CN112028613A - 一种应用添加催化剂酚醛树脂的镁碳砖 - Google Patents

一种应用添加催化剂酚醛树脂的镁碳砖 Download PDF

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CN112028613A
CN112028613A CN202010911517.1A CN202010911517A CN112028613A CN 112028613 A CN112028613 A CN 112028613A CN 202010911517 A CN202010911517 A CN 202010911517A CN 112028613 A CN112028613 A CN 112028613A
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曹丽云
龚育才
彭仁
俞晓东
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Abstract

本发明公开了一种应用添加催化剂酚醛树脂的镁碳砖,涉及镁碳砖技术领域,配料含有A组分、B组分和C组分,所述A组分、B组分和C组分之间的含量比为3:1:1,所述A组分由电熔镁砂、鳞片状石墨和结合剂组成,其中,电熔镁砂、鳞片状石墨和结合剂之间的含量比为3:1:4,所述B组分由陶瓷和四氧化三铁粉末组成,按含量比计,陶瓷:四氧化三铁粉末=3:1,所述C组分体系由玻璃纤维和催化剂组成,按含量比计,玻璃纤维:催化剂=2:1。该应用添加催化剂酚醛树脂的镁碳砖中,铁催化酚醛树脂的使用促进了镁碳砖的结构性重排,并导致了纳米管和更多的陶瓷晶须形成,改善了镁碳砖在高温下的性能,显著提高了镁碳砖的抗氧化性和机械强度。

Description

一种应用添加催化剂酚醛树脂的镁碳砖
技术领域
本发明涉及镁碳砖技术领域,具体为一种应用添加催化剂酚醛树脂的镁碳砖。
背景技术
镁碳砖是以高熔点碱性氧化物氧化镁(熔点2800℃)和难以被炉渣侵润的高熔点碳素材料作为原料,添加各种非氧化物添加剂,用炭质结合剂结合而成的不烧碳复合耐火材料。镁碳砖主要用于转炉、交流电弧炉、直流电弧炉的内衬,钢包的渣线等部位。
镁碳砖具有良好的耐高温性能,抗渣能力强,抗热震性好,高温蠕变低,近年来,低碳镁碳砖的开发成为研究的热点。
然而当碳含量降低时,镁碳砖的抗热震性、柔韧性以及承受苛刻热机械应力时的断裂韧性均会下降,现代为了解决这些问题,尝试采用纳米碳源如碳纳米管、石墨烯或氧化石墨纳米薄膜、纳米炭黑等,通过纳米结构基质来改善含碳耐火材料的性能,虽然应用纳米碳有效改善了镁碳砖的物理和热机械性能,但是纳米碳成本高且不易分散均匀。
发明内容
针对现有技术的不足,本发明提供了一种应用添加催化剂酚醛树脂的镁碳砖,解决了上述背景技术中提出的问题。
为实现以上目的,本发明通过以下技术方案予以实现:一种应用添加催化剂酚醛树脂的镁碳砖,其配料含有A组分、B组分和C组分,所述A组分、B组分和C组分之间的含量比为3:1:1,所述A组分由电熔镁砂、鳞片状石墨和结合剂组成,其中,电熔镁砂、鳞片状石墨和结合剂之间的含量比为3:1:4,所述B组分由陶瓷和四氧化三铁粉末组成,按含量比计,陶瓷:四氧化三铁粉末=3:1,所述C组分体系由玻璃纤维和催化剂组成,按含量比计,玻璃纤维:催化剂=2:1。
可选的,所述A组分中,结合剂为沥青变性酚醛树脂。
可选的,所述沥青变性酚醛树脂的原料为乳化沥青和酚醛树脂,其中乳化沥青和酚醛树脂的用量比例为2:1,沥青变性酚醛树脂的制备方法为:在乳化沥青中加入酚醛树脂,融合均匀。
可选的,所述B组分中,陶瓷选用碳化硅陶瓷。
可选的,所述陶瓷的处理过程为:将碳化硅陶瓷粉碎后研磨,得到碳化硅陶瓷粉末,碳化硅陶瓷粉末过100目筛,加入粘合剂,搅拌均匀,常温下静置保存。
可选的,所述粘合剂为环氧树脂、醋酸乙烯树脂、氯化橡胶中的任意一种。
可选的,所述催化剂为铁催化剂,所述铁催化剂的制备过程如下:
①取3份硝酸铁[Fe3(NO3)3.9H2O],加入到乙醇溶剂中,在25℃下搅拌1h,得到均匀溶液;
②取6份热固性酚醛树脂(固定碳含量为65%),将所得溶液缓慢加入酚醛树脂中并继续搅拌1h。
可选的,该应用添加催化剂酚醛树脂的镁碳砖的制备包括下述工艺步骤:
①以金属铝粉为抗氧化剂,将电熔镁砂和鳞片状石墨分别加入到结合剂沥青变性酚醛树脂中,搅拌1h得混合体A;
②将四氧化三铁粉末均匀加入到加入有粘合剂的陶瓷粉末中,搅拌混合得混合体B;
③将混合体A和混合体B进行混合,搅拌1h后加入玻璃纤维,继续搅拌1h;
④加入催化剂,混合30min后,置于可控温度的环境下困料12h;
⑤装入模具,在150MPa下加压成型,并在200℃下固化24h;
⑥装入氧化铝匣钵中埋焦炭与鳞片石墨的混合粉,置于电炉中以3℃/min的升温速率加热到800-1400℃,并保温3h。
本发明提供了一种应用添加催化剂酚醛树脂的镁碳砖,具备以下有益效果:该应用添加催化剂酚醛树脂的镁碳砖中,铁催化酚醛树脂的使用促进了镁碳砖的结构性重排,并导致了纳米管和更多的陶瓷晶须形成,改善了镁碳砖在高温下的性能,通过在含碳耐火材料基质中原位生成纳米碳和新的陶瓷结合相可以增强基质结合,有效改善镁碳砖的性能,而新生成的陶瓷相可以显著改善镁碳砖的抗氧化性和机械强度,降低了镁碳砖的气孔率,提高镁碳砖的致密度和抗侵蚀性,达到了添加纳米碳的相同效果,且较纳米碳更好。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。
实施例1
一种应用添加催化剂酚醛树脂的镁碳砖,其配料含有A组分、B组分和C组分,所述A组分、B组分和C组分之间的含量比为3:1:1,所述A组分由电熔镁砂、鳞片状石墨和结合剂组成,其中,电熔镁砂、鳞片状石墨和结合剂之间的含量比为3:1:4,所述B组分由陶瓷和四氧化三铁粉末组成,按含量比计,陶瓷:四氧化三铁粉末=3:1,所述C组分体系由玻璃纤维和催化剂组成,按含量比计,玻璃纤维:催化剂=2:1;
A组分中,结合剂为沥青变性酚醛树脂,沥青变性酚醛树脂的原料为乳化沥青和酚醛树脂,其中乳化沥青和酚醛树脂的用量比例为2:1,沥青变性酚醛树脂的制备方法为:在乳化沥青中加入酚醛树脂,融合均匀;
进一步地,沥青变性酚醛树脂软化点大于95度,游离酚小于1.5%,冷抗折强度大于6MPa,流动性好,固含量高,挥发酚含量低,其作为镁碳砖结合剂使用时,能改善耐火材料的高温性能,从而有效提高了镁碳砖的产品质量;
B组分中,陶瓷选用碳化硅陶瓷,
进一步地,碳化硅陶瓷具有高强度、高硬度及耐高温性能,在1200℃~1400℃使用仍能保持高的抗弯强度,同时还具有良好的导热性、抗氧化性、导电性和高的冲击韧度,在镁碳砖中添加碳化硅陶瓷,保证了镁碳砖的产品品质,填补了低碳镁碳砖强度、韧性不足的缺陷;
陶瓷的处理过程为:将碳化硅陶瓷粉碎后研磨,得到碳化硅陶瓷粉末,碳化硅陶瓷粉末过100目筛,加入粘合剂,搅拌均匀,常温下静置保存,其中,粘合剂为环氧树脂、醋酸乙烯树脂、氯化橡胶中的任意一种;
进一步地,加入粘合剂使得碳化硅陶瓷粉末具有强粘性,能够更好地融入镁碳砖原料中;
催化剂为铁催化剂,所述铁催化剂的制备过程为:①取3份硝酸铁[Fe3(NO3)3.9H2O],加入到乙醇溶剂中,在25℃下搅拌1h,得到均匀溶液;②取6份热固性酚醛树脂(固定碳含量为65%),将所得溶液缓慢加入酚醛树脂中并继续搅拌1h;
由于铁催化剂在氧化物-C材料基质中的催化效应,促进了源于酚醛树脂的玻璃碳和添加的金属抗氧化剂原位形成的晶体碳结构和一些陶瓷相晶须的生成,故添加铁催化剂的酚醛树脂可以提高氧化物-C质耐火材料的强度和柔韧性。
实施例2
一种应用添加催化剂酚醛树脂的镁碳砖的制备包括下述工艺步骤:
①以金属铝粉为抗氧化剂,将电熔镁砂和鳞片状石墨分别加入到结合剂沥青变性酚醛树脂中,搅拌1h得混合体A;
②将四氧化三铁粉末均匀加入到加入有粘合剂的陶瓷粉末中,搅拌混合得混合体B;
③将混合体A和混合体B进行混合,搅拌1h后加入玻璃纤维,继续搅拌1h;
④加入催化剂,混合30min后,置于可控温度的环境下困料12h;
⑤装入模具,在150MPa下加压成型,并在200℃下固化24h;
⑥装入氧化铝匣钵中埋焦炭与鳞片石墨的混合粉,置于电炉中以3℃/min的升温速率加热到800-1400℃,并保温3h。
综上,该应用添加催化剂酚醛树脂的镁碳砖中,铁催化酚醛树脂的加入导致了镁碳砖中石墨化碳的形成,与镁碳砖中常用的常规酚醛树脂相比,这种石墨结构更稳定,且随着铁催化剂在酚醛树脂中比例的增加,石墨化碳的数量也随之增加,铁催化酚醛树脂的使用促进了镁碳砖的结构性重排,并导致了纳米管和更多的陶瓷晶须形成,改善了镁碳砖在高温下的性能,通过在含碳耐火材料基质中原位生成纳米碳和新的陶瓷结合相可以增强基质结合,有效改善镁碳砖的性能,而新生成的陶瓷相可以显著改善镁碳砖的抗氧化性和机械强度,降低了镁碳砖的气孔率,提高镁碳砖的致密度和抗侵蚀性,达到了添加纳米碳的相同效果,且较纳米碳更好。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。

Claims (8)

1.一种应用添加催化剂酚醛树脂的镁碳砖,其特征在于:应用添加催化剂酚醛树脂的镁碳砖镁碳砖配料含有A组分、B组分和C组分,所述A组分、B组分和C组分之间的含量比为3:1:1,所述A组分由电熔镁砂、鳞片状石墨和结合剂组成,其中,电熔镁砂、鳞片状石墨和结合剂之间的含量比为3:1:4,所述B组分由陶瓷和四氧化三铁粉末组成,按含量比计,陶瓷:四氧化三铁粉末=3:1,所述C组分体系由玻璃纤维和催化剂组成,按含量比计,玻璃纤维:催化剂=2:1。
2.根据权利要求1所述的一种应用添加催化剂酚醛树脂的镁碳砖,其特征在于:所述A组分中,结合剂为沥青变性酚醛树脂。
3.根据权利要求2所述的一种应用添加催化剂酚醛树脂的镁碳砖,其特征在于:所述沥青变性酚醛树脂的原料为乳化沥青和酚醛树脂,其中乳化沥青和酚醛树脂的用量比例为2:1,沥青变性酚醛树脂的制备方法为:在乳化沥青中加入酚醛树脂,融合均匀。
4.根据权利要求1所述的一种应用添加催化剂酚醛树脂的镁碳砖,其特征在于:所述B组分中,陶瓷选用碳化硅陶瓷。
5.根据权利要求4所述的一种应用添加催化剂酚醛树脂的镁碳砖,其特征在于:所述陶瓷的处理过程为:将碳化硅陶瓷粉碎后研磨,得到碳化硅陶瓷粉末,碳化硅陶瓷粉末过100目筛,加入粘合剂,搅拌均匀,常温下静置保存。
6.根据权利要求5所述的一种应用添加催化剂酚醛树脂的镁碳砖,其特征在于:所述粘合剂为环氧树脂、醋酸乙烯树脂、氯化橡胶中的任意一种。
7.根据权利要求1所述的一种应用添加催化剂酚醛树脂的镁碳砖,其特征在于:所述催化剂为铁催化剂,所述铁催化剂的制备过程如下:
①取3份硝酸铁[Fe3(NO3)3.9H2O],加入到乙醇溶剂中,在25℃下搅拌1h,得到均匀溶液;
②取6份热固性酚醛树脂(固定碳含量为65%),将所得溶液缓慢加入酚醛树脂中并继续搅拌1h。
8.根据权利要求1所述的一种应用添加催化剂酚醛树脂的镁碳砖,其特征在于:该应用添加催化剂酚醛树脂的镁碳砖的制备包括下述工艺步骤:
①以金属铝粉为抗氧化剂,将电熔镁砂和鳞片状石墨分别加入到结合剂沥青变性酚醛树脂中,搅拌1h得混合体A;
②将四氧化三铁粉末均匀加入到加入有粘合剂的陶瓷粉末中,搅拌混合得混合体B;
③将混合体A和混合体B进行混合,搅拌1h后加入玻璃纤维,继续搅拌1h;
④加入催化剂,混合30min后,置于可控温度的环境下困料12h;
⑤装入模具,在150MPa下加压成型,并在200℃下固化24h;
⑥装入氧化铝匣钵中埋焦炭与鳞片石墨的混合粉,置于电炉中以3℃/min的升温速率加热到800-1400℃,并保温3h。
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