CN113461410B - 一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖及其生产方法 - Google Patents
一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖及其生产方法 Download PDFInfo
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Abstract
本发明提供一种添加氮化钛包裹莫来石的Al‑Al2O3滑板砖及其生产方法。按重量百分比计，原料组成为：54‑74％的刚玉、6‑12％活性氧化铝微粉、10‑30％的电熔莫来石、5‑10％的金属铝粉，外加上述原料总量3‑4％的热固性酚醛树脂。通过引入氮化钛包裹的电熔莫来石原料，并利用金属结合技术，克服了传统滑板砖对碳的依赖，解决了含碳耐火材料碳含量降低对其抗侵蚀性、热震稳定性的不利影响，采用免烧免浸生产工艺，降低了生产成本，缩短了生产周期，同时又使滑板砖具有强度、抗氧化性、热震稳定性、抗侵蚀性优越，使用寿命长、安全系数高等特点。
Description
技术领域
本发明涉及一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖及其生产方法，属于功能耐火材料技术领域。
背景技术
我国中低品位矾土储量巨大，约占矾土资源的60％，实现中低品位矾土资源的高效、综合利用是实现耐火行业持续绿色发展的重要途径。利用中低品位矾土通过电熔法制备莫来石，形成的电熔莫来石形成其固有的针状结构，莫来石是常压下Al2O3-SiO2系统中唯一稳定的二元化合物，其熔点为1890±90℃。具有耐火度高、抗热震性能好、荷重软化温度高、抗蠕变、高温体积稳定性好、抗化学侵蚀、电绝缘性强等性质，属高级耐火材料，有利于提高耐火材料的综合性能。中低品位矾土制备的莫来石中TiO2含量较高。TiO2会反应生成碳氮化钛固溶体固溶在莫来石中。碳氮化钛固溶体是一种性能优良的非氧化物陶瓷材料，具有高熔点、高硬度、耐侵蚀和优异的抗氧化性等特性，在一些研究中表明，碳氮化钛固溶体的存在能显著增强莫来石陶瓷材料的强度和硬度，并且有利于莫来石的致密化。
非氧化物具有高温性能优异、热膨胀系数小、抗侵蚀性好的特点，使其成为碳的理想替代材料，非氧化物耐火材料的应用，使得耐火材料的转向新型非氧化物-氧化物复合耐火材料的方向发展，氧化物-非氧化物耐火材料与含碳耐火材料相比具有较好的抗氧化性。滑板砖通常采用含碳耐火材料，使其具有优异的抗侵蚀性和热震稳定性，然而含碳耐火材料在高温下易发生碳氧化，破坏产品结构，影响制品寿命，并且在使用过程中容易污染钢水，不符合洁净钢的冶炼要求，限制了其应用。研发既能适应普通钢的连铸又能适应特殊钢的连铸，同时满足生产洁净钢和品种钢冶炼要求的无碳滑板，势在必行。
发明内容
针对现有技术的不足，本发明的目的是提供一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖及其生产方法。通过引入氮化钛包裹的电熔莫来石原料，并利用金属结合技术，克服了传统滑板砖对碳的依赖，解决了含碳耐火材料碳含量降低对其抗侵蚀性、热震稳定性的不利影响，采用免烧免浸生产工艺，降低了生产成本，缩短了生产周期，同时又使滑板砖具有强度、抗氧化性、热震稳定性、抗侵蚀性优越，使用寿命长、安全系数高等特点。
为了实现上述目的，本发明所采用的技术方案是：
一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖，按重量百分比计，原料组成为：54-74％的刚玉、6-12％活性氧化铝微粉、10-30％的电熔莫来石、5-10％的金属铝粉，外加上述原料总量3-4％的热固性酚醛树脂。
所述刚玉为板状刚玉，其粒度范围为：1mm<粒度1≤2mm、0.5mm<粒度2≤1mm、0.044mm<粒度3≤0.5mm、0<粒度4≤0.044mm，不同粒度的重量比为：粒度1：粒度2：粒度 3：粒度4＝0-20：18-22：20-24：11-14。
所述活性氧化铝微粉的型号为RG4000和CL370，RG4000和CL370的重量比为1:1。
所述电熔莫来石的粒度范围为：1mm≤粒度≤2mm。
所述电熔莫来石是利用中低品位或废弃矾土，经过2000℃高温电熔制备得到的，按重量百分比计，电熔莫来石的主要组分重量含量为Al2O3：70-75％，SiO2：10-15％，TiO2：5-8％。
所述滑板砖的生产方法，包括以下步骤：
(1)将电熔莫来石在氮气气氛下，于1300℃热处理5-8h，得到氮化钛包裹的电熔莫来石原料，备用；
(2)按配比称取各原料，先将除酚醛树脂外的所有原料投入高速混练机中，以200-300 转/分钟的转速混合2-5min，然后向高速混练机中加入酚醛树脂，继续以200-300转/分钟的转速混练30-40min后，得到成型用泥料，在温度20-35℃，湿度40-50％的恒温恒湿条件下困料 8-12h后进行压制成型，得到滑板砖坯体；
(3)将坯体自然干燥24h后，送入干燥器烘干，干燥温度为200-230℃，在此温度下干燥8-10h；
(4)干燥后产品再经加箍、磨制、涂布，即制成本发明产品。
干燥器升温时在100℃之前的升温速率为5-10℃/h，100℃之后的升温速率为10-15℃/h。
本发明有益效果：
本发明利用中低品位或废弃矾土制备的含Ti2O3电熔莫来石，制备了添加氮化钛包裹的莫来石的Al-Al2O3滑板砖，该产品制备原料中不含碳，产品无需沥青浸渍，具有节能和环保优势，降低了生产成本，提高经济效益，为大力发展国家产业政策鼓励的节能型、利废型、保健型、生态型的耐火材料技术和产品提供了参考。
1、本发明产品的混料过程使用高速混练机，采用所有原料一次性投入混料的工艺路线，打破了传统先加颗粒料，再加树脂，最后加入预混合粉料的原料分次加入的混料方式，提高了泥料的稳定性。
2、本发明产品中加入电熔莫来石原料，该原料采用中低品位或废弃矾土制备而成，使用前经过1300℃氮气气氛下热处理，在莫来石外层形成氮化钛非氧化物层，经过热处理后的莫来石含有莫来石、氧化铝、碳氮化钛、氮化钛等物相，该莫来石具有传统莫来石低热膨胀系数的特点，同时还具有碳氮化钛和氮化钛熔点高、耐磨性好、抗氧化性强、抗侵蚀性好的特点，并具有良好的导热性和化学稳定性的优异性能，能改善滑板砖的热震稳定性。
3、本发明产品在使用过程中原位生成Ti(C,N)和Al2OC-AlN等非氧化物增强相，提升了滑板的高温使用性能。其中，电熔莫来石中的Ti2O3与酚醛树脂残碳或者N2反应分别形成TiC、 TiN，TiC与TiN固溶形成Ti(C,N)；金属铝在高温熔融状态下与氮气或Al2O3反应分别生成 AlN、Al2O，AlN、Al2O与酚醛树脂的残碳反应生成Al2OC-AlN固溶体。与采用传统滑板相比，在滑板材料组成设计、提高富钛耐火原料利用价值方面有创新，实现了含高钛的低品位或废弃矾土的高效利用，又降低了滑板制备过程中对烧结刚玉的依赖。
4、本发明所得产品为金属和非金属结合滑板，非氧化物结合相一方面通过电熔莫来石原料预处理，在莫来石原料外层形成氮化钛非氧化物包裹层，将该非氧化物直接引入到滑板砖中改善滑板砖的性能，另一方面莫来石中的Ti在高温下原位生成碳氮化钛非氧化物增强相，改善滑板砖的性能。
5、本发明产品的无碳滑板砖，只有少量的树脂残碳，在很大程度上减小了滑动机构对钢液的增碳污染，为洁净钢的发展提供基础和保证；
6、本发明产品无需高温烧成，无需沥青浸渍和干馏工序，简化了生产工序，大大降低了生产成本；
7、经测试，本发明产品的性能指标为：显气孔率3-8％、体积密度3.00-3.15g/cm3、常温耐压强度140-210MPa、常温抗折强度13-18MPa，高温抗折强度30-55MPa。根据 YB/T5049-2019《滑板砖》行业标准中HBLT-80牌号(不浸渍)指标要求：显气孔率≤13％、体积密度≥2.90g/cm3、常温耐压强度≥80MPa。本发明各项理化性能均达到行业标准，说明本发明产品具有较好的物理性能。
附图说明
图1热处理前电熔莫来石原料的XRD图；
图2热处理后电熔莫来石原料的XRD图；
图3所得滑板砖产品使用后的XRD图；
其中，X1、X2、X3分别对应实施例1、实施例2、实施例3所得滑板砖产品；
图4所得滑板砖产品使用后，产品中Ti(C,N)的SEM图。
具体实施方式
以下结合实施例对本发明的具体实施方式作进一步详细说明。
实施例1：
一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖，按重量百分比计，原料组成为：74％的板状刚玉、3％的CL370、3％的RG4000、10％的电熔莫来石、10％的金属铝粉，外加上述原料总量3％的热固性酚醛树脂。
板状刚玉的粒度范围为：1mm<粒度1≤2mm、0.5mm<粒度2≤1mm、0.044mm<粒度3≤0.5 mm、0<粒度4≤0.044mm，不同粒度的重量比为：粒度1：粒度2：粒度3：粒度4＝20：22：20：12。
电熔莫来石的粒度范围为：1≤粒度≤2mm；电熔莫来石是利用中低品位或废弃矾土经过 2000℃高温电熔制备的含Ti2O3电熔莫来石，按重量百分比计，电熔莫来石的主要组分重量含量为Al2O3：70-75％，SiO2：10-15％，TiO2：5-8％。
该滑板砖的生产方法，包括以下步骤：
(1)将电熔莫来石在氮气气氛下，于1300℃热处理5-8h，得到氮化钛包裹的电熔莫来石原料，备用；
其中，热处理前后电熔莫来石原料的X射线衍射(XRD)图，如图1(热处理前)、图2(热处理后)所示。
(2)按配比称取各原料，先将除酚醛树脂外的所有原料投入高速混练机中，以200-300 转/分钟的转速混合2-5min，然后向高速混练机中加入酚醛树脂，继续以200-300转/分钟的转速混练30-40分钟后，得到成型用泥料，在温度20-35℃，湿度40％-50％的恒温恒湿条件下困料8-12小时后进行压制成型，得到滑板砖坯体；
(3)将坯体自然干燥24小时后，送入干燥器烘干，干燥温度为200-230℃，100℃之前的升温速率为5-10℃/h，100℃之后的升温速率为10-15℃/h，干燥温度达到目标温度后保温 8-10h；
其中，由于热固性酚醛树脂的特性，100℃之前树脂聚合反应进行，此时为树脂分子链结构形成的关键，升温不宜过快，升温过快会导致固化的结构破坏，使固化后的结构强度降低。
(4)干燥后产品再经加箍、磨制、涂布，即制成本发明产品。
其中，所得产品使用后的XRD图谱如图3(X1)所示，扫描电子显微镜(SEM)图如图4(右图为左图的局部放大图)所示，并对图4中点2处进行EDS能谱分析，结果如下表1(点 2位置上各原子的百分比at％)所示。结合图3、图4和表1可知，所的产品在高温使用过程中原位生成Ti(C,N)和Al2OC-AlN等非氧化物增强相。
表1图4中点2的EDS能谱分析结果(at％)
| 项目 | Si | Al | O | N | C | Ti |
| 点2 | 6.23 | 11.38 | 45.66 | 6.03 | 9.92 | 20.78 |
所得产品的性能指标为：显气孔率3％、体积密度3.15g/cm3、常温耐压强度210MPa、常温抗折强度18MPa，高温抗折强度(1400℃×0.5h埋碳)55MPa。残余抗折强度保持率72.8％(1100℃风冷3次)，产品的热震稳定性和强度较好。
实施例2：
一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖，按重量百分比计，原料组成为：64％的板状刚玉、3％的CL370、3％的RG4000、20％的电熔莫来石、10％的金属铝粉，外加上述原料总量3.5％的热固性酚醛树脂。
板状刚玉的粒度范围为：1mm<粒度1≤2mm、0.5mm<粒度2≤1mm、0.044mm<粒度3≤0.5 mm、0<粒度4≤0.044mm，不同粒度的重量比为：粒度1：粒度2：粒度3：粒度4＝10：22：20：12。
电熔莫来石的粒度范围为：1≤粒度≤2mm；电熔莫来石是利用中低品位或废弃矾土经过 2000℃高温电熔制备的含Ti2O3电熔莫来石，按重量百分比计，电熔莫来石的主要组分重量含量为Al2O3：70-75％，SiO2：10-15％，TiO2：5-8％。
该滑板砖的生产方法与实施例1相同，所得产品的性能指标为：显气孔率5.7％、体积密度3.08g/cm3、常温耐压强度184MPa、常温抗折强度16MPa，高温抗折强度(1400℃×0.5h 埋碳)53MPa。残余抗折强度保持率75.9％(1100℃风冷3次)，产品的热震稳定性和强度较好。
实施例3：
一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖，按重量百分比计，原料组成为：54％的板状刚玉、3％的CL370、3％的RG4000、30％的电熔莫来石、10％的金属铝粉，外加上述原料总量4％的热固性酚醛树脂。
板状刚玉的粒度范围为：1mm<粒度1≤2mm、0.5mm<粒度2≤1mm、0.044mm<粒度3≤0.5 mm、0<粒度4≤0.044mm，不同粒度的重量比为：粒度1：粒度2：粒度3：粒度4＝0：22： 20：12。
电熔莫来石的粒度范围为：1≤粒度≤2mm；电熔莫来石是利用中低品位或废弃矾土经过 2000℃高温电熔制备的含Ti2O3电熔莫来石，按重量百分比计，电熔莫来石的主要组分重量含量为Al2O3：70-75％，SiO2：10-15％，TiO2：5-8％。
该滑板砖的生产方法与实施例1相同，所得产品的性能指标为：显气孔率8％、体积密度 3.00g/cm3、常温耐压强度175MPa、常温抗折强度14MPa，高温抗折强度50MPa。残余抗折强度保持率83.4％(1100℃风冷3次)，产品的热震稳定性和强度较好。
实施例4：
一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖，按重量百分比计，原料组成为：64％的板状刚玉、4％的CL370、4％的RG4000、20％的电熔莫来石、8％的金属铝粉，外加上述原料总量3.5％的热固性酚醛树脂。
板状刚玉的粒度范围为：1mm<粒度1≤2mm、0.5mm<粒度2≤1mm、0.044mm<粒度3≤0.5 mm、0<粒度4≤0.044mm，不同粒度的重量比为：粒度1：粒度2：粒度3：粒度4＝10：22：20：12。
电熔莫来石的粒度范围为：1≤粒度≤2mm；电熔莫来石是利用中低品位或废弃矾土经过 2000℃高温电熔制备的含Ti2O3电熔莫来石，按重量百分比计，电熔莫来石的主要组分重量含量为Al2O3：70-75％，SiO2：10-15％，TiO2：5-8％。
该滑板砖的生产方法与实施例1相同，所得产品的性能指标为：显气孔率6.2％、体积密度3.07g/cm3、常温耐压强度172MPa、常温抗折强度15MPa，高温抗折强度(1400℃×0.5h 埋碳)42MPa。残余抗折强度保持率74.5％(1100℃风冷3次)，产品的热震稳定性和强度较好。
实施例5：
一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖，按重量百分比计，原料组成为：63％的板状刚玉、6％的CL370、6％的RG4000、20％的电熔莫来石、5％的金属铝粉，外加上述原料总量3.5％的热固性酚醛树脂。
板状刚玉的粒度范围为：1mm<粒度1≤2mm、0.5mm<粒度2≤1mm、0.044mm<粒度3≤0.5 mm、0<粒度4≤0.044mm，不同粒度的重量比为：粒度1：粒度2：粒度3：粒度4＝10：20：22：11。
电熔莫来石的粒度范围为：1≤粒度≤2mm；电熔莫来石是利用中低品位或废弃矾土经过 2000℃高温电熔制备的含Ti2O3电熔莫来石，按重量百分比计，电熔莫来石的主要组分重量含量为Al2O3：70-75％，SiO2：10-15％，TiO2：5-8％。
该滑板砖的生产方法与实施例1相同，所得产品的性能指标为：显气孔率6.8％、体积密度3.06g/cm3、常温耐压强度140MPa、常温抗折强度13MPa，高温抗折强度(1400℃×0.5h 埋碳)30MPa。残余抗折强度保持率70.4％(1100℃风冷3次)，产品的热震稳定性和强度较好。
实施例6：
一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖，按重量百分比计，原料组成为：63％的板状刚玉、6％的CL370、6％的RG4000、20％的电熔莫来石、5％的金属铝粉，外加上述原料总量3.5％的热固性酚醛树脂。
板状刚玉的粒度范围为：1mm<粒度1≤2mm、0.5mm<粒度2≤1mm、0.044mm<粒度3≤0.5 mm、0<粒度4≤0.044mm，不同粒度的重量比为：粒度1：粒度2：粒度3：粒度4＝10：18：24：11。
电熔莫来石的粒度范围为：1≤粒度≤2mm；电熔莫来石是利用中低品位或废弃矾土经过 2000℃高温电熔制备的含Ti2O3电熔莫来石，按重量百分比计，电熔莫来石的主要组分重量含量为Al2O3：70-75％，SiO2：10-15％，TiO2：5-8％。
该滑板砖的生产方法与实施例1相同，所得产品的性能指标为：显气孔率7.1％、体积密度3.06g/cm3、常温耐压强度145MPa、常温抗折强度13MPa，高温抗折强度(1400℃×0.5h 埋碳)32MPa。残余抗折强度保持率68.1％(1100℃风冷3次)，产品的热震稳定性和强度较好。
Claims (4)
1.一种添加氮化钛包裹莫来石的Al-Al2O3滑板砖，其特征在于，按重量百分比计，原料组成为：54-74%的刚玉、6-12 %活性氧化铝微粉、10-30 %的电熔莫来石、5-10%的金属铝粉，外加上述原料总量3-4%的热固性酚醛树脂；
所述电熔莫来石是利用中低品位或废弃矾土，经过2000℃高温电熔制备得到的，按重量百分比计，电熔莫来石的主要组分重量含量为Al2O3：70-75 %，SiO2：10-15 %，TiO2：5-8%；
所述滑板砖的生产方法，包括以下步骤：
（1）将电熔莫来石在氮气气氛下，于1300℃热处理5-8h，得到氮化钛包裹的电熔莫来石原料，备用；
（2）按配比称取各原料，先将除酚醛树脂外的所有原料投入高速混练机中，以200-300转/分钟的转速混合2-5min，然后向高速混练机中加入酚醛树脂，继续以200-300转/分钟的转速混练30-40min后，得到成型用泥料，在温度20-35℃，湿度40-50%的恒温恒湿条件下困料8-12h后进行压制成型，得到滑板砖坯体；
（3）将坯体自然干燥24h后，送入干燥器烘干，干燥温度为200-230℃，在此温度下干燥8-10h；干燥器升温时在100℃之前的升温速率为5-10℃/h，100℃之后的升温速率为10-15℃/h；
（4）干燥后产品再经加箍、磨制、涂布，即制成本发明产品。
2.如权利要求1所述的滑板砖，其特征在于，所述刚玉为板状刚玉，其粒度范围为：1mm<粒度1≤2 mm、0.5mm<粒度2≤1 mm、0.044mm<粒度3≤0.5 mm、0<粒度4≤0.044 mm，不同粒度的重量比为：粒度1：粒度2：粒度3：粒度4=0-20：18-22：20-24：11-14。
3.如权利要求1所述的滑板砖，其特征在于，所述活性氧化铝微粉的型号为RG4000和CL370，RG4000和CL370的重量比为1:1。
4.如权利要求1所述的滑板砖，其特征在于，所述电熔莫来石的粒度范围为：1mm≤粒度≤2 mm。
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