CN107814562A - 一种有机硅和白云石复合改性的铝镁碳砖的生产方法 - Google Patents

一种有机硅和白云石复合改性的铝镁碳砖的生产方法 Download PDF

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CN107814562A
CN107814562A CN201710940429.2A CN201710940429A CN107814562A CN 107814562 A CN107814562 A CN 107814562A CN 201710940429 A CN201710940429 A CN 201710940429A CN 107814562 A CN107814562 A CN 107814562A
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dolomite
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晋元龙
陈德全
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Ma'an Mountain Bao Long Building Material Co Ltd
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Abstract

一种有机硅和白云石复合改性的铝镁碳砖，其特征在于，首先采用溶胶‑凝胶结合原位生成法制备有机硅改性的酚醛树脂；其次高温煅烧制备白云石粉；然后以电熔镁砂为原料，鳞片石墨为碳源和抗氧剂，有机硅改性的酚醛树脂为结合剂，进行混料；最后将混合好的物料经困料、加压成型、干燥、微波热处理，得到有机硅和白云石复合改性的铝镁碳砖。本发明的铝镁碳砖，采用有机硅和白云石复合改性，氧化钙含量高，抗热震稳定性好，抗氧性佳，抗剥落性较好；用微波加热的方法对镁碳砖进行热处理，具有均匀快速加热、烧结温度低、改善材料显微结构、无污染、节能高效等特点。

Description

一种有机硅和白云石复合改性的铝镁碳砖的生产方法
技术领域
本发明属于材料领域，具体涉及一种有机硅和白云石复合改性的铝镁碳砖的生产方法。
背景技术
镁碳砖具有优异的抗渣侵蚀性，较理想的热震稳定性、热传导性和组织致密性，是钢铁冶金工业中广泛使用的一种耐火材料，主要应用于炼钢转炉、电炉和钢包精炼炉以及钢包渣线上。目前镁碳砖的热处理主要采用燃料燃烧提供热源或电热窑炉，这种方法热处理时间长，热效率低，环境污染严重，产品质量不能得到保证。微波加热是利用材料对微波产生热效应的新型加热技术，具有均匀快速加热、烧结温度低、改善材料显微结构、无污染、节能高效等特点。
发明内容
本发明的目的在于提供一种节能高效的有机硅和白云石复合改性的铝镁碳砖的生产方法。
为了实现上述目的，本发明采用了如下技术方案：
一种有机硅和白云石复合改性的铝镁碳砖，其特征在于，首先采用溶胶-凝胶结合原位生成法制备有机硅改性的酚醛树脂；其次高温煅烧制备白云石粉；然后以电熔镁砂为原料，鳞片石墨为碳源和抗氧剂，有机硅改性的酚醛树脂为结合剂，进行混料；最后将混合好的物料经困料、加压成型、干燥、微波热处理，得到有机硅和白云石复合改性的铝镁碳砖。
所述的有机硅和白云石复合改性的铝镁碳砖，其特征在于，其由如下步骤制备而成：
（1）将苯酚和37%的甲醛溶液以1：1.1-1.2的质量比加入到反应容器中，边搅拌边加入相当于苯酚0.02-0.03倍重量份的正硅酸乙酯，搅拌均匀后，滴加相当于苯酚0.02-0.04倍重量份的氢氧化钠加去离子水配置成的10%的氢氧化钠溶液，搅拌均匀后开始加热，迅速加热至50℃，磁力搅拌50-60min，控制升温速率为0.5℃/min升温至85-95℃，继续恒温磁力搅拌2-3h，加入醋酸溶液中和至体系pH为6.5-7；然后控制温度为65-70℃，0.08-0.09MPa的真空条件下，真空脱水3-4h，得到有机硅改性酚醛树脂；
（2）将白云石破碎成60-80mm的颗粒，置于高温竖窑进行间歇式富氧化煅烧，煅烧温度为1250-1450℃，煅烧1.5-2h出一次窑，进出窑次数为3-5次，冷却至室温，粉碎研磨至粒度小于0.088mm，得到白云石粉；
（3）将骨料电熔镁砂颗粒加入到混碾机中混合3-5min，加入0.02-0.03倍重量份的白云石粉，继续混合2-3min，得到预混料；将预混料和2/3的有机硅改性酚醛树脂加入到混炼机中混炼，使得酚醛树脂将预混料完全包裹，加入电熔镁砂细粉、鳞片石墨和铝粉，继续混炼4-5min，加入剩余的有机硅改性酚醛树脂，继续混炼8-10min，出料；
（4）将混炼好的物料困料5-6h，用液压机加压成型，压力为450-500MPa，保压1min；成型后的铝镁碳砖置于干燥箱中，经200-230℃热处理20-24h，再置于600-700W的微波炉中，微波热处理20-30min，得到有机硅和白云石复合改性的铝镁碳砖。
所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（1）中醋酸溶液的浓度为0.04-0.05mol/L。
所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（3）中骨料电熔镁砂颗粒的粒度为3-1mm。
所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（3）中有机硅改性酚醛树脂加入前需进行热处理使其成为流动性好的液态。
所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（3）中电熔镁砂细粉为电熔镁砂粉碎研磨成180-200目的颗粒。
所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（3）中预混料、有机硅改性酚醛树脂、电熔镁砂细粉、鳞片石墨和铝粉的质量比为1：0.05-0.06：0.02-0.03：0.06-0.08：0.06-0.07。
采用上述的技术方案，本发明的有益效果为：
本发明采用采用溶胶-凝胶结合原位生成法制备有机硅改性的酚醛树脂，正硅酸乙酯水解产生的Si—OH，不仅与酚羟基发生酯化反应和、与酚醛树脂中的苄羟基共缩聚反应和形成了含C—O—Si键结构的三维网络外，还能相互之间发生聚合形成了Si—O—Si的聚合链，Si—O—Si的聚合链不断的伸展，链之间不断的交联，最终形成了线性交联的三维无规则的网络结构；这些无规则的网络结构与酚醛树脂基体之间相互缠绕形成互穿网络结构；本发明以有机硅改性的酚醛树脂作为结合剂制备铝镁碳砖，有机硅改性的酚醛树脂固化时，互穿网络结构在一定程度上提高结合剂与材料之间的机械互锁力，从而达到进一步提高结合强度的效果。白云石经富氧间歇式煅烧会生成氧化镁和氧化钙，氧化钙可以起到调节酚醛树脂结合剂的pH值的作用；由于氧化钙的存在，酚醛树脂结合剂偏向强碱性，可以在常温下固化，产生强度，同时，氧化钙也会和酚醛树脂中的酚羟基发生反应起到交联作用，提高酚醛树脂的抗氧化能力；另外，氧化钙添加到镁碳砖中有利于提高镁碳砖基质的钙硅比，减少高温液相，增强对低碱度钢渣的抗侵蚀性，镁碳砖中氧化钙含量提高也有利于提高抗热震性，还有利于净化钢水，提高钢材质量。本发明的铝镁碳砖，采用有机硅和白云石复合改性，氧化钙含量高，抗热震稳定性好，抗氧性佳，抗剥落性较好；用微波加热的方法对镁碳砖进行热处理，具有均匀快速加热、烧结温度低、改善材料显微结构、无污染、节能高效等特点。
具体实施方式
本实施例的有机硅和白云石复合改性的铝镁碳砖，其由如下步骤制备而成：
（1）将苯酚和37%的甲醛溶液以1：1.2的质量比加入到反应容器中，边搅拌边加入相当于苯酚0.03倍重量份的正硅酸乙酯，搅拌均匀后，滴加相当于苯酚0.04倍重量份的氢氧化钠加去离子水配置成的10%的氢氧化钠溶液，搅拌均匀后开始加热，迅速加热至50℃，磁力搅拌60min，控制升温速率为0.5℃/min升温至90℃，继续恒温磁力搅拌3h，加入醋酸溶液中和至体系pH为6.5；然后控制温度为70℃，0.08MPa的真空条件下，真空脱水4h，得到有机硅改性酚醛树脂；
（2）将白云石破碎成80mm的颗粒，置于高温竖窑进行间歇式富氧化煅烧，煅烧温度为1450℃，煅烧2h出一次窑，进出窑次数为3次，冷却至室温，粉碎研磨至粒度小于0.088mm，得到白云石粉；
（3）将骨料电熔镁砂颗粒加入到混碾机中混合5min，加入0.03倍重量份的白云石粉，继续混合3min，得到预混料；将预混料和2/3的有机硅改性酚醛树脂加入到混炼机中混炼，使得酚醛树脂将预混料完全包裹，加入电熔镁砂细粉、鳞片石墨和铝粉，继续混炼5min，加入剩余的有机硅改性酚醛树脂，继续混炼10min，出料；
（4）将混炼好的物料困料6h，用液压机加压成型，压力为500MPa，保压1min；成型后的铝镁碳砖置于干燥箱中，经230℃热处理20h，再置于700W的微波炉中，微波热处理20min，得到有机硅和白云石复合改性的铝镁碳砖。
本实施例的步骤（1）中醋酸溶液的浓度为0.05mol/L。
本实施例的步骤（3）中骨料电熔镁砂颗粒的粒度为3-1mm。
本实施例的步骤（3）中有机硅改性酚醛树脂加入前需进行热处理使其成为流动性好的液态。
本实施例的步骤（3）中电熔镁砂细粉为电熔镁砂粉碎研磨成200目的颗粒。
本实施例的步骤（3）中预混料、有机硅改性酚醛树脂、电熔镁砂细粉、鳞片石墨和铝粉的质量比为1：0.06：0.03：0.06：0.07。

Claims (7)

1.一种有机硅和白云石复合改性的铝镁碳砖，其特征在于，首先采用溶胶-凝胶结合原位生成法制备有机硅改性的酚醛树脂；其次高温煅烧制备白云石粉；然后以电熔镁砂为原料，鳞片石墨为碳源和抗氧剂，有机硅改性的酚醛树脂为结合剂，进行混料；最后将混合好的物料经困料、加压成型、干燥、微波热处理，得到有机硅和白云石复合改性的铝镁碳砖。
2.根据权利要求书1所述的有机硅和白云石复合改性的铝镁碳砖，其特征在于，其由如下步骤制备而成：
（1）将苯酚和37%的甲醛溶液以1：1.1-1.2的质量比加入到反应容器中，边搅拌边加入相当于苯酚0.02-0.03倍重量份的正硅酸乙酯，搅拌均匀后，滴加相当于苯酚0.02-0.04倍重量份的氢氧化钠加去离子水配置成的10%的氢氧化钠溶液，搅拌均匀后开始加热，迅速加热至50℃，磁力搅拌50-60min，控制升温速率为0.5℃/min升温至85-95℃，继续恒温磁力搅拌2-3h，加入醋酸溶液中和至体系pH为6.5-7；然后控制温度为65-70℃，0.08-0.09MPa的真空条件下，真空脱水3-4h，得到有机硅改性酚醛树脂；
（2）将白云石破碎成60-80mm的颗粒，置于高温竖窑进行间歇式富氧化煅烧，煅烧温度为1250-1450℃，煅烧1.5-2h出一次窑，进出窑次数为3-5次，冷却至室温，粉碎研磨至粒度小于0.088mm，得到白云石粉；
（3）将骨料电熔镁砂颗粒加入到混碾机中混合3-5min，加入0.02-0.03倍重量份的白云石粉，继续混合2-3min，得到预混料；将预混料和2/3的有机硅改性酚醛树脂加入到混炼机中混炼，使得酚醛树脂将预混料完全包裹，加入电熔镁砂细粉、鳞片石墨和铝粉，继续混炼4-5min，加入剩余的有机硅改性酚醛树脂，继续混炼8-10min，出料；
（4）将混炼好的物料困料5-6h，用液压机加压成型，压力为450-500MPa，保压1min；成型后的铝镁碳砖置于干燥箱中，经200-230℃热处理20-24h，再置于600-700W的微波炉中，微波热处理20-30min，得到有机硅和白云石复合改性的铝镁碳砖。
3.根据权利要求书2所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（1）中醋酸溶液的浓度为0.04-0.05mol/L。
4.根据权利要求书2所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（3）中骨料电熔镁砂颗粒的粒度为3-1mm。
5.根据权利要求书2所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（3）中有机硅改性酚醛树脂加入前需进行热处理使其成为流动性好的液态。
6.根据权利要求书2所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（3）中电熔镁砂细粉为电熔镁砂粉碎研磨成180-200目的颗粒。
7.根据权利要求书2所述的有机硅和白云石复合改性的铝镁碳砖的制备方法，其特征在于，步骤（3）中预混料、有机硅改性酚醛树脂、电熔镁砂细粉、鳞片石墨和铝粉的质量比为1：0.05-0.06：0.02-0.03：0.06-0.08：0.06-0.07。
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