CN112390616A - 一种耐火材料的烧结成型工艺 - Google Patents

一种耐火材料的烧结成型工艺 Download PDF

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CN112390616A
CN112390616A CN202011266658.9A CN202011266658A CN112390616A CN 112390616 A CN112390616 A CN 112390616A CN 202011266658 A CN202011266658 A CN 202011266658A CN 112390616 A CN112390616 A CN 112390616A
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parts
refractory material
component
phenolic resin
mass
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李善平
李欣
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Xinhua Dongtai Special Refractory Co ltd
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Xinhua Dongtai Special Refractory Co ltd
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  • Compositions Of Oxide Ceramics (AREA)

Abstract

本发明公开了一种耐火材料的烧结成型工艺，其利用粒径＜1mm的氧化镁、碳化硅、碳化硼、氮化铝或者氮化硅的比例混合物作为基质；利用具有三类不同粒径的耐碱粘土、煅烧铝土矿、堇青石的比例混合物作为骨料；利用粒径为1~3mm的珍珠岩、蛭石、泡沫氧化铝的比例混合物作为轻质填料通过双组份的结合剂进行混合后制备，其在结合剂添加有炭素材料改性的酚醛树脂，并将双组份的结合剂分两次加入进行混料并在混料完成后压制成耐火材料生坯，耐火材料生坯进行三段式热处理后随炉自然冷却至室温即得成品。本发明制得耐火材料具有优良的热震性能和致密性，使得材料具有稳定裂纹扩展的特征，使得产品的致密性和热震性能得到了提升，力学性能也得到了提升。

Description

一种耐火材料的烧结成型工艺
技术领域
本发明涉及耐火材料技术领域，具体涉及一种耐火材料的烧结成型工艺。
背景技术
耐火材料是指耐火度不低于1580℃的无机非金属材料，它是为高温技术服务的基础材料，是用作高温窑炉等热工设备的结构材料，以及工业高温容器和部件的材料。耐火材料广泛应用于钢铁、水泥、陶瓷、玻璃、化工、有色等高温工业相关领域，是高温工业的重要基础材料和不可或缺的重要支撑材料,在现代工业体系中具有重要地位。随着近年来我国基础工业的快速发展，我国已经成为世界上最大的耐火材料生产大国和消费国。
在现有技术中，大部分耐火材料是以天然矿石（如耐火粘土、硅石、菱镁矿、白云石）为原料制造的，也有采用某些工业原料和人工合成原料（如工业氧化铝、碳化硅、合成莫来石、合成尖晶石等）的，因此，耐火材料的种类很多。耐火材料按照其耐火度来划分可分为普通、高级和特级耐火制品，按其密度来划分可分为轻质及重质耐火材料，随着耐火材料的技术进步以及钢铁、水泥、玻璃、有色等高温工业生产工艺和装备的不断升级，对耐火材料的质量水平提出了更好的要求，低档耐火材料的市场空间将不断萎缩，高档耐火材料的比重不断扩大，其中需求度较高的主要为轻质的高级或者特级耐火材料，这一类耐火材料除要求有较轻的质量和较为稳定的耐火性能外，还要求能够承受相应的物理化学变化及机械作用。而常用的无机非金属材料的机械韧性较差是无机非金属和材料中普遍存在的一个问题，使得无机非金属材料的耐火材料的机械韧性也较差，影响到了其高温时候的抗热震性能，在使用过程中容易发生开裂、剥落等情况，降低了耐火材料的使用寿命。
因而，如何在目前工艺的基础上，提高相关耐火材料的结构强度、稳定性及抗热震性能具有重要的意义。
发明内容
本发明所解决的技术问题在于提供一种耐火材料的烧结成型工艺，以解决上述技术背景中的缺陷。
本发明所解决的技术问题采用以下技术方案来实现：
一种耐火材料的烧结成型工艺，利用以下质量份组分的原料进行制备：
基质：氧化镁30~35份、碳化硅10~17份、碳化硼3~7份、 氮化铝或者氮化硅1~3份；所述基质中的各组分均为粒径＜1mm的颗粒物；
骨料：耐碱粘土75~90份、煅烧铝土矿10~15份、堇青石7~9份；其中，耐碱粘土采用Al2O3含量为25%~30%的耐碱粘土，堇青石被粉碎为粉末并过筛分级；骨料中粒径为1.0~3.0mm的颗粒的比例为30~40%、粒径为0.1~1.0mm的颗粒的比例为40~50%，以及余量粒径＜0.1mm的颗粒，且不同粒径的颗粒在耐碱粘土、煅烧铝土矿、堇青石中等比例均匀分布；
轻质填料：珍珠岩40~60份、蛭石20~40份、泡沫氧化铝15~25份，其中，所述轻质填料中各原料均为粒径为1~3mm的颗粒物；
结合剂为双组份结合剂：A组分为炭素材料改性的酚醛树脂20~30份，而B组分为硅酸钙水泥10~15份、聚乙烯醇9~10份、乙二醇3~5份、木质素磺酸钠3~5份、水30~50份；
所述用于酚醛树脂改性的炭素材料为石墨烯、纳米炭黑、碳纳米管的一种或者任意比例的混合物，将所述炭素材料加入酚醛树脂中进行超声辅助分散90~120min后即得炭素材料改性的酚醛树脂，所述炭素材料在酚醛树脂中的加入量为0.3~0.5%；
制备时，将质量比为20~30%的基质、质量比为30~40%的骨料以及余量的轻质填料按照总质量比100%的比例混合制得耐火材料干料，同时将结合剂中的B组分混合后制浆料，将耐火材料干料与浆料按照质量比6:1~8:1的比例混合完成后进行搅拌，搅拌60~90min，然后加入结合剂中的A组分，进行搅拌，搅拌20~30min后将原料入模具压制成耐火材料生坯；
将成型后的耐火材料生坯投入炉内进行热处理，热处理时进行三段式热处理，控制低温区温度为120~200℃，升温速率为30℃/h，并保温30~50min，中温区温度为450~600℃，升温速率为50℃/h，并保温90~120min，高温区温度为1200~1650℃，升温速率为80℃/h，并保温3~5h；热处理完成后随炉自然冷却至室温即得成品。
作为进一步限定，在进行耐火材料干料混合时可以添加占混合料总质量1~3%的硅微粉以及0.3~0.5%的白炭黑来改善成型后的耐火材料生坯的烧结性能，并提高成品耐火材料的抗裂变性能。
作为进一步限定，所述模具为厚度大于15mm的板料模具或者是砖坯模具。
作为进一步限定，所述结合剂中的B组分中还添加有占组分总质量0.03~1.0%的聚羧酸减水剂以及占组分总质量0.1~0.3%的煤油作为粉尘抑制剂。
有益效果：本发明一种耐火材料的烧结成型工艺可用于制备耐火砖或者耐火板，其制备的耐火材料通过不同粒径的基料以及骨料的结合组成增强组合物，以提高耐火材料整体结构的完整性，并在保证耐火性能的情况下提高其致密度，使得耐火材料具有优良的抗热震性能和抗裂变性能，而轻质填料的使用则能用于降低耐火材料的质量，并在成型后消除内部机械应力，进一步提高断裂韧性；而双组份结合剂的使用配合炭素材料改性的酚醛树脂可使酚醛树脂热解炭化后形成晶粒尺寸更大、层间距更小的玻璃状可镶嵌结构次生碳，或原位形成纳米碳纤维以及纳米碳管，从而达到显著改善低碳镁碳耐火材料的抗热震性及高温强度的目的。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例一：
耐火材料利用以下质量份组分的原料进行制备：
基质：氧化镁30份、碳化硅10份、碳化硼3份、 氮化铝1份；所述基质中的各组分均为粒径＜1mm的颗粒物；
骨料：耐碱粘土75份、煅烧铝土矿10份、堇青石7份；其中，耐碱粘土采用Al2O3含量为25%的耐碱粘土，堇青石被粉碎为粉末并过筛分级；骨料中粒径为1.0~3.0mm的颗粒的比例为30%、粒径为0.1mm的颗粒的比例为40%以及40%的粒径＜0.1mm的颗粒，不同粒径的颗粒在耐碱粘土、煅烧铝土矿、堇青石中等比例均匀分布；
轻质填料：珍珠岩40份、蛭石20份、泡沫氧化铝15份，其中，所述轻质填料中各原料均为粒径为2~3mm的颗粒物；
结合剂为双组份结合剂：
A组分为炭素材料改性的酚醛树脂20份，该改性酚醛树脂中添加有占酚醛树脂重量0.3%的炭素材料，该炭素材料为碳纳米管与纳米炭黑的质量比3:1的比例混合物，将该炭素材料加入酚醛树脂中进行超声辅助分散90min后即得炭素材料改性的酚醛树脂；
B组分为硅酸钙水泥10份、聚乙烯醇9份、乙二醇3份、木质素磺酸钠3份、水30份；
制备时，将质量比为20%的基质、质量比为30%的骨料以及质量比50%的轻质填料混合制得耐火材料干料，同时将结合剂中的B组分混合后制浆料，将耐火材料干料与浆料按照质量比6:1的比例混合完成后进行搅拌，搅拌60min，然后加入结合剂中的A组分，进行搅拌，搅拌20min后将将原料入长宽高为230mm×114mm×65mm的砖坯模具压制成耐火材料生坯；
将成型后的耐火材料生坯投入炉内进行热处理，热处理时进行三段式热处理，控制低温区温度为120℃，升温速率为30℃/h，并保温30min，中温区温度为450℃，升温速率为50℃/h，并保温90min，高温区温度为1200℃，升温速率为80℃/h，并保温3h；热处理完成后随炉自然冷却至室温即得耐火砖成品。
实施例二：
耐火材料利用以下质量份组分的原料进行制备：
基质：氧化镁35份、碳化硅17份、碳化硼7份、 氮化铝3份；所述基质中的各组分均为粒径＜1mm的颗粒物；
骨料：耐碱粘土90份、煅烧铝土矿15份、堇青石9份；其中，耐碱粘土采用Al2O3含量为30%的耐碱粘土，堇青石被粉碎为粉末并过筛分级；骨料中粒径为1.0~3.0mm的颗粒的比例为40%、粒径为0.1mm的颗粒的比例为50%以及10%的粒径＜0.1mm的颗粒，不同粒径的颗粒在耐碱粘土、煅烧铝土矿、堇青石中等比例均匀分布；
轻质填料：珍珠岩60份、蛭石40份、泡沫氧化铝25份，其中，所述轻质填料中各原料均为粒径为1~3mm的颗粒物；
结合剂为双组份结合剂：
A组分为炭素材料改性的酚醛树脂30份，该改性酚醛树脂中添加有占酚醛树脂重量0.5%的炭素材料，该炭素材料为碳纳米管与纳米炭黑的质量比3:1的比例混合物，将该炭素材料加入酚醛树脂中进行超声辅助分散120min后即得炭素材料改性的酚醛树脂；
B组分为硅酸钙水泥15份、聚乙烯醇10份、乙二醇5份、木质素磺酸钠5份、水50份；
制备时，将质量比为30%的基质、质量比为40%的骨料以及质量比30%的轻质填料混合制得耐火材料干料，同时将结合剂中的B组分混合后制浆料，将耐火材料干料与浆料按照质量比8:1的比例混合完成后进行搅拌，搅拌90min，然后加入结合剂中的A组分，进行搅拌，搅拌30min后将原料入长宽高为230mm×114mm×65mm的砖坯模具压制成耐火材料生坯；
将成型后的耐火材料生坯投入炉内进行热处理，热处理时进行三段式热处理，控制低温区温度为200℃，升温速率为30℃/h，并保温50min，中温区温度为600℃，升温速率为50℃/h，并保温120min，高温区温度为1650℃，升温速率为80℃/h，并保温5h；热处理完成后随炉自然冷却至室温即得耐火砖成品。
实施例三：
耐火材料利用以下质量份组分的原料进行制备：
基质：氧化镁32份、碳化硅15份、碳化硼6份、 氮化铝2份；所述基质中的各组分均为粒径＜1mm的颗粒物；
骨料：耐碱粘土80份、煅烧铝土矿12份、堇青石8份；其中，耐碱粘土采用Al2O3含量为28%的耐碱粘土，堇青石被粉碎为粉末并过筛分级；骨料中粒径为1.0~3.0mm的颗粒的比例为35%、粒径为0.1mm的颗粒的比例为45%以及20%的粒径＜0.1mm的颗粒，不同粒径的颗粒在耐碱粘土、煅烧铝土矿、堇青石中等比例均匀分布；
轻质填料：珍珠岩50份、蛭石30份、泡沫氧化铝20份，其中，所述轻质填料中各原料均为粒径为1~3mm的颗粒物；
结合剂为双组份结合剂：
A组分为炭素材料改性的酚醛树脂25份，该改性酚醛树脂中添加有占酚醛树脂重量0.4%的炭素材料，该炭素材料为碳纳米管与纳米炭黑的质量比3:1的比例混合物，将该炭素材料加入酚醛树脂中进行超声辅助分散100min后即得炭素材料改性的酚醛树脂；
B组分为硅酸钙水泥12份、聚乙烯醇9.5份、乙二醇4份、木质素磺酸钠4份、水40份；
制备时，将质量比为25%的基质、质量比为35%的骨料以及质量比40%的轻质填料混合制得耐火材料干料，同时将结合剂中的B组分混合后制浆料，将耐火材料干料与浆料按照质量比7:1的比例混合完成后进行搅拌，搅拌80min，然后加入结合剂中的A组分，进行搅拌，搅拌25min后将原料入长宽高为230mm×114mm×65mm的砖坯模具压制成耐火材料生坯；
将成型后的耐火材料生坯投入炉内进行热处理，热处理时进行三段式热处理，控制低温区温度为160℃，升温速率为30℃/h，并保温40min，中温区温度为550℃，升温速率为50℃/h，并保温110min，高温区温度为1450℃，升温速率为80℃/h，并保温4h；热处理完成后随炉自然冷却至室温即得耐火砖成品。
实施例四：
耐火材料利用以下质量份组分的原料进行制备：
基质：氧化镁33份、碳化硅16份、碳化硼6份、 氮化铝2份；所述基质中的各组分均为粒径＜1mm的颗粒物；
骨料：耐碱粘土85份、煅烧铝土矿13份、堇青石8份；其中，耐碱粘土采用Al2O3含量为27%的耐碱粘土，堇青石被粉碎为粉末并过筛分级；骨料中粒径为1.0~3.0mm的颗粒的比例为35%、粒径为0.1mm的颗粒的比例为45%以及20%的粒径＜0.1mm的颗粒，不同粒径的颗粒在耐碱粘土、煅烧铝土矿、堇青石中等比例均匀分布；
轻质填料：珍珠岩50份、蛭石30份、泡沫氧化铝20份，其中，所述轻质填料中各原料均为粒径为1~3mm的颗粒物；
结合剂为双组份结合剂：
A组分为炭素材料改性的酚醛树脂25份，该改性酚醛树脂中添加有占酚醛树脂重量0.4%的炭素材料，该炭素材料为石墨烯、纳米炭黑、碳纳米管的质量比1:1:1的比例混合物，将该炭素材料加入酚醛树脂中进行超声辅助分散110min后即得炭素材料改性的酚醛树脂；
B组分为硅酸钙水泥12份、聚乙烯醇10份、乙二醇4份、木质素磺酸钠5份、水45份；
制备时，将质量比为25%的基质、质量比为35%的骨料以及质量比40%的轻质填料混合制得耐火材料干料，同时将结合剂中的B组分混合后制浆料，将耐火材料干料与浆料按照质量比7:1的比例混合完成后进行搅拌，搅拌80min，然后加入结合剂中的A组分，进行搅拌，搅拌25min后将原料入长宽高为230mm×114mm×65mm的砖坯模具压制成耐火材料生坯；
将成型后的耐火材料生坯投入炉内进行热处理，热处理时进行三段式热处理，控制低温区温度为180℃，升温速率为30℃/h，并保温40min，中温区温度为500℃，升温速率为50℃/h，并保温105min，高温区温度为1350℃，升温速率为80℃/h，并保温4h；热处理完成后随炉自然冷却至室温即得耐火砖成品。
实施例五：
耐火材料利用以下质量份组分的原料进行制备：
基质：氧化镁32份、碳化硅15份、碳化硼6份、 氮化铝2份；所述基质中的各组分均为粒径＜1mm的颗粒物；
骨料：耐碱粘土80份、煅烧铝土矿12份、堇青石8份；其中，耐碱粘土采用Al2O3含量为28%的耐碱粘土，堇青石被粉碎为粉末并过筛分级；骨料中粒径为1.0~3.0mm的颗粒的比例为35%、粒径为0.1mm的颗粒的比例为45%以及20%的粒径＜0.1mm的颗粒，不同粒径的颗粒在耐碱粘土、煅烧铝土矿、堇青石中等比例均匀分布；
轻质填料：珍珠岩50份、蛭石30份、泡沫氧化铝20份，其中，所述轻质填料中各原料均为粒径为1~3mm的颗粒物；
结合剂为双组份结合剂：
A组分为炭素材料改性的酚醛树脂25份，该改性酚醛树脂中添加有占酚醛树脂重量0.4%的炭素材料，该炭素材料为碳纳米管与纳米炭黑的质量比3:1的比例混合物，将该炭素材料加入酚醛树脂中进行超声辅助分散100min后即得炭素材料改性的酚醛树脂；
B组分为硅酸钙水泥12份、聚乙烯醇9.5份、乙二醇4份、木质素磺酸钠4份、水40份；
制备时，将质量比为25%的基质、质量比为35%的骨料以及质量比40%的轻质填料加入混合容器中，一并加入占基质、骨料和轻质填料总质量2%的硅微粉以及0.4%的白炭黑，将混合物进行干混制得耐火材料干料，同时将结合剂中的B组分混合后制浆料，将耐火材料干料与浆料按照质量比7:1的比例混合完成后进行搅拌，搅拌80min，然后加入结合剂中的A组分，进行搅拌，搅拌25min后将原料入长宽高为230mm×114mm×65mm的砖坯模具压制成耐火材料生坯；
将成型后的耐火材料生坯投入炉内进行热处理，热处理时进行三段式热处理，控制低温区温度为160℃，升温速率为30℃/h，并保温40min，中温区温度为550℃，升温速率为50℃/h，并保温110min，高温区温度为1450℃，升温速率为80℃/h，并保温4h；热处理完成后随炉自然冷却至室温即得耐火砖成品。
将实施例一~实施例五的技术条件下制得的耐火砖成品与市售的两款耐火砖作为对比例一以及对比例二进行性能测试，其结果如下：
实施例一 实施例二 实施例三 实施例四 实施例五 对比例一 对比例二
气孔率 5.10% 5.70% 6.00% 6.40% 6.20% 7.80% 7.20%
体积密度 3.24g/cm3 3.03g/cm3 3.17g/cm3 3.12g/cm3 3.09g/cm3 3.94g/cm3 4.22g/cm3
常温耐压强度 （25℃） 93.4MPa 90.2MPa 101.3MPa 101.5MPa 105.0MPa 84.2MPa 87.7MPa
高温耐压强度（1100℃） 48.4MPa 54.6MPa 58.2MPa 62.1MPa 64.7MPa 49.4MPa 42.3MPa
常温断裂强度 （25℃） 5.4MPa 5.6MPa 6.1MPa 6.1MPa 6.4MPa 4.8MPa 4.6MPa
高温断裂强度（1100℃） 4.2MPa 4.6MPa 4.8MPa 5.1MPa 5.3MPa 3.7MPa 3.4MPa
热震稳定性 （水冷） 7 8 9 9 10 7 6
耐火等级 特级 特级 特级 特级 特级 特级 特级
由上表可以看出，本发明的实施例的技术方案相比于现有技术的实施例，其质量更轻，且物理强度和热震稳定性要更加优异，且能保证有效耐火性能。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (5)

1.一种耐火材料的烧结成型工艺，其特征在于，利用以下质量份组分的原料进行制备：
基质：氧化镁30~35份、碳化硅10~17份、碳化硼3~7份、 氮化铝或者氮化硅1~3份；所述基质中的各组分均为粒径＜1mm的颗粒物；
骨料：耐碱粘土75~90份、煅烧铝土矿10~15份、堇青石7~9份；其中，耐碱粘土采用Al2O3含量为25%~30%的耐碱粘土，堇青石被粉碎为粉末并过筛分级；骨料中粒径为1.0~3.0mm的颗粒的比例为30~40%、粒径为0.1~1.0mm的颗粒的比例为40~50%，以及余量粒径＜0.1mm的颗粒，且不同粒径的颗粒在耐碱粘土、煅烧铝土矿、堇青石中等比例均匀分布；
轻质填料：珍珠岩40~60份、蛭石20~40份、泡沫氧化铝15~25份，其中，所述轻质填料中各原料均为粒径为1~3mm的颗粒物；
结合剂为双组份结合剂：A组分为炭素材料改性的酚醛树脂20~30份，而B组分为硅酸钙水泥10~15份、聚乙烯醇9~10份、乙二醇3~5份、木质素磺酸钠3~5份、水30~50份；
所述用于酚醛树脂改性的炭素材料为石墨烯、纳米炭黑、碳纳米管的一种或者任意比例的混合物，将所述炭素材料加入酚醛树脂中进行超声辅助分散90~120min后即得炭素材料改性的酚醛树脂，所述炭素材料在酚醛树脂中的加入量为0.3~0.5%；
制备时，将质量比为20~30%的基质、质量比为30~40%的骨料以及余量的轻质填料按照总质量比100%的比例混合制得耐火材料干料，同时将结合剂中的B组分混合后制浆料，将耐火材料干料与浆料按照质量比6:1~8:1的比例混合完成后进行搅拌，搅拌60~90min，然后加入结合剂中的A组分，进行搅拌，搅拌20~30min后将原料入模具压制成耐火材料生坯；
将成型后的耐火材料生坯投入炉内进行热处理，热处理时进行三段式热处理，控制低温区温度为120~200℃，升温速率为30℃/h，并保温30~50min，中温区温度为450~600℃，升温速率为50℃/h，并保温90~120min，高温区温度为1200~1650℃，升温速率为80℃/h，并保温3~5h；热处理完成后随炉自然冷却至室温即得成品。
2.根据权利要求1所述的耐火材料的烧结成型工艺，其特征在于，在进行耐火材料干料混合时添加有占混合料总质量1~3%的硅微粉以及0.3~0.5%的白炭黑。
3.根据权利要求1所述的耐火材料的烧结成型工艺，其特征在于，所述模具为厚度大于15mm的板料模具或者是砖坯模具。
4.根据权利要求1所述的耐火材料的烧结成型工艺，其特征在于，所述结合剂中的B组分中添加有占组分总质量0.03~1.0%的聚羧酸减水剂。
5.根据权利要求1所述的耐火材料的烧结成型工艺，其特征在于，所述结合剂中的B组分中添加有占组分总质量0.1~0.3%的煤油作为粉尘抑制剂。
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