CN109569504B - 一种用于吸附有机气体的水铝英石材料及其制备方法 - Google Patents
一种用于吸附有机气体的水铝英石材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种用于吸附有机气体的水铝英石材料及其制备方法。所述的水铝英石材料的制备是在铝硅酸盐纳米矿物水铝英石的水热合成过程中,通过置换原料中的硅烷,直接将有机基团引入水铝英石内表面,从而制备出疏水性的水铝英石材料。所制备的水铝英石材料的单颗粒呈空心球状,其外径约5nm,内径约3nm;该材料比表面积和孔容较大,对苯、甲苯和环己烷等有机气体具有良好的吸附性能。此外,本发明提供的用于吸附有机气体的水铝英石材料的制备方法简单,制备条件温和,能耗低,无污染,应用前景广阔。
Description
技术领域
本发明涉及有机气体吸附领域,具体涉及一种用于吸附有机气体的水铝英石材料及其制备方法。
背景技术
有机气体是一类常见的大气污染物,它们主要来源于化石燃料的燃烧、汽车尾气的排放、建筑及装修材料中有机溶剂的挥发等。大多数有机气体具有刺激性和毒性,可致癌、致畸、致突变,还可充当光化学烟雾的前驱体,对环境和人类健康危害严重。目前,有机气体的治理方法主要包括吸附法、燃烧法、生物法和光催化降解法等。其中,吸附法由于工艺成熟,能耗低,去除效率高等优点,应用最广泛,也最经济有效。
吸附剂是吸附法应用的关键。纳米空心球材料由于具有丰富的微孔、较高的比表面积和较大的孔容等特殊的结构和性质,近年来被应用于吸附甲醛、丙酮和乙醚等有机气体。然而,复杂的制备流程和高昂的经济成本制约着纳米空心球材料在有机气体吸附领域的实际应用。因此,亟需寻找制备工艺简单、价格低廉的纳米空心球材料。
水铝英石(1~2SiO2·Al2O3·5~6H2O)是一种天然矿物,属于低结晶度的纳米空心球状铝硅酸盐矿物。它广泛产出于土壤等多种地质环境中,在我国有着丰富的储量;同时,也可通过简单的水热反应进行制备,是目前仅有的可通过水热法进行批量合成的单壁纳米空心球材料。
水铝英石由一层卷曲的似三水铝石片构成外部骨架,骨架内侧的铝羟基被原硅酸基团或其低聚体取代。其空心球外径约5.0nm,球壁厚度约0.7~1.0nm,球壁上分布着直径约0.35nm的孔洞。水铝英石丰富的微孔以及高的比表面积(约为几百至一千平方米每克)使其对废水中的重金属离子(如铅离子、镉离子等)和各种阴离子(如氟离子、磷酸根、砷酸根等)具有良好的吸附性。然而,水铝英石表面含有大量的羟基(包括外表面的铝羟基和内表面的硅羟基),呈现出较强的亲水性,这显著降低了其对有机气体分子,尤其是疏水性有机气体分子(如苯、甲苯等)的亲和性。研究表明,通过对吸附剂进行硅烷化改性,使其表面由亲水性转变为疏水性,能够显著提升其对有机气体分子的吸附性。然而,由于水铝英石颗粒非常细小且球壁上的孔洞极其细微,通过普通的硅烷化改性方法难以改善其表面的疏水性以提高其对有机气体的吸附性能。
中国发明专利《一种通过超声制备有机无机杂化中空纳米球的方法》(专利号:106317425A)通过超声法制备了一种有机-无机杂化中空纳米球。该纳米球是将水、pH调节剂、硅烷偶联剂和油相混合后超声处理,加入自由基引发剂引发聚合反应,然后洗涤得到。该材料壳层由含硅聚合物构成,且带有双键聚合后的有机链段部分,为有机-无机杂化结构,兼具亲水和亲油的特性。然而,该材料制备方法属于界面乳液聚合法,需要用到带双键的硅烷偶联剂、乙酸异戊酯等酯类(油相)和自由基引发剂,生产成本较高,且易造成污染。另外,所得中空纳米球材料的粒径为亚微米级(100nm以上),限制了其在真正纳米尺度(0.1~100nm)上的应用。
发明内容
本发明的目的在于克服纳米空心球材料制备工艺复杂,价格高昂,以及水铝英石纳米空心球材料亲水性强且表面难以改性的缺点,提供一种用于吸附有机气体的水铝英石材料及其制备方法。本发明的用于吸附有机气体的水铝英石材料不但具有独特的纳米空心球状结构、丰富的微孔和较高的比表面积,而且其内表面含有有机基团,疏水性较强。同时,所制备的水铝英石材料对苯、甲苯和环己烷等有机气体具有良好的吸附性能。
本发明的用于吸附有机气体的水铝英石材料是通过以下方法制备的,是将液态硅烷和铝源通过水热反应制备得到,所述的液态硅烷是液态含有有机基团的硅烷。
优选,该方法包括以下步骤:
a.将液态硅烷按照初始Si/Al摩尔比为0.5~1.0的比例加入到浓度为0.02~0.2M的铝源溶液中,充分搅拌,得到混合溶液;
b.将浓度为0.05~0.5M的NaOH溶液滴加至步骤a)所得的混合溶液中,继续搅拌,得到水铝英石材料的前躯体悬浮液;
c.将步骤b)所得的前躯体悬浮液于室温下老化8~24h后转移至反应釜内,于80~150℃下水热反应24~120h;
d.待步骤c)所得的反应产物冷却后滴加稀氨水至pH为7~8使悬浮液聚沉,然后离心分离得到沉淀物;
e.将步骤d)所得沉淀物渗析4~7d,冷冻干燥并研磨,得到用于吸附有机气体的水铝英石材料。
所述步骤a)中的液态硅烷选自三乙氧基甲基硅烷、三乙氧基乙基硅烷、氨甲基三乙氧基硅烷或氨乙基三乙氧基硅烷中的一种以上。
所述步骤a)中的铝源溶液为AlCl3、Al(ClO4)3、Al(NO3)3或Al2(SO4)3溶液。
所述步骤b)中NaOH溶液的加入量是以OH/Al摩尔比=2为准,所述继续搅拌的时间为1h。
所述步骤b)中NaOH溶液的滴加速度为0.5~10mL/min。
本发明还请求保护根据上述方法制得的用于吸附有机气体的水铝英石材料。所述的水铝英石材料具有纳米空心球状结构,且其内表面含有有机基团,呈现较强的疏水性。
与现有技术相比,本发明具有以下有益效果:
(1)从成分、体相结构和孔结构来看,本发明所制备的用于吸附有机气体的水铝英石材料属于典型的纳米空心球材料,其粒径仅为几纳米,目前尚未见到任何类似材料的报道。
(2)本发明在水铝英石水热合成工艺的基础上,通过置换原料中的硅源,创造性地将有机基团引入水铝英石纳米空心球的内表面,实现了内表面的选择性改性,也克服了水铝英石由于球壁孔洞极其细小而难以进行硅烷化改性的缺点。同时,所制备的水铝英石纳米空心球内表面完全有机化,呈现较强的疏水性。
(3)本发明制备的水铝英石材料具有较高的比表面积和较大的孔容(其比表面积和孔容可分别达396.5m2/g和0.23cm3/g),且对苯、甲苯和环己烷等有机气体具有较高的吸附量(其对苯、甲苯和环己烷的动态平衡吸附量最高可分别达180.1、165.2和139.5mg/g)。另外,所得材料的孔结构分布更加有序,有利于有机气体分子的扩散以及材料的脱附再生。
综上所述,本发明率先通过置换水铝英石水热合成过程中的硅烷,制备出具有纳米空心球结构的疏水性水铝英石材料,且所制备的水铝英石材料具有较高的比表面积、较大的孔容,以及良好的有机气体吸附性能。该制备方法具有工艺简单、能耗低、无污染、所需的原材料少等优势,应用前景广阔。
附图说明
图1为实施例1所制备的用于吸附有机气体的水铝英石材料的原子力显微镜图。
图2为实施例2所制备的用于吸附有机气体的水铝英石材料的红外光谱图。
图3为实施例3所制备的用于吸附有机气体的水铝英石材料的苯动态吸附穿透曲线。
具体实施方式
以下实施例是对本发明的进一步说明,而不是对本发明的限制。
实施例1
(1)将15.44g氨甲基三乙氧基硅烷加入到800mL浓度为0.2M的AlCl3溶液中,充分搅拌,所得混合溶液的初始Si/Al摩尔比为0.5;
(2)将640mL浓度为0.5M的NaOH溶液以0.5mL/min的速率滴加至步骤(1)所得混合溶液中(此时OH/Al摩尔比为2),继续搅拌1h,得到水铝英石材料的前躯体悬浮液;
(3)将步骤(2)所得前躯体悬浮液于室温下老化24h后转移至反应釜内,于150℃条件下水热反应24h;
(4)待步骤(3)所得的反应产物冷却后滴加稀氨水至pH为7~8使悬浮液聚沉,然后离心分离得到沉淀物;
(5)将步骤(4)所得沉淀物渗析4d,冷冻干燥并研磨,得到用于吸附有机气体的水铝英石材料。
图1为本实施例所制备的用于吸附有机气体的水铝英石材料的原子力显微镜图。图1b为图1a上白色直线所在位置的截面高度曲线。由图1a可看到,所制备的水铝英石材料呈纳米球状(部分颗粒发生了团聚)。由图1b可看出,该材料的粒径为3~5nm。
根据Brunauer-Emmett-Teller(BET)法测得本实施例所制备的用于吸附有机气体的水铝英石材料的比表面积为289.6m2/g,总孔体积为0.14cm3/g。
通过动态吸附实验测得本实施例所制备的用于吸附有机气体的水铝英石材料对苯、甲苯和环己烷的气体分子的动态平衡吸附量分别为143.5、122.1和117.6mg/g。
实施例2
(1)将14.24g三乙氧基甲基硅烷加入到800mL浓度为0.1M的Al(ClO4)3溶液中,充分搅拌,所得混合溶液的初始Si/Al摩尔比为1.0;
(2)将1600mL浓度为0.1M的NaOH溶液以10.0mL/min的速率滴加至步骤(1)所得混合溶液中(此时OH/Al摩尔比为2),继续搅拌1h,得到水铝英石材料的前躯体悬浮液;
(3)将步骤(2)所得前躯体悬浮液老化8h后转移至反应釜内,于80℃条件下水热反应120h;
(4)待步骤(3)所得的反应产物冷却后滴加稀氨水至pH为7~8使悬浮液聚沉,然后离心分离得到沉淀物;
(5)将步骤(4)所得沉淀物渗析7d,冷冻干燥并研磨,得到用于吸附有机气体的水铝英石材料。
图2为本实施例所制备的用于吸附有机气体的水铝英石材料的红外光谱图。图中与甲基有关的特征红外吸收带(2971、2912、1271和782cm-1)的出现表明甲基已被成功引入水铝英石的结构中。
根据BET法测得本实施例所制备的用于吸附有机气体的水铝英石材料的比表面积为396.5m2/g,总孔体积为0.23cm3/g。
通过动态吸附实验测得本实施例所制备的用于吸附有机气体的水铝英石材料对苯、甲苯和环己烷的气体分子的动态平衡吸附量分别为180.1、165.2和139.5mg/g。
实施例3
(1)将17.28g三乙氧基乙基硅烷加入到3000mL浓度为0.02M的Al2(SO4)3溶液中,充分搅拌,所得混合溶液的初始Si/Al摩尔比为0.75;
(2)将1200mL浓度为0.2M的NaOH溶液以5.0mL/min的速率滴加至步骤(1)所得混合溶液中(此时OH/Al摩尔比为2),继续搅拌1h,得到水铝英石材料的前躯体悬浮液;
(3)将步骤(2)所得前躯体悬浮液老化12h后转移至反应釜内,于100℃条件下水热反应48h;
(4)待步骤(3)所得的反应产物冷却后滴加稀氨水至pH为7~8使悬浮液聚沉,然后离心分离得到沉淀物;
(5)将步骤(4)所得沉淀物渗析7d,冷冻干燥并研磨,得到用于吸附有机气体的水铝英石材料。
图3为本实施例所制备的用于吸附有机气体的水铝英石材料的氮气吸脱附等温线。根据国际理论与应用化学联合会(IUPAC)的建议,该等温线属于I型等温线,表明该材料主要含微孔,具有较高的比表面积和孔容。
根据BET法测得本实施例所制备的用于吸附有机气体的水铝英石材料的比表面积为197.3m2/g,总孔体积为0.09cm3/g。
通过动态吸附实验测得本实施例所制备的用于吸附有机气体的水铝英石材料对苯、甲苯和环己烷的气体分子的动态平衡吸附量分别为121.0、113.8和109.8mg/g。
以上仅是本发明的优选实施方式,应当指出的是,上述优选实施方式不应视为对本发明的限制,本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说,在不脱离本发明的精神和范围内,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (3)
1.一种用于吸附有机气体的水铝英石材料的制备方法,其特征在于,包括以下步骤:
a.将液态硅烷按照初始Si/Al摩尔比为0.5~1.0的比例加入到浓度为0.02~0.2M的铝源溶液中,充分搅拌,得到混合溶液;
b.将浓度为0.05~0.5M的NaOH溶液以0.5~10mL/min的滴加速度滴加至步骤a)所得的混合溶液中,NaOH溶液的加入量是以OH/Al摩尔比=2为准,继续搅拌1h,得到水铝英石材料的前躯体悬浮液;
c.将步骤b)所得的前躯体悬浮液于室温下老化8~24h后转移至反应釜内,于80~150℃下水热反应24~120h;
d.待步骤c)所得的反应产物冷却后滴加稀氨水至pH为7~8使悬浮液聚沉,然后离心分离得到沉淀物;
e.将步骤d)所得沉淀物渗析4~7d,冷冻干燥并研磨,得到用于吸附有机气体的水铝英石材料;
所述的液态硅烷选自三乙氧基甲基硅烷、三乙氧基乙基硅烷、氨甲基三乙氧基硅烷或氨乙基三乙氧基硅烷中的一种以上;
所述的铝源溶液为AlCl3、Al(ClO4)3、Al(NO3)3或Al2(SO4)3溶液。
2.一种用于吸附有机气体的水铝英石材料,其特征在于,是根据权利要求1所述的制备方法制备得到。
3.根据权利要求2所述的用于吸附有机气体的水铝英石材料,其特征在于,所述的水铝英石材料具有纳米空心球状结构,且其内表面含有有机基团,呈现疏水性。
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