CN107971039B - 由有机铝废弃物制备氧化铝载体或复合氧化物载体的方法 - Google Patents
由有机铝废弃物制备氧化铝载体或复合氧化物载体的方法 Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 34
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- 238000000034 method Methods 0.000 title claims abstract description 17
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- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
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Abstract
本发明涉及一种由有机铝废弃物制备氧化铝载体或复合氧化物载体的方法，该方法包括将有机铝废弃物20～100％、组分A 0～80％、助挤剂0～10％充分混合后，在步骤a)得到的混合物中加入胶溶剂捏合成可塑体，控制可塑体的干基含量为20～80％；在将可塑体进行挤条成型、干燥、焙烧得氧化铝载体或复合氧化物载体。本发明方法制备的氧化铝载体或复合氧化物载体具有方法简单、耗水量小、成本低廉、孔容大、机械强度高的特点，适合用于多种催化剂领域。
Description
技术领域
本发明属于无机材料制备领域，涉及一种氧化铝载体或复合氧化物载体的制备方法，更具体的说，本发明涉及一种由有机铝废弃物制备氧化铝载体或复合氧化物载体的方法。
背景技术
有机铝化合物包括烷基铝、烷基卤化铝、烷基氢化铝、烷基烷氧基铝、芳基铝、以及含氮、含硫、含磷等的有机铝化合物，因其原料金属铝量大，产品产量大，作为有机金属化合物，反应性高，广泛用于橡胶行业、洗涤日用品、农药、医药、纺织等行业用于生产高分子聚合物、直链高级α-烯烃、直链高级α-醇、杀虫剂、杀菌剂、洗涤剂、有机金属化合物等。以上行业的生产过程中，特别是医药、农药行业，多会生成大量的有机铝废弃物，目前大量的有机铝废弃物被当作有机垃圾或含铝废渣进行处理。
研究表明，大量的有机铝废弃物的主要成分是高碳醇、酯与氧化铝的水合物，包括拟薄水铝石、氢氧化铝等组成。由于有机铝化合物主要由高纯铝锭或铝屑制备，因此有机铝废弃物中的无机物基本不含其他杂质，是制备氧化铝载体或含氧化铝的复合氧化物的优良原料。以有机铝废弃物为原料制备氧化铝载体或复合氧化物载体是一种变废为宝、绿色节能的新工艺。首先，该技术可减少废弃物排放，降低废渣处理费用；其次，有机铝废弃物中的有机物在载体成型过程还可起到扩孔剂的效果，可提高载体孔容、孔径；第三，焙烧过程通过回收挥发出的有机物废气引入燃烧室作为燃烧气的补充，还可起到降低能耗的作用。
发明内容：
本发明的目的是克服现有技术存在的上述不足提供一种利用有机铝废弃物制备氧化铝载体或复合氧化物载体的方法，该方法操作简单、耗水量小、成本低廉、孔容大、机械强度高的特点，适合用于多种催化剂领域。
为解决上述技术问题，本发明通过以下技术方法予以实现：
一种由有机铝废弃物制备氧化铝载体或复合氧化物载体的方法，其特征在于按以下步骤进行：
a)以混合物总质量计，将下列质量百分比的原料充分混合，：
有机铝废弃物，20～100％
组分A，0～80％
助挤剂0～10％，
有机铝废弃物选自废弃的含有有机物和氧化铝或氧化铝水合物的混合物，有机物包括醇、醚、酯、酚、醛、酮、烃、羧酸、胺、碳水化合物中的一种或几种；组分A为氧化铝、氧化硅、氧化镁、氧化钙、氧化锌、氧化钛、氧化锆、拟薄水铝石、氢氧化铝、硅胶、硅溶胶、氢氧化镁、氢氧化钙、氢氧化锌、碱式碳酸镁、碳酸钙、碱式碳酸锌中的一种或几种；助挤剂选自田菁粉、甲基纤维素、羟丙基甲基纤维素、羧甲基纤维素钠、淀粉、聚乙烯醇中的一种或几种；
b)在步骤a)得到的混合物中加入胶溶剂捏合成可塑体，控制可塑体的干基含量为20～80％；胶溶剂选自水、无机酸溶液、有机酸溶液或硅溶胶中的一种或几种；
c)将步骤b)得到的可塑体进行挤条成型、干燥、焙烧得氧化铝载体或复合氧化物载体。
在上述技术方案中所述的有机铝废弃物优选为含有有机物和拟薄水铝石的混合物。
根据本发明所述的制备方法，步骤c)中干燥、焙烧过程挥发出的有机物作为部分燃烧气加热干燥窑炉或焙烧窑炉以降低窑炉的能耗。
与现有技术相比，本发明所述制备法通过将有机铝废弃物作为原料制备氧化铝载体或复合氧化物载体，整个过程简单易行、能耗低，制得的载体具有孔容大、强度高、磨耗低的特点。
具体实施方式
下面结合具体实施例对本发明的技术方案作进一步说明。实施例1-9原料有机铝废弃物，以丙醇铝水解所得的有机铝废弃物(其中氧化铝含量62％，异丙醇含量12％)为例进行介绍，并不限于该有机铝废弃物，对本发明技术方案无限定作用。
实施例1
将300g有机铝废弃物与3g羧甲基纤维素充分混合，加入质量浓度3％硝酸溶液260g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在120℃干燥8小时，550℃焙烧5小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
实施例2
将300g有机铝废弃物、50g拟薄水铝石与10g羧甲基纤维素钠充分混合，加入质量浓度1％硝酸380g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在120℃干燥8小时，550℃焙烧5小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
实施例3
将300g有机铝废弃物、100g氧化镁、4g羟丙基甲基纤维素充分混合，加入质量浓度6％硝酸410g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在120℃干燥8小时，600℃焙烧5小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
实施例4
将300g有机铝废弃物、300g氧化硅、10g淀粉充分混合，加入硅溶胶450g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在100℃干燥12小时，600℃焙烧5小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
实施例5
将300g有机铝废弃物、50g二氧化钛、10g羧甲基纤维素充分混合，加入质量浓度3％硝酸300g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在100℃干燥12小时，700℃焙烧5小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
实施例6
将300g有机铝废弃物、20g氢氧化钙、50g羧甲基纤维素充分混合，加入水300g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在80℃干燥24小时，700℃焙烧3小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
实施例7
将300g有机铝废弃物、10g氢氧化铝、50g羧甲基纤维素充分混合，加入质量浓度10％醋酸溶液300g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在120℃干燥5小时，650℃焙烧8小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
实施例8
将300g有机铝废弃物、5g氧化锌与15g羧甲基纤维素充分混合，加入质量浓度3％硝酸溶液300g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在120℃干燥5小时，450℃焙烧8小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
实施例9
将60g有机铝废弃物、240g拟薄水铝石与3g羧甲基纤维素充分混合，加入质量浓度3％硝酸溶液260g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在120℃干燥5小时，550℃焙烧8小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
对比例1
将300g拟薄水铝石与3g羧甲基纤维素充分混合，加入质量浓度3％硝酸溶液260g，在捏合机中捏合得到可塑体，经挤压通过孔板制成3mm的圆柱，在120℃干燥5小时，550℃焙烧8小时得到圆柱形氧化铝载体，其载体组成、比表面、孔容、孔径、粒径、强度指标见表1。
表1实施例1-8及对比例制得的载体理化性能指标
实施例10
按实施例1中各物料配比制备5吨氧化铝载体，进行尾气回用对比实验，焙烧时将生成的尾气引入燃烧器作为部分燃气，与尾气直接排放相比，可节省天然气85m3/吨产品。
Claims (3)
1.一种氧化铝载体或复合氧化物载体的制备方法，其特征在于按以下步骤进行：
a）以混合物总质量计，将下列质量百分比的原料充分混合：
有机铝废弃物， 20~100%
组分A， 0~80%
助挤剂 0~10%
其中，有机铝废弃物为废弃的含有有机物和氧化铝或氧化铝水合物的混合物，有机物包括醇、醚、酯、酚、醛、酮、烃、羧酸、胺、碳水化合物中的一种或几种；组分A为氧化铝、氧化硅、氧化镁、氧化钙、氧化锌、氧化钛、氧化锆、拟薄水铝石、氢氧化铝、硅胶、硅溶胶、氢氧化镁、氢氧化钙、氢氧化锌、碱式碳酸镁、碳酸钙、碱式碳酸锌中的一种或几种；助挤剂选自田菁粉、甲基纤维素、羟丙基甲基纤维素、羧甲基纤维素钠、淀粉、聚乙烯醇中的一种或几种；
b）在步骤a）得到的混合物中加入胶溶剂捏合成可塑体，控制可塑体的干基含量为20~80%；胶溶剂选自水、无机酸溶液、有机酸溶液或硅溶胶中的一种或几种；
c）将步骤b）得到的可塑体进行挤条成型、干燥、焙烧得氧化铝载体或复合氧化物载体。
2.按照权利要求1所述的制备方法，其特征在于，所述的有机铝废弃物为含有有机物和拟薄水铝石的混合物。
3.按照权利要求1所述的制备方法，其特征在于，所述的步骤c）中干燥和/或焙烧过程挥发出的有机物作为部分燃烧气加热干燥窑炉或焙烧窑炉以降低窑炉的能耗。
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