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CN112708928B - 一种氧化铝晶粒及其制备方法 - Google Patents

一种氧化铝晶粒及其制备方法 Download PDF

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Publication number
CN112708928B
CN112708928B CN201911020895.4A CN201911020895A CN112708928B CN 112708928 B CN112708928 B CN 112708928B CN 201911020895 A CN201911020895 A CN 201911020895A CN 112708928 B CN112708928 B CN 112708928B
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Prior art keywords
alumina
crystal
crystal grain
powder
carrying
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CN201911020895.4A
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CN112708928A (zh
Inventor
杨卫亚
隋宝宽
凌凤香
张会成
王少军
沈智奇
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Sinopec Dalian Petrochemical Research Institute Co ltd
China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
Sinopec Dalian Research Institute of Petroleum and Petrochemicals
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Application filed by China Petroleum and Chemical Corp, Sinopec Dalian Research Institute of Petroleum and Petrochemicals filed Critical China Petroleum and Chemical Corp
Priority to CN201911020895.4A priority Critical patent/CN112708928B/zh
Priority to EP20878216.9A priority patent/EP4050130A4/en
Priority to JP2022524238A priority patent/JP7368619B2/ja
Priority to US17/755,241 priority patent/US20220380933A1/en
Priority to KR1020227017435A priority patent/KR102735447B1/ko
Priority to PCT/CN2020/123485 priority patent/WO2021078292A1/zh
Publication of CN112708928A publication Critical patent/CN112708928A/zh
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    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
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  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Catalysts (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

本发明公开了一种氧化铝晶粒及其制备方法。该氧化铝晶粒为单晶结构，具有近似正八面体立体形貌，所述的氧化铝晶粒的8个面属于γ态氧化铝的｛111｝晶面族，晶粒大小为25‑100μm。氧化铝晶粒的制备方法如下：（1）将拟薄水铝石粉体焙烧后，加入无机钠盐，研磨处理至一定粒度，研磨后的粉料用洗涤去除钠盐后，配成悬浊液，加入有机酸，进行高速剪切处理；（2）向物料中加入有机胺与有机碱混合物，混合均匀；（3）物料进行密闭水热处理，处理完毕后，固液分离，干燥、焙烧，得到产物。本发明的氧化铝晶粒具有灵活的晶面分布可控性，制备方法简单易行、成本低廉，具有较强的可操作性，在催化、吸附领域具有良好应用前景。

Description

一种氧化铝晶粒及其制备方法
技术领域
本发明属于无机材料制备领域，具体地涉及一种氧化铝晶粒及其制备方法。
背景技术
活性氧化铝具有比表面积大、孔结构可调、表面存在不同性质的酸性中心、较高的机械强度和热稳定性等良好的物化性质，被广泛用作炼油加氢催化等领域的催化剂载体，氧化铝的性质是影响催化剂的性能的关键性因素之一。氧化铝是一种由初级晶粒组成的晶体材料，初级粒子的晶面通过由底层向上（Bottom-Up）方式决定了氧化铝的上述物化性质并最终体现到催化剂的催化性能上。
氧化铝晶粒各种晶面具有不同的原子密度和原子对称性，导致各晶面的电子结构、表面能和化学活性等性质差别较大。通过调变氧化铝晶粒生长的制约因素，调控氧化铝晶粒的晶面类型和比例，可实现从源头出发对氧化铝的比表面、孔结构、酸性及原子、分子化学环境等关键物化性质的深度调控。
当前，以氧化铝（γ-氧化铝）为载体的工业加氢催化剂，氧化铝主要是以（110）、（111）及（100）晶面分布为主，其中（110）晶面分布一般为70%左右。氧化铝的三种晶面及其分布可对加氢催化剂活性相产生显著的影响，并分别使催化剂表现出各具特色的加氢脱硫及烯烃饱和性能。因此，如果能够灵活调控氧化铝（110）、（111）及（100）晶面的相对比例，使其分别达到优势分布，并确定优势晶面对加氢催化剂催化性能的影响规律，可为新型加氢催化剂载体的开发提供理论指导。然而，由于晶体生长习性的限制，氧化铝（110）晶面的优势分布状况在常规的合成方法中难以进行有效的调控，不能实现（111）及（100）晶面的优势分布，难以反映出具体晶面对催化剂催化性能的影响，不利于根据晶粒的表面晶面性质对催化剂的活性、选择性进行调控。
氧化铝表面晶面的类型及分布的调控，目前在世界范围仍然是一个亟待解决的重大科学难题。
Mater. Lett. 2013,94,104-107利用离子液体合成得到八面体形貌的含氟铝化合物，尺寸为5μm左右。该方法原料为价格昂贵的离子液体及含氟原料，易造成环境污染，不利于大规模生产，且该产物不适用于炼油加氢催化领域。
【精细石油化工，2014，31（5）：38-43】，研究了单晶小颗粒γ-氧化铝表面性质与晶面特性之间的关系，发现氧化铝晶体主要暴露（110）晶面族和（111）晶面族，其中（110）晶面族表面占70.4%，（111）晶面族表面占29.6%。
【当代化工，2015，44（5）：951-954】制备了包含（110）晶面且还具有（752）、（541）等高指数表面晶面的纳米γ-氧化铝单晶颗粒。但是氧化铝高指数晶面活性较高、界面能量较大，在热力学上较难稳定存在，不适合作为催化材料用于催化反应领域。
【石油炼制与化工，2013，44（9）：47-50】通过向水热体系加入硝酸钠的方法，可以在一定程度上改变氧化铝单晶颗粒的晶面分布范围，但是受氧化铝晶体学内在习性的制约，氧化铝晶面仍然是以（110）为主导。
CN201610494090.3提供了一种微米尺寸的八面体氧化铝的制备方法。将无机铝盐与有机添加剂溶于溶剂中形成溶液，在水热釜中经过110-200℃热处理1-48小时，得到八面体氧化铝前驱体，该八面体氧化铝尺寸在1-20μm之间。由产物经200℃焙烧（烘干）的XRD谱可以看出，该八面体氧化铝不具有薄水铝石或拟薄水铝石结构，按照氧化铝晶型转化规律，在500-700℃常规焙烧条件下将不能转化为γ-氧化铝，难以很好地满足催化领域的应用要求。
发明内容
针对现有技术的不足，本发明提供了一种氧化铝晶粒及其制备方法。本发明的氧化铝晶粒，具有灵活的晶面分布可控性，制备方法简单易行、成本低廉，具有较强的可操作性，在催化、吸附领域具有良好应用前景。
本发明的氧化铝晶粒为单晶结构，具有近似正八面体立体形貌，所述的氧化铝晶粒的8个面属于γ态氧化铝的｛111｝晶面族，分别为（111）、（-111）、（1-11）、（11-1）、（-1-1-1）、（1-1-1）、（-11-1）和（-1-11）晶面；所述的氧化铝晶粒， 8个面的形状为近等边三角形，边长为11-50μm。氧化铝晶粒的晶粒大小为25-100μm。
本发明的氧化铝晶粒的制备方法，包括如下内容：
（1）将拟薄水铝石粉体焙烧后，加入无机钠盐，研磨处理至一定粒度，研磨后的粉料用洗涤去除钠盐后，配成一定浓度的悬浊液，加入有机酸，进行高速剪切处理；
（2）向步骤（1）得到的物料中加入一定量有机胺与有机碱混合物，混合均匀；
（3）步骤（2）得到的物料进行密闭水热处理，处理完毕后，固液分离，干燥、焙烧，得到产物。
本发明方法中，步骤（1）所述的焙烧条件为：350-650℃，优选为400-550℃，焙烧时间1-12小时，优选2-5小时。
本发明方法中，步骤（1）所述的研磨处理，采用高能球磨机进行，将粉体处理至1000目以上粉体粒度，粉体粒度优选为2000-10000目。球磨机的操作条件以获得满足要求的粉体粒度为标准来灵活调整。
本发明方法中，步骤（1）所述的无机钠盐为硝酸钠、氯化钠或硫酸钠中的一种或多种，无机钠盐用量占氧化铝粉体的0.1wt%-10wt%。
本发明方法中，步骤（1）所配制的氧化铝悬浊液质量浓度为20-200g/L，优选为50-100g/L。
本发明方法中，步骤（1）所配制的氧化铝悬浊液的溶剂为水与醇的混合物，所述的醇为甲醇和/或乙醇，优选为水与乙醇的混合物，水/醇的质量比为1-5。
本发明方法中，步骤（1）所述的有机酸为甲酸、乙酸或柠檬酸中的一种或多种，有机酸用量为氧化铝粉体质量的0.1wt%-10wt%，优选为0.5wt%-5wt%。
本发明方法中，步骤（1）所述的高速剪切条件为：转速2000-50000转/分钟，时间1-60分钟，优选条件为转速5000-50000转/分钟，时间5-45分钟。
本发明方法中，所述有机胺为甲胺、二甲胺、三甲胺、乙胺、二乙胺、正丙胺、异丙胺、正丁胺、乙醇胺、1，2-丙二胺、己二胺、苄胺或苯乙胺中的一种或多种。
本发明方法中，步骤（2）所述有机碱为四甲基氢氧化铵、四乙基氢氧化铵或四丙基氢氧化铵中的一种或多种；有机胺与有机碱的质量比0.1-1.0：1。有机胺在物料体系中的浓度为30-300g/L，优选为50-100g/L；有机碱在物料体系中的浓度为20-200g/L，优选为30-100g/L。
本发明方法中，步骤（3）所述的密闭水热条件为：60-250℃下水热处理2-72小时，优选为120-180℃。
本发明方法中，步骤（3）中所述的干燥温度不大于200℃，优选为不大于120℃，干燥程度为在干燥温度下物料恒重。
本发明方法中，步骤（3）所述的焙烧条件为：450-750℃焙烧1-24小时，优选500-650℃焙烧3-12小时。
本发明的氧化铝晶粒在催化剂及吸附领域有着广阔的应用前景，如作为馏分油加氢催化剂载体组分，尤其适用于重质油催化剂的制备。
附图说明
图1为实施例1制备的氧化铝晶粒的扫描电镜照片。
图2为实施例1制备的氧化铝晶粒的电子衍射谱图谱图。
图3、4分别为实施例1中200℃烘干及550℃后的氧化铝晶粒的XRD谱图。
具体实施方式
下面通过实施例对本发明方法加以详细的说明。氧化铝晶粒形状及尺寸根据扫描电镜观察与测量。晶型采用X射线衍射表征，通过电子衍射分析判断样品颗粒是单晶或多晶。根据扫描电镜图像，以八面体晶粒的两个顶端的长度作为晶粒大小。
实施例1
拟薄水铝石粉体500℃焙烧6小时后均匀掺入占其质量2%的氯化钠，用球磨机研磨成微粉，筛取5000目左右的粉末，用蒸馏水洗涤除掉氯化钠，然后配成25g/L的悬浊液，该悬浊液的溶剂为水与乙醇的混合物，两者的质量比为4。向悬浊液中加入部分乙酸，使乙酸用量为氧化铝前体质量的1.5%。采用高速剪切搅拌器（20000转/分钟），室温下剪切搅拌15分钟。往体系中加入乙醇胺及四乙基氢氧化铵，最终两者的浓度分别为25g/L及25g/L，搅拌均匀后，密闭体系并升温到180℃水热处理6小时。将120℃下干燥后的产物分别于200℃烘干及550℃下焙烧6小时。两种处理温度得到的产物的XRD谱表明，分别是拟薄水铝石及γ-氧化铝。经扫描电镜观察，烘干或焙烧温度对形貌无明显影响，产物皆为八面体颗粒形状，产物切片的电子衍射谱为规则排列的衍射斑点，因此颗粒具有单晶结构。按照有关晶体学生长规律可知，该八面体只可能暴露｛111｝族晶面。八面体晶粒尺寸大小约36μm，八面体｛111｝族晶面近似为等边三角形，其边长约16μm。该八面体晶粒体理论上｛111｝族晶面所占比例为100%。
实施例2
拟薄水铝石粉体650℃焙烧3小时后均匀掺入占其质量5%的硫酸钠，用球磨机研磨成微粉，筛取10000目左右的粉末，用蒸馏水洗涤除掉硫酸钠，然后配成质量浓度20g/L的水悬浊液，该悬浊液的溶剂为水与甲醇的混合物，两者的质量比率为1。向悬浊液中加入甲酸，使甲酸用量为氧化铝前体质量的2.5%。采用高速剪切搅拌器（10000转/分钟），室温下处理25分钟。往体系中加入三乙醇胺及四甲基氢氧化铵，最终两者的浓度分别为20g/L及35g/L，搅拌均匀后，密闭体系并升温到200℃水热处理6小时。将120℃下干燥后的产物分别于200℃烘干及550℃下焙烧6小时。两种处理温度得到的产物的XRD谱表明，分别是拟薄水铝石及γ-氧化铝。经扫描电镜观察，烘干或焙烧温度对形貌无明显影响，产物皆为八面体颗粒形状，产物切片的电子衍射谱为规则排列的衍射斑点，因此颗粒具有单晶结构。按照有关晶体学生长规律可知，该八面体只可能暴露｛111｝族晶面。八面体晶粒尺寸大小约27μm，八面体｛111｝族晶面近似为等边三角形，其边长约12μm。该八面体晶粒体理论上｛111｝族晶面所占比例为100%。
实施例3
拟薄水铝石粉体600℃焙烧4小时后均匀掺入占其质量3%的硫酸钠，用球磨机研磨成微粉，筛取10000目左右的粉末，用蒸馏水洗涤除掉硫酸钠，然后配成质量浓度35g/L的水悬浊液，该悬浊液的溶剂为水与甲醇的混合物，两者的质量比率为2。向悬浊液中加入部分乙酸，使乙酸用量为氧化铝前体质量的1.5%。采用高速剪切搅拌器（10000转/分钟），室温下处理20分钟。往体系中加入苯乙胺及四丙基氢氧化铵，最终两者的浓度分别为35g/L及20g/L，搅拌均匀后，密闭体系并升温到150℃水热处理6小时。将120℃下干燥后的产物分别于200℃烘干及550℃下焙烧6小时。两种处理温度得到的产物的XRD谱表明，分别是拟薄水铝石及γ-氧化铝。经扫描电镜观察，烘干或焙烧温度对形貌无明显影响，产物皆为八面体颗粒形状，产物切片的电子衍射谱为规则排列的衍射斑点，因此颗粒具有单晶结构。按照有关晶体学生长规律可知，该八面体只可能暴露｛111｝族晶面。八面体晶粒尺寸大小约67μm，八面体｛111｝族晶面近似为等边三角形，其边长约34μm。该八面体晶粒体理论上｛111｝族晶面所占比例为100%。
对比例1
按照CN201610494090.3实施例1提供的方法了制备八面体氧化铝晶粒。所得产物由产物分别经200℃及550℃焙烧5小时。200℃焙烧物不具有拟薄水铝石或薄水铝石结构，550℃焙烧物不能形成γ-氧化铝。

Claims (14)

1.一种氧化铝晶粒，其特征在于：氧化铝晶粒为单晶结构，具有近似正八面体立体形貌，氧化铝晶粒的8个面属于γ态氧化铝的｛111｝晶面族，分别为（111）、（-111）、（1-11）、（11-1）、（-1-1-1）、（1-1-1）、（-11-1）和（-1-11）晶面；氧化铝晶粒的晶粒大小为25-100μm；所述的氧化铝晶粒 8个面的形状为近等边三角形，边长为11-50μm。
2.一种权利要求1所述的氧化铝晶粒的制备方法，其特征在于包括如下内容：（1）将拟薄水铝石粉体焙烧后，加入无机钠盐，研磨处理至一定粒度，研磨后的粉料用洗涤去除钠盐后，配成一定浓度的悬浊液，加入有机酸，进行高速剪切处理；（2）向步骤（1）得到的物料中加入一定量有机胺与有机碱混合物，混合均匀；（3）步骤（2）得到的物料进行密闭水热处理，处理完毕后，固液分离，干燥、焙烧，得到产物；步骤（3）所述的焙烧条件为：450-750℃焙烧1-24小时。
3.根据权利要求2所述的方法，其特征在于：步骤（1）所述的焙烧条件为：350-650℃，焙烧时间1-12小时。
4.根据权利要求2所述的方法，其特征在于：步骤（1）所述的研磨处理采用高能球磨机进行，将粉体处理至1000目以上粉体粒度。
5.根据权利要求2所述的方法，其特征在于：步骤（1）所述的无机钠盐为硝酸钠、氯化钠或硫酸钠中的一种或多种，无机钠盐用量占氧化铝粉体的0.1wt%-10wt%。
6.根据权利要求2所述的方法，其特征在于：步骤（1）所配制的氧化铝悬浊液质量浓度为20-200g/L。
7.根据权利要求2所述的方法，其特征在于：步骤（1）所配制的氧化铝悬浊液的溶剂为水与醇的混合物，所述的醇为甲醇和/或乙醇，水/醇的质量比为1-5：1。
8.根据权利要求2所述的方法，其特征在于：步骤（1）所述的有机酸为甲酸、乙酸或柠檬酸中的一种或多种，有机酸用量为氧化铝粉体质量的0.1wt%-10wt%。
9.根据权利要求2所述的方法，其特征在于：步骤（1）所述的高速剪切条件为：转速2000-50000转/分钟，时间1-60分钟。
10.根据权利要求2所述的方法，其特征在于：所述有机胺为甲胺、二甲胺、三甲胺、乙胺、二乙胺、正丙胺、异丙胺、正丁胺、乙醇胺、1，2-丙二胺、己二胺、苄胺或苯乙胺中的一种或多种。
11.根据权利要求2所述的方法，其特征在于：步骤（2）所述有机碱为四甲基氢氧化铵、四乙基氢氧化铵或四丙基氢氧化铵中的一种或多种。
12.根据权利要求2所述的方法，其特征在于：步骤（2）所述有机胺与有机碱的质量比0.1-1.0：1；有机胺在物料体系中的浓度为30-300g/L，有机碱在物料体系中的浓度为20-200g/L。
13.根据权利要求2所述的方法，其特征在于：步骤（3）所述的密闭水热条件为：60-250℃下水热处理2-72小时。
14.一种权利要求1所述的氧化铝晶粒在催化、吸附领域中的应用。
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