CN106588059B - 一种石灰回转窑用预制件及其制备方法 - Google Patents

一种石灰回转窑用预制件及其制备方法 Download PDF

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CN106588059B
CN106588059B CN201611243860.3A CN201611243860A CN106588059B CN 106588059 B CN106588059 B CN 106588059B CN 201611243860 A CN201611243860 A CN 201611243860A CN 106588059 B CN106588059 B CN 106588059B
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alumina spinel
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毛利民
袁林
刘锡俊
魏瀚
胡建辉
王俊涛
陈雪峰
徐如林
尹超男
叶亚红
周严敦
陈松林
赵洪亮
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Abstract

本发明公开了一种以富镁镁铝尖晶石废砖为主原料的石灰回转窑用预制件及其制备方法，其技术方案是：按重量百分比，由1～3mm的富镁镁铝尖晶石废砖35～40%、0.088～1mm富镁镁铝尖晶石废砖18～25%、≤0.088mm富镁镁铝尖晶石废砖粉30～35%、≤0.03mm氮化硅细粉3～6%、≤0.246mm金属铝粉0.05～1%及复合结合剂4～6%构成；外加水占主料总重量的5～6%；所述复合结合剂由重量百分比20～40%的硅微粉和重量百分比60～80%的铝酸盐水泥组成，其中硅微粉重量百分比SiO2含量≥93%，铝酸盐水泥重量百分比Al2O3含量≥68.75%；其制备方法包括破碎、筛分、研磨、配料、成型、烘干和热处理等工序。本发明以上述废砖为主原料，价格低廉，引入氮化硅、金属铝粉及复合结合剂显著改善该预制件性能及质量。

Description

一种石灰回转窑用预制件及其制备方法
技术领域
本发明涉及耐火材料工业领域，特别是一种石灰回转窑用预制件及其制备方法。
背景技术
目前，国内石灰石矿山产品中 0-30mm 细粒级品通常约占总产量的 30-40%，这部分石灰石无法借助套筒窑、麦尔兹窑、弗卡斯窑等窑炉以生产活性石灰，而回转窑可以直接煅烧 0-50mm 的细粒级石灰石，建设石灰回转窑生产线不但能充分利用石灰石矿山资源，且符合石灰行业可持续发展需要。
石灰回转窑内衬主要采用高铝砖、粘土砖、镁铬砖或镁铬质预制件及浇注料等耐火材料砌筑。虽然石灰回转窑的煅烧温度一般控制在 1100-1200℃，其中气体介质温度在1350℃左右，但是，在回转窑运转过程中，镁铬质材料中的铬会与石灰石原料中的CaO及少量其他碱金属物质发生反应，生成有毒的六价铬化合物（R2CrO4），其生成量由原制品中的初始含量0.04×10-6急剧升高至1000×10-6，其浓度值已大大超过环保标准值。这就意味着回转窑使用后的镁铬质废弃物必须进行特别的处理，才能不污染环境。因此，开发石灰回转窑内衬用无铬预制件，替代原含铬部件的使用，对于消除铬公害降低环境治理成本具有重要意义。
发明内容
本发明提供了一种以富镁的镁铝尖晶石废砖为主原料的石灰回转窑用预制件及其制备方法，利用该方法可以生产出具有较好的耐压强度、耐高温和抗热震稳定性的石灰回转窑用无铬的镁铝质预制件。
本发明提供的一种石灰回转窑用预制件的组分、粒度及重量百分比含量如下：
富镁镁铝尖晶石废砖 1～3mm 35～40%
富镁镁铝尖晶石废砖 0.088～1mm 18～25%
富镁镁铝尖晶石废砖粉 ≤0.088mm 30～35%
氮化硅细粉 ≤0.03mm 3～6%
金属铝粉 ≤0.246mm 0.05～1%
复合结合剂 / 4～6%
外加水 / 5～6%
上述富镁镁铝尖晶石废砖含重量百分比MgO：80～84%，Al2O3：10～12%，体积密度：2.85～2.95g/cm3。富镁镁铝尖晶石废砖是高温工业窑炉停炉大修或重建拆除的用后废品，由于其中的含镁物相易水化，难再烧结，多作为废弃物或废砖料处理。将富镁镁铝尖晶石废砖表面粘附的残留物去除后，其物质组成与富镁镁铝尖晶石砖相比差别很小，但其价格约是原富镁镁铝尖晶石砖的四分之一至七分之一。
所述氮化硅细粉重量百分比Si3N4含量≥96%；所述金属铝粉重量百分比活性Al含量≥98%。所述复合结合剂由重量百分比20～40%的硅微粉和重量百分比60～80%的铝酸盐水泥组成，硅微粉重量百分比SiO2含量≥93%，铝酸盐水泥重量百分比Al2O3含量≥68.75%。
一种石灰回转窑用镁铝质预制件的制备方法，该方法包括以下步骤：
a. 将富镁镁铝尖晶石废砖去除表面残留物，经破碎处理后，再用3mm、1mm和0.088mm筛筛分后，制成粒度为1～3mm和0.088～1mm的颗粒，对于≤0.088mm的筛下物进行粉磨处理，制成粉磨原料；
b. 按照前述重量百分比含量进行称量配料，经混合、成型、养护制得坯体，再经110℃×24小时烘干、750℃的预热处理和1650～1700℃高温热处理制得镁铝尖晶石预制件。
本发明与现有同类技术相比，其显著的有益效果体现在：
采用的骨料是粒度小于3mm的富镁镁铝尖晶石废砖颗粒，价格低廉，通过筛分获得1～3mm和0.088～1mm两种粒度的颗粒，再将≤0.088mm的颗粒研磨成≤0.088mm的富镁镁铝尖晶石废砖粉，充分利用减少资源浪费，能显著降低镁铝质预制件生产成本。
采用硅微粉、铝酸盐水泥作为预制件的复合结合剂提高了预制件的烘干和烧后强度，这是因为SiO2微粉比表面积约为20m3/g左右，平均粒径在2μm左右，它可以有效的填充气孔提高预制件的致密度，同时它与H2O 或OH﹣发生凝聚反应，从而使预制件110℃烘干强度升高；在预热处理过程中，预制件材料中的SiO2与Al2O3于750℃首先开始发生莫来石化反应，形成犬牙交错的莫来石结合相，提高预制件材料的中温强度；向预制件组分里引入的Si3N4细粉，在随后的高温热处理作用下，部分氧化后生成活性很高的 SiO2，SiO2进而与 Si3N4和Al2O3反应生成 O＇-SiAlON 结合相（化学式可表示为Si2-ZAlZO1+ZN2-Z，其中Z=0～0.4），它与稳定的莫来石相一起，进一步提高了材料高温时的强度。由于该预制件材料及基质中的固—固结合率大大提高，从而显著提高该预制件的高温强度及抗侵蚀性能。
向预制件组分里引入适量的金属铝粉，不会显著降低预制件固结硬化后的强度，而是可以显著提高预制件材料干燥和硬化时的防爆性，因为Al作为活泼的两性金属，能够与酸、碱反应放出氢气，铝粉与铝酸盐水泥水化生成的OH﹣及水反应生成氢气，提高了预制件坯体的透气度，有利于预制件在烘干和硬化过程中水分的排出，提高了预制件的防爆性，缩短了预制件硬化和干燥所需的时间。另外，在高温作用下，预制件基质中镁铝尖晶石呈方镁石和镁铝尖晶石二相共存状态，这种不匹配导致了在尖晶石骨料周围产生了环向拉伸应力和显微裂纹，缓冲了预制件材料因温度变化而产生的热应力，有效的防止材料因热冲击而产生的损毁，从而提高了预制件的抗热震稳定性。
实施例1
以富镁镁铝尖晶石废砖为原料，将废砖表面残留物去除，破碎，再经3mm、1mm筛筛分，制成粒度为1～3mm和≤1mm的两种颗粒物；由球磨机或其他磨粉设备对≤1mm的颗粒物进行进一步研磨，经1mm和0.088mm筛筛分，得到0.088～1mm和≤0.088mm的富镁镁铝尖晶石废砖粉；将上述1～3mm 、0.088～1mm和≤0.088mm的三种富镁镁铝尖晶石废砖颗粒及粉料作为原料，外加氮化硅细分、金属铝粉、复合结合剂以及水，具体配比如下：
富镁镁铝尖晶石废砖 1～3mm 40.0
富镁镁铝尖晶石废砖 0.088～1mm 18.0
富镁镁铝尖晶石废砖粉 ≤0.088mm 34.95
氮化硅细粉 ≤0.03mm 3.0
金属铝粉 ≤0.246mm 0.05
复合结合剂 4.0
外加水 6.0
其中富镁镁铝尖晶石废砖含重量百分比MgO：80～84%，Al2O3：10～12%，体积密度：2.85～2.95 g/cm3。复合结合剂由重量百分比40%的硅微粉和重量百分比60%的铝酸盐水泥组成。按照上述配比进行原料称重后混合均匀，进行成型和养护制得坯体，再经110℃×24小时烘干、750℃的预热处理和1650～1700℃高温热处理制得镁铝尖晶石预制件。成品理化性能分析结果见表2。
实施例2
以富镁镁铝尖晶石废砖为原料，将废砖表面残留物去除，破碎，再经3mm、1mm筛筛分，制成粒度为1～3mm和≤1mm的两种颗粒物；由球磨机或其他磨粉设备对≤1mm的颗粒物进行进一步研磨，经1mm和0.088mm筛筛分，得到0.088～1mm和≤0.088mm的富镁镁铝尖晶石废砖粉；将上述1～3mm 、0.088～1mm和≤0.088mm的三种富镁镁铝尖晶石废砖颗粒及粉料作为原料，外加氮化硅细分、金属铝粉、复合结合剂以及水，具体配比如下：
富镁镁铝尖晶石废砖 1～3mm 33.0
富镁镁铝尖晶石废砖 0.088～1mm 25.0
富镁镁铝尖晶石废砖粉 ≤0.088mm 32.44
氮化硅细粉 ≤0.03mm 3.5
金属铝粉 ≤0.246mm 0.06
复合结合剂 6.0
外加水 5.0
其中富镁镁铝尖晶石废砖含重量百分比MgO：80～84%，Al2O3：10～12%，体积密度：2.85～2.95 g/cm3。复合结合剂由重量百分比25%的硅微粉和重量百分比75%的铝酸盐水泥组成。按照上述配比进行原料称重后混合均匀，进行成型和养护制得坯体，再经110℃×24小时烘干、750℃的预热处理和1650～1700℃高温热处理制得镁铝尖晶石预制件。成品理化性能分析结果见表2。
实施例3
以富镁镁铝尖晶石废砖为原料，将废砖表面残留物去除，破碎，再经3mm、1mm筛筛分，制成粒度为1～3mm和≤1mm的两种颗粒物；由球磨机或其他磨粉设备对≤1mm的颗粒物进行进一步研磨，经1mm和0.088mm筛筛分，得到0.088～1mm和≤0.088mm的富镁镁铝尖晶石废砖粉；将上述1～3mm 、0.088～1mm和≤0.088mm的三种富镁镁铝尖晶石废砖颗粒及粉料作为原料，外加氮化硅细分、金属铝粉、复合结合剂以及水，具体配比如下：
富镁镁铝尖晶石废砖 1～3mm 35.0
富镁镁铝尖晶石废砖 0.088～1mm 23.2
富镁镁铝尖晶石废砖粉 ≤0.088mm 30.0
氮化硅细粉 ≤0.03mm 6.0
金属铝粉 ≤0.246mm 0.8
复合结合剂 5.0
外加水 6.0
其中富镁镁铝尖晶石废砖含重量百分比MgO：80～84%，Al2O3：10～12%，体积密度：2.85～2.95 g/cm3。复合结合剂由重量百分比20%的硅微粉和重量百分比80%的铝酸盐水泥组成。按照上述配比进行原料称重后混合均匀，进行成型和养护制得坯体，再经110℃×24小时烘干、750℃的预热处理和1650～1700℃高温热处理制得镁铝尖晶石预制件。成品理化性能分析结果见表2。
对比例1
以富镁镁铝尖晶石废砖为原料，将废砖表面残留物去除，破碎，再经3mm、1mm筛筛分，制成粒度为1～3mm和≤1mm的两种颗粒物；由球磨机或其他磨粉设备对≤1mm的颗粒物进行进一步研磨，经1mm和0.088mm筛筛分，得到0.088～1mm和≤0.088mm的富镁镁铝尖晶石废砖粉；将上述1～3mm 、0.088～1mm和≤0.088mm的三种富镁镁铝尖晶石废砖颗粒及粉料作为原料，外加氮化硅细分、金属铝粉、复合结合剂以及水，具体配比如下：
富镁镁铝尖晶石废砖 1～3mm 36.0
富镁镁铝尖晶石废砖 0.088～1mm 23.5
富镁镁铝尖晶石废砖粉 ≤0.088mm 34.5
复合结合剂 6.0
外加水 5.5
其中富镁镁铝尖晶石废砖含重量百分比MgO：80～84%，Al2O3：10～12%，体积密度：2.85～2.95 g/cm3。复合结合剂由重量百分比20%的硅微粉和重量百分比80%的铝酸盐水泥组成。按照上述配比进行原料称重后混合均匀，进行成型和养护制得坯体，再经110℃×24小时烘干、750℃的预热处理和1650～1700℃高温热处理制得镁铝尖晶石预制件。成品理化性能分析结果见表2。
对比例2
选取富镁的1～3mm、0.088～1mm和≤0.088mm的镁铝尖晶石颗粒及粉料作为原料，外加氮化硅细粉、金属铝粉、复合结合剂以及水，具体配比如下：
镁铝尖晶石 1～3mm 40.0
镁铝尖晶石 0.088～1mm 18.0
镁铝尖晶石 ≤0.088mm 34.95
氮化硅细粉 ≤0.03mm 3.0
金属铝粉 ≤0.246mm 0.05
复合结合剂 4.0
外加水 6.0
其中镁铝尖晶石重量百分比MgO含量≥84.0%，Al2O3含量≤10.0%，体积密度≥2.95g/cm3。复合结合剂由重量百分比40%的硅微粉和重量百分比60%的铝酸盐水泥组成。按照上述配比进行原料称重后混合均匀，进行成型和养护制得坯体，再经110℃×24小时烘干、750℃的预热处理和1650～1700℃高温热处理制得镁铝尖晶石预制件。成品理化性能分析结果见表2。
对比例3
选取富镁的1～3mm、0.088～1mm和≤0.088mm的镁铝尖晶石废砖颗粒及粉料作为原料，外加铝酸盐水泥结合剂以及水，具体配比如下：
镁铝尖晶石废砖 1～3mm 36.0
镁铝尖晶石废砖 0.088～1mm 23.5
镁铝尖晶石废砖粉 ≤0.088mm 34.5
铝酸盐水泥 6.0
外加水 5.5
其中镁铝尖晶石废砖含重量百分比MgO：80～84%，Al2O3：10～12%，体积密度：2.85～2.95 g/cm3。所用结合剂为铝酸盐水泥。按照上述配比进行原料称重后混合均匀，进行成型和养护制得坯体，再经110℃×24小时烘干、750℃的预热处理和1650～1700℃高温热处理制得镁铝尖晶石预制件。成品理化性能分析结果见表2。
表1 主料和添加剂的用量
Figure DEST_PATH_IMAGE002
表2 成品理化性能指标对比
检测项目 实施例1 实施例2 实施例3 对比例1 对比例2 对比例3
MgO，wt% 74.4 76.0 74.1 77.1 80.6 77.0
Al<sub>2</sub>O<sub>3</sub>，wt% 12.8 12.1 12.4 12.7 11.3 14.9
体积密度，g/cm<sup>3</sup> 2.86 2.90 2.93 2.81 2.87 2.78
显气孔率，% 19 18 17 23 18 26
常温耐压强度，MPa 50 53 55 39 50 19
烧后线变化率（1500℃×2h），% 0.30 0.29 0.28 0.57 0.30 0.86
荷重软化温度（T<sub>0.6</sub>），℃ 1600 1650 1680 1550 1600 1310
抗热震性 (950空冷)，次 13 16 17 6 17 2
加入复合结合剂、氮化硅细粉及金属铝粉的试样的体积密度、常温耐压强度、抗热震性、烧后线变化率和荷重软化温度等性能检测指标明显优于未加入添加剂及复合结合剂的对比试样。
对比例1与上述实施例的对比，表明加入氮化硅细粉和金属铝粉后，可以使实施例制品的荷重软化温度提高50～130℃；对比例2与实施例的试样性能相差不大，说明采用镁铝尖晶石废砖或镁铝尖晶石的颗粒及粉料作为原料，只要配加合适的添加剂，产品的常温耐压强度和抗热震性都能达到使用要求；对比例3与实施例的对比，说明单纯采用镁铝尖晶石废砖原料，如果不配加合适的外加剂，则预制件的荷重软化温度只有1310℃，显然它已不适合在石灰回转窑内衬上使用。因此，本发明的原料配方及制备工艺具有独创性，在固体废物利用、降低生产成本等方面具有重要的实用价值。

Claims (2)

1.一种石灰回转窑用镁铝质预制件，其特征在于，采用如下原料制备得到：
组分 粒度 重量百分比含量
富镁镁铝尖晶石废砖 1～3mm 35～40%
富镁镁铝尖晶石废砖 0.088～1mm 18～25%
富镁镁铝尖晶石废砖粉 ≤0.088mm 30～35%
氮化硅细粉 ≤0.03mm 3～6%
金属铝粉 ≤0.246mm 0.05～1%
复合结合剂 / 4～6%
外加水 / 5～6%
其中，所述富镁镁铝尖晶石废砖是高温工业窑炉停炉大修或重建拆除的用后废品，所述富镁镁铝尖晶石废砖含重量百分比MgO：80～84%，Al2O3：10～12%，体积密度：2.85～2.95g/cm3；
所述氮化硅细粉重量百分比Si3N4含量≥96%；所述金属铝粉重量百分比活性Al含量≥98%；所述复合结合剂由重量百分比20～40%的硅微粉和重量百分比60～80%的铝酸盐水泥组成，硅微粉重量百分比SiO2含量≥93%，铝酸盐水泥重量百分比Al2O3含量≥68.75%。
2.如权利要求1所述的一种石灰回转窑用镁铝质预制件的制备方法，该方法包括以下步骤：
（1）将富镁镁铝尖晶石废砖去除表面残留物，经破碎处理后，再用3mm、1mm和0.088mm筛筛分后，制成粒度为1～3mm和0.088～1mm的颗粒，对于≤0.088mm的筛下物进行粉磨处理，制成粉磨原料；
（2） 按照权利要求1所述的重量百分比含量进行称量配料，经混合、成型、养护制得坯体，再经110℃×24小时烘干、750℃的预热处理和1650～1700℃高温热处理制得镁铝尖晶石预制件。
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