CN106745119B - 一种镁铝尖晶石粉末的合成方法 - Google Patents

一种镁铝尖晶石粉末的合成方法 Download PDF

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CN106745119B
CN106745119B CN201611030941.5A CN201611030941A CN106745119B CN 106745119 B CN106745119 B CN 106745119B CN 201611030941 A CN201611030941 A CN 201611030941A CN 106745119 B CN106745119 B CN 106745119B
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吕晓军
刘建华
张恒星
赖延清
李劼
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Abstract

本发明公开了一种镁铝尖晶石粉末的合成方法,以水溶性淀粉作为单体,以N‑N’‑亚甲基双丙烯酰胺为交联剂,过硫酸铵作为引发剂,加入到镁、铝无机盐生成镁铝尖晶石的反应体系中,搅拌条件下恒温水浴保温,得到前驱体,随后将前驱体干燥后煅烧,即得到高纯镁铝尖晶石微粉。采用本发明方法可制备纯度高、颗粒尺寸小、分散性好的MAS粉体,且该方法具有环保、成本低、周期短、操作方便、温度易控、粉体性能更加优良等优点。

Description

一种镁铝尖晶石粉末的合成方法
技术领域
本发明属于粉末冶金技术领域,具体涉及一种镁铝尖晶石粉末的合成方法。
背景技术
镁铝尖晶石(化学式为MgAl2O4,英文缩写MAS)之前主要用在耐火材料、耐磨材料和精细陶瓷等领域,近年来逐渐应用于电子、催化剂及其载体材料、透明陶瓷、尖晶石单晶等领域。这对MAS粉体的性能要求也就越来越高。MAS粉体的主要性能包括纯度、粒度和组成等。其中,纯度是衡量粉体性能优劣的关键指标,高纯MAS粉体的纯度一般大于99%。
目前,常见到的MAS粉体制备技术主要有:固相反应法、共沉淀法、溶剂蒸发法、溶胶-凝胶法等方法。这些制备技术都存在一定局限性:如固相反应法成本低廉、工艺简单,但存在转化率低、平均粒径大、颗粒形貌难以控制的问题;共沉淀法获得的粉体活性高、组分均匀,但粉体分散性差,易形成硬团聚;溶剂蒸发法基本解决了颗粒分散性问题,但是粉体多为中空结构,影响了粉体的应用;溶胶-凝胶法产品纯度较高,但是粉体分散困难。
为此,本发明提出一种制备高纯镁铝尖晶石微粉的高分子絮凝法。高分子絮凝法是以金属无机盐为主要原料,以无毒的淀粉为单体、以N-N’-亚甲基双丙烯酰胺为交联剂、以过氧化物为引发剂,制备得到絮凝状(非凝胶状)的前驱体,干燥煅烧后即得。与传统方法相比,本发明的高分子絮凝法具有环保、成本低、周期短、操作方便、温度易控、粉体性能更加优良等优点。更为重要的是由于在絮凝过程中所形成的聚合物网络使得MgAl2O4的接触机会减少,从而减少了团聚的产生,有希望获得纯度高、颗粒尺寸小和分散均匀的MAS粉体。
发明内容
本发明的目的旨在克服现有技术中的不足,提供一种镁铝尖晶石粉末的合成方法。采用本发明,可制备纯度高、颗粒尺寸小、分散性好的MAS粉体,且该方法具有环保、成本低、周期短、操作方便、温度易控、粉体性能更加优良等优点。采用高分子絮凝法制备得到的高纯MAS微粉,可以广泛应用于耐火材料、电子、催化剂及其载体材料、透明陶瓷、尖晶石单晶等领域。
本发明的目的是通过以下方式实现的。
一种镁铝尖晶石粉末的合成方法:以水溶性淀粉作为单体,以N-N’-亚甲基双丙烯酰胺为交联剂,过硫酸铵作为引发剂,加入到镁、铝无机盐生成镁铝尖晶石的反应体系中,搅拌条件下恒温水浴保温,得到前驱体,随后将前驱体干燥后煅烧,即得到高纯镁铝尖晶石微粉。
所述的镁铝尖晶石粉末的合成方法:
以2-16%质量浓度的水溶性淀粉作为单体,以2-16%质量浓度的N-N’-亚甲基双丙烯酰胺为交联剂;然后将N-N’-亚甲基双丙烯酰胺和水溶性淀粉溶液按2:1-12:1的体积比例配制成一定浓度的溶液,加入到镁、铝无机盐按化学计量比配制成的溶液中,水浴加热、搅拌,然后加入2-12%质量浓度的过硫酸铵作为引发剂,水浴搅拌保温,得到前驱体,随后将前驱体干燥后煅烧,即得到镁铝尖晶石微粉。
所述的镁铝尖晶石粉末的合成方法:采用镁、铝无机盐为原料,按摩尔比为Al2O3:MgO=1:1的比例配制成混合溶液。
所述的镁铝尖晶石粉末的合成方法,镁、铝无机盐混合溶液中镁、铝无机盐的浓度均为0.05g/ml-1g/ml。
所述的镁铝尖晶石粉末的合成方法:N-N’-亚甲基双丙烯酰胺和水溶性淀粉的混合溶液与镁、铝无机盐的混合溶液的体积比例为1:8-1:12。
所述的镁铝尖晶石粉末的合成方法:
将N-N’-亚甲基双丙烯酰胺和水溶性淀粉溶液加入到镁、铝无机盐配制成的溶液中,在75-85℃温度下水浴加热、搅拌至少10min,然后加入过硫酸铵,在搅拌条件下60-100℃下恒温水浴保温至少1h,得到前驱体。
所述的镁铝尖晶石粉末的合成方法:将前驱体在100-120℃下干燥至少24h后,在700-1000℃下煅烧至少2h,即得到高纯镁铝尖晶石微粉。
所述的镁铝尖晶石粉末的合成方法,镁无机盐原料包括碳酸镁、硝酸镁、硫酸镁中的一种或几种;铝无机盐原料包括碳酸铝、硝酸铝、硫酸铝中的一种或几种。
与现有技术相比,本发明具有下列优点:
(1)采用本发明得到的MAS粉体,杂质含量少、纯度高;
(2)采用本发明得到的MAS粉体,颗粒尺寸小和分散均匀;
(3)本发明制备工艺具有环保、成本低、周期短、操作方便、温度易控、实用性强的优点。
附图说明:
图1为本发明制备MAS粉体的步骤示意图;
图2为本发明制得的MAS粉体的XRD图;
图3为本发明制得的MAS粉体的SEM图。
具体实施方式
下面给出的实施例拟对本发明作进一步说明,但不能理解为是对本发明保护范围的限制,该领域的技术人员根据上述本发明的内容对本发明作出的一些非本质的改进和调整,仍属于本发明的保护范围。
实施例1
硝酸镁和硝酸铝,按MgO:Al2O3摩尔比为1:1配制成混合溶液。先配制浓度为3%的淀粉和浓度为3%的N-N’-亚甲基双丙烯酰胺,然后将N-N’-亚甲基双丙烯酰胺和水溶性淀粉按5:1的体积比例配制成一定浓度的溶液,并加入到镁、铝无机盐溶液(镁、铝无机盐的浓度均为0.05g/ml)中,两种混合溶液体积比为1:10。在80℃温度下水浴加热、搅拌10min,然后加入3%浓度的过硫酸铵作为引发剂,用恒温加热磁力搅拌器,在60℃下水浴保温1h,生成白色的絮状沉淀,得到前驱体。随后将前驱体在110℃下干燥24h后,在800℃下煅烧2h,得到纯度高于99.99%、颗粒尺寸小(0.1-10微米)和分散均匀的MAS微粉。
实施例2
硝酸镁和硝酸铝,按MgO:Al2O3摩尔比为1:1配制成混合溶液。先配制浓度为6%的淀粉和浓度为8%的N-N’-亚甲基双丙烯酰胺,然后将N-N’-亚甲基双丙烯酰胺和水溶性淀粉按8:1的体积比例配制成一定浓度的溶液,并加入到镁、铝无机盐溶液中(镁、铝无机盐的浓度均为0.5g/ml),两种混合溶液体积比为1:10。在80℃温度下水浴加热、搅拌10min,然后加入5%浓度的过硫酸铵作为引发剂,用恒温加热磁力搅拌器,在70℃下水浴保温1h,生成白色的絮状沉淀,得到前驱体。随后将前驱体在110℃下干燥24h后,在900℃下煅烧2h,得到纯度高于99.99%、颗粒尺寸小(0.1-10微米)和分散均匀的MAS微粉。
实施例3
硝酸镁和硝酸铝,按MgO:Al2O3摩尔比为1:1配制成混合溶液。先配制浓度为9%的淀粉和浓度为10%的N-N’-亚甲基双丙烯酰胺,然后将N-N’-亚甲基双丙烯酰胺和水溶性淀粉按10:1的体积比例配制成一定浓度的溶液,并加入到镁、铝无机盐溶液中(镁、铝无机盐的浓度均为0.8g/ml),两种混合溶液体积比为1:10。在80℃温度下水浴加热、搅拌10min,然后加入3%浓度的过硫酸铵作为引发剂,用恒温加热磁力搅拌器,在80℃下水浴保温1h,生成白色的絮状沉淀,得到前驱体。随后将前驱体在110℃下干燥24h后,在1000℃下煅烧2h,得到纯度高于99.99%、颗粒尺寸小(0.1-10微米)和分散均匀的MAS微粉。
实施例4
硝酸镁和硝酸铝,按MgO:Al2O3摩尔比为1:1配制成混合溶液。先配制浓度为15%的淀粉和浓度为15%的N-N’-亚甲基双丙烯酰胺,然后将N-N’-亚甲基双丙烯酰胺和水溶性淀粉按3:1的体积比例配制成一定浓度的溶液,并加入到镁、铝无机盐溶液(镁、铝无机盐的浓度均为1g/ml)中,两种混合溶液体积比为1:10。在80℃温度下水浴加热、搅拌10min,然后加入3%浓度的过硫酸铵作为引发剂,用恒温加热磁力搅拌器,在100℃下水浴保温1h,生成白色的絮状沉淀,得到前驱体。随后将前驱体在110℃下干燥24h后,在700℃下煅烧2h,得到纯度高于99.99%、颗粒尺寸小(0.1-10微米)和分散均匀的MAS微粉。
对比例:
操作步骤和原料添加比例同上述实施例,以丙烯酰胺为单体、以N-N’-亚甲基双丙烯酰胺为交联剂、以过氧化物为引发剂,制备出的凝胶作为前驱体,将凝胶干燥、煅烧即可得到亚微米级MAS粉体。制备得到的产品的性能进行对比发现纯度仅为95%,颗粒尺寸8-20微米的MAS微粉,而且分散不均匀。

Claims (2)

1.一种镁铝尖晶石粉末的合成方法,其特征在于:以水溶性淀粉作为单体,以2-16%质量浓度的水溶性淀粉作为单体,以2-16%质量浓度的N-N’-亚甲基双丙烯酰胺为交联剂;然后将N-N’-亚甲基双丙烯酰胺和水溶性淀粉溶液按2:1-12:1的体积比例配制成一定浓度的溶液,加入到镁、铝无机盐按化学计量比配制成的溶液中,水浴加热、搅拌,然后加入2-12%质量浓度的过硫酸铵作为引发剂,水浴搅拌保温,得到前驱体,随后将前驱体干燥后煅烧,即得到镁铝尖晶石微粉;
采用镁、铝无机盐为原料,按摩尔比为Al2O3:MgO=1:1的比例配制成混合溶液;镁、铝无机盐混合溶液中镁、铝无机盐的浓度均为0.05g/ml-1g/ml;N-N’-亚甲基双丙烯酰胺和水溶性淀粉的混合溶液与镁、铝无机盐的混合溶液的体积比例为1:8-1:12;将N-N’-亚甲基双丙烯酰胺和水溶性淀粉溶液加入到镁、铝无机盐配制成的溶液中,在75-85℃温度下水浴加热、搅拌至少10min,然后加入过硫酸铵,在搅拌条件下60-100℃下恒温水浴保温至少1h,得到前驱体;将前驱体在100-120℃下干燥至少24h后,在700-1000℃下煅烧至少2h,即得到高纯镁铝尖晶石微粉。
2.根据权利要求1所述的镁铝尖晶石粉末的合成方法,其特征在于,镁无机盐原料包括碳酸镁、硝酸镁、硫酸镁中的一种或几种;铝无机盐原料包括碳酸铝、硝酸铝、硫酸铝中的一种或几种。
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