CN108623313A - 一种氮化硅结合碳化硅复合耐火材料的制备方法 - Google Patents
一种氮化硅结合碳化硅复合耐火材料的制备方法 Download PDFInfo
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Abstract
本发明提供了一种氮化硅结合碳化硅复合耐火材料的制备方法,先将碳化硅、氮化硅和偶联剂混合,研磨,得到表面改性的碳化硅和氮化硅;再采用有机单体对硫酸钙晶须进行接枝反应,得到改性硫酸钙晶须;最后将表面改性的碳化硅和氮化硅、改性硫酸钙晶须、二氧化硅微粉、莫来石、红柱石、硅藻土加到结合剂的水溶液中,搅拌均匀后注入模型中成型,脱模后置于乙醇水溶液中脱水,脱水后干燥,得到坯体;将烘干的坯体置于高温炉中烧制,即得。本发明以莫来石为骨料,碳化硅、氮化硅和改性硫酸钙晶须为增强相制备了耐火材料,所得耐火材料具有良好的物理性能。
Description
技术领域
本发明属于耐火材料技术领域,具体涉及一种氮化硅结合碳化硅复合耐火材料的制备方法。
背景技术
耐火材料是高温行业中不可缺少的基础材料。耐火材料涉及钢铁、建材、有色金属冶炼、机械、化工等多项国民经济的支柱行业。这些行业中伴随着大量的高温化学反应,这就要求耐火材料除了能够耐受高温和化学侵蚀外,同时还要能够在这些恶劣条件下具有抵抗应力或者应对温度急剧变化的能力,并拥有足够长的使用寿命。目前,氧化物-非氧化物复合材料由于其本身具有的优越性能,已经逐渐发展成为新一代的优质高效耐火材料,并应用于许多高温关键部位。莫来石质材料作为一种传统的耐火材料, 具有耐火度高、热膨胀系数低、热震稳定性好、高湿抗蠕变性好、具有很高的耐磨性及耐剥落、抗侵蚀性等一系列良好的性能,一直以来都被广泛应用。但由于莫来石晶体的结构中的SiO4和AlO4四面体的空间的排列会随Al、Si比的变化而出现不同程度的周期性氧缺位,使得其晶格间的空隙较多,进而导致莫来石材料的强度较低,影响了其在工业生产中的应用。
碳化硅(SiC)是用石英砂、石油焦(或煤焦)、木屑等原料通过电阻炉高温冶炼而成,具有良好的力学性能,机械强度高于刚玉,脆而锋利,耐磨性能优良。氮化硅(Si3N4)是一种重要的结构陶瓷材料,与碳化娃一样也是一种共价键极强的非氧化物。碳化硅和氮化硅均为重要的耐高温硬质材料,但是如何同时应用碳化硅和氮化硅增强莫来石的强度,需要进一步研究。
发明内容
本发明的目的是解决现有莫来石耐火材料强度较低的问题,提供一种氮化硅结合碳化硅复合耐火材料的制备方法。
一种氮化硅结合碳化硅复合耐火材料的制备方法,包括以下步骤:
步骤1,以重量份计,将碳化硅10-20份、氮化硅10-20份和偶联剂2-5份混合,研磨,得到表面改性的碳化硅和氮化硅;
步骤2,以重量份计,将硬脂酸锌1-2份和硫酸钙晶须5-10份混合,混合物加至有机单体和交联剂的混合溶液20-30份中,混合,加入引发剂0.2-0.6份和催化剂0.1-0.4份,搅拌混合,加热反应,所得产物经洗涤、过滤、干燥处理,转移至马弗炉中,在250℃-400℃的温度条件下热处理15min-60min,得到改性硫酸钙晶须;
步骤3,以重量份计,将表面改性的碳化硅和氮化硅10份、改性硫酸钙晶须2份、二氧化硅微粉1-3份、莫来石20-30份、红柱石30-40份、硅藻土3-5份加到结合剂的水溶液3-6份中,搅拌均匀后注入模型中成型,脱模后置于乙醇水溶液中脱水,脱水后干燥,得到坯体;
步骤4,将烘干的坯体置于高温炉中烧制,即得。
优选地,所述偶联剂为硅烷偶联剂。
优选地,所述有机单体和交联剂的混合溶液是丙烯酰胺和N,N-亚甲基双丙酰胺的混合水溶液,丙烯酰胺和N,N-亚甲基双丙酰胺的质量比为10:1,丙烯酰胺在混合水溶液中的浓度为5wt.%。
优选地,所述引发剂为过硫酸铵,催化剂为四甲基乙二胺。
优选地,所述结合剂的水溶液是聚乙烯醇的水溶液,聚乙烯醇的浓度为6-10wt.%。
优选地,烧制条件为1450-1500℃,保温5-10h。
本发明以莫来石为骨料,碳化硅、氮化硅和改性硫酸钙晶须为增强相制备了耐火材料,所得耐火材料具有良好的物理性能。通过对硫酸钙晶须进行改性,可以增强碳化硅、氮化硅与莫来石的联结,使得莫来石的晶格间空隙都被碳化硅和氮化硅填充,改善了莫来石的强度,从而提高了耐火材料的强度。
具体实施方式
实施例1
一种氮化硅结合碳化硅复合耐火材料的制备方法,包括以下步骤:
步骤1,以重量份计,将碳化硅10份、氮化硅10份和硅烷偶联剂2份混合,研磨,得到表面改性的碳化硅和氮化硅;
步骤2,以重量份计,将硬脂酸锌1份和硫酸钙晶须5份混合,混合物加至有机单体丙烯酰胺和交联剂N,N-亚甲基双丙酰胺的混合溶液20份中,丙烯酰胺和N,N-亚甲基双丙酰胺的质量比为10:1,丙烯酰胺在混合水溶液中的浓度为5wt.%,混合,加入引发剂过硫酸铵0.2份和催化剂四甲基乙二胺0.1份,搅拌混合,加热反应,所得产物经洗涤、过滤、干燥处理,转移至马弗炉中,在250℃的温度条件下热处理60min,得到改性硫酸钙晶须;
步骤3,以重量份计,将表面改性的碳化硅和氮化硅10份、改性硫酸钙晶须2份、二氧化硅微粉1份、莫来石20份、红柱石30份、硅藻土3份加到结合剂聚乙烯醇的水溶液3份中,聚乙烯醇的浓度为6wt.%,搅拌均匀后注入模型中成型,脱模后置于乙醇水溶液中脱水,脱水后干燥,得到坯体;
步骤4,将烘干的坯体置于高温炉中烧制,烧制条件为1450℃、保温10h,即得。
按GB/T2997-2000对制品的体积密度和显气孔率进行测试,结果分别为14.84%、2.45g/cm3;按GB/T5998-2007对制品的加热线变化率进行测试,结果为0.67%;按GB/T5072-2008对制品的常温耐压强度进行测试,结果为127.8MPa;按GB/T3002-2004对制品的高温抗折强度进行测试,1100℃保温两小时后的结果为29.8MPa。
实施例2
一种氮化硅结合碳化硅复合耐火材料的制备方法,包括以下步骤:
步骤1,以重量份计,将碳化硅14份、氮化硅13份和硅烷偶联剂4份混合,研磨,得到表面改性的碳化硅和氮化硅;
步骤2,以重量份计,将硬脂酸锌1.5份和硫酸钙晶须7份混合,混合物加至有机单体丙烯酰胺和交联剂N,N-亚甲基双丙酰胺的混合溶液24份中,丙烯酰胺和N,N-亚甲基双丙酰胺的质量比为10:1,丙烯酰胺在混合水溶液中的浓度为5wt.%,混合,加入引发剂过硫酸铵0.4份和催化剂四甲基乙二胺0.2份,搅拌混合,加热反应,所得产物经洗涤、过滤、干燥处理,转移至马弗炉中,在250℃的温度条件下热处理60min,得到改性硫酸钙晶须;
步骤3,以重量份计,将表面改性的碳化硅和氮化硅10份、改性硫酸钙晶须2份、二氧化硅微粉1份、莫来石25份、红柱石38份、硅藻土4份加到结合剂聚乙烯醇的水溶液5份中,聚乙烯醇的浓度为8wt.%,搅拌均匀后注入模型中成型,脱模后置于乙醇水溶液中脱水,脱水后干燥,得到坯体;
步骤4,将烘干的坯体置于高温炉中烧制,烧制条件为1500℃、保温5h,即得。
按GB/T2997-2000对制品的体积密度和显气孔率进行测试,结果分别为14.32%、2.47g/cm3;按GB/T5998-2007对制品的加热线变化率进行测试,结果为0.72%;按GB/T5072-2008对制品的常温耐压强度进行测试,结果为126.3MPa;按GB/T3002-2004对制品的高温抗折强度进行测试,1100℃保温两小时后的结果为28.9MPa。
实施例3
一种氮化硅结合碳化硅复合耐火材料的制备方法,包括以下步骤:
步骤1,以重量份计,将碳化硅20份、氮化硅20份和硅烷偶联剂5份混合,研磨,得到表面改性的碳化硅和氮化硅;
步骤2,以重量份计,将硬脂酸锌1份和硫酸钙晶须5份混合,混合物加至有机单体丙烯酰胺和交联剂N,N-亚甲基双丙酰胺的混合溶液30份中,丙烯酰胺和N,N-亚甲基双丙酰胺的质量比为10:1,丙烯酰胺在混合水溶液中的浓度为5wt.%,混合,加入引发剂过硫酸铵0.6份和催化剂四甲基乙二胺0.4份,搅拌混合,加热反应,所得产物经洗涤、过滤、干燥处理,转移至马弗炉中,在400℃的温度条件下热处理15min,得到改性硫酸钙晶须;
步骤3,以重量份计,将表面改性的碳化硅和氮化硅10份、改性硫酸钙晶须2份、二氧化硅微粉1份、莫来石30份、红柱石40份、硅藻土3份加到结合剂聚乙烯醇的水溶液6份中,聚乙烯醇的浓度为10wt.%,搅拌均匀后注入模型中成型,脱模后置于乙醇水溶液中脱水,脱水后干燥,得到坯体;
步骤4,将烘干的坯体置于高温炉中烧制,烧制条件为1450℃、保温10h,即得。
按GB/T2997-2000对制品的体积密度和显气孔率进行测试,结果分别为14.76%、2.45g/cm3;按GB/T5998-2007对制品的加热线变化率进行测试,结果为0.63%;按GB/T5072-2008对制品的常温耐压强度进行测试,结果为130.2MPa;按GB/T3002-2004对制品的高温抗折强度进行测试,1100℃保温两小时后的结果为28.6MPa。
实施例4
本实施例与实施例2的区别在于:硫酸钙晶须没有经过改性。
一种氮化硅结合碳化硅复合耐火材料的制备方法,包括以下步骤:
步骤1,以重量份计,将碳化硅20份、氮化硅20份和硅烷偶联剂5份混合,研磨,得到表面改性的碳化硅和氮化硅;
步骤2,以重量份计,将表面改性的碳化硅和氮化硅10份、硫酸钙晶须2份、二氧化硅微粉1份、莫来石30份、红柱石40份、硅藻土3份加到结合剂聚乙烯醇的水溶液6份中,聚乙烯醇的浓度为10wt.%,搅拌均匀后注入模型中成型,脱模后置于乙醇水溶液中脱水,脱水后干燥,得到坯体;
步骤3,将烘干的坯体置于高温炉中烧制,烧制条件为1450℃、保温10h,即得。
按GB/T2997-2000对制品的体积密度和显气孔率进行测试,结果分别为19.25%、2.45g/cm3;按GB/T5998-2007对制品的加热线变化率进行测试,结果为0.89%;按GB/T5072-2008对制品的常温耐压强度进行测试,结果为87.3MPa;按GB/T3002-2004对制品的高温抗折强度进行测试,1100℃保温两小时后的结果为24.6MPa。
将实施例1至4所得试样在1100℃条件下保温15-20min后,再置于流动水槽内水冷3min,然后空气中冷却5min,如此反复热交替40次,测定试样的显气孔率和耐压强度,结果如下:
实施例1 | 实施例2 | 实施例3 | 实施例4 | |
显气孔率 | 30.78% | 29.15% | 31.52% | 40.24% |
常温耐压强度 | 98.2MPa | 97.5MPa | 99.6MPa | 53.2 MPa |
可以看出,经过多次反复热处理后,本发明的耐火材料仍然具有较高的耐压强度,说明改性硫酸钙晶须能增强碳化硅、氮化硅与莫来石之间的联结,防止热处理中氧气进入材料内部,保护碳化硅和氮化硅不发生氧化。
Claims (6)
1.一种氮化硅结合碳化硅复合耐火材料的制备方法,其特征在于:包括以下步骤:
步骤1,以重量份计,将碳化硅10-20份、氮化硅10-20份和偶联剂2-5份混合,研磨,得到表面改性的碳化硅和氮化硅;
步骤2,以重量份计,将硬脂酸锌1-2份和硫酸钙晶须5-10份混合,混合物加至有机单体和交联剂的混合溶液20-30份中,混合,加入引发剂0.2-0.6份和催化剂0.1-0.4份,搅拌混合,加热反应,所得产物经洗涤、过滤、干燥处理,转移至马弗炉中,在250℃-400℃的温度条件下热处理15min-60min,得到改性硫酸钙晶须;
步骤3,以重量份计,将表面改性的碳化硅和氮化硅10份、改性硫酸钙晶须2份、二氧化硅微粉1-3份、莫来石20-30份、红柱石30-40份、硅藻土3-5份加到结合剂的水溶液3-6份中,搅拌均匀后注入模型中成型,脱模后置于乙醇水溶液中脱水,脱水后干燥,得到坯体;
步骤4,将烘干的坯体置于高温炉中烧制,即得。
2.根据权利要求1所述的氮化硅结合碳化硅复合耐火材料的制备方法,其特征在于:所述偶联剂为硅烷偶联剂。
3.根据权利要求1所述的氮化硅结合碳化硅复合耐火材料的制备方法,其特征在于:所述有机单体和交联剂的混合溶液是丙烯酰胺和N,N-亚甲基双丙酰胺的混合水溶液,丙烯酰胺和N,N-亚甲基双丙酰胺的质量比为10:1,丙烯酰胺在混合水溶液中的浓度为5wt.%。
4.根据权利要求1所述的氮化硅结合碳化硅复合耐火材料的制备方法,其特征在于:所述引发剂为过硫酸铵,催化剂为四甲基乙二胺。
5.根据权利要求1所述的氮化硅结合碳化硅复合耐火材料的制备方法,其特征在于:所述结合剂的水溶液是聚乙烯醇的水溶液,聚乙烯醇的浓度为6-10wt.%。
6.根据权利要求1所述的氮化硅结合碳化硅复合耐火材料的制备方法,其特征在于:烧制条件为1450-1500℃,保温5-10h。
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