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Simplified waste-free process for synthesis of nanoporous compact alumina under technologically advantageous conditions

机译：在技​​术有利条件下，简化无废物的纳米多孔致密氧化铝的方法

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Precipitated ammonium aluminium carbonate hydroxide (NH _(4) Al(OH) _(2) CO _(3) ) is a promising precursor for preparation of nanostructured Al _(2) O _(3) . However, the experimental conditions, such as the low concentration of Al ~(3+) salt solution, high temperature and/or pressure, long reaction time, and excessive amount of the (NH _(4) ) _(2) CO _(3) precipitating agent, make this process expensive for large-scale production. Here, we report a simpler and cheaper route to prepare nanostructured alumina by partial neutralisation of a nearly saturated aqueous solution of Al(NO _(3) ) _(3) with (NH _(4) ) _(2) CO _(3) as a base at pH < 4. Synthesis in the acidic region led to formation of a polynuclear aluminium cluster (Al _(13) ), which is an important “green” solution precursor for large-area preparation of Al _(2) O _(3) thin films and nanoparticles. Control of the textural properties of the final alumina product during calcination of the prepared aluminium (oxy)hydroxide gel was accomplished by adding low-solubility aluminium acetate hydroxide (Al(OH)(CH _(3) COO) _(2) ) as a seed to the Al(NO _(3) ) _(3) solution before neutralisation. The large Brunauer–Emmett–Teller specific surface area (376 m ~(2) g ~(?1) ) and narrow pore size distribution (2–20 nm) of the prepared compact alumina suggest that the chelating effect of the acetate ions affects the structures of the forming transition aluminas, and the evolved gases produced by decomposition of Al(OH)(CH _(3) COO) _(2) and NH _(4) NO _(3) as a by-product of the reaction during calcination prevent particle agglomeration. Other advantages of the proposed process are its versatility and the ability to obtain high purity materials without producing large amounts of by-products without the need for washing and energy saving by using a low processing temperature, and the possibility of recycling the generated CO _(2) and NH _(3) gases as the (NH _(4) ) _(2) CO _(3) reagent.
机译：沉淀的碳酸铵氢氧化铝（NH _（4）Al（OH）_（2）CO _（3））是用于制备纳米结构Al _（2）O _（3）的有前体的前体。但是，实验条件，如低浓度的Al〜（3+）盐溶液，高温和/或压力，长反应时间，和量过多（NH _（4））_（2）CO _ （3）沉淀剂，使这一过程昂贵，用于大规模生产。在这里，我们通过部分中和含有近饱和的Al（NO _（3））_（3）的部分中和（NH _（4））_（2）CO _（）通过部分中和更简单和更便宜的途径来制备纳米结构氧化铝来制备纳米结构氧化铝3）作为pH的碱<4.酸性区域中的合成导致形成多核铝簇（Al _（13）），这是Al _的大面积制剂的重要“绿色”溶液前体（2 ）O _（3）薄膜和纳米颗粒。通过加入低溶解度氢氧化铝（Al（OH）（CH_（3）COO）_（2））来完成在制备铝（氧化铝）氢氧化铝凝胶期间的最终氧化铝产品的纹理性质在中和前的Al（NO _（3））_（3）溶液的种子。大型Brunauer-Emmett-extrer特定表面积（376 m〜（2）g〜（α1））和制备的紧凑氧化铝的窄孔径分布（2-20nm）表明醋酸乙酸离子的螯合作用会影响形成过渡铝的结构，以及通过分解Al（OH）（CH _（3）COO）_（2）和NH _（4）NO _（3）作为副产物的副产品产生的进化气体煅烧过程中的反应防止颗粒聚集。所提出的方法的其他优点是其多功能性和获得高纯度材料而不产生大量副产物的能力，而无需使用低处理温度洗涤和节能，以及再循环所产生的CO _（ 2）和NH _（3）气体作为（NH _（4））_（2）CO _（3）试剂。

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