所述三层结构与二氧化氯缓释片层、活性炭吸附层组合。
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