CN117019118B - 一种用于苯系废气的过滤材料及其制备方法 - Google Patents
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Abstract
本发明属于过滤分离材料技术领域,涉及一种用于苯系废气的过滤材料及其制备方法。该过滤材料的制备方法包括:将多孔膜置于制膜器中,浸没第一液体,50~60℃超声水浴4~8h,30℃真空干燥12~24h;再加入第二液体浸没,50~60℃超声水浴6~10h,30℃真空干燥12~24h。该过滤材料能够用于分离苯系废气,在获得气体高渗透通量和高耐用性的前提下,改善过滤材料的稳定性,制备方法简单,适合工业化生产。
Description
技术领域
本发明属于过滤分离材料技术领域,涉及一种用于苯系废气的过滤材料及其制备方法。
背景技术
苯系废气的来源包括运输和许多工厂或工业过程,包括化工,电力和制药厂,加油站,炼油,印刷,制鞋,食品加工,汽车,家具和纺织品制造等方面。同时,苯系废气也是重要的室内空气污染源之一。许多苯系废气具有致畸变性和致癌性,因而对人体的危害十分严重。由于苯系物结构的特点,开环需要的能量大,是典型的难降解工业废气之一。苯系废气具有难降解、开环后成分复杂、毒性大等特点。
CN107185482B公开了一种由改性海泡石吸附苯乙烯废气的方法,首先将低比表面积海泡石浸入一定比例的水中,恒温浸渍一段时间,溶液抽滤,将滤饼干燥、破碎;再浸入一定体积盐酸一段时间,将溶液抽滤,滤饼干燥、破碎即可得改性海泡石,然后将改性海泡石装入吸附塔,在0~80℃高效吸附含有苯乙烯的恶臭废气。CN107185482B公开了一种用于吸附苯乙烯废气的新型粘土复合吸附材料的制备方法,所述方法包括如下步骤:(1)将粘土加入到酸性溶液中,室温下搅拌,得到溶液A;(2)在溶液A中加入表面活性剂,室温下搅拌,得到溶液B;(3)在溶液B中再加入硅源、铝源搅拌;(4)将步骤(3)中得到的产物过滤洗涤至中性,干燥,然后粉碎成颗粒;(5)取过渡金属硝酸盐溶于去离子水中,溶解配成盐溶液,滴加在上诉颗粒上,搅拌,干燥,然后焙烧。但上述方法合成的材料,其吸附过滤性能提高有限,对于多种苯系物构成的苯系废气的过滤吸附性能不佳,实验步骤较为繁琐。
发明内容
本发明的目的在于实现苯系废气的吸附过滤和分离,实现苯系废气去除的高效稳定。
基于上述目的,本申请通过提供一种用于苯系废气的过滤材料及其制备方法来满足本领域的这种需要。
一方面,本发明涉及一种用于苯系废气的过滤材料的制备方法,其包括:将多孔膜置于制膜器中,浸没第一液体,50~60℃超声水浴4~8h,30℃真空干燥12~24h;再加入第二液体浸没,50~60℃超声水浴6~10h,30℃真空干燥12~24h;
所述第一液体的制备方法为:采用硅烷偶联剂对氧化石墨烯纳米片进行表面改性,加入丙酮,投入环氧树脂中,50~60℃超声水浴搅拌2~4h,注入固化剂和促进剂,继续50~60℃超声水浴搅拌1~3h;
所述第二液体的制备方法为:在搅拌条件下,将单宁酸溶解在三羟甲基氨基甲烷盐酸盐溶液中,然后加入乙醇与氨基丙基三乙氧基甲硅烷,最后投入针状活性炭、Co(NO3)2·6H2O和硫脲,80~90℃超声水浴搅拌12~24h。
进一步地,本申请提供的制备方法中,所述第一液体的制备方法为:每1L丙酮中,加入10~30g氧化石墨烯纳米片和40mg硅烷偶联剂,超声搅拌8h,然后离心干燥,制得改性氧化石墨烯纳米片;
每30~50mg所述改性氧化石墨烯纳米片,加入50~100mL丙酮,然后加入100~200g预热后的环氧树脂,50~60℃超声水浴搅拌2~4h,注入固化剂和促进剂,继续50~60℃超声水浴搅拌1~3h,制得淡黄色的所述第一液体。
进一步地,本申请提供的制备方法中,所述固化剂为MTHPA,所述促进剂为DMI-1,2。
进一步地,本申请提供的制备方法中,所述第二液体的制备方法为:在搅拌条件下,每50~100mg单宁酸溶解在50~100mL三羟甲基氨基甲烷盐酸盐溶液中,然后加入5~10mL乙醇与50~100mg氨基丙基三乙氧基甲硅烷,最后投入5~10g针状活性炭、1.2~1.5g Co(NO3)2·6H2O和0.3~0.5g硫脲,80~90℃超声水浴搅拌12~24h。
进一步地,本申请提供的制备方法中,所述三羟甲基氨基甲烷盐酸盐溶液的pH为8~9。
进一步地,本申请提供的制备方法中,任一所述真空干燥的真空度为100~140Pa。
进一步地,本申请提供的制备方法中,所述加入第二液体浸没前,擦干表面液体。
另一方面,本发明涉及一种用于苯系废气的过滤材料,其采用上述的方法制得。
另一方面,本发明涉及一种用于苯系废气的过滤器,其包含上述的过滤材料。
本发明与现有技术相比具有以下有益效果或者优点:
本发明提供的过滤材料,采用Co(NO3)2·6H2O和硫脲的加入,并选择针状活性炭,能够实现分离过滤苯系废气,防止了多种苯系物掺杂下对过滤/吸附性能的抑制作用。本发明提供的过滤材料,采用Co(NO3)2·6H2O和硫脲的加入,显著提高了对苯系废气分离效率;选择针状活性炭,显著提高了过滤材料的渗透通量,在获得气体高渗透通量和高耐用性的前提下,改善过滤材料的稳定性,制备方法简单,适合工业化生产。
具体实施方式
下面,结合实施例对本发明的技术方案进行说明,但是,本发明并不限于下述的实施例。
下述各实施例中实验方法和检测方法,如无特殊说明,均为常规方法;药剂和材料,如无特殊说明,均可在市场上购买得到;指标数据,如无特殊说明,均为常规测量方法。
实施例1
本实施例提供了一种用于苯系废气的过滤材料的制备。
(1)第一液体的制备:取1L丙酮,加入10g氧化石墨烯纳米片和40mg硅烷偶联剂(KH560),超声搅拌8h,然后离心干燥,制得改性氧化石墨烯纳米片。取30mg改性氧化石墨烯纳米片,加入50mL丙酮,然后加入100g预热后的环氧树脂,50℃超声水浴搅拌2h,注入0.5w%固化剂(MTHPA)和1w%促进剂(DMI-1,2),继续50℃超声水浴搅拌1h,制得淡黄色的第一液体。
(2)第二液体的制备:在搅拌条件下,取50mg单宁酸溶解在50mL三羟甲基氨基甲烷盐酸盐溶液(pH为8)中,然后加入5mL乙醇与50mg氨基丙基三乙氧基甲硅烷,最后投入5g针状活性炭、1.2g Co(NO3)2·6H2O和0.3g硫脲,80℃超声水浴搅拌12h。
(3)取将聚偏氟乙烯(PVDF)多孔膜放置在制膜器中,倒入第一液体,使第一液体完全浸没多孔膜,50℃超声水浴4h,30℃真空度为100Pa,真空干燥12h。擦干表面液体再倒入第二液体,50℃超声水浴6h,30℃真空度为100Pa,真空干燥12h。
实施例2
本实施例提供了一种用于苯系废气的过滤材料的制备。
(1)第一液体的制备:取1L丙酮,加入20g氧化石墨烯纳米片和40mg硅烷偶联剂(KH560),超声搅拌8h,然后离心干燥,制得改性氧化石墨烯纳米片。取40mg改性氧化石墨烯纳米片,加入70mL丙酮,然后加入150g预热后的环氧树脂,55℃超声水浴搅拌3h,注入0.5w%固化剂(MTHPA)和1w%促进剂(DMI-1,2),继续50℃超声水浴搅拌1h,制得淡黄色的第一液体。
(2)第二液体的制备:在搅拌条件下,取80mg单宁酸溶解在70mL三羟甲基氨基甲烷盐酸盐溶液(pH为8.5)中,然后加入7mL乙醇与80mg氨基丙基三乙氧基甲硅烷,最后投入7g针状活性炭、1.3g Co(NO3)2·6H2O和0.4g硫脲,85℃超声水浴搅拌18h。
(3)取将聚偏氟乙烯(PVDF)多孔膜放置在制膜器中,倒入第一液体,使第一液体完全浸没多孔膜,55℃超声水浴6h,30℃真空度为120Pa,真空干燥18h。擦干表面液体再倒入第二液体,55℃超声水浴8h,30℃真空度为120Pa,真空干燥18h。
实施例3
本实施例提供了一种用于苯系废气的过滤材料的制备。
(1)第一液体的制备:取1L丙酮,加入30g氧化石墨烯纳米片和40mg硅烷偶联剂(KH560),超声搅拌8h,然后离心干燥,制得改性氧化石墨烯纳米片。取50mg改性氧化石墨烯纳米片,加入100mL丙酮,然后加入200g预热后的环氧树脂,60℃超声水浴搅拌4h,注入0.5w%固化剂(MTHPA)和1w%促进剂(DMI-1,2),继续60℃超声水浴搅拌3h,制得淡黄色的第一液体。
(2)第二液体的制备:在搅拌条件下,取100mg单宁酸溶解在100mL三羟甲基氨基甲烷盐酸盐溶液(pH为9)中,然后加入10mL乙醇与100mg氨基丙基三乙氧基甲硅烷,最后投入10g针状活性炭、1.5g Co(NO3)2·6H2O和0.5g硫脲,90℃超声水浴搅拌24h。
(3)取将聚偏氟乙烯(PVDF)多孔膜放置在制膜器中,倒入第一液体,使第一液体完全浸没多孔膜,60℃超声水浴8h,30℃真空度为140Pa,真空干燥24h。擦干表面液体再倒入第二液体,60℃超声水浴10h,30℃真空度为140Pa,真空干燥24h。
对比例1
本对比例提供了一种过滤材料的制备。
本对比例制备方法同实施例2,区别在于,第二液体制备中未加入Co(NO3)2·6H2O和硫脲。
对比例2
本对比例提供了一种过滤材料的制备。
本对比例制备方法同实施例2,区别在于,第二液体制备采用普通活性炭。
对比例3
本对比例提供了一种吸附材料的制备。
制备方法参照CN107185482B。
实施例4
本实施例提供了上述过滤/吸附材料的性能测试试验。
将实施例1~3和对比例1~3制备得到的过滤/吸附材料封入过滤管中,过滤/吸附材料体积为50cm3,采用便携式气相色谱质谱仪(Inficon,HAPSITEER),配DB-5色谱柱(15m×0.32mm×1.0μm)对VOCs浓度进行检测。设置条件为:苯系废气包含苯、甲苯、二甲苯,其余为空气,气体流速为5L/min,气体温度设置为80℃,工作3h后试验结果如表1所示。
表1:废气各组分浓度变化
由表1可知,本发明提供的过滤材料,采用Co(NO3)2·6H2O和硫脲的加入,并选择针状活性炭,能够实现分离过滤苯系废气,防止了多种苯系物掺杂下对过滤/吸附性能的抑制作用,显著优于对比例1~3提供的技术方案。
将实施例1~3和对比例1~2制备得到的过滤材料放入膜池中,用于上述的苯系废气,测量分离因子和渗透率,其结构如表2所示。
表2:过滤材料性能
由表2可知,本发明提供的过滤材料,采用Co(NO3)2·6H2O和硫脲的加入,显著提高了对苯系废气分离效率;选择针状活性炭,显著提高了过滤材料的渗透通量,在获得气体高渗透通量和高耐用性的前提下,改善过滤材料的稳定性,制备方法简单,适合工业化生产。
如上所述,即可较好地实现本发明,上述的实施例仅仅是对本发明的优选实施方式进行描述,并非对本发明的范围进行限定,在不脱离本发明设计精神的前提下,本领域普通技术人员对本发明的技术方案做出的各种改变和改进,均应落入本发明确定的保护范围内。
Claims (7)
1.一种用于苯系废气的过滤材料的制备方法,其特征在于,包括:将多孔膜置于制膜器中,浸没第一液体,50~60℃超声水浴4~8h,30℃真空干燥12~24h;再加入第二液体浸没,50~60℃超声水浴6~10h,30℃真空干燥12~24h;
所述第一液体的制备方法为:采用硅烷偶联剂对氧化石墨烯纳米片进行表面改性,加入丙酮,投入环氧树脂中,50~60℃超声水浴搅拌2~4h,注入固化剂和促进剂,继续50~60℃超声水浴搅拌1~3h;每1L丙酮中,加入10~30g氧化石墨烯纳米片和40mg硅烷偶联剂,超声搅拌8h,然后离心干燥,制得改性氧化石墨烯纳米片;每30~50mg所述改性氧化石墨烯纳米片,加入50~100mL丙酮,然后加入100~200g预热后的环氧树脂,50~60℃超声水浴搅拌2~4h,注入固化剂和促进剂,继续50~60℃超声水浴搅拌1~3h,制得淡黄色的所述第一液体;
所述第二液体的制备方法为:在搅拌条件下,每50~100mg单宁酸溶解在50~100mL三羟甲基氨基甲烷盐酸盐溶液中,然后加入5~10mL乙醇与50~100mg氨基丙基三乙氧基甲硅烷,最后投入5~10g针状活性炭、1.2~1.5g Co(NO3)2·6H2O和0.3~0.5g硫脲,80~90℃超声水浴搅拌12~24h。
2.根据权利要求1所述的制备方法,其特征在于,所述固化剂为MTHPA,所述促进剂为DMI-1,2。
3.根据权利要求1所述的制备方法,其特征在于,所述三羟甲基氨基甲烷盐酸盐溶液的pH为8~9。
4.根据权利要求1所述的制备方法,其特征在于,任一所述真空干燥的真空度为100~140Pa。
5.根据权利要求1所述的制备方法,其特征在于,所述加入第二液体浸没前,擦干表面液体。
6.一种用于苯系废气的过滤材料,其特征在于,采用权利要求1~5任一项所述的方法制得。
7.一种用于苯系废气的过滤器,其特征在于,包含权利要求6所述的过滤材料。
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