CN105503212B - 一种镁碳砖及其制备方法 - Google Patents

一种镁碳砖及其制备方法 Download PDF

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CN105503212B
CN105503212B CN201510967318.1A CN201510967318A CN105503212B CN 105503212 B CN105503212 B CN 105503212B CN 201510967318 A CN201510967318 A CN 201510967318A CN 105503212 B CN105503212 B CN 105503212B
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曹丽云
张雪松
俞晓东
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JIANGSU SUJIA GROUP NEW MATERIAL CO Ltd
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Abstract

本发明涉及一种镁碳砖及其制备方法，包括组分按重量百分数计为：电熔镁砂颗粒60～75%，电熔镁砂细粉10～30%，碳素5～10%，抗氧化剂1～5%，结合剂1～3%，糠醛废液0.4～1%，制备时首先将电熔镁砂颗粒放入混炼机中干混2～15min，然后加入酚醛树脂和糠醛废液继续混合5～15min，接着向其中加入碳素，混合5～15min，最后加入电熔镁砂细粉和抗氧化剂继续混合8～15min形成泥料，混炼机转速定为950～1000r/min，混炼时间为10～60min，经过压制成型和烘干固化后制得镁碳砖。本发明制备方法简单，步骤易于操作，改进了镁碳砖混料的均匀性，提高镁碳砖的混料质量，降低工人的劳动强度，减少酚醛树脂的使用量，糠醛废液的加入使得混料过程中更均匀防止酚醛树脂结团现象的发生。

Description

一种镁碳砖及其制备方法
技术领域
本发明涉及一种镁碳砖及其制备方法，属于耐火材料制备技术领域。
背景技术
自上世纪70年代末，把碳引入耐火材料中引起了以镁碳砖为代表的冶炼耐火材料的一次革命。由于充分发挥了石墨碳的超高熔点，高温高强度、低热膨胀率的优势。含碳耐火制品具有耐火度高、抗渣侵性能好、耐热震性强及高温蠕变小等优点,在炼钢高炉、电炉、转炉、精炼炉连铸系统上广泛得到应用,使用寿命大幅度提高。同时,由于含碳制品大部分不需高温烧成，节省能源，制作工艺简单,，因而被全世界许多国家迅速推广应用。
镁碳砖通常使用酚醛树脂结合，酚醛树脂结合剂由于粘度较大，在混料过程中容易产生泥团，而且会黏在混料机的碾头上，难以清理，既增加了工人的劳动强度，又影响了砖的配比和质量，且生产酚醛树脂的主要原料是煤和石油，越用越少。
糠醛废液是生产糠醛产生的废水，含有醋酸、糠醛以及醇类、醛类、酮类、酯类、有机酸类等多种有机物，根据色谱、质谱分析，有机物达40余种，其中以醋酸、糠醛为主。废水水样显透明状，显淡黄色度，pH值大约为2，COD10000～20000m g/L，BOD大约为2500～3000mg/L，B/C为0.2～0.25，废水中含有大量的乙酸、蚁酸等有机酸，可生化性差，属于高浓度有机酸性废水。糠醛废液的处理工艺比较复杂，对环境影响较大。
发明内容
本发明的目的是为了解决现有技术中镁碳砖中酚醛树脂在混合过程中容易产生泥团影响原料混匀的问题，提供了一种酚醛树脂用量较少的镁碳砖及其制备方法。
本发明采用如下技术方案：一种镁碳砖，包括组分按重量百分数计为：电熔镁砂颗粒60～75％，电熔镁砂细粉10～30％，碳素5～10％，抗氧化剂1～5％，结合剂1～3％，糠醛废液0.4～1％。
进一步的，所述碳素为石墨，石墨的粒度为350～400目，石墨中碳含量大于94％；
进一步的，所述电熔镁砂颗粒大小为1～5mm。
进一步的，所述电熔镁砂细粉的粒度为300～350目。
进一步的，所述抗氧化剂为铝粉、铝镁合金粉、金属硅粉、碳化硅或碳化硼中的一种或几种。
进一步的，所述结合剂为酚醛树脂。
镁碳砖的制备方法，包括如下步骤：
(1)混炼：采用旋移循环式混炼机进行混炼，按原料配比分别称取电熔镁砂颗粒、电熔镁砂细粉、碳素、抗氧化剂、结合剂和糠醛废液，首先将电熔镁砂颗粒放入混炼机中干混2～15min，然后加入酚醛树脂和糠醛废液继续混合5～15min，接着向其中加入碳素，混合5～15min，最后加入电熔镁砂细粉和抗氧化剂继续混合8～15min形成泥料，混炼机转速定为950～1000r/min，混炼时间为10～60min；
(2)压制成型：将混炼完成的泥料加入模具中采用复合式真空摩擦压砖机进行压制成型制成砖坯，压力为2500-6300KN；
(3)烘烤固化：将砖坯置于隧道式干燥窑中烘烤固化得到镁碳砖，烘烤温度为150～300℃，烘烤时间为10～20h。
通过选用电熔镁砂颗粒提高镁碳砖的耐高温性、抗渣侵蚀性；通过碳素保持镁碳砖的高温强度、抗热震性、抗渣渗透性；通过抗氧化剂保护碳素和非氧化物不被氧化；通过添加糠醛废液解决酚醛树脂结合剂由于粘度较大，在混料过程中容易产生泥团且会黏在混料机的碾头上难以清理的问题，减轻了工人的劳动强度，又保证了砖的配比和质量。
本发明制备方法简单，步骤易于操作，改进了镁碳砖混料的均匀性，提高镁碳砖的混料质量，降低工人的劳动强度，减少酚醛树脂的使用量，降低了成本，糠醛废液的加入使得混料过程中更均匀防止酚醛树脂结团现象的发生。
具体实施方式
下面将结合具体实施例对本发明作进一步的说明。
实施例一：一种镁碳砖，包括组分按重量百分数计为：电熔镁砂颗粒75％，电熔镁砂细粉14％，石墨7.2％，铝粉1％，酚醛树脂2.1％，糠醛废液0.7％。
镁碳砖的制备方法，包括如下步骤：
(1)混炼：采用旋移循环式混炼机进行混炼，按原料配比分别称取电熔镁砂颗粒、电熔镁砂细粉、石墨、铝粉、酚醛树脂和糠醛废液，首先将电熔镁砂颗粒放入混炼机中干混5min，然后加入酚醛树脂和糠醛废液继续混合5min，接着向其中加入石墨，混合8min，最后加入电熔镁砂细粉和铝粉继续混合10min形成泥料，混炼机转速定为970r/min；
(2)压制成型：将混炼完成的泥料加入模具中采用复合式真空摩擦压砖机进行压制成型制成砖坯，压力为3000KN；
(3)烘烤固化：将砖坯置于隧道式干燥窑中烘烤固化，烘烤温度为200℃，烘烤时间为15h。
实施例二：一种镁碳砖，包括组分按重量百分数计为：电熔镁砂颗粒70％，电熔镁砂细粉20％，石墨5％，铝镁合金粉2％，酚醛树脂2.5％，糠醛废液0.5％。
镁碳砖的制备方法，包括如下步骤：
(1)混炼：采用旋移循环式混炼机进行混炼，按原料配比分别称取电熔镁砂颗粒、电熔镁砂细粉、石墨、铝镁合金粉、酚醛树脂和糠醛废液，首先将电熔镁砂颗粒放入混炼机中干混8min，然后加入酚醛树脂和糠醛废液继续混合10min，接着向其中加入石墨，混合10min，最后加入电熔镁砂细粉和铝镁合金粉继续混合12min形成泥料，混炼机转速定为980r/min；
(2)压制成型：将混炼完成的泥料加入模具中采用复合式真空摩擦压砖机进行压制成型制成砖坯，压力为3500KN；
(3)烘烤固化：将砖坯置于隧道式干燥窑中烘烤固化，烘烤温度为200℃，烘烤时间为20h。
实施例三：一种镁碳砖，包括组分按重量百分数计为：电熔镁砂颗粒65％，电熔镁砂细粉20％，石墨8％，金属硅粉4.2％，酚醛树脂2.4％，糠醛废液0.4％。
镁碳砖的制备方法，包括如下步骤：
(1)混炼：采用旋移循环式混炼机进行混炼，按原料配比分别称取电熔镁砂颗粒、电熔镁砂细粉、碳素、金属硅粉、酚醛树脂和糠醛废液，首先将电熔镁砂颗粒放入混炼机中干混10min，然后加入酚醛树脂和糠醛废液继续混合8min，接着向其中加入石墨，混合12min，最后加入电熔镁砂细粉和金属硅粉继续混合12min形成泥料，混炼机转速定为970r/min；
(2)压制成型：将混炼完成的泥料加入模具中采用复合式真空摩擦压砖机进行压制成型制成砖坯，压力为4000KN；
(3)烘烤固化：将砖坯置于隧道式干燥窑中烘烤固化，烘烤温度为250℃，烘烤时间为15h。
实施例四：一种镁碳砖，包括组分按重量百分数计为：电熔镁砂颗粒60，电熔镁砂细粉30％，石墨5％，碳化硅和碳化硼3％，酚醛树脂1％，糠醛废液1％。
镁碳砖的制备方法，包括如下步骤：
(1)混炼：采用旋移循环式混炼机进行混炼，按原料配比分别称取电熔镁砂颗粒、电熔镁砂细粉、石墨、碳化硅和碳化硼、酚醛树脂和糠醛废液，首先将电熔镁砂颗粒放入混炼机中干混2min，然后加入酚醛树脂和糠醛废液继续混合15min，接着向其中加入石墨，混合5min，最后加入电熔镁砂细粉和碳化硅、碳化硼继续混合15min形成泥料，混炼机转速定为950r/min，混炼时间为60min；
(2)压制成型：将混炼完成的泥料加入模具中采用复合式真空摩擦压砖机进行压制成型制成砖坯，压力为2500KN；
(3)烘烤固化：将砖坯置于隧道式干燥窑中烘烤固化，烘烤温度为150℃，烘烤时间为20h。
实施例五：一种镁碳砖，包括组分按重量百分数计为：电熔镁砂颗粒75％，电熔镁砂细粉10％，石墨6.6％，碳化硼5％，酚醛树脂3％，糠醛废液0.4％。
镁碳砖的制备方法，包括如下步骤：
(1)混炼：采用旋移循环式混炼机进行混炼，按原料配比分别称取电熔镁砂颗粒、电熔镁砂细粉、石墨、碳化硼、酚醛树脂和糠醛废液，首先将电熔镁砂颗粒放入混炼机中干混15min，然后加入酚醛树脂和糠醛废液继续混合5min，接着向其中加入石墨，混合15min，最后加入电熔镁砂细粉和碳化硼继续混合8min形成泥料，混炼机转速定为1000r/min，混炼时间为10min；
(2)压制成型：将混炼完成的泥料加入模具中采用复合式真空摩擦压砖机进行压制成型制成砖坯，压力为6300KN；
(3)烘烤固化：将砖坯置于隧道式干燥窑中烘烤固化，烘烤温度为300℃，烘烤时间为10h。
对比例：与实例一中原料组分相同，将其中糠醛废液用酚醛树脂替换，按同样的制备方法制成不含糠醛废液的镁碳砖。
参照GB/T2997---2000、GB/T5072.2---2004、GB/T3001---2000、GB/T3002---2004、GB/T 7320.1-2000检测对比例与实施例一制备的镁碳砖各项性能，包括显气孔率和体积密度、常温耐压强度、常温抗折强度、高温抗折强度和线膨胀率。
抗热震性试验：将实施例一和对比例中制备的镁碳砖进行抗热震性试验，制成40mm×40mm×160mm的试样，将试样加热到1100℃保温30min后，取出试样迅速放入室温水中急冷，重复以上过程至试样断裂，记录重复次数，以次数评价试样的抗热震性。
抗侵蚀性试验：将实施例一和对比例中制备的镁碳砖进行抗侵蚀性试验，制成坩埚试样尺寸内孔尺寸为采用静态抗侵蚀试验法，在坩埚试样内装填20g钢包渣，置于埋炭气氛下，于1500℃下保温3h，随炉冷却后将坩埚沿高度方向切开，测量坩埚中心截面的侵(渗透)面积S，计算其侵蚀指数S/S0×100％(S0为原坩埚中心孔的截面积)，以评价试样的抗侵蚀性。
各检测数据如下表1：
表1
项目 实施例一 对比例
体积密度(g/cm3) 3.11 3.11
显气孔率(％) 2.2 2.1
常温抗折强度(MPa) 9.24 9.02
常温耐压强度(MPa) 61.2 60.8
高温抗折强度(MPa) 8.04 7.84
抗热震性(次) 5 5
抗侵蚀指数(％) 11 12
线膨胀率(％) 0.12 0.13
由表1可知，同样条件下实施例一种添加糠醛废液的镁碳砖和对比例中不含糠醛废液的镁碳砖各项性能均相近，因此添加糠醛废液不会降低原有镁碳砖的抗热震性以及常温下的耐压和抗折强度等性能，添加糠醛废液能够降本增益。

Claims (1)

1.一种镁碳砖，其特征在于：包括组分按重量百分数计为：电熔镁砂颗粒60～75%，电熔镁砂细粉10～30%，碳素5～10%，抗氧化剂1～5%，结合剂1～3%，糠醛废液0.4～1%；所述碳素为石墨，石墨的粒度为350～400目，石墨中碳含量大于94%；所述电熔镁砂颗粒大小为1～5mm；所述电熔镁砂细粉的粒度为300～350目；所述抗氧化剂为铝粉、铝镁合金粉、金属硅粉、碳化硅或碳化硼中的一种或几种；所述结合剂为酚醛树脂；
制备方法包括如下步骤：
（1）混炼：采用旋移循环式混炼机进行混炼，按原料配比分别称取电熔镁砂颗粒、电熔镁砂细粉、碳素、抗氧化剂、结合剂和糠醛废液，首先将电熔镁砂颗粒放入混炼机中干混2～15min，然后加入酚醛树脂和糠醛废液继续混合5～15min，接着向其中加入碳素，混合5～15min，最后加入电熔镁砂细粉和抗氧化剂继续混合8～15min形成泥料，混炼机转速定为950～1000r/min，混炼时间为10～60min；
（2）压制成型：将混炼完成的泥料加入模具中采用复合式真空摩擦压砖机进行压制成型制成砖坯，压力为2500-6300KN；
（3）烘烤固化：将砖坯置于隧道式干燥窑中烘烤固化得到镁碳砖，烘烤温度为150～300℃，烘烤时间为10～20h。
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