CN107324796A - 一种碳/镁铝尖晶石复合粉 - Google Patents
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Abstract
本发明公开了一种碳/镁铝尖晶石复合粉,所述复合粉按质量百分比计,包括以下原料:28.6%~40.8%草酸镁,20.6%~28.6%过氧化镁,19.0%~22.2%氧化铝,19.8%~23.8%铝粉,各原料的质量百分比之和为100%。优选的,所述复合粉按质量百分比计,包括以下原料:33.4%草酸镁,22.2%过氧化镁,22.2%氧化铝,22.2%铝粉。本发明的复合粉,突破性的解决了含碳耐火材料中碳难分散均匀、易团聚的题,制备的复合粉晶粒细,能够在耐火材料领域得到更好的应用。
Description
技术领域
本发明属于无机复合材料技术领域,具体涉及一种新型碳/镁铝尖晶石复合粉。
背景技术
耐火材料是指耐火度不低于1500℃的一类无机非金属材料。耐火材料包括天然矿石以及按照一定的工业要求制造,具有一定的高温力学性能、良好的体积稳定性,并且是各种耐高温设备必需的材料。耐火材料广泛应用于化工、石油、冶金、机械制造、动力等工业领域,尤其在冶金工业中用量最大,在高温工业生产发展中起着不可替代的重要作用。
含碳耐火材料属于耐火材料的一种,含碳耐火材料中的碳与熔渣不润湿,能够提高耐火材料的抗渣侵蚀及热震稳定性能。但是,微米级碳制备工艺复杂、成本较高,且与氧化物混合过程中容易团聚,在耐火材料中分散困难。碳难分散的难题,限制了其优势的发挥。
发明内容
针对现有技术中存在的不足,本发明提出一种碳/镁铝尖晶石复合粉,复合粉中的碳有序度极高,将其添加到含碳耐火材料中,可显著改善含碳耐火材料的碳分散问题。
为实现上述目标,本发明采用如下技术方案:
一种碳/镁铝尖晶石复合粉,包括以下原料:草酸镁、过氧化镁、氧化铝和铝粉。
所述复合粉按质量百分比计,包括以下原料:28.6%~40.8%草酸镁,20.6%~28.6%过氧化镁,19.0%~22.2%氧化铝,19.8%~23.8%铝粉,各原料的质量百分比之和为100%。
优选的,所述复合粉按质量百分比计,包括以下原料:33.4%草酸镁,22.2%过氧化镁,22.2%氧化铝,22.2%铝粉。
所述草酸镁的纯度≥99.0%,所述氧化铝的纯度≥99.0%,所述铝粉的纯度≥99.0%,所述过氧化镁中氧化镁占比不超过70%。
上述复合粉的制备方法,包括以下步骤:将草酸镁、过氧化镁、氧化铝与铝粉按配方量混合后干压成型,通过自蔓延高温合成反应得到试样,将试样进行粉碎研磨即得碳/镁铝尖晶石复合粉。
将草酸镁、过氧化镁、氧化铝与铝粉按配比混合后干压成直径为20mm、高为30mm的圆柱形试样进行自蔓延高温合成反应。
上述复合粉添加到含碳耐火材料中的应用。
相较于现有技术,本发明的技术效果如下:
(1)本发明的复合粉,含有极高有序度的自由碳,将其添加到含碳耐火材料中,减少耐火材料碳的加入,可显著改善含碳耐火材料的碳分散问题,或者将其添加到普通耐火材料中,可制备出碳分散均匀的含碳耐火材料,本发明突破性的解决了含碳耐火材料中碳难分散均匀、易团聚的题。
(2)本发明的复合粉的制备方法,根据原位合成理论,只需一步即可完成,采用自蔓延高温合成,制备过程简单。
(3)本发明的复合粉的制备方法,其设备简单,生产成本大大降低,能耗低,更加节能环保。
附图说明
图1是本发明实施例1制备的碳/镁铝尖晶石复合粉的XRD图谱;
图2是本发明实施例1制备的碳/镁铝尖晶石复合粉的Raman图谱;
图3是本发明实施例1制备的碳/镁铝尖晶石复合粉的SEM图(图3a)及A、B、C三点的能谱图(分别为3b、3c、3d图);
图4是本发明实施例2制备的碳/镁铝尖晶石复合粉的XRD图谱;
图5是本发明实施例2制备的碳/镁铝尖晶石复合粉的Raman图谱;
图6是本发明实施例3制备的碳/镁铝尖晶石复合粉的XRD图谱;
图7是本发明实施例3制备的碳/镁铝尖晶石复合粉的Raman图谱。
以下结合附图对本发明作进一步的说明。
具体实施方式
下面结合附图和具体实施方式对本发明进行详细说明,不能认定本发明的具体实施只局限于这些说明。对于本发明所属技术领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干简单推演或替换,都应当视为属于本发明的保护范围。
本发明的制备碳/镁铝尖晶石复合粉不仅具备碳和镁铝尖晶石抗熔渣侵蚀的优势,更重要的是解决了碳的分散性问题,可以赋予耐火材料更优越的抗侵蚀性能。
本发明制备碳/镁铝尖晶石复合粉中,碳的粒径减小,比表面积增大,使得复合粉的应用在降低碳含量的同时,改善含碳耐火材料的抗侵蚀性能、抗热震性能;含镁铝尖晶石的耐火材料具有良好的抗侵蚀性,归因于镁铝尖晶石可以吸收钢渣低熔点氧化物形成固溶体而不生成低熔点氧化物,同时可以改变熔渣化学组成并提高熔渣的粘度,从而减缓熔渣的侵蚀。复合粉中尖晶石的颗粒、晶粒较小,使得尖晶石表面积、晶界含量提高,更有利于固溶钢渣中的低熔点氧化物,从而改善耐火材料抗熔渣渗透性能,而熔渣渗透是熔渣导致耐火材料熔损与剥落的先决条件,因此提高耐火材料的抗溶渣渗透性能对延长耐火材料服役寿命非常重要。本发明的复合粉,其活性高、晶粒细,且性能优异,使用温度有明显的提高,能够在耐火材料领域得到更好的应用。
实施例1
本实施例提供一种碳/镁铝尖晶石复合粉的制备方法,原料包括:草酸镁(纯度≥99.0%)、过氧化镁复合粉(含量≥30.0%,其余为氧化镁)、铝粉(纯度≥99.0%)和氧化铝(纯度≥99.0%)为原料,按质量百分比计,草酸镁为33.4%,过氧化镁为22.2%,氧化铝为22.2%,铝粉为22.2%;
包括以下步骤:将上述各混合均匀的原料装入模具中,再对其干压成型,压制成直径为20mm、高度为30mm的圆柱形试样;结束成型后,将试样进行脱模,然后放入自蔓延高温反应炉中,在试样上放置C-Ti引燃剂,自蔓延高温合成反应由置于试样上端的C-Ti反应产生的热量引发,而C和Ti反应则通过一根钨丝引发;在反应室内充满氩气,压力为1MPa,点火引燃试样发生自蔓延高温合成反应,而后待炉温降至室温后,关闭电源,卸压,开启炉门,将物料取出。对烧成的物料进行粉碎、研磨,即得碳/镁铝尖晶石复合粉。
对制备的碳/镁铝尖晶石复合粉进行X射线衍射分析,得到XRD图谱参见图1,由图1可知,该复合粉主要成分包括碳、镁铝尖晶石及氧化镁。对实施例制备的碳/镁铝尖晶石复合粉进行了拉曼光谱分析,得到的拉曼光谱图参见图2,由图2可知,制备的碳/镁铝尖晶石复合粉中含有碳,且在1350cm-1、1580cm-1及2700cm-1附近有很强的峰值,拉曼光谱图在1350cm-1与1580cm-1附近的两个峰是自由碳的D峰和G峰,G峰非常强并且尖锐,表明产物中存在有序度较高的自由碳。对实施例1制备的碳/镁铝尖晶石复合粉进行氧化称重法测定碳含量,测得碳/镁铝尖晶石复合粉中碳含量为1.77%。对实施例制备的碳/镁铝尖晶石复合粉进行了扫描电镜观察,如图3所示,结合A、B、C三点的能谱分析可以得出碳附着于镁铝尖晶石晶粒上,使其分散性得到改善。
实施例2:
本实施例提供一种碳/镁铝尖晶石复合粉的制备方法,与实施例1不同的是:按质量百分比计,草酸镁为28.6%,过氧化镁为28.6%,氧化铝为19.0%,铝粉为23.8%;
对制备的碳/镁铝尖晶石复合粉进行X射线衍射分析,得到XRD图谱参见图4,由图4可知,该复合粉主要成分包括碳、镁铝尖晶石及氧化镁。对实施例2制备的碳/镁铝尖晶石复合粉进行了拉曼光谱分析,得到的拉曼光谱图参见图5,由图5可知,制备的碳/镁铝尖晶石复合粉中含有碳。
实施例3:
本实施例与实施例1不同的是:按质量百分比计,草酸镁为40.8%,过氧化镁为20.6%,氧化铝为18.8%,铝粉为19.8%;
对制备的碳/镁铝尖晶石复合粉进行X射线衍射分析,得到XRD图谱参见图6,由图6可知,该复合粉主要成分包括碳、镁铝尖晶石及氧化镁。对实施例3制备的碳/镁铝尖晶石复合粉进行了拉曼光谱分析,得到的拉曼光谱图参见图7,由图7可知,制备的碳/镁铝尖晶石复合粉中含有碳。
Claims (7)
1.一种碳/镁铝尖晶石复合粉,其特征在于,所述复合粉包括以下原料:草酸镁、过氧化镁、氧化铝和铝粉。
2.如权利要求1所述复合粉,其特征在于,所述复合粉按质量百分比计,包括以下原料:28.6%~40.8%草酸镁,20.6%~28.6%过氧化镁,19.0%~22.2%氧化铝,19.8%~23.8%铝粉,各原料的质量百分比之和为100%。
3.如权利要求1所述复合粉,其特征在于,所述复合粉按质量百分比计,包括以下原料:33.4%草酸镁,22.2%过氧化镁,22.2%氧化铝,22.2%铝粉。
4.如权利要求1所述复合粉,其特征在于,所述草酸镁的纯度≥99.0%,所述氧化铝的纯度≥99.0%,所述铝粉的纯度≥99.0%,所述过氧化镁中氧化镁占比不超过70%。
5.如权利要求1-4任一权利要求所述复合粉,其特征在于,所述复合粉的制备方法,包括以下步骤:将草酸镁、过氧化镁、氧化铝与铝粉按配方量混合后干压成型,通过自蔓延高温合成反应得到试样,将试样进行粉碎研磨即得碳/镁铝尖晶石复合粉。
6.如权利要求5所述复合粉,其特征在于,将草酸镁、过氧化镁、氧化铝与铝粉按配比混合后干压成直径为20mm、高为30mm的圆柱形试样进行自蔓延高温合成反应。
7.权利要求1-4任一权利要求所述复合粉在含碳耐火材料中的应用。
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CN111732419A (zh) * | 2020-08-28 | 2020-10-02 | 北京利尔高温材料股份有限公司 | 一种性能优良的超低碳镁碳砖及其制备方法 |
CN114455967A (zh) * | 2022-01-27 | 2022-05-10 | 西安建筑科技大学 | 一种低碳耐火材料添加剂、制备方法及应用 |
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US4612297A (en) * | 1982-12-08 | 1986-09-16 | Toya Soda Manufacturing Co., Ltd. | Process for preparation of silicon nitride powder of good sintering property |
CN1144520A (zh) * | 1994-03-25 | 1997-03-05 | 弗博塞尔维斯股份有限公司 | 用于构成耐火组合物的化学混合物 |
CN101085707A (zh) * | 2006-04-27 | 2007-12-12 | 武汉科技大学 | 一种电熔镁铝尖晶石复合耐火材料及其生产方法 |
CN106187243A (zh) * | 2016-07-22 | 2016-12-07 | 武汉科技大学 | 一种水泥窑用尖晶石质耐火材料及其制备方法 |
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CN111732419A (zh) * | 2020-08-28 | 2020-10-02 | 北京利尔高温材料股份有限公司 | 一种性能优良的超低碳镁碳砖及其制备方法 |
CN114455967A (zh) * | 2022-01-27 | 2022-05-10 | 西安建筑科技大学 | 一种低碳耐火材料添加剂、制备方法及应用 |
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