CN108484149A - 一种NaA分子筛膜支撑体制备方法 - Google Patents
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Abstract
本发明提供的一种NaA分子筛膜支撑体制备方法,其以天然粘土矿物高岭土作为起始原料,外加剂分别为AlF3、V2O5、La2O3和有机添加剂PVA;将配好的粉料置于聚乙烯塑料桶中进行机械混和,混合时间为8h;将混合好的粉料分别在捏合机、练泥机和真空挤出机、烘箱中进行捏合、练泥、成型、干燥等工艺处理,最后烘干后的生坯在1500℃下程序控温炉中以5℃/min的升温速率煅烧制得;本发明使多孔莫来石分子筛膜支撑体的制备工艺大大简化,成本大大降低;且制备出的多孔莫来石支撑体其孔径、孔隙率和微观形貌可以通过控制制备过程参数进行调控此外制备出的多孔莫来石,不需酸滤或碱滤成孔,可直接满足要求,该特定微结构的多孔莫来石支撑体有广阔的应用前景。
Description
技术领域
本发明涉及膜材料制备领域,特别涉及一种NaA分子筛膜支撑体制备方法。
背景技术
膜技术是一种新型分离技术,具有高效节能,过程易控制,操作方便等特点。目前,一些新型的膜技术已经或正在实现工业化,渗透气化技术就是其中发展较快的一种。由于NaA分子筛膜在有机物脱水、共沸物的分离、污染物的去除及气体分离方面具有独特优势和良好的应用前景而成为近期无机膜材料研究的热点之一。
虽然NaA分子筛膜的研究取得了很多成果,但要真正实现工业应用还存在诸多困难,如支撑体微观形貌的控制问题,支撑体和分子筛层之间由于热应力的不同而存在粘附强度差的问题,对合成条件的控制和合成的重复性问题等。其中,分子筛膜支撑体的研究和发展水平制约着分子筛膜的研究及其工业化应用。分子筛膜常用的支撑体材料有氧化铝(Al2O3)、莫来石(3Al2O3·2SiO2)、多孔玻璃、不锈钢等。由于莫来石(3Al2O3·2SiO2)的元素组成和NaA分子筛的元素组成相似,因此,根据材料的相似相容性,采用莫来石作为支撑体材料有利于NaA膜的合成和稳定性的提高。NaA膜的制备对支撑体的要求是比较严格的,不仅要求支撑体具有一定的平均孔径(0.7-2μm)及均一的孔径分布,还要求具有较高的孔隙率(≥30%)。并且支撑体的微观结构对分子筛膜的合成及其性能也具有很大的影响。作为具有工业应用价值的NaA膜材料(外径10-30mm,长径比为50-100),对支撑体的强度和韧性也提出了很高的要求。为此,对多孔支撑体材料进行必要的增韧补强措施,提高其在实际应用过程中的可靠性就势在必行了。多年来各国研究者针对致密陶瓷的增韧补强相继提出了多种机理,如颗粒弥散增韧、相变增韧、晶须增韧、微裂纹增韧和协同增韧等,从而较好的改善了陶瓷材料的力学性能和使用性能,提高了其使用的可靠性。对于多孔陶瓷的增韧补强报道研究报道并不多,特别是原位生成晶须来提高多孔支撑体韧性方面的报道更少。
莫来石(3Al2O3·2SiO2)由于具有抗热震性好,耐火度高,高温强度和化学稳定性能好,熔点高(1890℃)和热膨胀系数低等性质被广泛应用于冶金、陶瓷、玻璃、化工0、国防、燃气等工业上。目前,国内外关于莫来石(3Al2O3·2SiO2)材料的研究主要集中在高性能莫来石粉体的制备、用于特定用途的致密莫来石陶瓷的制备、高孔隙率多孔莫来石陶瓷的制备。其主要用作玻璃窑炉和金属熔炉的内衬、耐火材料的骨料、陶瓷制品用的匣体及窑具,催化剂载体、高温过滤器等。
莫来石(3Al2O3·2SiO2)的人工合成方法有多种,李博文【CN99100545.7】以蓝晶石族矿物(包括蓝晶石、红柱石、硅线石三种同质异象矿物)的微米级粉体和氧化铝粉为主要原料,采用烧结法直接制备莫来石陶瓷。张世平,于殿顺【CN01107134.6】以高铝矾土、高岭土、粘土、硅石、氧化铝中的一种或多种物质为原料,人工合成莫来石。人工制备莫来石的方法还有中国专利【CN200410056132.2,CN200410009081.8,CN98101568.9】。上述方法均侧重于莫来石粉料的人工合成,而非多孔莫来石分子筛膜载体的制备。朱沛志,吴旦【CN00111735.1】采用矾土熟料、高岭土为主要原料,添加少量氧化镁与粘合剂,制备以莫来石晶相为主的蜂窝陶瓷载体,但其无法满足分子筛膜对支撑体孔径及其孔隙率的要求。高纯多孔莫来石陶瓷通常采用湿化学法(凝胶溶胶法,共沉淀法,水热合成法,化学气相沉积法)制备,但由于其生产费用昂贵,并且相对小的生产能力限制了它的应用。采用天然粘土矿物作为原料原位制备多孔莫来石陶瓷,则会使其成本大大降低,该方法也被一些研究者报道[1-4,JP90-173285],但基于粘土制备的多孔莫来石陶瓷中,由于在加热过程中形成大量的无定型SiO2玻璃相,从而造成其孔隙率很低通常小于30%,孔径也非常小,要增大其孔隙率和提高其孔径通常采用酸滤或碱滤或两种方法的结合,采用这种方法获得的多孔莫来石陶瓷对用于过滤为目的的载体,其孔径也不是足够的大(0.17-0.61μm),且强度也被大大的破坏。2001年中国科技大学孟广耀[5-6]课题组报道了采用高岭土为原料采用凝胶铸造工艺(Gelcasting process)制备出了孔隙率在(58.5%-63.9%),平均孔径在(0.76-1.31μm)多孔莫来石陶瓷,但制备出的多孔莫来石陶瓷并没有结晶良好的针状莫来石晶体产生,其和传统的采用粒子烧结法制备的多孔莫来石陶瓷微结构相似,且使用凝胶铸造工艺不利于大规模的工业生产。
莫来石晶须可以作为一种增强材料,提高金属和陶瓷的机械和热性能,更重要的是这种结晶完好的晶须结构具有好的吸附和催化性能,具有大的比表面积因此被广泛的研究。中国专利(CN92102982.9,CN200510044907.9)采用溶胶凝胶法制备莫来石晶须粉料,该晶须材料主要用作陶瓷增强材料。另外中国专利200480010571.8描述了通过形成一个或多个前驱体化合物和一些性能增强化合物的混合物在含氟气体中加热,制备出针状颗粒的莫来石组合物用来作为柴油机过滤器,但其无法满足分子筛膜对支撑体孔径及其孔隙率和微观结构性能的要求标准。
发明内容
本发明提供一种NaA分子筛膜支撑体制备方法,其具体制备步骤如下:
①将Al(OH)3和高岭土按照Al2O3:SiO2=7.18:2.82配比进行混合,形成混合料;
②向步骤①得到的混合料中加入AlF3、V2O5、La2O3和有机添加剂PVA;所述AlF3、V2O5、La2O3和PVA的添加量分别为Al(OH)3与高岭土混合料的8%、0.05%、0.1%和0.2%;
③步骤②将配好的粉料置于聚乙烯塑料桶中进行机械混和,混合时间为8h;
④将步骤③混合好的粉料添加质量浓度为2%的PVA水溶液,所述PVA水溶液的质量为Al(OH)3与高岭土混合料的10%;之后放入捏合机中,在室温下捏合30min形成块状的泥料;
⑤将步骤④得到的块状泥料放入练泥机中练泥1h,之后将练好的泥料放入真空挤出机的装料桶中,在保持真空度-0.1Mpa的压力下进行挤出成型的湿坯;
⑥将步骤⑤挤出的湿坯放入110℃烘箱中烘干8h,形成生坯;
⑦将步骤⑥烘干的生坯放入1500℃的程序控温炉中以5℃/min的升温速率在1400℃保温2h制得出高性能的多孔莫来石支撑体。
优选的,所述高岭土的化学分子式为:2SiO2·Al2O3·2H2O,其化学组成为46.54%的SiO2,39.5%的Al2O3,13.96%的H2O;
优选的,所述多孔莫来石支撑体的孔径在0.1-10μm,孔隙率在8%-60%。
本发明开发了一种新的制备多孔莫来石分子筛膜支撑体的方法,采用该方法生产出的多孔莫来石陶瓷伴生有结晶良好的莫来石晶须,其孔径在0.1-10μm,孔隙率在8%-60%内可调。由于其含有结晶完好的针状莫来石晶态,具有好的表面物理化学性质,同时具有高的韧性,并且其平均孔径和孔隙率可以达到分子筛膜对支撑体的要求,因此本发明制备出的多孔莫来石支撑体可以用来作为分子筛膜支撑体,尤其适合作为NaA分子筛膜支撑体。
Al(OH)3和AlF3组分的加入使高岭土产生一定孔隙的同时,分解的Al2O3和SiO2玻璃相反应生成具有针状结构的莫来石晶体;由于其具有完好的结晶状态和相互交叉的网状结构,使其具备高的孔隙率的同时还具备高的强度和韧性,同时由于结晶良好的莫来石晶须的生成,使其孔容和比表面积大大增加,表面物理化学性质大大改善,这样都有助于提高支撑体的性能。此外,通过制备过程参数的控制还可以获得不同孔径和孔隙率的多孔莫来石支撑体。
本发明采用原位固相反应的方法制备多孔莫来支撑体,使多孔莫来石支撑体的制备工艺大大简化,成本大大降低。采用化学合成的路线,原位制备出了多孔莫来支撑体并有结晶良好的莫来石晶须伴生;且制备出的多孔莫来石支撑体其孔径、孔隙率和微观形貌可以通过控制制备过程参数进行调控此外制备出的多孔莫来石分子筛膜支撑体,不需酸滤或碱滤成孔,可直接满足要求,该特定微结构的多孔莫来石支撑体有广阔的应用前景。
附图说明
图1为制备出的含有晶须伴生的多孔莫来石支撑体;
图2为制备出的含有晶须伴生的多孔莫来石支撑体;
图3为制备出的含有晶须伴生的多孔莫来石支撑体;
图4为制备出的含有晶须伴生的多孔莫来石支撑体;
图5为根据本发明所制备的多孔莫来石支撑体的XRD。
具体实施方式
下面对本发明的一个具体实施方式进行详细描述,但应当理解本发明的保护范围并不受具体实施方式的限制。
本发明实施例提供的一种NaA分子筛膜支撑体制备方法,其具体制备步骤如下:
①将Al(OH)3和高岭土按照Al2O3:SiO2=7.18:2.82配比进行混合,形成混合料;
②向步骤①得到的混合料中加入AlF3、V2O5、La2O3和有机添加剂PVA;所述AlF3、V2O5、La2O3和PVA的添加量分别为Al(OH)3与高岭土混合料的8%、0.05%、0.1%和0.2%;
③步骤②将配好的粉料置于聚乙烯塑料桶中进行机械混和,混合时间为8h;
④将步骤③混合好的粉料添加质量浓度为2%的PVA水溶液,所述PVA水溶液的质量为Al(OH)3与高岭土混合料的10%;之后放入捏合机中,在室温下捏合30min形成块状的泥料;
⑤将步骤④得到的块状泥料放入练泥机中练泥1h,之后将练好的泥料放入真空挤出机的装料桶中,在保持真空度-0.1Mpa的压力下进行挤出成型的湿坯;
⑥将步骤⑤挤出的湿坯放入110℃烘箱中烘干8h,形成生坯;
⑦将步骤⑥烘干的生坯放入1500℃的程序控温炉中以5℃/min的升温速率在1400℃保温2h制得出高性能的多孔莫来石支撑体。
优选的,所述高岭土的化学分子式为:2SiO2·Al2O3·2H2O,其化学组成为46.54%的SiO2,39.5%的Al2O3,13.96%的H2O;
优选的,所述多孔莫来石支撑体的孔径在0.1-10μm,孔隙率在8%-60%。
本发明采用原位固相反应的方法制备多孔莫来石支撑体,使多孔莫来石支撑体的制备工艺大大简化,成本大大降低。采用化学合成的路线,原位制备出了多孔莫来石支撑体并有结晶良好的莫来石晶须伴生;且制备出的多孔莫来石支撑体其孔径、孔隙率和微观形貌可以通过控制制备过程参数进行调控,此外制备出的多孔莫来石支撑体,不需酸滤或碱滤成孔,可直接满足要求,该特定微结构的多孔莫来石支撑体有广阔的应用前景。
上公开的仅为本发明的具体实施例,但是,本发明实施例并非局限于此,任何本领域的技术人员能思之的变化都应落入本发明的保护范围。
Claims (3)
1.一种NaA分子筛膜支撑体制备方法,其特征在于,其具体制备步骤如下:
①将Al(OH)3和高岭土按照Al2O3:SiO2=7.18:2.82配比进行混合,形成混合料;
②向步骤①得到的混合料中加入AlF3、V2O5、La2O3和有机添加剂PVA;所述AlF3、V2O5、La2O3和PVA的添加量分别为Al(OH)3与高岭土混合料的8%、0.05%、0.1%和0.2%;
③步骤②将配好的粉料置于聚乙烯塑料桶中进行机械混和,混合时间为8h;
④将步骤③混合好的粉料添加质量浓度为2%的PVA水溶液,所述PVA水溶液的质量为Al(OH)3与高岭土混合料的10%;之后放入捏合机中,在室温下捏合30min形成块状的泥料;
⑤将步骤④得到的块状泥料放入练泥机中练泥1h,之后将练好的泥料放入真空挤出机的装料桶中,在保持真空度-0.1Mpa的压力下进行挤出成型的湿坯;
⑥将步骤⑤挤出的湿坯放入110℃烘箱中烘干8h,形成生坯;
⑦将步骤⑥烘干的生坯放入1500℃的程序控温炉中以5℃/min的升温速率在1400℃保温2h制得出高性能的多孔莫来石支撑体。
2.根据权利要求1所述的一种NaA分子筛膜支撑体制备方法,其特征在于,所述高岭土的化学分子式为:2SiO2·Al2O3·2H2O,其化学组成为46.54%的SiO2,39.5%的Al2O3,13.96%的H2O。
3.根据权利要求2所述的一种NaA分子筛膜支撑体制备方法,其特征在于,所述多孔莫来石支撑体的孔径在0.1-10μm,孔隙率在8%-60%。
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