CN115304357B - 一种黄长石/铝酸钙两相材料及其制备方法 - Google Patents
一种黄长石/铝酸钙两相材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 37
- XFWJKVMFIVXPKK-UHFFFAOYSA-N calcium;oxido(oxo)alumane Chemical compound [Ca+2].[O-][Al]=O.[O-][Al]=O XFWJKVMFIVXPKK-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229910001719 melilite Inorganic materials 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000002893 slag Substances 0.000 claims abstract description 17
- RGKMZNDDOBAZGW-UHFFFAOYSA-N aluminum calcium Chemical compound [Al].[Ca] RGKMZNDDOBAZGW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 12
- 230000000996 additive effect Effects 0.000 claims abstract description 12
- 235000019738 Limestone Nutrition 0.000 claims abstract description 11
- 239000006028 limestone Substances 0.000 claims abstract description 11
- 239000011575 calcium Substances 0.000 claims abstract description 10
- 238000005245 sintering Methods 0.000 claims abstract description 10
- 239000006004 Quartz sand Substances 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 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 9
- 239000004927 clay Substances 0.000 claims abstract description 9
- 241000723420 Celtis Species 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 4
- 239000011148 porous material Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000011230 binding agent Substances 0.000 claims description 13
- 229920005551 calcium lignosulfonate Polymers 0.000 claims description 10
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 239000011362 coarse particle Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 4
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- QKYBEKAEVQPNIN-UHFFFAOYSA-N barium(2+);oxido(oxo)alumane Chemical compound [Ba+2].[O-][Al]=O.[O-][Al]=O QKYBEKAEVQPNIN-UHFFFAOYSA-N 0.000 claims description 2
- 238000000748 compression moulding Methods 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000011819 refractory material Substances 0.000 abstract description 10
- 230000035939 shock Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 17
- 229910052656 albite Inorganic materials 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000010304 firing Methods 0.000 description 5
- 239000002440 industrial waste Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229910017625 MgSiO Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 229910052661 anorthite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 229910001597 celsian Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 229910001678 gehlenite Inorganic materials 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- -1 na) 2 (Al Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000000930 thermomechanical effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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Abstract
本发明公开了一种黄长石/铝酸钙两相材料及其制备方法，涉及耐火材料技术领域，原料包括：铝钙渣50～75wt%，石灰石0～8wt%，石英砂10～20wt%，工业氧化铝2～5wt%，粘土1～10wt%，添加剂1～10wt%，高温烧成后主晶相为黄长石Ca2Al2SiO7和铝酸钙Ca23.90Al27.88O65.58。对传统的陶瓷制备工艺进行改良，制备出的多孔材料较铝钙渣相比，具有较强的热稳定性好、膨胀系数低等优点，还可以作为一种添加剂引入到耐火材料中，提高其烧结性能和热震稳定性。
Description
技术领域
本发明涉及耐火材料技术领域，特别是涉及一种黄长石/铝酸钙两相材料及其制备方法。
背景技术
耐火材料作为一种均质多相的无机非金属材料，具有较高的耐火度和优异的热机械性能，被广泛应用于高温窑炉和冶金行业。2020年我国的耐火材料生产量约为2477.49万吨，随着生产成本的提高和矿产资源的过度开采造成的环境污染，在耐火材料的生产过程中采用工业废料为原料成为一种选择。
黄长石是由铝、镁、铁的硅酸盐构成的一类硅酸盐类矿物，其化学通式为(Ca,Na)2(Al,Mg,Fe)[(Al,Si)SiO7]。钙铝黄长石（Ca2Al(Al,Si)O7）和镁黄长石(Ca2MgSiO7)是黄长石族中两种重要的化合物。黄长石具有体积密度低、热膨胀系数小等特点，尽管其熔点不高不能作为耐火材料的主晶相，但将其引入到耐火材料中作为第二相有助提高材料的烧结性能、力学强度和热震稳定性。
铝钙渣主要以铝灰和石灰石经高温合成的，分为烧结和熔融两种铝钙渣。铝灰的主要来源于金属铝、电解铝熔炼以及铝合金的生产过程中产生的废料。近年来，我国铝工业发展迅猛，已成为世界上主要的铝工业强国。炼铝过程中产生的铝灰渣是一种产量大、污染环境的工业废渣。刚出炉的工业废渣含有较高的金属铝，其中只有部分金属铝能得到回收，其余的含有少量金属铝的铝灰废渣被堆积在厂区或填埋，不仅造成资源的浪费，同时还会污染环境。
发明内容
本发明针对上述技术问题，克服现有技术的缺点，提供一种黄长石/铝酸钙两相材料，原料包括：铝钙渣50～75wt%，石灰石0～8wt%，石英砂10～20wt%，工业氧化铝2～5wt%，粘土1～10wt%，添加剂1～10wt%，高温烧成后主晶相为黄长石Ca2Al2SiO7和铝酸钙Ca23.90Al27.88O65.58。
本发明进一步限定的技术方案是：
前所述的一种黄长石/铝酸钙两相材料，铝钙渣粒径包括3-1mm，1-0.5mm，0.5-0.088mm和＜0.088mm。
前所述的一种黄长石/铝酸钙两相材料，两相材料具有均匀分布的气孔，显气孔率为25%～32%，体积密度1.5～2.0g/cm3。
前所述的一种黄长石/铝酸钙两相材料，添加剂为结合剂、脱模剂中的至少一种。。
前所述的一种黄长石/铝酸钙两相材料，添加剂包括结合剂和脱模剂，结合剂包括聚乙烯醇、木质素磺酸钙中的至少一种，占原料总重量的3～8wt%；脱模剂包括石蜡、硬脂酸钠中的至少一种，占原料总重量的0～1wt%。
本发明的另一目的在于提供一种黄长石/铝酸钙两相材料制备方法，包括以下步骤：
（1）分别按照质量百分比称量铝钙渣、石灰石、石英砂、工业氧化铝和粘土原料；
（2）将细粉部分在球磨机中预混2～6小时，使得预混粉的粒度小于350目且占比低于20%；
（3）将粗颗粒和预混粉在强力搅拌机中搅拌5～10分钟，随后加入添加剂继续混炼10～60分钟；
（4）将混炼均匀的坯料采用液压成型的方式在液压机中压制成型；
（5）将压制成型的坯体在真空干燥箱中进行干燥，真空度小于0.08Mpa，干燥温度为80～110℃，干燥时间15～24小时；
（6）将干燥后的坯体置于电炉中，采用温度梯度升温，热处理温度为1200～1400℃，保温时间为3～10小时，随炉冷却后即制得低膨胀、多孔的黄长石/铝酸钙两相材料。
前所述的一种黄长石/铝酸钙两相材料制备方法，在上述步骤（2）～（4）之间加入添加剂，混合均匀后使得粉料成型为生坯，其中水的添加量为1.5～10wt%。
前所述的一种黄长石/铝酸钙两相材料制备方法，在步骤（4）中，坯料在150～200MPa下保压10～100s，压制成型得到尺寸为Փ50mm×H50mm的坯体。
前所述的一种黄长石/铝酸钙两相材料制备方法，在步骤（6）中，热处理的控温制度为：①室温～1000℃，升温速率为5～10℃/min；②1000℃至目标温度，升温速率为3℃/min，并保温。
本发明的有益效果是：
（1）本发明以废弃的铝灰废渣和石灰石为主要原料制备黄长石/铝酸钙复合材料，不仅可以避免工业废料对生态环境的污染，而且降低了生产成本，变废为宝，使得工业原料再生利用，具有重要的社会意义和经济效益；
（2）本发明设备简单、成本低、对材料的成型没有特别限定，可以根据具体的设备工艺做出相应的调整；
（3）本发明在对压制成型的坯体干燥过程中采用真空干燥，真空度小于0.08MPa，避免了含铝钙渣的材料在干燥、固化过程因氧化钙的水化而开裂；
（4）本发明主要原料采用金属铝、电解铝熔炼以及铝合金生产过程中产生的工业废料，对传统的陶瓷制备工艺进行改良，制备出的多孔材料较铝钙渣相比，具有较强的热稳定性好、膨胀系数低等优点，还可以作为一种添加剂引入到耐火材料中，提高其烧结性能和热震稳定性。
附图说明
图1、2为黄长石/铝酸钙两相材料的XRD衍射图谱。
具体实施方式
实施例1
本实施例提供的一种黄长石/铝酸钙两相材料，原料：铝钙渣（＜0.088mm）68wt%，石灰石2wt%，石英砂19wt%，工业氧化铝1wt%，粘土10wt%，外加总质量的5%的木质素磺酸钙溶液为结合剂，按照质量进行称量。
先将细粉部分在行星式球磨机中预混3小时；
将粗颗粒和预混粉在强力搅拌机中搅拌10分钟，随后加入结合剂木质素磺酸钙进行混炼1小时；
将混炼均匀的坯料采用液压成型的方式在液压机中压制成型；
将压制成型的坯体在真空干燥箱中进行干燥，真空度小于0.08MPa，干燥温度为110℃，干燥时间20小时；
将干燥后的坯体置于电炉中，采用温度梯度升温，热处理温度为1200℃、1300℃、1400℃，保温时间均为为5h，随炉冷却后即制得低膨胀、多孔陶瓷。
通过对比不同烧成温度下物相组成，在1200℃下的物相组成为黄长石、铝酸钙和钙长石，当烧成温度高于1300℃时物相组成为黄长石和铝酸钙，且随着烧成温度的升高，材料的力学性能提高。
实施例2
本实施例提供的一种黄长石/铝酸钙两相材料，原料：铝钙渣（＜0.088mm）70wt%，石灰石2wt%，石英砂17wt%，工业氧化铝1wt%，粘土10wt%，外加总质量的3wt%的木质素磺酸钙溶液为结合剂和1wt%的硬脂酸钠为脱模剂，按照质量进行称量。
先将细粉部分在行星式球磨机中预混3小时；
将粗颗粒和预混粉在强力搅拌机中搅拌10分钟,随后加入结合剂木质素磺酸钙和脱模剂硬质酸钠继续混炼1小时；
将混炼均匀的坯料采用液压成型的方式在液压机中压制成型；
将压制成型的坯体在真空干燥箱中进行干燥，真空度小于0.08Mpa，干燥温度为110℃，干燥时间15小时；
将干燥后的坯体置于电炉中，采用温度梯度升温，热处理温度为1200℃、1300℃、1400℃，保温时间均为为5h，随炉冷却后即制得低膨胀、多孔陶瓷。
图1列出了经不同温度烧成后的低膨胀、多孔陶瓷的X射线衍射图谱。烧成温度为1200℃物相组成为黄长石、铝酸钙和硅酸钙，烧成温度为1300℃和1400℃时，物相组成为黄长石和铝酸钙，且在 1300℃烧成后黄长石的含量为59.5%，1400℃烧成后黄长石的含量为76.6%。考虑到黄长石优异的热震稳定性，因此，1400℃更适合低膨胀、多孔的黄长石/铝酸钙材料的制备。
实施例3
本实施例提供的一种黄长石/铝酸钙两相材料，原料：铝钙渣（＜0.088mm）72%，石灰石5wt%，石英砂10%，工业氧化铝3%，粘土10%，外加总质量的3wt%的木质素磺酸钙为结合剂，按照质量进行称量。
先将细粉部分在球磨机中预混3小时；
将粗颗粒和预混粉在强力搅拌机中搅拌10分钟，随后加入结合剂木质素磺酸钙进行混炼1小时；
将混炼均匀的坯料采用液压成型的方式在液压机中压制成型；
将压制成型的坯体在真空干燥箱中进行干燥，真空度小于0.08MPa，干燥温度为110℃，干燥时间18小时；
将干燥后的坯体采用感应加热，热处理温度约为1400℃，随炉冷却后即制得低膨胀、多孔的黄长石/铝酸钙复合材料，其黄长石含量高于80%，体积密度为1.8g/cm3，显气孔率为30%。
实施例4
本实施例提供的一种黄长石/铝酸钙两相材料，原料：铝钙渣（＜0.088mm）70wt%，石灰石5wt%，石英砂10wt%，工业氧化铝5wt%，粘土10wt%，外加总质量的3wt%的木质素磺酸钙为结合剂，按照质量进行称量。
先将细粉部分在球磨机中预混3小时；
将粗颗粒和预混粉在强力搅拌机中搅拌10分钟，随后加入结合剂木质素磺酸钙进行混炼1小时；
将混炼均匀的坯料采用液压成型的方式在液压机中压制成型；
将压制成型的坯体在真空干燥箱中进行干燥，真空度小于0.08MPa，干燥温度为110℃，干燥时间20小时；
将干燥后的坯体采用感应加热，热处理温度约为1400℃，随炉冷却后即制得低膨胀、多孔的黄长石/铝酸钙两相材料，且黄长石含量高于92.5%。图2为其X射线衍射图谱，该黄长石/铝酸钙两相材料的体积密度为2.1g/cm3，显气孔率为26%。
除上述实施例外，本发明还可以有其他实施方式。凡采用等同替换或等效变换形成的技术方案，均落在本发明要求的保护范围。
Claims (6)
1.一种黄长石/铝酸钙两相材料，其特征在于：原料包括：铝钙渣50～75wt%，石灰石0～8wt%，石英砂10～20wt%，工业氧化铝2～5wt%，粘土1～10wt%，添加剂1～10wt%，高温烧成后主晶相为黄长石Ca2Al2SiO7和铝酸钙Ca23.90Al27.88O65.58；
制备方法包括以下步骤：
（1）分别按照质量百分比称量铝钙渣、石灰石、石英砂、工业氧化铝和粘土原料；
（2）将细粉部分在球磨机中预混2～6小时，使得预混粉的粒度小于350目且占比低于20%；
（3）将粗颗粒和预混粉在强力搅拌机中搅拌5～10分钟，随后加入添加剂继续混炼10～60分钟；
（4）将混炼均匀的坯料采用液压成型的方式在液压机中压制成型；
（5）将压制成型的坯体在真空干燥箱中进行干燥，真空度小于0.08Mpa，干燥温度为80～110℃，干燥时间15～24小时；
（6）将干燥后的坯体置于电炉中，采用温度梯度升温，热处理温度为1200～1400℃，保温时间为3～10小时，随炉冷却后即制得低膨胀、多孔的黄长石/铝酸钙两相材料；
所述铝钙渣粒径包括3-1mm，1-0.5mm，0.5-0.088mm和＜0.088mm；
两相材料具有均匀分布的气孔，显气孔率为25%～32%，体积密度1.5～2.0g/cm3。
2.根据权利要求1所述的一种黄长石/铝酸钙两相材料，其特征在于：所述添加剂为结合剂、脱模剂中的至少一种。
3.根据权利要求1所述的一种黄长石/铝酸钙两相材料，其特征在于：所述添加剂包括结合剂和脱模剂，结合剂包括聚乙烯醇、木质素磺酸钙中的至少一种，占原料总重量的3～8wt%；脱模剂包括石蜡、硬脂酸钠中的至少一种，占原料总重量的0～1wt%。
4.根据权利要求1所述的一种黄长石/铝酸钙两相材料制备方法，其特征在于：在上述步骤（2）～（4）之间加入添加剂，混合均匀后使得粉料成型为生坯，其中水的添加量为1.5～10wt%。
5.根据权利要求1所述的一种黄长石/铝酸钙两相材料制备方法，其特征在于：在步骤（4）中，坯料在150～200MPa下保压10～100s，压制成型得到尺寸为Փ50mm×H50mm的坯体。
6.根据权利要求1所述的一种黄长石/铝酸钙两相材料制备方法，其特征在于：在步骤（6）中，热处理的控温制度为：①室温～1000℃，升温速率为5～10℃/min；②1000℃至目标温度，升温速率为3℃/min，并保温。
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