CN109603913A - 负载型多孔吸附催化材料及其制备方法和用途 - Google Patents
负载型多孔吸附催化材料及其制备方法和用途 Download PDFInfo
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Abstract
本发明提出了一种负载型多孔吸附催化材料的制备方法,包括以下步骤:将二氧化硅多孔块体材料浸入3~5mg/ml金属酞菁溶液中,于常温下超声10~20分钟,获得二氧化硅多孔块体改性材料;将步骤S1所得二氧化硅多孔块体改性材料洗涤干净后干燥,获得负载型多孔吸附催化材料。本发明还提供一种利用上述方法制备获得的负载型多孔吸附催化材料,该材料吸附甲醛,其去除甲醛的能力高。
Description
技术领域
本发明涉及催化材料技术领域,具体涉及一种负载型多孔吸附催化材料及其制备方法和用途。
背景技术
空气污染问题日益引起广泛重视,其中甲醛的污染问题尤其突出。甲醛作为一种室内污染气体,当浓度达到600微克/立方米时就会对人体的健康造成潜在的危害。近年来,室内空气中甲醛污染的净化方法主要有吸附法、光催化氧化法和化学处理法。吸附法是利用多孔的固体,如沸石、活性炭、多孔粘土等吸附剂,将存在与空气中的甲醛吸附在其表面,从而去除甲醛。光催化氧化法利用对光响应的催化剂,如TiO2、ZnO、WO3、ZnS等金属氧化物或硫化物,利用催化剂产生的羟基自由基和氧负离子将甲醛等有机物分子降解为二氧化碳和水。但应该看到,尽管吸附法具有快速、简单、成本等特点,但大部分吸附材料是微孔材料,其吸附用量大,易饱和,易堵塞,还有二次污染等问题。目前,发展的趋势是将吸附法与光催化氧化法相结合,利用多孔吸附和催化氧化机理,从而吸附降解甲醛,从而彻底解决室内空气中甲醛污染问题。
目前,已有改性二氧化硅用于室内空气净化的报道。专利(CN 108640121 A)公开了改性纳米二氧化硅、制备方法及在制备甲醛产品中的应用。主要是将纳米二氧化硅与γ-氨乙基氨丙基三甲氧基硅烷、青蒿素和/或甘草素复合,制备改性纳米二氧化硅,可以起到长效杀菌、抗菌、分解有害甲醛气体的作用。有人采用有序介孔材料(MCM-41或SBA-15)经胺基改性后来吸附甲醛,有一定的去除效果。也有人用氨基化壳聚糖/二氧化硅气凝胶来吸附甲醛,达到去除甲醛的目的。但目前二氧化硅作为载体,存在孔结构单一、孔结构不易调控的问题,且功能基团或离子负载量难以烤制,负载后易团聚、脱落等问题,极大影响二氧化硅吸附降解甲醛的性能。
专利《一种负载金属酞菁吸附剂及其制备方法和用途》(CN104759259B)公开了一种以二氧化硅为载体,负载金属酞菁的吸附剂,但其用于脱硫,并未告知其具有吸附甲醛的功效,且其用料(二氧化硅)为粉末状,难以回收。
综上,需要对现有技术做进一步改进。
发明内容
本发明要解决的技术问题是提出一种吸附效果佳,易于回收循环使用的负载型多孔吸附催化材料及其制备方法。
为解决上述技术问题,本发明提出一种负载型多孔吸附催化材料的制备方法,包括如下步骤:
S1、将二氧化硅多孔块体材料浸入3~5mg/ml金属酞菁溶液中,于常温(20~35℃)下超声10~20分钟(超声功率为600w~1000w),获得二氧化硅多孔块体改性材料;
S2、将步骤S1所得二氧化硅多孔块体改性材料洗涤干净后干燥,获得负载型多孔吸附催化材料。
作为本发明负载型多孔吸附催化材料的制备方法的改进:
每升金属酞菁溶液的配制方法为:
向3~5g金属酞菁中加入酰胺类溶剂定容至1L,金属酞菁溶解于酰胺类溶剂中,获得3~5mg/mL金属酞菁溶液。
作为本发明负载型多孔吸附催化材料的制备方法的进一步:
所述金属酞菁为酞菁钴或酞菁铁。
作为本发明负载型多孔吸附催化材料的制备方法的进一步:
所述酰胺类溶剂为N,N-二甲基甲酰胺或N,N-二甲基乙酰胺。
作为本发明负载型多孔吸附催化材料的制备方法的进一步:
所述二氧化硅多孔块体是阶层多孔二氧化硅块体材料或大孔二氧化硅块体。
注:上述阶层多孔二氧化硅块体材料为现有材料,例如可选用按照专利号为201410188449.5的发明专利《阶层多孔氧化硅的制备方法》制备获得的阶层多孔二氧化硅块体材料。
上述大孔二氧化硅块体材料为块体材料,例如可选用按照《溶胶-凝胶伴随相分离制备SiO2多孔块体,物理化学学报,2013,29(3),646-652》中所提出的方法制备获得的大孔二氧化硅块体材料。
为解决上述技术问题,本发明还提出一种利用上述制备方法制备获得的负载型多孔吸附催化材料。
为解决上述技术问题,本发明还提出上述负载型多孔吸附催化材料的用途:
所述负载型多孔吸附催化材料用于吸附甲醛。
作为本发明负载型多孔吸附催化材料的用途的改进:
所述负载型多孔吸附催化材料对甲醛(浓度为300ppm)的去除率≥95%。
本发明的技术优势在于:
1、本发明采用的载体为阶层多孔二氧化硅块体材料或大孔二氧化硅块体材料,上述两种材料为具有贯通大孔、共连续骨架的大孔多孔块体材料,其均具有高热稳定性和化学稳定性,比表面积高,具有强的吸附性能;贯通大孔有利于金属酞菁溶液的传输,实现较大的负载量,骨架上的介孔和强的毛细管小,利于抑制金属钛菁的缔合,提高其分散性,从而提高金属酞菁的催化活性;且骨架上的羟基易与钛菁环的基团通过共价键结合,且稳定性,不易脱落;多孔块体的形状可调,具有易回收和再生循环性能,便于实际生产应用。
2、本发明制备所得的负载型多孔吸附催化材料,多孔吸附与氧化催化相结合去除甲醛,其去除甲醛的能力高,甲醛(浓度为300ppm)去除率达95%以上。
具体实施方式
下面结合具体实施例对本发明进行进一步描述,但本发明的保护范围并不仅限于此。
实施例1-1、负载型多孔吸附催化材料的制备方法:
本实施例中以阶层多孔二氧化硅块体材料为载体,酞菁钴(蓝黑色)为光催化材料,N,N-二甲基甲酰胺为溶剂。
本实施例中阶层多孔二氧化硅块体材料按照专利号为201410188449.5的发明专利《阶层多孔氧化硅的制备方法》所提出的方法,以三嵌段共聚物聚氧乙烯-聚氧丙烯-聚氧乙烯(PluronicP123)为模板剂制备的拥有贯通大孔、共连续骨架、骨架上有规则球形介孔的阶层多孔二氧化硅块体材料,即,该专利实施例2-2所制备获得的阶层多孔二氧化硅块体材料,其比表面积为708m2/g。
具体制备方法如下:
S1、向5g的酞菁钴中加入N,N-二甲基甲酰胺定容至1L,酞菁钴溶解于N,N-二甲基甲酰胺中,获得浓度为5mg/mL的酞菁钴溶液;
S2、采用过量浸渍法将阶层多孔二氧化硅块体材料浸入到步骤S1所得酞菁钴溶液中,在常温(25℃)超声20min(超声功率为900w),此时阶层多孔二氧化硅块体材料被酞菁钴溶液充分浸渍,获得阶层多孔二氧化硅块体改性材料。
注:过量浸渍法为现有技术,故无需对其进行详细介绍,也无需告知阶层多孔二氧化硅块体材料和酞菁钴溶液的用量比,相关领域的技术人员即可轻易再现本发明,并达到本法明所告知的技术效果。
S3、将步骤S2所得阶层多孔二氧化硅块体改性材料用水充分洗涤至洗涤液无色(即,洗涤液中没有蓝黑色的酞菁钴),之后放入烘箱于60℃干燥至恒重,获得负载酞菁钴的多孔吸附催化材料。
采用常规甲醛检测设备检测到,利用10g所得多孔吸附催化材料对300ppm甲醛的去除率达97%。
实施例1-2、
本实施例中以阶层多孔二氧化硅块体材料为载体,酞菁铁(墨绿色)为光催化材料,N,N-二甲基乙酰胺为溶剂。
具体制备方法如下:
S1、向4g的酞菁铁中加入N,N-二甲基乙酰胺定容至1L,酞菁铁溶解于N,N-二甲基乙酰胺中,获得浓度为4mg/mL的酞菁铁溶液;
S2、采用过量浸渍法将阶层多孔二氧化硅块体材料浸入到步骤S1所得酞菁铁溶液中,于常温(25℃)超声15min(超声功率为900w),此时阶层多孔二氧化硅块体材料被酞菁铁溶液充分浸渍,获得阶层多孔二氧化硅块体改性材料。
S3、将步骤S2所得阶层多孔二氧化硅块体改性材料用水充分洗涤至洗涤液无色(即,洗涤液中没有墨绿色的酞菁铁),之后放入烘箱于60℃干燥至恒重,获得负载酞菁铁的多孔吸附催化材料。
利用10g所得多孔吸附催化材料对300ppm甲醛的去除率达96%。
实施例2-1、负载型多孔吸附催化材料的制备方法:
本实施例中大孔二氧化硅块体材料为载体,酞菁铁(墨绿色)为光催化材料,N,N-二甲基乙酰胺为溶剂;
本实施例中大孔二氧化硅块体材料按照《溶胶-凝胶伴随相分离制备SiO2多孔块体,物理化学学报,2013,29(3),646-652》中所提出的方法:
即,以正硅酸甲酯为前驱体,0.01mol·L-1盐酸为催化剂,环氧丙烷为凝胶促进剂,聚氧化乙烯(Mv=10000)为相分离诱导剂,在PEO/TMOS摩尔比为0.0018的条件下,制备获得的具有贯通大孔、共连续骨架的大孔多孔块体材料,即,大孔二氧化硅块体材料。该大孔二氧化硅块体材料大孔孔径分布在1-3μm之间,比表面积达719m2·g-1,孔体积为0.48m3·g-1。
具体制备方法如下:
S1、向3g的酞菁铁中加入N,N-二甲基乙酰胺定容至1L,酞菁铁溶解于N,N-二甲基乙酰胺中,获得浓度为3mg/mL的酞菁铁溶液;
S2、采用过量浸渍法将大孔二氧化硅块体材料浸入到步骤S1所得酞菁铁溶液中,在常温(25℃)超声10min(超声功率为900w),此时大孔二氧化硅块体材料被酞菁铁溶液充分浸渍,获得大孔二氧化硅块体改性材料。
S3、将步骤S2所得大孔二氧化硅块体改性材料用水充分洗涤至洗涤液无色(即,洗涤液中没有墨绿色的酞菁铁),之后放入烘箱于60℃干燥至恒重,获得负载酞菁铁的多孔吸附催化材料。
利用10g所得多孔吸附催化材料对300ppm甲醛的去除率达95%。
实施例2-2、负载型多孔吸附催化材料的制备方法:
本实施例中大孔二氧化硅块体材料为载体,酞菁钴(蓝黑色)为光催化材料,N,N-二甲基甲酰胺为溶剂;
具体制备方法如下:
S1、向3g的酞菁钴中加入N,N-二甲基甲酰胺定容至1L,酞菁钴溶解于N,N-二甲基甲酰胺中,获得浓度为3mg/mL的酞菁钴溶液;
S2、采用过量浸渍法将大孔二氧化硅块体材料浸入到步骤S1所得酞菁钴溶液中,在常温(25℃)超声10min(超声功率为900w),此时大孔二氧化硅块体材料被酞菁钴溶液充分浸渍,获得大孔二氧化硅块体改性材料。
S3、将步骤S2所得大孔二氧化硅块体改性材料用水充分洗涤至洗涤液无色(即,洗涤液中没有蓝黑色的酞菁钴),之后放入烘箱于60℃干燥至恒重,获得负载酞菁钴的多孔吸附催化材料。
利用10g所得多孔吸附催化材料对300ppm甲醛的去除率达95%。
最后,还需要注意的是,以上列举的仅是本发明的若干个具体实施例。显然,本发明不限于以上实施例,还可以有许多变形。本领域的普通技术人员能从本发明公开的内容直接导出或联想到的所有变形,均应认为是本发明的保护范围。
Claims (8)
1.负载型多孔吸附催化材料的制备方法,其特征是包括如下步骤:
S1、将二氧化硅多孔块体材料浸入3~5mg/ml金属酞菁溶液中,于常温下超声10~20分钟,获得二氧化硅多孔块体改性材料;
S2、将步骤S1所得二氧化硅多孔块体改性材料洗涤干净后干燥,获得负载型多孔吸附催化材料。
2.根据权利要求1所述的负载型多孔吸附催化材料的制备方法,其特征是:
每升金属酞菁溶液的配制方法为:
向3~5g金属酞菁中加入酰胺类溶剂定容至1L,金属酞菁溶解于酰胺类溶剂中,获得3~5mg/mL金属酞菁溶液。
3.根据权利要求2所述的负载型多孔吸附催化材料的制备方法,其特征是:
所述金属酞菁为酞菁钴或酞菁铁。
4.根据权利要求3所述的负载型多孔吸附催化材料的制备方法,其特征是:
所述酰胺类溶剂为N,N-二甲基甲酰胺或N,N-二甲基乙酰胺。
5.根据权利要求1~4任一所述的负载型多孔吸附催化材料的制备方法,其特征是:
所述二氧化硅多孔块体是阶层多孔二氧化硅块体材料或大孔二氧化硅块体。
6.如权利要求1~5任一所述的制备方法制备获得的负载型多孔吸附催化材料。
7.如权利要求6所述负载型多孔吸附催化材料的用途,其特征是:
所述负载型多孔吸附催化材料用于吸附甲醛。
8.根据权利要求7所述负载型多孔吸附催化材料的用途,其特征是:
所述负载型多孔吸附催化材料对甲醛的去除率≥95%。
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