CN113731359A - 一种块状炭气凝胶电吸附材料及制备方法以及吸附剂 - Google Patents
一种块状炭气凝胶电吸附材料及制备方法以及吸附剂 Download PDFInfo
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Abstract
本发明涉及复合材料技术领域,尤其涉及一种块状炭气凝胶电吸附材料及制备方法以及吸附剂,该方法将回收的香烟过滤嘴直接通过溶解再生以及冷冻干燥技术得到废醋纤维素基气凝胶,并且通过原位生长在其表面加载ZIF‑8材料,得到复合气凝胶,随后在管式炉中炭化,得到比表面积大于或者等于1000m2/g的块状凝胶电吸附材料。本发明原料来源简单,生产成本较低,且反应过程简单。由块状炭气凝胶电吸附材料制成的吸附剂既可实现对带电离子的吸附,又便于进行回收利用,减少了对环境造成的二次污染,对于废水的处理具有重大意义。
Description
技术领域
本发明涉及复合材料技术的领域,具体为一种块状炭气凝胶电吸附材料及制备方法以及吸附剂。
背景技术
在过去的几十年里,随着轻工业的快速发展,染料污染问题已经成为废水处理的一个挑战。此外,大多数有机染料是有毒的,可能会破坏生态系统,对人类健康造成风险。因此,针对废水中有机染料的处理,发展了许多技术,如膜分离、化学氧化、电化学氧化降解、吸附、光催化降解等方法。其中,吸附法因其简单而受到广泛关注。
电吸附是一种高效、清洁处理废水的技术。电吸附过程中,水中的阳离子和阴离子在外场作用下被迫向电荷相反的电极移动,并在电极表面上形成电双层,从而实现对离子的储存。目前,电吸附技术被广泛应用于淡化海水等领域。主要的电吸附材料包括活性炭、石墨烯、碳气凝胶等具有高比面积和导电性等优良特性的电极材料。
近年来,许多高比表面积吸附剂被用于去除废水中的有机染料,如活性炭、石墨烯基材料、金属有机框架等。但目前吸附剂多为粉末形式,难以回收利用,易造成二次污染。
发明内容
针对现有技术中粉末状吸附剂难以回收,容易造成二次污染的问题,本发明提供一种块状炭气凝胶电吸附材料及制备方法以及吸附剂。
本发明是通过以下技术方案来实现:
一种块状炭气凝胶电吸附材料的制备方法,制备步骤如下:
S1,将废醋酸纤维素在溶解剂中进行溶解,并在-15~-10℃下冰冻处理,获得冰冻废醋酸纤维素;
S2,将冰冻废醋酸纤维素进行48~72h冷冻干燥,得到废醋酸纤维素基气凝胶;
S3,在废醋酸纤维素基气凝胶表面通过原位生长的方式加载ZIF-8材料,得到复合气凝胶;
S4,对复合气凝胶进行炭化,炭化温度为800~1000℃,炭化时间为60~180min,得到块状炭气凝胶电吸附材料。
优选的,所述废醋酸纤维素由回收的香烟过滤嘴提供。
优选的,所述溶解剂按质量百分比记,包括7wt%的氢氧化钠、12wt%的尿素溶液和81wt%水。
优选的,在S2中,包括以下步骤:
S21,将冰冻废醋酸纤维素在常温下进行解冻,并加入50~200mL乙醇进行搅拌并静置24~48h,得到混合液;
S22,将混合液进行离心洗涤,直至获得中性的离心液;
S23,将离心液进行透析,获得钠离子含量为0.01~0.02mmol的透析液;
S24,将透析液分散在20~100ml去离子水中,并通过冷冻干燥得到废醋酸纤维素基气凝胶。
优选的,在S3中,包括以下步骤:
S31,将1~4mmol的硝酸锌溶于25mL甲醇溶液中,获得硝酸锌-甲醇溶液;
S32,将4~16mmol的2-甲基咪唑溶于25mL甲醇溶液中,获得2-甲基咪唑-甲醇溶液;
S33,将S21获得的硝酸锌-甲醇溶液和SS2获得的2-甲基咪唑-甲醇溶液进行搅拌,获得ZIF-8混合溶液;
S34,将S2中得到的废醋酸纤维素基气凝胶浸泡在SS3中的混合溶液中浸泡12~24h,得到中间体;
S35,将中间体冷冻干燥,得到ZIF-8修饰的复合气凝胶。
优选的,硝酸锌和2-甲基咪唑的摩尔比例为1:4。
优选的,在S3中,进行炭化时通入保护气体。
优选的,所述保护气体为氮气,流量为200~400mL/min。
一种块状炭气凝胶电吸附材料,由块状炭气凝胶电吸附材料的制备方法制备得到,所述块状炭气凝胶电吸附材料的比表面积大于或者等于1000m2/g。
一种吸附剂,吸附剂由块状炭气凝胶电吸附材料制成。
与现有技术相比,发明具有以下有益效果:
本发明一种块状炭气凝胶电吸附材料的制备方法通过冻干将废醋酸纤维素的分子链与ZIF-8材料的分子链进行胶连,从而获得稳定态的复合气凝胶,之后通过炭化对复合气凝胶进行结构稳定和性能改善,工艺简单,经过溶解和冻干即可实现制备。
一种块状炭气凝胶电吸附材料的制备方法获得的块状炭气凝胶电吸附材料既可实现对带电离子的吸附,又便于进行回收利用,减少了对环境造成的二次污染,对于废水的处理具有重大意义。
本发明一种块状炭气凝胶电吸附材料的制备方法的原料来源简单,有助于香烟过滤嘴的回收利用,生产成本较低,符合绿色环保的发展理念。
在炭化过程中引入了氮元素,有助于炭气凝胶结构的稳定并极大的改善了材料的比表面积和导电性。
附图说明
图1是本发明实施例1制备的炭气凝胶电吸附材料的扫描电镜图;
图2是本发明实施例3制备的炭气凝胶电吸附材料的扫描电镜图;
图3是本发明实施例5制备的炭气凝胶电吸附材料的扫描电镜图。
具体实施方式
下面结合具体的实施例对本发明做进一步的详细说明,所述是对本发明的解释而不是限定。
本发明还公开了一种块状炭气凝胶电吸附材料的制备方法,制备步骤如下:
S1,将1~4g的废醋酸纤维素在溶解剂进行溶解,并在-15~-10℃下经过24~48h的冰冻处理,获得冰冻废醋酸纤维素。其中,废醋酸纤维素由回收的香烟过滤嘴提供;溶解剂按质量百分比记,包括7wt%的氢氧化钠、12wt%的尿素溶液和81wt%水。
S2,将冰冻废醋酸纤维素在冷冻干燥机中进行48~72h冷冻干燥,得到废醋酸纤维素基气凝胶;
S21,将冰冻废醋酸纤维素在常温10~30℃下进行解冻,并加入50~200mL乙醇进行搅拌并静置24~48h,得到混合液;
S22,将混合液进行离心洗涤,直至获得中性的离心液;
S23,将离心液进行透析,透析转速为200~500r/min,透析时间为48~72h,获得钠离子含量为0.01~0.02mmol的透析液;
S24,将透析液分散在20~100ml去离子水中,并通过冷冻干燥得到废醋酸纤维素基气凝胶。
S3,在废醋酸纤维素基气凝胶表面通过原位生长的方式加载ZIF-8材料,得到复合气凝胶;其中,硝酸锌和2-甲基咪唑的摩尔比例为1:4。
S31,将1~4mmol的硝酸锌溶于25mL甲醇溶液中,获得硝酸锌-甲醇溶液;
S32,将4~16mmol的2-甲基咪唑溶于25mL甲醇溶液中,获得2-甲基咪唑-甲醇溶液;
S33,将S21获得的硝酸锌-甲醇溶液和SS2获得的2-甲基咪唑-甲醇溶液进行搅拌,搅拌时间为10~20min,获得ZIF-8混合溶液;
S34,将S2中得到的废醋酸纤维素基气凝胶浸泡在SS3中的混合溶液中浸泡12~24h,得到中间体;
S35,将中间体在冷冻干燥机中进行48~72h冷冻干燥,得到ZIF-8修饰的复合气凝胶。
S4,对复合气凝胶在管式炉中进行炭化,炭化温度为800~1000℃,炭化时间为60~180min,升温速率为2~5℃/min。在炭化时,通入氮气,氮气的流量为200~400mL/min,得到比表面积大于或者等于1000m2/g的块状炭气凝胶电吸附材料。
本发明还公开了一种吸附剂,吸附剂由块状炭气凝胶吸附材料制成,这种吸附剂不仅能够对废水中的有机染料进行吸附,还便于人员对处理后的吸附剂进行回收,减少了对水的二次污染,对废水处理有着重要意义。
实施例1
将3.5g氢氧化钠和6g尿素溶于40.5g去离子水中,将回收的1g废醋酸纤维素溶于制备的氢氧化钠/尿素溶液中,冰冻24h后在常温下解冻,并加入50ml的乙醇进行搅拌后,静置24h。然后将混合液离心洗涤至中性,随后透析48h后分散在20ml去离子水中,放置在冷冻干燥机中冻干得到废醋酸纤维素气凝胶。配置1mmol的硝酸锌和4mmol的2-甲基咪唑分别溶于25ml甲醇溶液,然后将两溶液混合搅拌10min。将制备的废醋酸纤维素气凝胶放置在混合溶液中静置12h从而得到ZIF-8修饰的复合气凝胶。将复合气凝胶放置管式炉中进行炭化,炭化温度为800℃,升温速率5℃/min,保温时间60min,氮气流量200ml/min。其扫描电镜图如图1所示,其表面可以看到多孔结构,经康塔比表面积测试仪器测得其比表面积约为1020m2/g。
实施例2
将3.5g氢氧化钠和6g尿素溶于40.5g去离子水中,将回收的2g废醋酸纤维素溶于制备的氢氧化钠/尿素溶液中,冰冻24h后在常温下解冻,并加入50ml的乙醇进行搅拌后,静置24h。然后将混合液离心洗涤至中性,随后透析48h后分散在20ml去离子水中,放置在冷冻干燥机中冻干得到废醋酸纤维素气凝胶。配置4mmol的硝酸锌和16mmol的2-甲基咪唑分别溶于25ml甲醇溶液,然后将两溶液混合搅拌10min。将制备的废醋酸纤维素气凝胶放置在混合溶液中静置12h从而得到ZIF-8修饰的复合气凝胶。将复合气凝胶放置管式炉中进行炭化,炭化温度为850℃,升温速率2℃/min,保温时间80min,氮气流量200ml/min。其表面可以看到多孔结构,经康塔比表面积测试仪器测得其比表面积约为1100m2/g。
实施例3
将14g氢氧化钠和24g尿素溶于162g去离子水中,将回收的4g废醋酸纤维素溶于制备的氢氧化钠/尿素溶液中,冰冻36h后在常温下解冻,并加入200ml的乙醇进行搅拌后,静置36h。然后将混合液离心洗涤至中性,随后透析72h后分散在100ml去离子水中,放置在冷冻干燥机中冻干得到废醋酸纤维素气凝胶。配置4mmol的硝酸锌和16mmol的2-甲基咪唑分别溶于25ml甲醇溶液,然后将两溶液混合搅拌15min。将制备的废醋酸纤维素气凝胶放置在混合溶液中静置24h从而得到ZIF-8修饰的复合气凝胶。将复合气凝胶放置管式炉中进行炭化,炭化温度为900℃,升温速率2℃/min,保温时间120min,氮气流量300ml/min。其扫描电镜图如图2所示,可以看到均匀规整的孔分布,经康塔比表面积测试仪器测得其比表面积高达1400m2/g。
实施例4
将14g氢氧化钠和24g尿素溶于162g去离子水中,将回收的4g废醋酸纤维素溶于制备的氢氧化钠/尿素溶液中,冰冻36h后在常温下解冻,并加入200ml的乙醇进行搅拌后,静置36h。然后将混合液离心洗涤至中性,随后透析72h后分散在100ml去离子水中,放置在冷冻干燥机中冻干得到废醋酸纤维素气凝胶。配置4mmol的硝酸锌和16mmol的2-甲基咪唑分别溶于25ml甲醇溶液,然后将两溶液混合搅拌15min。将制备的废醋酸纤维素气凝胶放置在混合溶液中静置24h从而得到ZIF-8修饰的复合气凝胶。将复合气凝胶放置管式炉中进行炭化,炭化温度为950℃,升温速率2℃/min,保温时间100min,氮气流量300ml/min。经康塔比表面积测试仪器测得其比表面积为1260m2/g。
实施例5
将7g氢氧化钠和12g尿素溶于81g去离子水中,将回收的2g废醋酸纤维素溶于制备的氢氧化钠/尿素溶液中,冰冻48h后在常温下解冻,并加入100ml的乙醇进行搅拌后,静置24h。然后将混合液离心洗涤至中性,随后透析60h后分散在50ml去离子水中,随后放置在冷冻干燥机中冻干得到废醋酸纤维素气凝胶。配置2mmol的硝酸锌和8mmol的2-甲基咪唑分别溶于25ml甲醇溶液,然后将两溶液混合搅拌20min。将制备的废醋酸纤维素气凝胶放置在混合溶液中静置18h从而得到ZIF-8修饰的复合气凝胶。将复合气凝胶放置管式炉中进行炭化,炭化温度为1000℃,升温速率3℃/min,保温时间180min,氮气流量400ml/min。其扫描电镜图如图3所示,经康塔比表面积测试仪器测得其表面积为1346m2/g。
Claims (10)
1.一种块状炭气凝胶电吸附材料的制备方法,其特征在于,制备步骤如下:
S1,将废醋酸纤维素在溶解剂中进行溶解,并在-15~-10℃下冰冻处理,获得冰冻废醋酸纤维素;
S2,将冰冻废醋酸纤维素进行48~72h冷冻干燥,得到废醋酸纤维素基气凝胶;
S3,在废醋酸纤维素基气凝胶表面通过原位生长的方式加载ZIF-8材料,得到复合气凝胶;
S4,对复合气凝胶进行炭化,炭化温度为800~1000℃,炭化时间为60~180min,得到炭气凝胶电吸附材料。
2.根据权利要求1所述的块状炭气凝胶电吸附材料的制备方法,其特征在于,所述废醋酸纤维素由回收的的香烟过滤嘴提供。
3.根据权利要求1所述的块状炭气凝胶电吸附材料的制备方法,其特征在于,所述溶解剂按质量百分比记,包括7wt%的氢氧化钠、12wt%的尿素溶液和81wt%的水。
4.根据权利要求1所述的块状炭气凝胶电吸附材料的制备方法,其特征在于,在S2中,包括以下步骤:
S21,将冰冻废醋酸纤维素在常温下进行解冻,并加入50~200mL乙醇进行搅拌并静置24~48h,得到混合液;
S22,将混合液进行离心洗涤,直至获得中性的离心液;
S23,将离心液进行透析,获得钠离子含量为0.01~0.02mmol的透析液;
S24,将透析液分散在20~100ml去离子水中,并通过冷冻干燥得到废醋酸纤维素基气凝胶。
5.根据权利要求1所述的块状炭气凝胶电吸附材料的制备方法,其特征在于,在S3中,包括以下步骤:
S31,将1~4mmol的硝酸锌溶于25mL甲醇溶液中,获得硝酸锌-甲醇溶液;
S32,将4~16mmol的2-甲基咪唑溶于25mL甲醇溶液中,获得2-甲基咪唑-甲醇溶液;
S33,将S21获得的硝酸锌-甲醇溶液和SS2获得的2-甲基咪唑-甲醇溶液进行搅拌,获得ZIF-8混合溶液;
S34,将S2中得到的废醋酸纤维素基气凝胶浸泡在SS3中的混合溶液中浸泡12~24h,得到中间体;
S35,将中间体进行48~72h冷冻干燥,得到ZIF-8修饰的复合气凝胶。
6.根据权利要求5所述的块状炭气凝胶电吸附材料的制备方法,其特征在于,硝酸锌和2-甲基咪唑的摩尔比例为1:4。
7.根据权利要求1所述的块状炭气凝胶电吸附材料的制备方法,其特征在于,在S3中,进行炭化时通入保护气体。
8.根据权利要求7所述的块状炭气凝胶电吸附材料的制备方法,其特征在于,所述保护气体为氮气,流量为200~400mL/min。
9.一种块状炭气凝胶电吸附材料,其特征在于,由权利要求1-8任意一项所述的方法制备得到,所述块状炭气凝胶电吸附材料的比表面积大于或者等于1000m2/g。
10.一种吸附剂,其特征在于,所述吸附剂由如权利要求1所述的块状炭气凝胶电吸附材料制成。
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