CN108083830A - 一种焦炉和热风炉专用导热硅砖及其制备方法 - Google Patents
一种焦炉和热风炉专用导热硅砖及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种焦炉和热风炉专用导热硅砖及其制备方法,属于导热材料技术领域。本发明将硅石,氧化铁,氧化钙,铝粉,电石,石墨,木质素磺酸钙球磨搅拌,过筛,得混合粉末;将所得混合粉末,石灰乳,改性炭化椰壳纤维湿碾压混练,压制成型,得湿砖坯;将所得湿砖坯真空冷冻干燥,得干燥砖坯;将所得干燥砖坯充氮高温烧结,降温,得预处理导热硅砖;将所得预处理导热硅砖充氧高温烧结,降温,即得焦炉和热风炉专用导热硅砖。本发明提供的焦炉和热风炉专用导热硅砖具有优异的导热性能,抗热震性和高温强度。
Description
技术领域
本发明公开了一种焦炉和热风炉专用导热硅砖及其制备方法,属于导热材料技术领域。
背景技术
硅砖是最常见的硅石耐火材料,具有很长的应用历史,因其具有较高的高温强度和荷重软化温度,较好的高温性能及较强的抗酸性渣侵蚀能力等优良的性能,在工业生产中广泛应用,主要用于焦炉、玻璃熔窑和大型高炉的热风炉的耐火材料。生产硅砖的主要原料为硅石、矿化剂(如石灰和赤铁矿)和结合剂。后者使砖坯在成型后达到需要的强度。对硅砖进行烧成时矿化剂促进石英发生转化。
硅砖作为焦炉和热风炉的耐火材料,在烧成过程中所受环境温度急剧变化的作用,称之为热冲击(或称热震)。在热冲击下,硅砖内部产生热应力,当其值达到制品的强度极限值时,制品即开裂或断裂。硅砖是非均质的脆性材料,由于其比金属制品的热膨胀率大、导热率和弹性小以及抗张强度低等,故在烧成过程中易出现裂纹且在热冲击作用下不断扩展,最终发生断裂。硅砖在烧成时,由于晶形转变则产生较大的体积膨胀,尤其易产生裂纹甚至开裂。
近年来,随着焦炉均向大型化发展,对焦炉硅砖的质量技术要求也更严格苛刻。如要求炭化室等部位所用硅砖应残余石英少、具有更高的致密度、导热性、高温强度及抗热震性能,由此可增加硅砖墙体的强度与传热能力,减薄燃烧室与焦化室的隔墙,缩短结焦时间提高焦炉的焦炭生产效率。因此,开发应用一种具有高致密度、高导热性、高温强度及抗热震性能良好的硅质耐火材料,成为焦炉耐火材料研究与生产领域的重要课题。
因此,如何改善传统硅砖导热性能及抗热震性能不佳,高温强度低的缺点,以获取更高综合性能的硅砖,是其推广与应用于更广阔的领域,满足工业生产需求亟待解决的问题。
发明内容
本发明主要解决的技术问题是:针对传统硅砖导热性能及抗热震性能不佳,高温强度低的缺点,提供了一种焦炉和热风炉专用导热硅砖及其制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
一种焦炉和热风炉专用导热硅砖,是由以下重量份数的原料组成:30~40份硅石,10~20份石灰乳,5~8份氧化铁,5~8份铝粉,2~3份电石,5~8份氧化钙,10~20份改性炭化椰壳纤维,5~8份石墨,5~8份木质素磺酸钙;
所述焦炉和热风炉专用导热硅砖的制备步骤为:
(1)按原料组成称量各原料;
(2)将硅石,氧化铁,氧化钙,铝粉,电石,石墨,木质素磺酸钙球磨搅拌,过筛,得混合粉末;
(3)将上述所得混合粉末,石灰乳,改性炭化椰壳纤维湿碾压混练,压制成型,得湿砖坯;
(4)将上述所得湿砖坯真空冷冻干燥,得干燥砖坯;
(5)将上述所得干燥砖坯充氮高温烧结,得预处理导热硅砖;
(6)将上述所得预处理导热硅砖充氧高温烧结,降温,即得焦炉和热风炉专用导热硅砖。
所述改性炭化椰壳纤维的制备过程为:将椰壳纤维充氮保温炭化,降温,得炭化椰壳纤维;将炭化椰壳纤维与酪素溶液按质量比1:50~1:100搅拌混合,浸泡,过滤,得预处理炭化椰壳纤维;按重量份数计,将10~20份预处理炭化椰壳纤维,20~30份氟化钠溶液和5~6份纳米铁粉搅拌混合,浸渍,减压蒸馏,即得改性炭化椰壳纤维。
步骤(2)所述过筛为过80~100目的筛。
步骤(5)所述充氮的速率为60~90mL/min;所述高温烧结温度为1400~1600℃。
步骤(6)所述充氧速率为10~20mL/min;所述高温烧结温度为1300~1500℃。
本发明的有益效果是:
(1)本发明通过添加改性炭化椰壳纤维,在充氮高温烧结过程中,首先,硅石熔融渗透进改性炭化椰壳纤维中,在高温、氟化钠和纳米铁粉的催化条件下,硅石中二氧化硅与改性炭化椰壳纤维中炭发生反应,生成坚硬的碳化硅,生成的碳化硅形成坚硬的碳化硅纤维骨架,碳化硅纤维骨架错综穿插在体系中,一方面,增强体系的抗热震性和高温强度,另一方面,碳化硅起到良好的导热性能,同时,体系中的石墨与二氧化硅,在充氮高温条件下反应,生成坚硬的氮化硅填料,填充在体系中,进一步增强体系的导热性能,抗热震性和高温强度;
(2)本发明通过添加氧化铁,铝粉和电石,在充氧高温烧结过程中,首先,电石在高温条件下遇到体系中产生的水分反应生成乙炔,乙炔燃烧,引发氧化铁和铝粉发生反应,生成氧化铝和铁,一方面,氧化铝和铁的生成,增强体系的导热性能,抗热震性和高温强度,另一方面,改性炭化椰壳纤维中未反应的炭在高温充氧的条件下,反应生成气体消耗殆尽,在体系中形成孔隙结构,生成的铁在高温条件下融化,将体系中形成孔隙填充,在使用过程中,承受急剧温度变化时,体系中的铁反复的膨胀和收缩可排除填充在体系中的杂质,减少残留夹杂物的尺寸,从而使其成分趋于均匀,组织趋于致密,细化晶粒,改善体系的性能,进一步增强导热硅砖的抗热震性和高温强度。
具体实施方式
将椰壳纤维置于炭化炉中,并以60~90mL/min速率向炉内通入氮气,于温度为550~650℃条件下,于氮气保护条件下,保温炭化2~3h,随炉降至室温,得炭化椰壳纤维;将炭化椰壳纤维与质量浓度为3~8g/L酪素溶液按质量比1:50~1:100加入烧杯中,再将烧杯移至数显测速恒温磁力搅拌器中,于温度为30~40℃,转速为300~400r/min条件下,加热搅拌混合40~60min,停止搅拌,保温静置浸泡1~2h,得浸泡液,随后将浸泡液过滤,得预处理炭化椰壳纤维;按重量份数计,将10~20份预处理炭化椰壳纤维,20~30份质量分数为8~10%的氟化钠溶液和5~6份纳米铁粉加入单口烧瓶中,于转速为200~300r/min条件下,搅拌混合20~30min后,静置浸渍1~2h,得浸渍液,将浸渍液移至旋转蒸发仪中,于温度为80~100℃,转速为80~100r/min,压力为200~300kPa条件下,减压蒸馏30~40min,得改性炭化椰壳纤维;按重量份数计,依次取30~40份硅石,10~20份石灰乳,5~8份氧化铁,5~8份铝粉,2~3份电石,5~8份氧化钙,10~20份改性炭化椰壳纤维,5~8份石墨,5~8份木质素磺酸钙,先将硅石,氧化铁,氧化钙,铝粉,电石,石墨,木质素磺酸钙置于球磨机中,于转速为500~600r/min条件下,球磨混合40~60min后,过80~100目的筛,得混合粉末;将所得混合粉末,石灰乳,改性炭化椰壳纤维加入湿碾机中,湿碾压混练20~30min,并压制成型,得湿砖坯;将所得湿砖坯真空冷冻干燥,干燥18~24h,得干燥砖坯;将所得干燥砖坯置于隧道窑中,并以60~90mL/min速率向窑内通入氮气,于温度为1400~1600℃条件下,于氮气保护条件下,高温烧结3~4h后,停止通入氮气,并以10~20mL/min速率向窑内通入氧气,待窑内温度自然降温至1300~1500℃后,于氧气氛围下,保温烧结5~6h,随炉降至室温,即得焦炉和热风炉专用导热硅砖。
实例1
将椰壳纤维置于炭化炉中,并以90mL/min速率向炉内通入氮气,于温度为650℃条件下,于氮气保护条件下,保温炭化3h,随炉降至室温,得炭化椰壳纤维;将炭化椰壳纤维与质量浓度为8g/L酪素溶液按质量比1:100加入烧杯中,再将烧杯移至数显测速恒温磁力搅拌器中,于温度为40℃,转速为400r/min条件下,加热搅拌混合60min,停止搅拌,保温静置浸泡2h,得浸泡液,随后将浸泡液过滤,得预处理炭化椰壳纤维;按重量份数计,将20份预处理炭化椰壳纤维,30份质量分数为10%的氟化钠溶液和6份纳米铁粉加入单口烧瓶中,于转速为300r/min条件下,搅拌混合30min后,静置浸渍2h,得浸渍液,将浸渍液移至旋转蒸发仪中,于温度为100℃,转速为100r/min,压力为300kPa条件下,减压蒸馏40min,得改性炭化椰壳纤维;按重量份数计,依次取40份硅石,20份石灰乳,8份氧化铁,8份铝粉,3份电石,8份氧化钙,20份改性炭化椰壳纤维,8份石墨,8份木质素磺酸钙,先将硅石,氧化铁,氧化钙,铝粉,电石,石墨,木质素磺酸钙置于球磨机中,于转速为600r/min条件下,球磨混合60min后,过100目的筛,得混合粉末;将所得混合粉末,石灰乳,改性炭化椰壳纤维加入湿碾机中,湿碾压混练30min,并压制成型,得湿砖坯;将所得湿砖坯真空冷冻干燥,干燥24h,得干燥砖坯;将所得干燥砖坯置于隧道窑中,并以90mL/min速率向窑内通入氮气,于温度1600℃条件下,于氮气保护条件下,高温烧结4h后,停止通入氮气,并以20mL/min速率向窑内通入氧气,待窑内温度自然降温至1500℃后,于氧气氛围下,保温烧结6h,随炉降至室温,即得焦炉和热风炉专用导热硅砖。
实例2
按重量份数计,依次取40份硅石,20份石灰乳,8份氧化铁,8份铝粉,3份电石,8份氧化钙,20份椰壳纤维,8份石墨,8份木质素磺酸钙,先将硅石,氧化铁,氧化钙,铝粉,电石,石墨,木质素磺酸钙置于球磨机中,于转速为600r/min条件下,球磨混合60min后,过100目的筛,得混合粉末;将所得混合粉末,石灰乳,椰壳纤维加入湿碾机中,湿碾压混练30min,并压制成型,得湿砖坯;将所得湿砖坯真空冷冻干燥,干燥24h,得干燥砖坯;将所得干燥砖坯置于隧道窑中,并以90mL/min速率向窑内通入氮气,于温度1600℃条件下,于氮气保护条件下,高温烧结4h后,停止通入氮气,并以20mL/min速率向窑内通入氧气,待窑内温度自然降温至1500℃后,于氧气氛围下,保温烧结6h,随炉降至室温,即得焦炉和热风炉专用导热硅砖。
实例3
将椰壳纤维置于炭化炉中,并以90mL/min速率向炉内通入氮气,于温度为650℃条件下,于氮气保护条件下,保温炭化3h,随炉降至室温,得炭化椰壳纤维;将炭化椰壳纤维与质量浓度为8g/L酪素溶液按质量比1:100加入烧杯中,再将烧杯移至数显测速恒温磁力搅拌器中,于温度为40℃,转速为400r/min条件下,加热搅拌混合60min,停止搅拌,保温静置浸泡2h,得浸泡液,随后将浸泡液过滤,得预处理炭化椰壳纤维;按重量份数计,将20份预处理炭化椰壳纤维,30份质量分数为10%的氟化钠溶液和6份纳米铁粉加入单口烧瓶中,于转速为300r/min条件下,搅拌混合30min后,静置浸渍2h,得浸渍液,将浸渍液移至旋转蒸发仪中,于温度为100℃,转速为100r/min,压力为300kPa条件下,减压蒸馏40min,得改性炭化椰壳纤维;按重量份数计,依次取40份硅石,20份石灰乳,8份氧化钙,20份改性炭化椰壳纤维,8份石墨,8份木质素磺酸钙,先将硅石,氧化钙,石墨,木质素磺酸钙置于球磨机中,于转速为600r/min条件下,球磨混合60min后,过100目的筛,得混合粉末;将所得混合粉末,石灰乳,改性炭化椰壳纤维加入湿碾机中,湿碾压混练30min,并压制成型,得湿砖坯;将所得湿砖坯真空冷冻干燥,干燥24h,得干燥砖坯;将所得干燥砖坯置于隧道窑中,并以90mL/min速率向窑内通入氮气,于温度1600℃条件下,于氮气保护条件下,高温烧结4h后,停止通入氮气,并以20mL/min速率向窑内通入氧气,待窑内温度自然降温至1500℃后,于氧气氛围下,保温烧结6h,随炉降至室温,即得焦炉和热风炉专用导热硅砖。
对比例:河北某材料科技有限公司生产的硅砖。
将实例1至3所得的焦炉和热风炉专用导热硅砖及对比例产品进行性能检测,具体检测方法如下:
1.导热性能:按照GB/T2608检测试件导热系数;
2.抗热震性:按照GB/T2608检测试件1000℃热膨胀率;
3.高温强度:按照GB/T2608检测试件1000℃抗弯强度;
具体检测结果如表1所示:
表1
检测项目 | 实例1 | 实例2 | 实例3 | 对比例 |
导热系数(W/(m·K)) | 0.815 | 0.547 | 0.671 | 0.232 |
热膨胀率(1000℃)/% | 1.21 | 1.25 | 1.29 | 1.36 |
抗弯强度(1000℃)/MPa | 2.5 | 2.1 | 1.9 | 0.5 |
由表1检测结果可知,本发明技术方案制备的焦炉和热风炉专用导热硅砖具有优异的导热性能及抗热震性的特点,同时,其高温强度也显著提高,在导热材料行业的发展中具有广阔的前景。
Claims (5)
1.一种焦炉和热风炉专用导热硅砖,其特征在于:是由以下重量份数的原料组成:30~40份硅石,10~20份石灰乳,5~8份氧化铁,5~8份铝粉,2~3份电石,5~8份氧化钙,10~20份改性炭化椰壳纤维,5~8份石墨,5~8份木质素磺酸钙;
所述焦炉和热风炉专用导热硅砖的制备步骤为:
(1)按原料组成称量各原料;
(2)将硅石,氧化铁,氧化钙,铝粉,电石,石墨,木质素磺酸钙球磨搅拌,过筛,得混合粉末;
(3)将上述所得混合粉末,石灰乳,改性炭化椰壳纤维湿碾压混练,压制成型,得湿砖坯;
(4)将上述所得湿砖坯真空冷冻干燥,得干燥砖坯;
(5)将上述所得干燥砖坯充氮高温烧结,得预处理导热硅砖;
(6)将上述所得预处理导热硅砖充氧高温烧结,降温,即得焦炉和热风炉专用导热硅砖。
2.根据权利要求1所述一种焦炉和热风炉专用导热硅砖,其特征在于:所述改性炭化椰壳纤维的制备过程为:将椰壳纤维充氮保温炭化,降温,得炭化椰壳纤维;将炭化椰壳纤维与酪素溶液按质量比1:50~1:100搅拌混合,浸泡,过滤,得预处理炭化椰壳纤维;按重量份数计,将10~20份预处理炭化椰壳纤维,20~30份氟化钠溶液和5~6份纳米铁粉搅拌混合,浸渍,减压蒸馏,即得改性炭化椰壳纤维。
3.根据权利要求1所述一种焦炉和热风炉专用导热硅砖,其特征在于:步骤(2)所述过筛为过80~100目的筛。
4.根据权利要求1所述一种焦炉和热风炉专用导热硅砖,其特征在于:步骤(5)所述充氮的速率为60~90mL/min;所述高温烧结温度为1400~1600℃。
5.根据权利要求1所述一种焦炉和热风炉专用导热硅砖,其特征在于:步骤(6)所述充氧速率为10~20mL/min;所述高温烧结温度为1300~1500℃。
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