CN113856652B - 一种VOCs高分子吸附材料及其合成方法 - Google Patents
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Abstract
本发明属于减震支座复合材料技术领域,尤其涉及一种VOCs高分子吸附材料及其合成方法。本发明所述VOCs高分子吸附材料为球形,所以在装填为柱状吸附体应用时气体为层流通过,具有操作压力低的优点;吸附材料表面多孔,具有吸附效率高的优点;吸附材料本身具有强疏水性,空气中的水蒸气不影响吸附过程;吸附材料表面经过适度改性,对极性和非极性挥发性有机物具有高的吸附能力。本发明所公开的吸附材料合成方法,合成设备简单,原材料易得,合成操作条件温和,具有生产效率高和成本低的优点。
Description
技术领域
本发明属于吸附材料技术领域,尤其涉及一种VOCs高分子吸附材料及其合成方法。
背景技术
挥发性有机物(VOCs)通常指在常温下,沸点在260℃以下的各种有机化合物,主要由烷烃类、芳烃类、烯烃类、卤代烃类、酯类、醛类、酮类和其他类有机化合物组成。如日常生活中常用的天然气(甲烷)、打火机用的燃气(丁烷)液化石油气(多种烷烃的混合物)以及汽油(主要烷烃、少量烯烃等的混合物)等都是烷烃类的挥发性VOC;轮胎修补用的粘合剂的溶剂主要芳烃类(甲苯)VOC;日常生活中用的PVC管材是卤代烃类VOC的来源(氯乙烯);空调制冷剂用的氯氟烃也是VOC中卤代烃的代表;酯类和酮类VOC一般来源于各种溶剂;醛类则主要来源于工业生产。自然燃烧和人工燃烧以及人类的工业活动是挥发性有机物在自然界中的主要来源。挥发性有机物参与自然界的物质循环过程,是形成PM2.5和臭氧合成主要因素,进而引起雾霾以及光化学烟雾污染,影响人的健康。
大多数挥发性有机物(VOCs)本身就是对人体有害的物质,有些还具有致癌性,代表性的有多环芳烃和亚硝胺等物质,有些具有诱导致癌性如卤代烃、芳香胺等物质。挥发性有机物(VOCs)是环境大气和室内空气污染的主要因素之一,因此VOCs的采集与测定对于监控大气中的污染程度、保护环境大气和维护人的健康具有重要现实意义。
现有技术中常见的VOCs吸附材料有活性炭、石墨化炭黑、改性活性炭、多孔无机材料如氧化铝硅藻土、以及高分子材料如二苯并呋喃多孔聚合物等。活性炭系列吸附材料(含活性炭和改性活性炭)具有成本低廉的优点,对苯系物系列的挥发性有机物具有很好的吸附能力,但也存在诸多缺陷如活性点容易被破坏造成使用缩短寿命短,疏水性不够在吸附过程中容易被水蒸气干扰降低吸附效率;无机材料吸附剂具有强度大,成本低的优点,但存在极性大,吸附挥发性有机物时极容易容易吸水而降低吸附效率;石墨化炭黑拥有良好的吸附性能和稳定性,但是生产条件需3000℃以上的高温且需要稀有气体环境,致使成本高昂;苯并呋喃系列材料合成难度大,合成后需粉碎为无定形物后筛分使用,存在一致性的问题等。
发明内容
为解决上述现有技术中存在的问题,本发明提供了一种VOCs高分子吸附材料,本发明所合成的高分子VOCS吸附材料具有疏水性强、解吸温度低、比表面大等优点。
为实现上述目的,本发明采用如下技术方案:
本发明的一个发明目的是公开了一种VOCs高分子吸附材料,所述VOCs高分子吸附材料为球形多孔材料,在其球形表面和孔内表面的分子层级结构式包括:
本发明的另一个发明目的是公开了一种VOCs高分子吸附材料的合成方法,具体包括以下合成步骤:
S1.高分子微球的合成
具体反应结构式如下:
具体包括以下步骤:
(1)在装配好水浴锅、电动搅拌器和回流冷凝器的1000毫升三颈瓶中,加入300-700毫升1%的明胶水溶液,加入100-200毫升的二乙烯苯溶液(溶解有过氧化二苯甲酰0.2-1.5克,30-50毫升甲苯,10-30毫升庚烷),开动搅拌器搅拌,同时通入氮气,在通入氮气的同时开启回流冷凝水,用搅拌速度控制液滴大小,逐步提高搅拌速度至300-500转/分左右,保持此搅拌速度通氮气搅拌10-40分钟;
(2)开启恒温水浴锅,设置温度为60-80摄氏度,在上述温度下保温反应8-24小时,升温至85-95摄氏度,保温反应2-6小时后降温出料,将反应物抽滤,并用大量热水洗涤三次以上,经过60目和100目筛分,取60-100目之间部分干燥备用;
(3)将60-100目之间珠体用索氏提取器丙酮溶液提取三次,烘干备用;
S2.高分子微球改性
具体反应结构式如下:
具体包括以下步骤:
取上述经过严格干燥的微球10-20克,用50-100份二氯乙烷溶液溶胀,所述二氯乙烷溶液其中包含50-70份二氯乙烷、5-15份无水SnCl4、2-10份乙酰氯、10-20份1-氯丁烷,将上述反应底物转移至装配有恒温水浴锅、电动搅拌器和回流冷凝器(上端装配有干燥装置)的250毫升三颈瓶中,通入干燥的氮气排除氧气,设置温度为40-65摄氏度,保温反应8-16小时,反应完毕,将反应底物抽滤后用丙酮提取三次,干燥至恒重,得改性DVB吸附材料。
有益效果
本发明公开了一种VOCs高分子吸附材料,这种吸附材料为球形,所以在装填为柱状吸附体应用时气体为层流通过,具有操作压力低的优点;吸附材料表面多孔,具有吸附效率高的优点;吸附材料本身具有强疏水性,空气中的水蒸气不影响吸附过程;吸附材料表面经过适度改性,对极性和非极性挥发性有机物具有高的吸附能力。
本发明所公开的吸附材料合成方法,合成设备简单,原材料易得,合成操作条件温和,具有生产效率高和成本低的优点。
附图说明
图1:本发明所合成的VOCs吸附材料吸附53种可挥发性有机物GC-MS谱图。
具体实施方式
以下,将详细地描述本发明。在进行描述之前,应当理解的是,在本说明书和所附的权利要求书中使用的术语不应解释为限制于一般含义和字典含义,而应当在允许发明人适当定义术语以进行最佳解释的原则的基础上,根据与本发明的技术方面相应的含义和概念进行解释。因此,这里提出的描述仅仅是出于举例说明目的的优选实例,并非意图限制本发明的范围,从而应当理解的是,在不偏离本发明的精神和范围的情况下,可以由其获得其他等价方式或改进方式。
以下实施例仅是作为本发明的实施方案的例子列举,并不对本发明构成任何限制,本领域技术人员可以理解在不偏离本发明的实质和构思的范围内的修改均落入本发明的保护范围。除非特别说明,以下实施例中使用的试剂和仪器均为市售可得产品。
实施例1
VOCs高分子吸附材料的合成,具体包括以下合成步骤:
S1.高分子微球的合成,具体包括以下步骤:
(1)在装配好水浴锅、电动搅拌器和回流冷凝器的1000毫升三颈瓶中,加入300毫升1%的明胶水溶液,加入100毫升的二乙烯苯溶液(溶解有过氧化二苯甲酰0.2克,30毫升甲苯,10毫升庚烷),开动搅拌器搅拌,同时通入氮气,在通入氮气的同时开启回流冷凝水,用搅拌速度控制液滴大小,逐步提高搅拌速度至300转/分左右,保持此搅拌速度通氮气搅拌10分钟;
(2)开启恒温水浴锅,设置温度为60摄氏度,在上述温度下保温反应8小时,升温至85摄氏度,保温反应2小时后降温出料,将反应物抽滤,并用大量热水洗涤三次以上,经过60目和100目筛分,取60-100目之间部分干燥备用;
(3)将60-100目之间珠体用索氏提取器丙酮溶液提取三次,烘干备用;
S2.高分子微球改性
取上述经过严格干燥的微球10克,用50份二氯乙烷溶液溶胀,所述二氯乙烷溶液其中包含50份二氯乙烷、5份无水SnCl4、2份乙酰氯、10份1-氯丁烷,将上述反应底物转移至装配有恒温水浴锅、电动搅拌器和回流冷凝器(上端装配有干燥装置)的250毫升三颈瓶中,通入干燥的氮气排除氧气,设置温度为40摄氏度,保温反应8小时,反应完毕,将反应底物抽滤后用丙酮提取三次,干燥至恒重,得改性DVB吸附材料。
实施例2
VOCs高分子吸附材料的合成,具体包括以下合成步骤:
S1.高分子微球的合成,具体包括以下步骤:
(1)在装配好水浴锅、电动搅拌器和回流冷凝器的1000毫升三颈瓶中,加入700毫升1%的明胶水溶液,加入200毫升的二乙烯苯溶液(溶解有过氧化二苯甲酰1.5克,50毫升甲苯,30毫升庚烷),开动搅拌器搅拌,同时通入氮气,在通入氮气的同时开启回流冷凝水,用搅拌速度控制液滴大小,逐步提高搅拌速度至500转/分左右,保持此搅拌速度通氮气搅拌40分钟;
(2)开启恒温水浴锅,设置温度为80摄氏度,在上述温度下保温反应24小时,升温至95摄氏度,保温反应6小时后降温出料,将反应物抽滤,并用大量热水洗涤三次以上,经过60目和100目筛分,取60-100目之间部分干燥备用;
(3)将60-100目之间珠体用索氏提取器丙酮溶液提取三次,烘干备用;
S2.高分子微球改性
取上述经过严格干燥的微球20克,用100份二氯乙烷溶液溶胀,所述二氯乙烷溶液其中包含70份二氯乙烷、15份无水SnCl4、10份乙酰氯、20份1-氯丁烷,将上述反应底物转移至装配有恒温水浴锅、电动搅拌器和回流冷凝器(上端装配有干燥装置)的250毫升三颈瓶中,通入干燥的氮气排除氧气,设置温度为65摄氏度,保温反应16小时,反应完毕,将反应底物抽滤后用丙酮提取三次,干燥至恒重,得改性DVB吸附材料。
实施例3
VOCs高分子吸附材料的合成,具体包括以下合成步骤:
S1.高分子微球的合成,具体包括以下步骤:
(1)在装配好水浴锅、电动搅拌器和回流冷凝器的1000毫升三颈瓶中,加入500毫升1%的明胶水溶液,加入150毫升合适比例的的二乙烯苯溶液(其中含有合适比例的二乙烯苯75毫升溶解有过氧化二苯甲酰0.75克,50毫升甲苯,25毫升庚烷),开动搅拌器搅拌,同时通入氮气,在通入氮气的同时开启回流冷凝水。用搅拌速度控制液滴大小,逐步提高搅拌速度至450转/分左右。保持此搅拌速度通氮气搅拌30分钟。
(2)开启恒温水浴锅,设置温度为70摄氏度,在上述温度下70摄氏度保温反应12小时。升温至90摄氏度,保温反应4小时后降温出料。将反应物抽滤,并用大量热水洗涤三次以上,经过60目和100目筛分,取60-100目之间部分干燥备用
(3)将60-100目之间珠体用索氏提取器丙酮溶液提取三次,烘干备用。
S2.高分子微球改性
取上述经过严格干燥的微球20克,用100毫升二氯乙烷溶胀。加入100二氯乙烷溶液:其中包含70毫升二氯乙烷,10毫升无水SnCl4,5毫升乙酰氯,15毫升1-氯丁烷。将上述反应底物转移至装配有恒温水浴锅、电动搅拌器和回流冷凝器(上端装配有干燥装置)的250毫升三颈瓶中,通入干燥的氮气排除氧气。设置温度为60摄氏度,保温反应12小时以上。反应完毕,将反应底物抽滤后用丙酮提取三次,干燥至恒重,得改性DVB吸附材料。
本发明通过烷基化反应和酰基化反应,烷基化反应增加苯环支链,增加疏水性和对非极性有机物的吸附能力,酰基化反应加入羰基,部分增加极性,以增强对极性挥发性有机物如醇类和酮类的吸附能力。
本发明所合成的VOCs吸附材料吸附53种可挥发性有机物GC-MS谱图如图1所示,53种可挥发性有机物的具体数据如下表1所示。
表1.吸附53种可挥发性有机物GC-MS数据
由图1可以看出,本发明所合成的VOCs吸附材料对极性和非极性挥发性有机物均具有高的吸附能力。
以上实施例仅用以说明本发明的技术方案,而非对其进行限制;尽管参照前述实施例对本发明进行了详细的说明,对于本领域的普通技术人员来说,依然可以对前述实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或替换,并不使相应技术方案的本质脱离本发明所要求保护的技术方案的精神和范围。
Claims (4)
1.一种VOCs高分子吸附材料,其特征在于,所述VOCs高分子吸附材料为球形多孔材料,在其球形表面和孔内表面的分子层级结构式包括:
所述的VOCs高分子吸附材料的合成方法,包括以下合成工艺:
S1.高分子微球的合成;
S2.高分子微球改性;
所述S1.高分子微球的合成,具体包括以下步骤:
(1)在反应容器中加入300-700毫升1%的明胶水溶液,加入100-200毫升的二乙烯苯溶液,所述二乙烯苯溶液中溶解有过氧化二苯甲酰、甲苯、庚烷,搅拌、通入氮气、开启回流冷凝水,搅拌反应10-40分钟;
(2)将反应体系升温至温度为60-80摄氏度,保温反应8-24小时,然后升温至85-95摄氏度,保温反应2-6小时,然后将反应物降温出料;
(3)将反应物后处理,即得到产物高分子微球;
所述S2高分子微球改性,具体包括以下步骤:
取S1所得高分子微球10-20克,用50-100份二氯乙烷溶液溶胀,所述二氯乙烷溶液中包含二氯乙烷、无水SnCl4、乙酰氯、1-氯丁烷,将上述反应底物转移至反应容器中,通入干燥的氮气排除氧气,设置温度为40-65摄氏度,保温反应8-16小时,反应完毕,将反应底物抽滤后用丙酮提取三次,干燥至恒重,即得到最终产物。
2.根据权利要求1所述的一种VOCs高分子吸附材料,其特征在于,步骤1中所述二乙烯苯溶液中溶解有过氧化二苯甲酰0.2-1.5克、甲苯30-50毫升,庚烷10-30毫升。
3.根据权利要求1所述的一种VOCs高分子吸附材料,其特征在于,步骤3中所述反应物后处理具体包括以下步骤:将反应物抽滤,并用热水洗涤三次以上,经过60目和100目筛分,取60-100目之间部分干燥备用;将60-100目之间珠体于索氏提取器中用丙酮溶液提取三次,烘干备用,即得到高分子微球。
4.根据权利要求1所述的一种VOCs高分子吸附材料,其特征在于,所述二氯乙烷溶液中包含50-70份二氯乙烷、5-15份无水SnCl4、2-10份乙酰氯、10-20份1-氯丁烷。
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