CN113058548A - 一种用于VOCs吸附的整体式分子筛吸附剂的制备方法 - Google Patents
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,包括(1)配置柠檬酸溶液,在室温下搅拌;(2)称取分子筛粉末加入到上述柠檬酸溶液中,搅拌形成浆液;(3)将聚四氟乙烯微粉放置在不同形状的模具中,然后将步骤(2)中得到的分子筛浆液滴加到模具中成型,然后在室温下干燥;(4)将干燥后的样品在马弗炉中500‑550℃焙烧4‑6h,即得到整体式分子筛吸附剂。本发明制备方法简单,易操作,不需要添加粘结剂;制备的整体式分子筛吸附剂机械强度高,在干燥条件下,其对甲苯的吸附量达到298mg/g;成型的吸附剂机械强度高,可以达到15N,接近目前工业挤条型分子筛的强度,具有实际工业应用价值。
Description
技术领域
本发明属于吸附剂技术领域,涉及一种用于VOCs吸附的整体式分子筛吸附剂的制备方法。
背景技术
挥发性有机物(VOCs)是指熔点低于室温、沸点在50-260℃之间的挥发性有机化合物的总称,广泛分布在空气、土壤、水体中,并且VOCs种类繁多,主要有烃类、卤代烃、芳香烃、酮类、酯类等。其主要来源于工业源、移动源、生活源,近几年VOCs的排放量一直呈现递增趋势。VOCs种类复杂,严重危害人体的神经及免疫系统,造成呼吸道感染、神经错乱等问题,还可能致癌、致畸、致突变,此外大部分VOCs会形成二次污染,形成光化学烟雾等,严重破坏环境质量及人体健康,因此对VOCs的治理迫在眉睫。
目前对于VOCs控制的方法主要有吸收法、吸附法、催化氧化法、生物降解法等,其中吸附法操作简单,成本较低,净化效率高等特点,成为了应用较广泛的处理方法之一。分子筛具有独特的孔结构,较大的比表面积,较好的稳定性,是一种理想的吸附材料。在实际工业应用中需要将粉末状的分子筛组装成具有一定的宏观形貌和高机械强度的整体式材料进行实际应用。目前工业上通常采用加入粘结剂的方法使分子筛成型。使用的粘结剂分为有机粘结剂和无机粘结剂,有机类粘结剂如合成树脂、聚氨酯、表面活性剂等,此类粘结剂多与无机粘结剂混合使用,一般不能单独使用。无机类粘结剂如粘土、高岭土、硅胶、氧化铝等。成型过程是将分子筛粉末与粘结剂混合,并加入一定量的水,混合均匀。之后采用挤条、喷雾、滚球等方式成型。为了达到分子筛的强度要求,对于粘土类粘合剂需要加至分子筛质量的10%以上。由于加入了较大量的粘结剂,并且粘结剂在煅烧时不能被去除,使得成型的分子筛中实际分子筛含量下降,降低了应用性能。此外,这些成型方式对技术及设备要求较高,物耗能耗较大。因此,以快速且简便的方法制备具有高机械强度的整体式分子筛,并且不影响分子筛本身的应用性能仍然是一个挑战。
发明内容
本发明所要解决的技术问题是克服现有技术的缺陷,提出了一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,该制备方法简单,无需添加粘结剂,并且成型的吸附剂机械强度高,达到15N,接近目前工业挤条型分子筛的强度;此外,表现出优异的吸附性能,在干燥条件下,其对甲苯的吸附量达到298mg/g,比涂覆法制备的整体式分子筛吸附剂的甲苯吸附量高317.9%,比挤压成型的整体式分子筛吸附剂的吸附量高122.0%,具有实际工业应用价值。
为解决上述技术问题,本发明提出了如下技术方案:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,包括以下步骤:
(1)配置柠檬酸溶液,在室温下搅拌;
(2)称取分子筛粉末加入到上述柠檬酸溶液中,搅拌形成浆液;
(3)将聚四氟乙烯微粉放置在不同形状的模具中,然后将步骤(2)中得到的分子筛浆液滴加到模具中成型,然后在室温下干燥;
(4)将干燥后的样品在马弗炉中500-550℃焙烧4-6h,即得到整体式分子筛吸附剂。
所述的步骤(1)中,柠檬酸浓度为1-5mol/L。
所述的步骤(1)中搅拌5-10min。
所述的步骤(2),加入的分子筛质量与柠檬酸溶液的固液比为0.7-1.3g/ml
所述的步骤(2)中搅拌5-10min。
所述的分子筛粉末为Y、Beta、ZSM-5、SSZ-13或SAPO-34分子筛。
所述的不同形状的模具包括球形、立方形、三角形、圆柱形、蜂窝状中的一种或几种。
本发明的有益效果是:制备方法简单,易操作,不需要添加粘结剂;制备的整体式分子筛吸附剂机械强度高,制备方法不影响对VOCs的吸附性能,在干燥条件下,其对甲苯的吸附量达到298mg/g,比涂覆法制备的整体式分子筛吸附剂的甲苯吸附量高317.9%,比挤压成型的整体式分子筛吸附剂的吸附量高122.0%,表现出优异的吸附性能;与原始粉末分子筛相比,对水蒸气的吸附量下降了9%,提高了其疏水性。此外,成型的吸附剂机械强度高,可以达到15N,接近目前工业挤条型分子筛的强度,具有实际工业应用价值。
具体实施方式
下面具体实施例对本发明技术方案作进一步详细描述,所描述的具体实施例仅对本发明进行解释说明,并不用于限制本发明。
实施例1:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,步骤如下:
(1)称取1.0927g柠檬酸溶解在1.3ml去离子水中搅拌5min配制成4mol/L的柠檬酸溶液;
(2)将1.000g Y型分子筛加入到上述柠檬酸溶液中搅拌7min,形成均匀的浆液;固液比为0.77g/ml;
(3)将聚四氟乙烯微粉放置在球性模具中,然后将上述分子筛浆液滴加到每一个球形模具中,形成小球状分子筛吸附剂,在室温下干燥12h;
(4)将干燥后的小球状分子筛吸附剂在马弗炉中550℃焙烧6h,即得到整体式分子筛吸附剂。机械强度达到14N/颗。
实施例2:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,步骤如下:
(1)称取0.2731g柠檬酸溶解在1.2ml去离子水中搅拌5min配制成1mol/L的柠檬酸溶液;
(2)将1.000g Y型分子筛加入到上述柠檬酸溶液中搅拌5min,形成均匀的浆液;固液比为0.83g/ml;
(3)将聚四氟乙烯微粉放置在球性模具中,然后将上述分子筛浆液滴加到每一个球形模具中,形成小球状分子筛吸附剂,在室温下干燥12h;
(4)将干燥后的小球状分子筛吸附剂在马弗炉中500℃焙烧6h,即得到整体式分子筛吸附剂。机械强度达到2N/颗。
实施例3:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,步骤如下:
(1)称取2.4166g柠檬酸溶解在2.3ml去离子水中搅拌7min配制成5mol/L的柠檬酸溶液;
(2)将1.620g Y型分子筛加入到上述柠檬酸溶液中搅拌10min,形成均匀的浆液;固液比为0.7g/ml;
(3)将聚四氟乙烯微粉放置在球性模具中,然后将上述分子筛浆液滴加到每一个球形模具中,形成小球状分子筛吸附剂,在室温下干燥15h;
(4)将干燥后的小球状分子筛吸附剂在马弗炉中550℃焙烧6h,即得到整体式分子筛吸附剂。机械强度达到11N/颗。
实施例4:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,步骤如下:
(1)称取1.0927g柠檬酸溶解在1.3ml去离子水中搅拌10min配制成4mol/L的柠檬酸溶液;
(2)将1.700g Y型分子筛加入到上述柠檬酸溶液中搅拌10min,形成均匀的浆液;固液比为1.3g/ml;
(3)将聚四氟乙烯微粉放置在球性模具中,然后将上述分子筛浆液滴加到每一个球形模具中,形成小球状分子筛吸附剂,在室温下干燥18h;
(4)将干燥后的小球状分子筛吸附剂在马弗炉中550℃焙烧5h,即得到整体式分子筛吸附剂。
实施例5:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,步骤如下:
(1)称取1.0927g柠檬酸溶解在1.3ml去离子水中搅拌5min配制成4mol/L的柠檬酸溶液;
(2)将1.000g Beta型分子筛加入到上述柠檬酸溶液中搅拌7min,形成均匀的浆液;固液比为0.77g/ml;
(3)将聚四氟乙烯微粉放置在球性模具中,然后将上述分子筛浆液滴加到每一个球形模具中,形成小球状分子筛吸附剂,在室温下干燥12h;
(4)将干燥后的小球状分子筛吸附剂在马弗炉中550℃焙烧4h,即得到整体式分子筛吸附剂。
实施例6:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,步骤如下:
(1)称取1.0927g柠檬酸溶解在1.3ml去离子水中搅拌5min配制成4mol/L的柠檬酸溶液;
(2)将1.000g ZSM-5型分子筛加入到上述柠檬酸溶液中搅拌10min,形成均匀的浆液;固液比为0.77g/ml;
(3)将聚四氟乙烯微粉放置在球性模具中,然后将上述分子筛浆液滴加到每一个球形模具中,形成小球状分子筛吸附剂,在室温下干燥10h;
(4)将干燥后的小球状分子筛吸附剂在马弗炉中530℃焙烧6h,即得到整体式分子筛吸附剂。
实施例7:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,步骤如下:
(1)称取1.0927g柠檬酸溶解在1.3ml去离子水中搅拌5min配制成4mol/L的柠檬酸溶液;
(2)将1.000g Y型分子筛加入到上述柠檬酸溶液中搅拌7min,形成均匀的浆液;固液比为0.77g/ml;
(3)将聚四氟乙烯微粉放置在立方形模具中,然后将上述分子筛浆液滴加到立方形模具中,形成整体式分子筛吸附剂,在室温下干燥12h;
(4)将干燥后的立方形分子筛吸附剂在马弗炉中520℃焙烧6h,即得到整体式分子筛吸附剂。
实施例8:
一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,步骤如下:
(1)称取1.0927g柠檬酸溶解在1.3ml去离子水中搅拌5min配制成4mol/L的柠檬酸溶液;
(2)将1.000g Y型分子筛加入到上述柠檬酸溶液中搅拌7min,形成均匀的浆液;固液比为0.77g/ml;
(3)将聚四氟乙烯微粉放置在三角形模具中,然后将上述分子筛浆液滴加到三角形模具中,形成整体式分子筛吸附剂,在室温下干燥12h;
(4)将干燥后的三角形分子筛吸附剂在马弗炉中550℃焙烧6h,即得到整体式分子筛吸附剂。
根据上述实施例可知,以上范围的柠檬酸浓度都适用于整体式分子筛的制备。但是当柠檬酸浓度低于2M时,整体式吸附剂的机械强度较小。该制备方法具有普适性,对于不同种类的分子筛都可以制备整体式吸附剂,并且具有不同形状。相比于其他分子筛成型方法操作简单,灵活性强。
实施例9:
整体式分子筛吸附剂对甲苯气体吸附的应用,以实施例1-3样品为代表:称取0.1g整体式分子筛于吸附装置的石英管反应器中,在吸附开始前对吸附剂进行预处理,200℃加热2小时并进行氮气吹扫去除材料中吸附的水及其他有机杂质。预处理结束后冷却至室温吸附,吸附总流量保持45ml/min,甲苯的初始浓度为1000ppm。通过气相色谱在线检测出口浓度,当出口浓度达到初始浓度的95%,则认为吸附饱和。通过穿透曲线积分面积公式计算甲苯的吸附量。结果发现,以实施例1-3为代表的样品对甲苯的吸附量可以达到262-298mg/g(表1),比涂覆法制备的整体式分子筛吸附剂的甲苯吸附量高317.9%[1],比挤压成型的整体式分子筛吸附剂的吸附量高122.0%[2]。此方法形成的各种整体式分子筛吸附剂具有优异的吸附性能。
表1实施例1-3样品对甲苯和水蒸气的吸附量
参考文献:
[1]罗小会,张文霞,宋宇鹏,等.负载分子筛的蜂窝状陶瓷对VOCs的吸脱附性能[C]//环境工程2019年全国学术年会论文集(中册).2019.
[2]王喜芹,李凯,魏冰,栾志强.硅改性制备疏水性沸石分子筛蜂窝体[J].环境科学.2011,32(12):3653-3656.
本发明公开和提出的技术方案,本领域技术人员可通过借鉴本文内容,适当改变条件路线等环节实现,尽管本发明的方法和制备技术已通过较佳实施例子进行了描述,相关技术人员明显能在不脱离本发明内容、精神和范围内对本文所述的方法和技术路线进行改动或重新组合,来实现最终的制备技术。特别需要指出的是,所有相类似的替换和改动对本领域技术人员来说是显而易见的,他们都被视为包括在本发明精神、范围和内容中。
Claims (7)
1.一种用于VOCs吸附的整体式分子筛吸附剂的制备方法,其特征是包括以下步骤:
(1)配置柠檬酸溶液,在室温下搅拌;
(2)称取分子筛粉末加入到上述柠檬酸溶液中,搅拌形成浆液;
(3)将聚四氟乙烯微粉放置在不同形状的模具中,然后将步骤(2)中得到的分子筛浆液滴加到模具中成型,然后在室温下干燥;
(4)将干燥后的样品在马弗炉中500-550℃焙烧4-6h,即得到整体式分子筛吸附剂。
2.如权利要求1所述的制备方法,其特征是步骤(1)中,柠檬酸浓度为1-5mol/L。
3.如权利要求1所述的制备方法,其特征是步骤(1)中搅拌5-10min。
4.如权利要求1所述的制备方法,其特征是步骤(2),加入的分子筛质量与柠檬酸溶液的固液比为0.7-1.3g/ml。
5.如权利要求1所述的制备方法,其特征是步骤(2)中搅拌5-10min。
6.如权利要求1所述的制备方法,其特征是分子筛粉末为Y、Beta、ZSM-5、SSZ-13或SAPO-34分子筛。
7.如权利要求1所述的制备方法,其特征是不同形状的模具包括球形、立方形、三角形、圆柱形、蜂窝状中的一种或几种。
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