CN106256802A - 一种有机硅/酚醛树脂结合剂及其制备耐火材料的应用 - Google Patents

一种有机硅/酚醛树脂结合剂及其制备耐火材料的应用 Download PDF

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CN106256802A
CN106256802A CN201610648721.2A CN201610648721A CN106256802A CN 106256802 A CN106256802 A CN 106256802A CN 201610648721 A CN201610648721 A CN 201610648721A CN 106256802 A CN106256802 A CN 106256802A
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organosilicon
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丁冬海
肖国庆
杨少雨
李延军
任耘
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Xian University of Architecture and Technology
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Abstract

本发明属于耐火材料领域，主要涉及一种有机硅/酚醛树脂结合剂及其制备耐火材料的应用，所述复合耐火材料原料包括不同粒径的SiC骨料、鳞片石墨、有机硅树脂、酚醛树脂，可以应用于砌筑冶金炉内衬的定型砖或者导流管、控流器等耐火功能器件。本发明在酚醛树脂中引入含有Si‑O‑Si主链的有机硅树脂，在烧成或者高温服役过程中，通过高温裂解、碳热还原在酚醛树脂热解碳骨架中原位生成SiC，SiC氧化后生成高粘度的氧化硅玻璃薄膜，对氧气的渗透有阻碍作用，有利于改善耐火材料的抗氧化性能。有机硅/酚醛树脂结合剂比目前使用的商用酚醛树脂或沥青结合剂具有更高的残碳率，所制备的SiC复相耐火材料具有更高的力学强度与抗氧化性能。

Description

一种有机硅/酚醛树脂结合剂及其制备耐火材料的应用
技术领域
本发明属耐火材料领域，特别涉及一种有机硅/酚醛树脂结合剂及其制备耐火材料的应用。
技术背景
含碳耐火材料在20世纪70年代开始商业化生产，现在已经成为应用于BOF炉、钢包、电弧炉、滑板、连铸设备等钢铁熔炼容器或技术最重要的一类耐火材料。由于类似石墨结构碳素组元的存在，它们表现出较好的抗冲击性能与抗侵蚀性能。含碳耐火材料的性能由碳源、结合剂、抗氧化剂及氧化物骨料决定。与烧结耐火材料相比，结合剂对含碳耐火材料起着更为重要的作用。结合剂不仅可以赋予坯体强度，使其能够装卸、砌体堆垛，而且烧结后以碳骨架的形式存在。含碳耐火材料常用的有机结合剂不影响其耐火度，而且可以提供碳源。酚醛树脂作为结合剂，是世界上最早实现工业化生产的，能够满足耐火材料生产与应用环境所提出的环境安全、高残碳率、热解生成三维结构的碳骨架、储存稳定、好的流动性与骨料结合好、价格合理等要求。但是，酚醛树脂碳化属于典型的固相碳化，生成的碳是无定形玻璃碳，抗氧化性能较差，一定程度上限制了含碳耐火材料的服役时间。耐火材料用酚醛树脂结合剂的改性主要集中于催化热解与无机纳米粒子改性两个方面。催化热解主要通过在酚醛树脂中混入过渡金属，提高热解碳的石墨化程度或者原位生成碳纳米管；无机纳米粒子改性主要是在酚醛树脂中掺入纳米黏土、石墨烯、碳化硼来提高酚醛树脂热解碳的抗氧化性能。前一种方法对酚醛树脂热解碳抗氧化性能提高的程度有限，后一种方法存在纳米粒子容易团聚、不易分散的问题。
发明内容
针对现有技术的缺陷和不足，本发明提出一种有机硅/酚醛树脂结合剂及其制备耐火材料的应用，结合剂比商用酚醛树脂结合剂相比，残炭率可提高约20％，本方法可以在酚醛树脂热解碳中原位生成SiC，改善其结合含碳耐火材料的抗氧化性能；本发明采用的方法工艺简单、原料价格低廉、容易控制。
本发明提出如下技术解决方案：
一种有机硅/酚醛树脂结合剂，该结合剂包括有机硅树脂和酚醛树脂。
具体的，有机硅树脂占结合剂质量分数的5％～15％，余下为酚醛树脂，两者百分比总和为100％。
更具体的，所述的酚醛树脂为热固性甲阶酚醛树脂，热固性甲阶酚醛树脂的水分含量≤4％，热固性甲阶酚醛树脂的残碳量≥42％；所述的有机硅树脂为聚甲基有机硅树脂。
所述的有机硅/酚醛树脂结合剂用于制备耐火材料的应用。
具体的，以SiC作为骨料和细粉，石墨为碳源，结合剂为所述的有机硅酚醛树脂结合剂，上述原料经压坯烧制后得到耐火材料。
更具体的，所述的SiC的粒径范围包括：0～0.068mm，0.1～0.5mm和0.5～1mm三种，其纯度为SiC含量大于90％，0.1～0.5mm和0.5～1mm粒径的SiC为骨料，0～0.068mm粒径的SiC为细粉；石墨为高纯鳞片石墨，粒径为300μm，固定碳含量为99.9％。
还有，按质量百分比计，骨料为60％，细粉为25％，碳源为8％，结合剂为7％。
另外，烧制的具体过程为：将压制好的坯体放入气氛烧结炉中，真空度为5KPa以下，通入惰性保护气体，以5℃/min升温速度升温至1400℃，保温2小时，降温后取出制品即得耐火材料。
本发明的优点包括：
(1)本发明的结合剂比商用酚醛树脂结合剂相比，残炭率可提高约20％；
(2)本方法可以在酚醛树脂热解碳中原位生成SiC，改善其结合含碳耐火材料的抗氧化性能；
(3)本发明采用的方法工艺简单、原料价格低廉、容易控制。
具体实施方式
本发明的有机硅/酚醛树脂结合剂包括有机硅树脂和酚醛树脂。具体的，有机硅树脂占结合剂质量分数的5％～15％，余下为酚醛树脂，两者百分比总和为100％。更具体的，酚醛树脂为热固性甲阶酚醛树脂，热固性甲阶酚醛树脂的水分含量≤4％，热固性甲阶酚醛树脂的残碳量≥42％，平均分子量为400；所述的有机硅树脂为聚甲基有机硅树脂，最好为，聚甲基苯基有机硅树脂，聚甲基苯基有机硅树脂的平均分子量为1200。
优选的，按质量百分比计，有机硅树脂在树脂结合剂中占5％。
优选的，按质量百分比计，有机硅树脂在树脂结合剂中占10％。
优选的，按质量百分比计，有机硅树脂在树脂结合剂中占15％。
有机硅/酚醛树脂结合剂用于制备耐火材料的应用，具体过程为：选取不同粒径的SiC作为骨料、细粉及鳞片石墨作为碳源；将颗粒状有机硅树脂与酚醛树脂按一定质量分数混合研磨后溶于无水乙醇中；水泥搅拌机混料，将两种树脂溶液混合、搅拌均匀；经干燥、压坯成型、固化后在1400℃温度下烧成。
采用的SiC粒径范围包括：0～0.068mm，0.1～0.5mm，0.5～1mm三种，SiC含量大于90％，0.1～0.5mm和0.5～1mm粒径的SiC为骨料，0～0.068mm粒径的SiC为细粉；鳞片石墨粒径300μm，按质量分数7％外加，固化后在惰性气氛炉中烧成，烧成温度为1400℃。
具体的，所述的球磨工艺参数为：树脂结合剂与介质球的质量比为2：1，酚醛树脂与无水乙醇的质量比为1：4，球磨时间为1小时，球磨机转速为400r/min；烧成工艺参数：保护气体为氮气或氩气，流量500ml/min，以5℃/min升温速度升温至1400℃，保温2小时。
以下是发明人给出的实施例，本发明不限于以下的实施例，在本发明给出的范围内，均能制备出符合要求的SiC-C复合耐火材料。
实施例1：
结合剂为纯商用热固性甲阶酚醛树脂，研磨后溶于无水乙醇中得树脂结合剂溶液。
树脂结合剂与介质球的质量比为2：1，球磨时间为1小时，球磨机转速为400r/min；将粗颗粒和中颗粒的SiC(0.5～1mm：45wt％，0.1～0.5mm：25wt％)倒入水泥搅拌池内搅拌混合均匀，将配制好的树脂结合剂溶液按照外加树脂结合剂7wt％倒入混合均匀的颗粒料内，继续混合至结合剂完全包裹，再倒入SiC细粉(0～0.044mm:30wt％)，再搅拌0.5小时至细粉、颗粒、结合剂混合均匀。成型后120℃固化。烧成具体工艺参数：保护气体为氮气，以5℃/min的速度升到1400℃后保温2小时。取出，测试制品的抗折强度、抗压强度、体积密度，分别为：11.37MPa、49.43MPa、3.27g/cm3。根据烧成前后制品重量差计算得到结合剂残碳率为46％，用差示扫描量热曲线中氧化放热峰值对应的温度表征试样的抗氧化性能，氧化峰值温度为546℃。
实施例2：
聚甲基苯基有机硅树脂在结合剂中含量为5wt％，热固性甲阶酚醛树脂为95wt％，混合研磨后溶于无水乙醇中即得树脂结合剂溶液。
树脂结合剂与介质球的质量比为2：1，球磨时间为1小时，球磨机转速为400r/min；将粗颗粒和中颗粒的SiC(0.5～1mm：45wt％，0.1～0.5mm:25wt％)导入水泥搅拌池内搅拌混合均匀，将配制好的树脂结合剂溶液按照外加树脂结合剂7wt％倒入混合均匀的颗粒料内，继续混合至结合剂完全包裹，再倒入SiC细粉(0～0.044mm:30wt％)，再搅拌0.5小时至细粉、颗粒、结合剂混合均匀。成型后120℃固化。烧成具体工艺参数：保护气体为氮气，以5℃/min的速度升到1400℃保温2小时。取出，测试制品的抗折强度、抗压强度、体积密度，分别为：13.41MPa、54.64MPa、3.25g/cm3。根据烧成前后制品重量差计算得到结合剂残碳率为53％，比实施例1提高7％。用差示扫描量热曲线中氧化放热峰值对应的温度表征试样的抗氧化性能，氧化峰值温度为618℃，比实施例1提高了约72℃。
实施例3：
聚甲基苯基有机硅树脂在结合剂中含量为10wt％，热固性甲阶酚醛树脂为90wt％，混合研磨后溶于无水乙醇中得到树脂结合剂。
树脂结合剂与介质球的质量比为2：1，球磨时间为1小时，球磨机转速为400r/min；将粗颗粒和中颗粒的SiC(0.5～1mm：45wt％，0.1～0.5mm:25wt％)导入水泥搅拌池内搅拌混合均匀，将配制好的树脂结合剂溶液按照外加树脂结合剂7wt％倒入混合均匀的颗粒料内，继续混合至结合剂完全包裹，再倒入SiC细粉(0～0.044mm:30wt％)，再搅拌0.5小时至细粉、颗粒、结合剂混合均匀。成型后在120℃温度下固化。烧成具体工艺参数：保护气体为氮气，以5℃/min的速度升到1400℃保温2小时。取出，测试制品的抗折强度、抗压强度、体积密度，分别为：15.36MPa、52.28MPa、3.24g/cm3。根据烧成前后制品重量差计算得到结合剂残碳率为59％，比实施例2提高6％。用差示扫描量热曲线中氧化放热峰值对应的温度表征试样的抗氧化性能，氧化峰值温度为673℃，比实施例2提高了约55℃。
实施例4：
聚甲基苯基有机硅树脂在结合剂中含量为15wt％，热固性甲阶酚醛树脂85wt％，混合研磨后溶于无水乙醇中即得树脂结合剂溶液。
树脂结合剂与介质球的质量比为2：1，球磨时间为1小时，球磨机转速为400r/min；将粗颗粒和中颗粒的SiC(0.5～1mm：45wt％，0.1～0.5mm:25wt％)导入水泥搅拌池内搅拌混合均匀，将配制好的树脂结合剂溶液按照外加树脂结合剂7wt％倒入混合均匀的颗粒料内，继续混合至结合剂完全包裹，再倒入SiC细粉(0～0.044mm:30wt％)，再搅拌0.5小时至细粉、颗粒、结合剂混合均匀。成型后120℃固化。烧成具体工艺参数：保护气体为氮气，以5℃/min的速度升到1400℃保温2小时。取出，测试制品的抗折强度、抗压强度、体积密度，分别为：16.29MPa、56.73MPa、3.22g/cm3。根据烧成前后制品重量差计算得到结合剂残碳率为61％，比实施例3提高2％。用差示扫描量热曲线中氧化放热峰值对应的温度表征试样的抗氧化性能，氧化峰值温度为709℃，比实施例3提高了约36℃。

Claims (8)

1.一种有机硅/酚醛树脂结合剂，其特征在于，该结合剂包括有机硅树脂和酚醛树脂。
2.如权利要求1所述的有机硅/酚醛树脂结合剂，其特征在于，有机硅树脂占结合剂质量分数的5％～15％，余下为酚醛树脂，两者百分比总和为100％。
3.如权利要求1或2所述的有机硅/酚醛树脂结合剂，其特征在于，所述的酚醛树脂为热固性甲阶酚醛树脂，热固性甲阶酚醛树脂的水分含量≤4％，热固性甲阶酚醛树脂的残碳量≥42％；所述的有机硅树脂为聚甲基有机硅树脂。
4.权利要求1、2或3所述的有机硅/酚醛树脂结合剂用于制备耐火材料的应用。
5.如权利要求4所述的应用，其特征在于，以SiC作为骨料和细粉，石墨为碳源，结合剂为权利要求1、2或3所述的有机硅酚醛树脂结合剂，上述原料经压坯烧制后得到耐火材料。
6.如权利要求5所述的应用，其特征在于，所述的SiC的粒径范围包括：0～0.068mm，0.1～0.5mm和0.5～1mm三种，其纯度为SiC含量大于90％，0.1～0.5mm和0.5～1mm粒径的SiC为骨料，0～0.068mm粒径的SiC为细粉；石墨为高纯鳞片石墨，粒径为300μm，固定碳含量为99.9％。
7.如权利要求5或6所述的应用，其特征在于，按质量百分比计，骨料为60％，细粉为25％，碳源为8％，结合剂为7％。
8.如权利要求5或6所述的应用，其特征在于，烧制的具体过程为：将压制好的坯体放入气氛烧结炉中，真空度为5KPa以下，通入惰性保护气体，以5℃/min升温速度升温至1400℃，保温2小时，降温后取出制品即得耐火材料。
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Application publication date: 20161228