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CN106582545A - 一种净化含苯废气的气凝胶吸附剂及其制备方法 - Google Patents

一种净化含苯废气的气凝胶吸附剂及其制备方法 Download PDF

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CN106582545A
CN106582545A CN201611255433.7A CN201611255433A CN106582545A CN 106582545 A CN106582545 A CN 106582545A CN 201611255433 A CN201611255433 A CN 201611255433A CN 106582545 A CN106582545 A CN 106582545A
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silicon
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何小波
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Beijing University of Chemical Technology
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Abstract

本发明涉及一种净化含苯废气气凝胶吸附剂及其制备方法。本发明吸附剂以含硅铝气凝胶为基体，含有0.1％～30％的助剂组分，助剂组分是含Cu、Ca、Ba和Mg物质中一种或几种物质。本发明吸附剂克服了现有技术吸附剂吸附容量低，再生性差等缺陷，大大提高了吸附剂对苯的去除率。本发明吸附剂非常适用于含苯废气的净化处理。

Description

一种净化含苯废气的气凝胶吸附剂及其制备方法
技术领域
本发明涉及一种吸附剂及其制备方法，特别是用于净化含苯废气的负载型含硅铝气凝胶吸附剂及其制备方法。
背景技术
各种工业生产过程中，经常产生一些有毒有害物质，特别是一些含苯废气，这些含苯废气的排放会带来严重的环境污染。目前，对这类废气的治理方法主要有吸附法、燃烧法、洗涤法、催化氧化等，其中吸附法以其工艺简单、操作方便、净化效率高而应用广泛，其中采用的吸附剂主要为活性炭。另外，用于含苯的吸附剂一般需要负载其它金属组分，以提高吸附速率和吸附容量。但是活性炭吸附剂大多吸附容量较低，而且不易再生，运行费用较高。
含硅铝气凝胶是由金属离子和有机配体相互桥联形成的一种新型多孔材料，具有高比表面积、大孔容、结构和功能可调等显著优点，因而在吸附领域表现出巨大的应用潜力。
发明内容
针对现有技术的不足，本发明提供一种净化含苯废气的负载型含硅铝气凝胶吸附剂及其制备方法，提高了含苯废气中苯的去除效率，本发明吸附剂可以适用于各种含苯废气的吸附净化处理。
本发明净化含苯废气吸附剂以含硅铝气凝胶为基体，含有0.1％～30％(占含硅铝气凝胶重量)的助剂组分，助剂组分是含Cu、Ca、Ba和Mg等物质中一种或几种物质的盐类。
本发明净化含苯废气吸附剂的制备过程包括以下步骤：
(l)制备含硅铝气凝胶颗粒；
(2)配制含助剂组分的浸渍溶液；
(3)用浸渍溶液浸渍含硅铝气凝胶基体0.01～60小时，浸渍时间优选为0.1～20小时。需要负载多种添加组分时，可以采用共浸，也可以采用分浸方式；
(4)进行活化，得到改性负载型含硅铝气凝胶吸附剂。
上述步骤(l)中所述的含硅铝气凝胶颗粒先采用水热法制备，金属离子前驱体选用硝酸铬或者氯化铬，有机配体是对苯二甲酸或1,3,5-苯三甲酸或它们的混合，然后根据需要进行成型。含硅铝气凝胶的比表面积为1000～4000m2/g，孔径大小为0.5～10nm。含硅铝气凝胶的颗粒大小可以根据使用需要确定，一般可以是直径2～5mm球型、条形、三叶草型等，条形或三叶草形颗粒的长度一般为2～l0mm。
上述步骤(2)中所述的浸渍溶液可以根据本领域常规知识配制，选择所需助剂组分的化合物，配制浓度适宜的水溶液。需要负载多种组分时，可以分别配制浸渍溶液进行分浸，也可以配制混合溶液进行共浸，优选共浸。溶液的浓度一般为重量浓度为0.5％～30％。溶质一般选择盐类
步骤(4)所述的活化采用常规操作方式，包括干燥和焙烧，干燥一般在常温～150℃下进行1～60小时，焙烧一般在180～400℃、优选200～300℃惰性气体环境下进行0.5～30小时、优选1～10小时。
本发明方法采用含硅铝气凝胶作为吸附材料，提高了含苯废气中苯的去除效果。可能的原因是：含硅铝气凝胶是具有很高比表面积的多孔性物质，同时也是吸附能力较强的物质，其孔道绝大部分是为微孔，具有强烈的吸附作用，而少量的大孔主要起大孔和中孔、微孔的桥梁作用，使吸附质能迅速进入中微孔。经实验表明，本发明吸附剂用于含苯废气净化处理时，具有较快的吸附速率、较高的吸附容量和良好的再生性能。
具体实施方式
实施例1
制取含硅铝气凝胶
采用水热合成法，由金属盐(例如Cr(NO3)2等)，有机配体(例如均苯三甲酸)，在水作为溶剂的条件下混合均匀，在220℃下反应，即得到产物含硅铝气凝胶，将所得产品于75℃下烘干24小时，除去空穴中的有机溶剂。
将浓度为2％(质量浓度)的Na2SiO3溶液混入粉状含硅铝气凝胶中，Na2SiO3溶液的体积比与含硅铝气凝胶炭粉的体积比为1：1，挤压成型，在300℃用水蒸气进行活化处理5小时。
5％浓度(质量浓度)的Cu(NO3)2溶液在上述制备的含硅铝气凝胶颗粒中浸泡30min，混合溶液与含硅铝气凝胶颗粒的体积比为1:1。然后在110℃下烘干，再在200℃氮气气氛下活化5小时，制备吸附剂。
将300mg/m3的含苯废气通入由上述方法制备的吸附剂，在常温、空速为1000h-1条件下，苯的去除效果如表1。
实施例2
含硅铝气凝胶基体制备如实例1
5％浓度(质量浓度)的CaCl2溶液在上述制备的含硅铝气凝胶颗粒中浸泡1200min，混合溶液与含硅铝气凝胶颗粒的体积比为1:1。然后在130℃下烘干，再在300℃氮气气氛下活化30小时，制备一系列吸附剂。
将300mg/m3的含苯废气通入由上述方法制备的吸附剂，在常温、空速为1000h-1条件下，苯的去除效果如表1。
实施例3
含硅铝气凝胶基体制备如实例1
5％浓度(质量浓度)的Mg(NO3)2溶液在上述制备的含硅铝气凝胶颗粒中浸泡80min，混合溶液与含硅铝气凝胶颗粒的体积比为1:1。然后在150℃下烘干，再在300℃氮气气氛下活化2小时，制备一系列吸附剂。
将300mg/m3的含苯废气通入由上述方法制备的吸附剂，在常温、空速为1000h-1条件下，苯的去除效果如表1。
实施例4
含硅铝气凝胶基体制备如实例1
5％浓度(质量浓度)的BaCl2溶液在上述制备的含硅铝气凝胶颗粒中浸泡500min，混合溶液与含硅铝气凝胶颗粒的体积比为1:1。然后在100℃下烘干，再在200℃氮气气氛下活化10小时，制备一系列吸附剂。
将300mg/m3的含苯废气通入由上述方法制备的吸附剂，在常温、空速为1000h-1条件下，苯的去除效果如表1。
实施例5
5％浓度(质量浓度)的Cu(NO3)2溶液在活性炭颗粒中浸泡30min，混合溶液与活性炭颗粒的体积比为1:1。然后在110℃下烘干，再在200℃氮气气氛下活化5小时，制备吸附剂。
将300mg/m3的含苯废气通入由上述方法制备的吸附剂，在常温、空速为1000h-1条件下，苯的去除效果如表1。
表1
实例 基体 助剂 苯的进口浓度(mg/m3) 苯的出口浓度(mg/m3) 苯的去除率(％)
1 含硅铝气凝胶 Cu(NO3)2 300 5.4 98.2
2 含硅铝气凝胶 CaCl2 300 3.3 98.9
3 含硅铝气凝胶 Mg(NO3)2 300 7.2 97.6
4 含硅铝气凝胶 BaCl2 300 5.7 98.1
5 活性炭 Cu(NO3)2 300 41.1 86.3

Claims (10)

1.一种净化含苯废气的气凝胶吸附剂，以含硅铝气凝胶为基体，含有0.1～30％的助剂组分(以含硅铝气凝胶重量计)，助剂组分是含Cu、Ca、Ba和Mg物质中一种或几种物质。
2.按照权利要求l所述的气凝胶吸附剂，其特征在于所述的基体是金属有机骨架含硅铝气凝胶。
3.按照权利要求2所述的气凝胶吸附剂，其特征在于所述的助剂组分为含Cu、Ca、Ba和Mg物质中一种或几种，含量以含硅铝气凝胶重量计为0.1～30％。
4.按照权利要求l所述的气凝胶吸附剂，其特征在于所述的助剂是所选元素的盐。
5.一种权利要求1～4所述任一气凝胶吸附剂的制备方法，包括以下步骤：
(1)制备含硅铝气凝胶颗粒；
(2)配制含助剂组分的浸渍溶液；
(3)用浸渍溶液浸渍含硅铝气凝胶颗粒0.01～60小时；
(4)进行活化，得到改性负载型含硅铝气凝胶气凝胶吸附剂。
6.按照权利要求5所述的方法，其特征在于在步骤(1)所述含硅铝气凝胶，采用水热法制备，金属离子前驱体选用硝酸铬或者氯化铬，有机配体是对苯二甲酸或者1,3,5-苯三甲酸或者它们的混合。
7.按照权利要求5所述的方法，其特征在于在步骤(1)所述含硅铝气凝胶,其比表面积为1000～4000m2/g，孔径大小为0.5～10nm。
8.按照权利要求5所述的方法，其特征在于步骤(3)所述的浸渍时间为0.1～20小时。
9.按照权利要求5所述的方法，其特征在于步骤(4)所述的活化包括干燥和焙烧，干燥在常温～150℃下进行1～50小时，焙烧一般在180～300℃惰性气体环境下进行0.5～30小时。
10.按照权利要求5所述的方法，其特征在于步骤(2)所述浸渍溶液的重量浓度为0.5％～40％，溶质选择盐类。
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