CN111099905B - 一种高铝耐火砖及其制备方法 - Google Patents
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Abstract
本发明涉及一种高铝耐火砖及其制备方法,属于建筑材料技术领域。在本发明技术方案中,通过在单分散聚苯乙烯微球表面填充致密玻璃转化层,通过由于玻璃料与粘土在熔烧过程中形成复杂的釉瓷,进一步提高材料的结构性能,改善材料的耐火强度,同时采用高铝矾土材料为主要基材,经高温煅烧后,高铝矾土微粉在高温条件下充填于砖体孔隙中,促进烧结,能够有效提高砖体的力学强度、耐高温性和持久使用性有效耐火并提高材料的力学性能。
Description
技术领域
本发明涉及一种高铝耐火砖及其制备方法,属于建筑材料技术领域。
背景技术
高温窑炉或高温设备的内衬、绝热层等部位主要采用高铝耐火材料,这些高温设备有间歇和连续式两大类运行方式。在连续性运行的设备中,连续的热流通过围护结构向外传递,最终散发到大气或大地中为热损失的主要方式。围护结构中材料的导热系数λ与设备的热损失成正比。因此这类设备应以高铝耐火材料的λ趋向于0最终追求目标。在间歇式或短期运行的热工设备中,设备的热损失既与围护材料的导热系数有关,也与内衬材料本身的比热容有关。轻质高铝耐火耐火材料是晶相、非晶相等固相和气相组成的多相体系,高铝耐火材料导热是通过晶体点阵或晶格振动和气相导热完成。由于晶格振动的能量是量子化的,通常把晶格振动的“量子”称为声子。声子的传递与固体的结构有关,由于声子在晶格系的每个干扰处都会发生碰撞造成散射,从而使材料的导热率下降。从单晶体到多晶体,从多晶固体到多孔固体,导热率逐步下降1个到2个数量级。除声子导热外,高铝耐火耐火材料还通过辐射进行能量传递。低温时,因这部分能量微乎其微,可以忽略不计,但高温时,这部分辐射能就大了,辐射能E与温度T的四次方成正比[8-9],必须加以考虑。在高铝耐火耐火材料中,气相占有很大比例(>50%),通常气相以气孔的方式存在,气孔里的温差对形成热传递的可能性大多数是很少的,即使直径在5mm以下的气孔也几乎不能形成气流。
高铝耐火材料内部热传递大多排除对流这一形式。高铝耐火砖是一种轻质、高强、低导热率的材料,与致密材料相比具有低密度、低导热率、保温性能优良等特点。与普通高铝耐火材料相比具有强度高、使用温度高等特点,不但可以做高铝耐火层,也可以与火焰直接接触,是轻型高温窑炉理想的内衬材料。由于其原材料丰富、价格相对低廉,被广泛应用于各种烧成窑、加热装置、均热炉的高铝耐火层和内衬,增加了窑炉的蓄热效果与减轻了窑炉的重量,但是现有的高铝耐火砖材料性能不佳,特别是力学性能受到材料内部结构的影响,导致其性能降低,使用时效性较差,所以对其进行有效的改进很有必要。
发明内容
本发明的目的在于提供一种高铝耐火砖及其制备方法,以解决现有技术中的问题。
为实现上述目的,本发明提供如下技术方案:
一种高铝耐火砖,由下列重量份物质组成:
45~50份高铝矾土分散粉末;
10~15份磷酸溶液;
6~8份单分散聚苯乙烯颗粒;
15~20份分散浆液;
所述分散浆液是由二氧化硅、氧化铝、氧化铁、生石灰、氧化镁、氧化钾和氧化钠,经高温熔融后水淬处理,研磨并与聚乙烯醇溶液混合制备而成。
所述高铝矾土分散粉末粒径为500目。
所述磷酸溶液浓度优选为质量分数50%。
一种高铝耐火砖的制备方法具体制备步骤为:
S1、按重量份数计,分别称量45~50份质量分数60%乙醇、3~5份苯乙烯单体、0.1~0.2份过硫酸钾和0.1~0.2份亚硫酸钠置于三口烧瓶中,搅拌混合并通氮气排除空气,待通入完成后,搅拌混合并保温反应,静置冷却至室温并收集反应液,按质量比1:1,将反应液与无水乙醇搅拌混合并离心分离,收集下层沉淀并干燥6~8h,得单分散聚苯乙烯颗粒;本发明技术方案采用沉淀聚合的方法,以乙醇溶液为反应介质,过硫酸钾和亚硫酸钠为引发剂制备得到单分散聚苯乙烯微球,由于本反应体系在反应初始阶段并不是均一的溶液,形成了单体小液滴,聚苯乙烯微球在单体小液滴中成核与生长,有效形成单分散性能的微球颗粒;
S2、按重量份数计,分别称量45~50份二氧化硅、10~15份氧化铝、0.1~0.2份氧化铁、20~30份生石灰、5~8份氧化镁、1~2份氧化钾和1~2份氧化钠置于刚玉坩埚中,搅拌混合并加热熔融,程序升温并收集熔融液水淬冷却,收集冷却物并置于球磨机中球磨处理,过500目筛并收集过筛颗粒,按质量比1:5,将过筛颗粒与质量份数10%聚乙烯醇溶液搅拌混合并超声分散,收集得分散浆液;由于玻璃料与粘土在熔烧过程中形成复杂的釉瓷,其熔体流动性好,形成涂层后具有十分光滑致密的表面,无连通气孔,因而具有十分优异的耐腐蚀和抗氧化性能,同时难熔氧化物微细颗粒对瓷釉起到强化和锚固作用,改善了玻璃质瓷釉的耐热性、抗热震性,由于釉浆涂层是通过高温熔烧而成的,在熔烧过程中玻璃质的熔体与工件基体表面产生了良好的润湿和化学结合,涂层附着牢固,填充材料内部的同时,有效密实材料的内部结构,进一步提高材料的结构性能,改善材料的耐火强度;
S3、取高铝矾土并研磨分散,过500目筛并收集分散粉末,得高铝矾土分散粉末;
S4、按重量份数计,分别称量45~50份高铝矾土分散粉末、10~15份质量分数50%磷酸溶液、15~20份分散浆液和6~8份单分散聚苯乙烯颗粒置于搅拌机中,搅拌混合并收集混合浆液,将混合浆液浇注至模具中压制成型并保温干燥,升温加热并保温烧制,静置冷却至室温,得高铝耐火砖。通过玻璃料与粘土在熔烧过程中形成复杂的釉瓷粘结成一定形状的固体,即保留在内部空隙中,形成核壳结构,核壳结构高铝质耐火砖通过致密层与火焰接触,充分利用其致密耐火的特点形成耐火屏障,利用球形空隙内叠套的酥松的耐火固态颗粒,有效减少热射线的传输的平均自由程,使大部分热量能够保留在核壳结构中,有效耐火并提高材料的力学性能。
所述氮气通入速率为25~30mL/min。
步骤S2所述程序升温为按5℃/min升温至1300~1500℃。
步骤S4所述压制成型压力为5~10MPa。
步骤S4所述升温加热并保温烧制为按10℃/min升温至1000~1100℃,保温烧制1~2h。
与现有技术相比,本发明的有益效果是:(1)本发明技术方案采用沉淀聚合的方法,以乙醇溶液为反应介质,过硫酸钾和亚硫酸钠为引发剂制备得到单分散聚苯乙烯微球,由于本反应体系在反应初始阶段并不是均一的溶液,形成了单体小液滴,聚苯乙烯微球在单体小液滴中成核与生长,有效形成单分散性能的微球颗粒,通过以聚苯乙烯分散颗粒为主要材料,通过对其表面填充致密玻璃转化层,通过由于玻璃料与粘土在熔烧过程中形成复杂的釉瓷,其熔体流动性好,形成涂层后具有十分光滑致密的表面,无连通气孔,因而具有十分优异的耐腐蚀和抗氧化性能,同时难熔氧化物微细颗粒对瓷釉起到强化和锚固作用,改善了玻璃质瓷釉的耐热性、抗热震性,由于釉浆涂层是通过高温熔烧而成的,在熔烧过程中玻璃质的熔体与工件基体表面产生了良好的润湿和化学结合,涂层附着牢固,填充材料内部的同时,有效密实材料的内部结构,进一步提高材料的结构性能,改善材料的耐火强度;
(2)本发明技术方案采用高铝矾土材料为主要基材,经高温煅烧后,高铝矾土微粉在高温条件下充填于砖体孔隙中,促进烧结,能够有效提高砖体的力学强度、耐高温性和持久使用性,同时通过填充的聚苯乙烯微球材料在升温时,被浆料浸渍后的聚苯乙烯微球材料在高温环境下明显收缩并持续炭化分解,这样在高铝砖内部形成孔隙,覆着在微球表面的浆料颗粒随温度升高逐渐脱水,通过玻璃料与粘土在熔烧过程中形成复杂的釉瓷粘结成一定形状的固体,即保留在内部空隙中,形成核壳结构,核壳结构高铝质耐火砖通过致密层与火焰接触,充分利用其致密耐火的特点形成耐火屏障,利用球形空隙内叠套的酥松的耐火固态颗粒,有效减少热射线的传输的平均自由程,使大部分热量能够保留在核壳结构中,有效耐火并提高材料的力学性能。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
按重量份数计,分别称量45~50份质量分数60%乙醇、3~5份苯乙烯单体、0.1~0.2份过硫酸钾和0.1~0.2份亚硫酸钠置于三口烧瓶中,搅拌混合并通氮气排除空气,控制氮气通入速率为25~30mL/min,待通入完成后,搅拌混合并置于75~80℃下保温反应10~12h,静置冷却至室温并收集反应液,按质量比1:1,将反应液与无水乙醇搅拌混合并离心分离,收集下层沉淀并置于45~50℃烘箱中,干燥6~8h,得单分散聚苯乙烯颗粒;按重量份数计,分别称量45~50份二氧化硅、10~15份氧化铝、0.1~0.2份氧化铁、20~30份生石灰、5~8份氧化镁、1~2份氧化钾和1~2份氧化钠置于刚玉坩埚中,搅拌混合并加热熔融,按5℃/min升温至1300~1500℃保温熔融2~3h,收集熔融液并水淬冷却,收集冷却物并置于球磨机中球磨处理1~2h,过500目筛并收集过筛颗粒,按质量比1:5,将过筛颗粒与质量份数10%聚乙烯醇溶液搅拌混合并置于200~300W下超声分散10~15min,收集得分散浆液;取高铝矾土并研磨分散,过500目筛并收集高铝矾土分散粉末,再按重量份数计,分别称量45~50份高铝矾土分散粉末、10~15份质量分数50%磷酸溶液、15~20份分散浆液和6~8份单分散聚苯乙烯颗粒置于搅拌机中,搅拌混合并收集混合浆液,将混合浆液浇注至模具中压制成型并置于100~110℃下保温干燥1~2h后,再按10℃/min升温至1000~1100℃,保温烧制1~2h后,静置冷却至室温,得高铝耐火砖。
实施例1
按重量份数计,分别称量45份质量分数60%乙醇、3份苯乙烯单体、0.1份过硫酸钾和0.1份亚硫酸钠置于三口烧瓶中,搅拌混合并通氮气排除空气,控制氮气通入速率为25mL/min,待通入完成后,搅拌混合并置于75℃下保温反应10h,静置冷却至室温并收集反应液,按质量比1:1,将反应液与无水乙醇搅拌混合并离心分离,收集下层沉淀并置于45℃烘箱中,干燥6h,得单分散聚苯乙烯颗粒;按重量份数计,分别称量45份二氧化硅、10份氧化铝、0.1份氧化铁、20份生石灰、5份氧化镁、1份氧化钾和1份氧化钠置于刚玉坩埚中,搅拌混合并加热熔融,按5℃/min升温至1300℃保温熔融2h,收集熔融液并水淬冷却,收集冷却物并置于球磨机中球磨处理1h,过500目筛并收集过筛颗粒,按质量比1:5,将过筛颗粒与质量份数10%聚乙烯醇溶液搅拌混合并置于200W下超声分散10min,收集得分散浆液;取高铝矾土并研磨分散,过500目筛并收集高铝矾土分散粉末,再按重量份数计,分别称量45份高铝矾土分散粉末、10份质量分数50%磷酸溶液、15份分散浆液和6份单分散聚苯乙烯颗粒置于搅拌机中,搅拌混合并收集混合浆液,将混合浆液浇注至模具中压制成型并置于100℃下保温干燥1h后,再按10℃/min升温至1000℃,保温烧制1h后,静置冷却至室温,得高铝耐火砖。
实施例2
按重量份数计,分别称量47份质量分数60%乙醇、4份苯乙烯单体、0.1份过硫酸钾和0.1份亚硫酸钠置于三口烧瓶中,搅拌混合并通氮气排除空气,控制氮气通入速率为27mL/min,待通入完成后,搅拌混合并置于77℃下保温反应11h,静置冷却至室温并收集反应液,按质量比1:1,将反应液与无水乙醇搅拌混合并离心分离,收集下层沉淀并置于47℃烘箱中,干燥7h,得单分散聚苯乙烯颗粒;按重量份数计,分别称量47份二氧化硅、12份氧化铝、0.1份氧化铁、25份生石灰、7份氧化镁、1份氧化钾和1份氧化钠置于刚玉坩埚中,搅拌混合并加热熔融,按5℃/min升温至1400℃保温熔融2h,收集熔融液并水淬冷却,收集冷却物并置于球磨机中球磨处理1h,过500目筛并收集过筛颗粒,按质量比1:5,将过筛颗粒与质量份数10%聚乙烯醇溶液搅拌混合并置于250W下超声分散12min,收集得分散浆液;取高铝矾土并研磨分散,过500目筛并收集高铝矾土分散粉末,再按重量份数计,分别称量47份高铝矾土分散粉末、12份质量分数50%磷酸溶液、17份分散浆液和7份单分散聚苯乙烯颗粒置于搅拌机中,搅拌混合并收集混合浆液,将混合浆液浇注至模具中压制成型并置于105℃下保温干燥1h后,再按10℃/min升温至1050℃,保温烧制1h后,静置冷却至室温,得高铝耐火砖。
实施例3
按重量份数计,分别称量50份质量分数60%乙醇、5份苯乙烯单体、0.2份过硫酸钾和0.2份亚硫酸钠置于三口烧瓶中,搅拌混合并通氮气排除空气,控制氮气通入速率为30mL/min,待通入完成后,搅拌混合并置于80℃下保温反应12h,静置冷却至室温并收集反应液,按质量比1:1,将反应液与无水乙醇搅拌混合并离心分离,收集下层沉淀并置于50℃烘箱中,干燥8h,得单分散聚苯乙烯颗粒;按重量份数计,分别称量50份二氧化硅、15份氧化铝、0.2份氧化铁、30份生石灰、8份氧化镁、2份氧化钾和2份氧化钠置于刚玉坩埚中,搅拌混合并加热熔融,按5℃/min升温至1500℃保温熔融3h,收集熔融液并水淬冷却,收集冷却物并置于球磨机中球磨处理2h,过500目筛并收集过筛颗粒,按质量比1:5,将过筛颗粒与质量份数10%聚乙烯醇溶液搅拌混合并置于300W下超声分散15min,收集得分散浆液;取高铝矾土并研磨分散,过500目筛并收集高铝矾土分散粉末,再按重量份数计,分别称量50份高铝矾土分散粉末、15份质量分数50%磷酸溶液、20份分散浆液和8份单分散聚苯乙烯颗粒置于搅拌机中,搅拌混合并收集混合浆液,将混合浆液浇注至模具中压制成型并置于110℃下保温干燥2h后,再按10℃/min升温至1100℃,保温烧制2h后,静置冷却至室温,得高铝耐火砖。
实施例4
按重量份数计,分别称量50份质量分数60%乙醇、3~5份苯乙烯单体、0.2份过硫酸钾和0.2份亚硫酸钠置于三口烧瓶中,搅拌混合并通氮气排除空气,控制氮气通入速率为30mL/min,待通入完成后,搅拌混合并置于80℃下保温反应12h,静置冷却至室温并收集反应液,按质量比1:1,将反应液与无水乙醇搅拌混合并离心分离,收集下层沉淀并置于50℃烘箱中,干燥8h,得单分散聚苯乙烯颗粒;取高铝矾土并研磨分散,过500目筛并收集高铝矾土分散粉末,再按重量份数计,分别称量50份高铝矾土分散粉末、15份质量分数50%磷酸溶液、20份分散浆液和8份单分散聚苯乙烯颗粒置于搅拌机中,搅拌混合并收集混合浆液,将混合浆液浇注至模具中压制成型并置于110℃下保温干燥2h后,再按10℃/min升温至1100℃,保温烧制2h后,静置冷却至室温,得高铝耐火砖。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何标记视为限制所涉及的权利要求。
对实施例1、实施例2、实施例3、实施例4进行性能测试,所述的实施例4为未添加分散浆液制备的高铝耐火砖:
按照《GB/T3001-2007耐火材料常温抗折强度试验方法》和《GB/T 5072-2008耐火材料常温耐压强度试验方法》测试耐火材料常温抗折耐压强度;采用《GB/T30873-2014耐火材料抗热震性试验方法》测试材料热震稳定性。具体测试结果如表1所示。
表1性能对照表
(1)将本发明实施例1、实施例2、实施例3、实施例4进行对比,实施例4的抗热震性能远远小于实施例1、实施例2和实施例3,说明本发明技术方案通过对聚苯乙烯微球表面填充致密玻璃转化层,通过由于玻璃料与粘土在熔烧过程中形成复杂的釉瓷,其熔体流动性好,形成涂层后具有十分光滑致密的表面,无连通气孔,因而具有十分优异的耐腐蚀和抗氧化性能,同时难熔氧化物微细颗粒对瓷釉起到强化和锚固作用,改善了玻璃质瓷釉的耐热性、抗热震性,由于釉浆涂层是通过高温熔烧而成的,在熔烧过程中玻璃质的熔体与工件基体表面产生了良好的润湿和化学结合,涂层附着牢固,填充材料内部的同时,有效密实材料的内部结构,进一步提高材料的结构性能,改善材料的耐火强度。
(2)本发明技术方案实施例1,2,3对比实施例4,实施例4的抗折性能和耐压强度远远小于实施例1、实施例2和实施例3,说明本发明技术方案采用高铝矾土材料为主要基材,经高温煅烧后,高铝矾土微粉在高温条件下充填于砖体孔隙中,促进烧结,能够有效提高砖体的力学强度、耐高温性和持久使用性,同时通过填充的聚苯乙烯微球材料在升温时,被浆料浸渍后的聚苯乙烯微球材料在高温环境下明显收缩并持续炭化分解,这样在高铝砖内部形成孔隙,覆着在微球表面的浆料颗粒随温度升高逐渐脱水,通过玻璃料与粘土在熔烧过程中形成复杂的釉瓷粘结成一定形状的固体,即保留在内部空隙中,形成核壳结构,核壳结构高铝质耐火砖通过致密层与火焰接触,充分利用其致密耐火的特点形成耐火屏障,利用球形空隙内叠套的酥松的耐火固态颗粒,有效减少热射线的传输的平均自由程,使大部分热量能够保留在核壳结构中,有效耐火并提高材料的力学性能。
Claims (7)
1.一种高铝耐火砖,其特征在于,具体制备步骤为:
S1、按重量份数计,分别称量45~50份质量分数60%乙醇、3~5份苯乙烯单体、0.1~0.2份过硫酸钾和0.1~0.2份亚硫酸钠置于三口烧瓶中,搅拌混合并通氮气排除空气,待通入完成后,搅拌混合并保温反应,静置冷却至室温并收集反应液,按质量比1:1,将反应液与无水乙醇搅拌混合并离心分离,收集下层沉淀并干燥6~8h,得单分散聚苯乙烯颗粒;
S2、按重量份数计,分别称量45~50份二氧化硅、10~15份氧化铝、0.1~0.2份氧化铁、20~30份生石灰、5~8份氧化镁、1~2份氧化钾和1~2份氧化钠置于刚玉坩埚中,搅拌混合并加热熔融,程序升温并收集熔融液水淬冷却,收集冷却物并置于球磨机中球磨处理,过500目筛并收集过筛颗粒,按质量比1:5,将过筛颗粒与质量份数10%聚乙烯醇溶液搅拌混合并超声分散,收集得分散浆液;
S3、取高铝矾土并研磨分散,过500目筛并收集分散粉末,得高铝矾土分散粉末;
S4、按重量份数计,分别称量45~50份高铝矾土分散粉末、10~15份质量分数50%磷酸溶液、15~20份分散浆液和6~8份单分散聚苯乙烯颗粒置于搅拌机中,搅拌混合并收集混合浆液,将混合浆液浇注至模具中压制成型并保温干燥,升温加热并保温烧制,静置冷却至室温,得高铝耐火砖。
2.根据权利要求1所述的一种高铝耐火砖,其特征在于,所述高铝矾土分散粉末粒径为500目。
3.根据权利要求1所述的一种高铝耐火砖,其特征在于,所述磷酸溶液浓度优选为质量分数50%。
4.根据权利要求1所述的一种高铝耐火砖,其特征在于,所述氮气通入速率为25~30mL/min。
5.根据权利要求1所述的一种高铝耐火砖,其特征在于,步骤S2所述程序升温为按5℃/min升温至1300~1500℃。
6.根据权利要求1所述的一种高铝耐火砖,其特征在于,步骤S4所述压制成型压力为5~10MPa。
7.根据权利要求1所述的一种高铝耐火砖,其特征在于,步骤S4所述升温加热并保温烧制为按10℃/min升温至1000~1100℃,保温烧制1~2h。
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