CN112209739A - 一种轻质高强镁铝尖晶石空心球多孔陶瓷及其制备方法 - Google Patents
一种轻质高强镁铝尖晶石空心球多孔陶瓷及其制备方法 Download PDFInfo
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- 229910052596 spinel Inorganic materials 0.000 title claims abstract description 78
- 239000011029 spinel Substances 0.000 title claims abstract description 78
- 239000011777 magnesium Substances 0.000 title claims abstract description 69
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 69
- -1 magnesium aluminate Chemical class 0.000 title claims abstract description 69
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000004568 cement Substances 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 18
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- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000005187 foaming Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 238000005266 casting Methods 0.000 claims abstract description 4
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- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 229920002401 polyacrylamide Polymers 0.000 claims description 14
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 11
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 7
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 7
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 7
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 7
- 238000013329 compounding Methods 0.000 claims description 6
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- 239000002245 particle Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical group [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 14
- 239000012071 phase Substances 0.000 description 13
- 239000011159 matrix material Substances 0.000 description 8
- 239000000395 magnesium oxide Substances 0.000 description 7
- 235000012245 magnesium oxide Nutrition 0.000 description 7
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- 238000002441 X-ray diffraction Methods 0.000 description 3
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明公开了一种轻质高强镁铝尖晶石空心球多孔陶瓷及其制备方法。以质量百分含量表示，多孔陶瓷由原料镁铝尖晶石空心球60～80％、氧化铝微粉16.5～33％和铝酸钙水泥3.5～7％组成；另外加入结合剂、发泡剂和稳泡剂。首先将配制的稳泡剂和发泡剂加入结合剂中搅拌溶解，得到发泡溶液；然后加入铝酸钙水泥和氧化铝微粉搅匀，得到发泡浆料，接着加入镁铝尖晶石空心球搅匀得到泥料；所得泥料浇注成型、养护、脱模，得到多孔陶瓷坯体，坯体经干燥、高温炉加热保温，得到轻质高强镁铝尖晶石空心球多孔陶瓷。相比于传统空心球多孔陶瓷，本发明产品具有高强度、低导热系数、良好的体积稳定性及适用于碱性和超高温环境中。
Description
一、技术领域：
本发明属于无机化工技术领域，具体涉及一种轻质高强镁铝尖晶石空心球多孔陶瓷及其制备方法。
二、背景技术：
随着经济和社会的发展，社会日常生产所需要的能源消耗逐渐增加，不可再生能源日渐枯竭，能源危机日益严重，同时钢铁工业、有色冶金工业、建筑材料工业、超高温陶瓷及功能材料等各个工业领域对材料的使用要求也是更加的严苛。因此，为了满足这些高温工业对材料使用要求以及减少能源的浪费，迫切需要开发一种轻质、高强、耐火度高、热导率低的高温窑炉碱性内衬材料。而目前常用高温隔热空心球材料通常为氧化铝空心球制品和氧化锆空心球制品，适用于酸性或中性条件下。另外传统空心球制品体积密度较大，其密度为 1.4～1.6g/cm3，这就导致其重量较大并且热导率高，蓄热大。
空心球多孔陶瓷的强度主要与基质对于空心球的结合强度有关，基质对空心球结合强度高则制品强度高，样品破坏呈穿球断裂，基质对空心球结合强度低则制品强度低，样品破坏呈沿球断裂。合适的基质组成可以在不降低制品使用温度条件下使其具有高的强度。镁铝尖晶石具有很高的熔点(2150℃)，一般使用温度为1600～2000℃，不但可以用作耐碱隔热层还可以用作工作面砖。另外，铝酸钙水泥是目前耐火材料浇注料常用的一种水泥，具有高的耐火度、水化强度高的优点。铝酸钙水泥与基质中的氧化铝粉配合，经高温烧成后生成六铝酸钙(熔点为1875℃)，为高温相，具有良好的抗碱蒸汽腐蚀能力，此外还具有力学性能好、热震稳定性好等优点。因此，六铝酸钙结合的镁铝尖晶石空心球制品是碱性环境下高温隔热材料的优良选择。
三、发明内容：
本发明要解决的技术问题是：针对目前市场缺乏高强、低导热的碱性空心球制品问题，本发明提供一种轻质高强镁铝尖晶石空心球多孔陶瓷及其制备方法。本发明技术方案以镁铝尖晶石空心球(球璧为镁铝尖晶石相，球心为方镁石相)为轻质骨料，氧化铝微粉和铝酸钙水泥为基质，聚丙烯酰胺溶液为结合剂，十二烷基硫酸钠为发泡剂，十二醇和羧甲基纤维素钠一定比例复配为稳泡剂，经混料、成型、干燥、烧成制备得到轻质高强镁铝尖晶石空心球多孔陶瓷。本发明发泡剂的加入使得气孔率进一步增大，体积密度降低；在高温条件下烧成，基质中铝酸钙水泥与氧化铝微粉反应生成片状耐高温六铝酸钙，提高镁铝尖晶石空心球之间的结合强度和基质耐高温性能，主晶相MgAlO4和结合相CA6形成的二元体系生成液相的温度可以超过1800℃，主晶相MgAlO4和MgO形成的二元体系生成液相的温度也可以超过1800℃，都有希望能用于2000℃以上耐高温的碱性环境。因此，本发明制备得到的轻质高强镁铝尖晶石空心球多孔陶瓷具有质轻、高强、耐高温和适用于中性和碱性环境等优势。
为了解决上述问题，本发明采取的技术方案是：
本发明提供一种轻质高强镁铝尖晶石空心球多孔陶瓷，以质量百分含量表示，所述轻质高强镁铝尖晶石空心球多孔陶瓷由原料镁铝尖晶石空心球60～ 80％、氧化铝微粉16.5～33％和铝酸钙水泥3.5～7％组成；另外，加入占三种原料总重量24～30％的结合剂聚丙烯酰胺溶液、占三种原料总重量0.03～0.05％的发泡剂十二烷基硫酸钠和占三种原料总重量0.03～0.05％的稳泡剂。
根据上述的轻质高强镁铝尖晶石空心球多孔陶瓷，所述镁铝尖晶石空心球的粒径为0.5～0.9mm。
根据上述的轻质高强镁铝尖晶石空心球多孔陶瓷，所述氧化铝微粉的d50为 2.3μm。
根据上述的轻质高强镁铝尖晶石空心球多孔陶瓷，所述铝酸钙水泥为 Secar71铝酸钙水泥。
根据上述的轻质高强镁铝尖晶石空心球多孔陶瓷，所述聚丙烯酰胺溶液的质量百分浓度为33％。
根据上述的轻质高强镁铝尖晶石空心球多孔陶瓷，所述稳泡剂是由十二醇和羧甲基纤维素钠复配而成，十二醇与羧甲基纤维素钠复配过程中二者的混合比例为4∶6。
另外，提供一种上述轻质高强镁铝尖晶石空心球多孔陶瓷的制备方法，所述制备方法包括以下步骤：
a、首先按照上述轻质高强镁铝尖晶石空心球多孔陶瓷的配比比例配制各种原料；
b、将配制的稳泡剂和发泡剂十二烷基硫酸钠加入结合剂聚丙烯酰胺溶液中进行搅拌溶解，搅拌均匀后得到发泡溶液；然后加入铝酸钙水泥和氧化铝微粉搅拌均匀，得到发泡浆料，接着加入镁铝尖晶石空心球进行搅拌，搅拌混匀后得到泥料；
c、将步骤b所得泥料倒入模具中进行浇注成型，所得成型样品在模具中室温下养护24h，然后60℃养护10h后脱模，得到镁铝尖晶石空心球多孔陶瓷坯体；
d、将步骤c所得坯体进行烘干，得到干燥坯体；
e、将步骤d所得干燥的镁铝尖晶石空心球多孔陶瓷坯体，在高温炉中升温至1700℃，保温2～8h；然后随炉冷却至室温，得到轻质高强镁铝尖晶石空心球多孔陶瓷。
根据上述的轻质高强镁铝尖晶石空心球多孔陶瓷的制备方法，步骤d中所述烘干的具体过程为：将所得坯体放入烘箱中，在110℃条件下烘干10h，得到干燥坯体。
根据上述的轻质高强镁铝尖晶石空心球多孔陶瓷的制备方法，步骤e中高温炉中升温的制度为：由室温～300℃过程中升温速率为3℃/min，300～1100℃升温过程中控制升温速率为5℃/min，1100～1700℃升温过程中控制升温速率为 3℃/min。
本发明的积极有益效果：
1、本发明技术方案中，加入发泡剂和稳泡剂，制备得到的多孔陶瓷相比于致密耐火材料具有体积密度低、显气孔率高、热容量、低导热系数和隔热性好的特点。
2、本发明技术方案中，以铝酸钙水泥和氧化铝微粉为基质材料，且二者配比在高温下全部形成片状结构的六铝酸钙结合相，使基质的常温强度和高温强度大大提高，同时使主晶相MgAlO4和结合相CA6形成的二元体系生成液相的温度较高，该材料有希望能用于2000℃以上超高温的碱性环境。因此，本发明材料多孔陶瓷相比于普通隔热材料具有高强度、使用温度高和耐碱性环境腐蚀等特点。
3、本发明技术方案中，采用的镁铝尖晶石空心球，内部包含了一个体积占比5％以下的氧化镁(熔点2800℃)芯球，能够进一步保障镁铝尖晶石空心球的耐高温性能和耐碱侵蚀性能。
四、附图说明：
图1不同粒径镁铝尖晶石空心球原料的XRD图谱；
由图1可知，镁铝尖晶石空心球原料主要成分为MgAlO4和MgO，且显微结构分析表明空心球璧的主要组成为MgAlO4相，内部主要是MgO相小芯球。
图2不同镁铝尖晶石空心球加入量所得多孔陶瓷的XRD图谱；
图2中A1#、A2#、A3#、A4#和A5#分别代表的是实施例1、实施例2、实施例3、实施例4和实施例5。
由图2可知，所得各试样主要的物相为MA、MgO和CA6，均为高温相，且显微结构分析表明MA主要位于空心球表面、MgO主要位于空心球内部，基质中主要为CA6。
五、具体实施方式：
以下结合实施例进一步阐述本发明，但并不限制本发明技术方案保护的范围。
以下实施例中采用的原料氧化铝微粉的d50为2.3μm，聚丙烯酰胺溶液的质量百分浓度为33％，稳泡剂是由十二醇和羧甲基纤维素钠复配而成，十二醇与羧甲基纤维素钠复配过程中二者的混合比例为4∶6。
实施例1：
本发明轻质高强镁铝尖晶石空心球多孔陶瓷，以质量百分含量表示，由原料0.9～0.6mm的镁铝尖晶石空心球40％、0.6～0.5mm的镁铝尖晶石空心球20％、氧化铝微粉33％和Secar71铝酸钙水泥7％组成；另外，加入占三种原料总重量 24％的结合剂聚丙烯酰胺溶液、占三种原料总重量0.043％的发泡剂十二烷基硫酸钠和占三种原料总重量0.04％的稳泡剂。
实施例2：
本发明轻质高强镁铝尖晶石空心球多孔陶瓷，以质量百分含量表示，由原料0.9～0.6mm的镁铝尖晶石空心球45％、0.6～0.5mm的镁铝尖晶石空心球20％、氧化铝微粉28.87％和Secar71铝酸钙水泥6.13％组成；另外，加入占三种原料总重量26％的结合剂聚丙烯酰胺溶液、占三种原料总重量0.04％的发泡剂十二烷基硫酸钠和占三种原料总重量0.05％的稳泡剂。
实施例3：
本发明轻质高强镁铝尖晶石空心球多孔陶瓷，以质量百分含量表示，由原料0.9～0.6mm的镁铝尖晶石空心球50％、0.6～0.5mm的镁铝尖晶石空心球20％、氧化铝微粉24.75％和Secar71铝酸钙水泥5.25％组成；另外，加入占三种原料总重量28％的结合剂聚丙烯酰胺溶液、占三种原料总重量0.03％的发泡剂十二烷基硫酸钠和占三种原料总重量0.04％的稳泡剂。
实施例4：
本发明轻质高强镁铝尖晶石空心球多孔陶瓷，以质量百分含量表示，由原料0.9～0.6mm的镁铝尖晶石空心球55％、0.6～0.5mm的镁铝尖晶石空心球20％、氧化铝微粉20.62％和Secar71铝酸钙水泥4.38％组成；另外，加入占三种原料总重量30％的结合剂聚丙烯酰胺溶液、占三种原料总重量0.05％的发泡剂十二烷基硫酸钠和占三种原料总重量0.045％的稳泡剂。
实施例5：
本发明轻质高强镁铝尖晶石空心球多孔陶瓷，以质量百分含量表示，由原料0.9～0.6mm的镁铝尖晶石空心球60％、0.6～0.5mm的镁铝尖晶石空心球20％、氧化铝微粉16.5％和Secar71铝酸钙水泥3.5％组成；另外，加入占三种原料总重量26％的结合剂聚丙烯酰胺溶液、占三种原料总重量0.04％的发泡剂十二烷基硫酸钠和占三种原料总重量0.05％的稳泡剂。
本发明实施例1～5所述轻质高强镁铝尖晶石空心球多孔陶瓷的制备方法，详见以下步骤：
a、首先按照实施例1～5任一项所述轻质高强镁铝尖晶石空心球多孔陶瓷的配比比例配制各种原料；
b、将配制的稳泡剂和发泡剂十二烷基硫酸钠加入结合剂聚丙烯酰胺溶液中进行搅拌溶解，搅拌均匀后得到发泡溶液；然后加入铝酸钙水泥和氧化铝微粉搅拌均匀，得到发泡浆料，接着加入镁铝尖晶石空心球进行搅拌，搅拌混匀后得到泥料；
c、将步骤b所得泥料倒入模具中进行浇注成型，所得成型样品在模具中室温下养护24h，然后60℃养护10h后脱模，得到镁铝尖晶石空心球多孔陶瓷坯体；
d、将步骤c所得镁铝尖晶石空心球多孔陶瓷坯体放入烘箱中，在110℃条件下烘干10h，得到干燥坯体；
e、将步骤d所得干燥的镁铝尖晶石空心球多孔陶瓷坯体，在高温炉中升温至1700℃(高温炉升温的具体过程为：由室温～300℃过程中升温速率为 3℃/min，300～1100℃升温过程中控制升温速率为5℃/min，1100～1700℃升温过程中控制升温速率为3℃/min)，保温6h；然后随炉冷却至室温，得到轻质高强镁铝尖晶石空心球多孔陶瓷。
实施例1～5制备所得产品镁铝尖晶石空心球多孔陶瓷的相关物理性能参数详见表1。
表1实施例1～5制备所得产品镁铝尖晶石空心球多孔陶瓷的相关物理性能参数
由表1可以看出，利用本发明技术方案制备得到的产品镁铝尖晶石空心球多孔陶瓷的强度在3.97～21.71MPa之间，体积密度在0.92～1.14g/cm3，重烧线变化在零附近，800℃导热系数在0.342～0.431W/(m·K)之间，相比于传统空心球多孔陶瓷，具有高强度、低密度、低导热系数、良好的体积稳定性、耐高温和适用于碱性环境等优点，综合使用效果良好。
Claims (9)
1.一种轻质高强镁铝尖晶石空心球多孔陶瓷，其特征在于：以质量百分含量表示，所述轻质高强镁铝尖晶石空心球多孔陶瓷由原料镁铝尖晶石空心球60～80％、氧化铝微粉16.5～33％和铝酸钙水泥3.5～7％组成；另外，加入占三种原料总重量24～30％的结合剂聚丙烯酰胺溶液、占三种原料总重量0.03～0.05％的发泡剂十二烷基硫酸钠和占三种原料总重量0.03～0.05％的稳泡剂。
2.根据权利要求1所述的轻质高强镁铝尖晶石空心球多孔陶瓷，其特征在于：所述镁铝尖晶石空心球的粒径为0.5～0.9mm。
3.根据权利要求1所述的轻质高强镁铝尖晶石空心球多孔陶瓷，其特征在于：所述氧化铝微粉的d50为2.3μm。
4.根据权利要求1所述的轻质高强镁铝尖晶石空心球多孔陶瓷，其特征在于：所述铝酸钙水泥为Secar71铝酸钙水泥。
5.根据权利要求1所述的轻质高强镁铝尖晶石空心球多孔陶瓷，其特征在于：所述聚丙烯酰胺溶液的质量百分浓度为33％。
6.根据权利要求1所述的轻质高强镁铝尖晶石空心球多孔陶瓷，其特征在于：所述稳泡剂是由十二醇和羧甲基纤维素钠复配而成，十二醇与羧甲基纤维素钠复配过程中二者的混合比例为4∶6。
7.一种权利要求1所述轻质高强镁铝尖晶石空心球多孔陶瓷的制备方法，其特征在于，所述制备方法包括以下步骤：
a、首先按照权利要求1所述轻质高强镁铝尖晶石空心球多孔陶瓷的配比比例配制各种原料；
b、将配制的稳泡剂和发泡剂十二烷基硫酸钠加入结合剂聚丙烯酰胺溶液中进行搅拌溶解，搅拌均匀后得到发泡溶液；然后加入铝酸钙水泥和氧化铝微粉搅拌均匀，得到发泡浆料，接着加入镁铝尖晶石空心球进行搅拌，搅拌混匀后得到泥料；
c、将步骤b所得泥料倒入模具中进行浇注成型，所得成型样品在模具中室温下养护24h，然后60℃养护10h后脱模，得到镁铝尖晶石空心球多孔陶瓷坯体；
d、将步骤c所得坯体进行烘干，得到干燥坯体；
e、将步骤d所得干燥的镁铝尖晶石空心球多孔陶瓷坯体，在高温炉中升温至1700℃，保温2～8h；然后随炉冷却至室温，得到轻质高强镁铝尖晶石空心球多孔陶瓷。
8.根据权利要求7所述的轻质高强镁铝尖晶石空心球多孔陶瓷的制备方法，其特征在于，步骤d中所述烘干的具体过程为：将所得坯体放入烘箱中，在110℃条件下烘干10h，得到干燥坯体。
9.根据权利要求7所述的轻质高强镁铝尖晶石空心球多孔陶瓷的制备方法，其特征在于，步骤e中高温炉中升温的制度为：由室温～300℃过程中升温速率为3℃/min，300～1100℃升温过程中控制升温速率为5℃/min，1100～1700℃升温过程中控制升温速率为3℃/min。
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