CN116947522A - 一种微孔刚玉砖及其制备方法 - Google Patents
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- 229910052593 corundum Inorganic materials 0.000 title claims abstract description 119
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- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 84
- 239000008187 granular material Substances 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 28
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 239000006229 carbon black Substances 0.000 claims abstract description 20
- 239000004927 clay Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims abstract description 8
- 150000004767 nitrides Chemical class 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims description 48
- 238000001035 drying Methods 0.000 claims description 34
- 238000000227 grinding Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 24
- 238000000465 moulding Methods 0.000 claims description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 18
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 16
- 239000005011 phenolic resin Substances 0.000 claims description 16
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- 241000276425 Xiphophorus maculatus Species 0.000 claims description 4
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 57
- 229910052742 iron Inorganic materials 0.000 abstract description 29
- 239000002893 slag Substances 0.000 abstract description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 18
- 239000003513 alkali Substances 0.000 abstract description 18
- 229910052751 metal Inorganic materials 0.000 abstract description 17
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- 229910052581 Si3N4 Inorganic materials 0.000 abstract description 7
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 29
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000009991 scouring Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
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- 230000009467 reduction Effects 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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- 238000010791 quenching Methods 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
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Abstract
本发明涉及炼铁高炉用耐火材料技术领域,尤其涉及一种微孔刚玉砖及其制备方法。微孔刚玉砖由包括颗粒料、细粉和树脂结合剂的原料制备得到;颗粒料为刚玉颗粒;颗粒料包括3~5mm、1~3mm和0~1mm三种颗粒级别;细粉按重量份数计包括:刚玉细粉15~21份;氧化铝微粉3~9份;金属硅粉3~7份;氮化硅铁3~7份;炭黑2~6份;结合粘土1~3份;所述细粉的粒度≤0.074mm。本发明通过调整制品配方,引入金属硅粉、氮化硅铁、纳米级炭黑、氧化铝微粉和结合粘土,并限定了原料组分的粒度范围,最终获得的微孔刚玉砖具有良好的抗渣、抗碱、抗铁水侵蚀性,而且具有较好的抗热震性能。
Description
技术领域
本发明涉及炼铁高炉用耐火材料技术领域,尤其涉及一种微孔刚玉砖及其制备方法。
背景技术
高炉是生产铁水的大型设备,其中高炉炉缸、炉底用耐火材料工况条件恶劣、寿命短是影响高炉整体使用寿命的薄弱环节之一。现有的高炉炉缸、炉底用的耐火材料和结构基本上分两大类:一是微孔和超微孔炭砖炉衬,二是氧化物陶瓷杯与炭砖复合炉衬。
微孔和超微孔炭砖的优点是炭素材料难润湿,渣铁难渗透,热传导好。它能把渣铁共凝等温线(1150℃)推至炉内,即在炭砖的表面与炉内铁水接触的地方形成一层固态保护膜层,这个膜层是渣铁在炭砖表面凝固形成渣皮,保护炭砖,达到高炉长寿的目的。但因高炉操作及除铁操作等原因,渣皮的稳定性较差,脆弱的渣皮一旦被破坏,炭砖就直接与铁水接触。炭砖的铁水熔蚀指数高达25%~30%;因炭砖的碳在铁水中的溶解度较高,导致了炭砖的化学侵蚀,炭砖的强度较低,抗高温铁水和熔渣的冲刷能力较差,特别是高炉出铁时,高温的铁水和熔渣形成环流,造成炉缸炭砖形成“马蹄形”冲蚀状态。炭砖的抗碱性较优,但是碱蒸气通过炭砖的气孔各裂纹深入炭砖内部,碱与碳的反应使炭砖催化而开裂,导致炉缸炭砖砌体形成环形裂缝,降低了炭砖的热导率,不利于渣皮的形成,继而加快了炭砖的损坏。炭砖的抗氧化性较差,也加速了其损坏速度。
氧化物陶瓷杯材质主要为氧化物耐火材料(如刚玉莫来石砖、棕刚玉碳化硅复合砖、刚玉浇注预制块、塑性相刚玉砖和微孔刚玉砖)。其导热性好,保温性差,能将1150℃渣铁凝固线和800~870℃的碱化学侵蚀线推往炉内和留在陶瓷杯内,形成渣皮保护炭砖并减少碱对炭砖的侵蚀。这类材料强度高,抗冲刷能力强;其铁水熔蚀指数很低,也不存在氧化问题。但是,陶瓷杯砖大多不是微孔或超微孔砖,渣铁和碱类物质通过气孔渗入砖体内部,降低了砖的耐火性能,受到化学侵蚀,砖的原有结构遭到破坏,强度大幅降低,抗冲刷能力也随之降低。实践证明,现有的陶瓷杯很难判定其准确的使用寿命。应用初期它对高炉炉缸、炉底炭砖起到了保护作用,但是,高炉的中、后期还是要靠炭砖维持,因此也难实现长寿。
现有的微孔刚玉砖抗渣性和抗碱性不好,抗热震性极差,而且微孔化效果也不好,很多企业不愿意使用国内的微孔刚玉砖。
现有微孔刚玉砖都是以刚玉作为主要原料,基质部分以金属硅粉、氮化硅或碳化硅、刚玉细粉和少量烧结剂预混,高压成型,长时间高温还原气氛烧结而成。一是烧成费用高,二是利用金属硅粉的较低熔点(1460℃)和可塑性,将刚玉砖在1460℃以上高温长时间烧成,金属硅高温下呈液相,逐步滑移占据填充砖中气孔位置,逐渐形成微孔或超微孔,加上氮化硅或碳化硅等具有良好的抗侵蚀,高的力学强度,较低的热膨胀率,较高的抗氧化性能等,因而使得微孔刚玉砖具有较好的抗渣、抗碱及抗铁水熔蚀性能。但是利用金属硅粉的较低熔点及可塑性滑移特点形成微孔化组织结构不是很理想,孔径分布及平均孔径还需改善和提高。另外,由于微孔刚玉砖是经高压、高温长时间烧成,砖强度特别高,常温耐压强度在120MPa以上,加上微孔或超微孔结构,导致砖的热震很差,做1100℃水冷热震,1次都做不了。
发明内容
有鉴于此,本发明要解决的技术问题在于提供一种微孔刚玉砖及其制备方法,本发明提供的微孔刚玉砖具有良好的抗渣、抗碱、抗铁水侵蚀性,而且具有较好的抗热震性能。
本发明提供了一种微孔刚玉砖,由包括组分a和树脂结合剂的原料制备得到;所述组分a包括颗粒料和细粉;
所述颗粒料为刚玉颗粒;
所述颗粒料包括3~5mm、1~3mm和0~1mm三种颗粒级别;
所述细粉按重量份数计包括:
所述细粉的粒度≤0.074mm。
优选的,所述刚玉颗粒的材质包括棕刚玉、致密刚玉、白刚玉、板状刚玉和高铝刚玉中的至少一种。
优选的,所述颗粒料和细粉的质量比为55~65:35~45;
所述3~5mm的颗粒料、1~3mm的颗粒料和0~1mm的颗粒料的质量比为15~21:25~35:9~15。
优选的,所述细粉中,氮化硅铁和结合粘土的粒度为≤0.074mm,刚玉细粉和金属硅粉的粒度为≤0.045mm,氧化铝微粉的粒度为≤5μm,炭黑的粒度为≤10nm。
优选的,所述刚玉细粉的材质包括棕刚玉、致密刚玉、白刚玉、板状刚玉和高铝刚玉中的至少一种;
所述氧化铝微粉为α氧化铝微粉;
所述炭黑为纳米级炭黑;
所述结合粘土为维罗泥;
所述树脂结合剂为热固性酚醛树脂;
所述组分a和树脂结合剂的质量比为100:3.5~4。
本发明还提供了一种上文所述的微孔刚玉砖的制备方法,包括以下步骤:
A)将细粉预混,得到预混粉;
B)将颗粒料干混后,与部分树脂结合剂混碾,再与所述预混粉混碾,然后与剩余树脂结合剂净混,制得泥料;
C)将所述泥料进行困料、筛分,然后机压成型,干燥,得到砖坯;
D)将所述砖坯在还原气气氛下1470~1480℃烧成,得到微孔刚玉砖。
优选的,步骤A)中,所述预混的转速为60~65rpm,时间为15~20min。
优选的,步骤B)中,
所述干混的时间为1~2min;
所述部分树脂结合剂占全部树脂结合剂质量的70%~80%;
与部分树脂结合剂混碾的时间为10~12min;
再与所述预混粉混碾的时间为4~5min;
所述净混的时间为20~25min。
优选的,步骤C)中,所述困料的温度为20~25℃,湿度为80%~85%,时间为18~24h;
所述筛分采用的筛子孔径为7~9mm;
所述机压成型后的成型体密度≥3.25g/cm3,显气孔率≤5%;
所述干燥包括:
先自然干燥24~36h后,再在天然气干燥窑内、200~250℃干燥24~36h。
优选的,步骤D)中,所述烧成的时间为35~40h。
本发明提供了一种微孔刚玉砖,由包括组分a和树脂结合剂的原料制备得到;所述组分a包括颗粒料和细粉;所述颗粒料为刚玉颗粒;所述颗粒料包括3~5mm、1~3mm和0~1mm三种颗粒级别;所述细粉按重量份数计包括:刚玉细粉15~21份;氧化铝微粉3~9份;金属硅粉3~7份;氮化硅铁3~7份;炭黑2~6份;结合粘土1~3份;所述细粉的粒度≤0.074mm。本发明通过调整制品配方,引入金属硅粉、氮化硅铁、纳米级炭黑、氧化铝微粉和结合粘土,并限定了原料组分的粒度范围,最终获得的微孔刚玉砖具有良好的抗渣、抗碱、抗铁水侵蚀性,而且具有较好的抗热震性能。
具体实施方式
下面将结合本发明实施例,对本发明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。
本发明提供了一种微孔刚玉砖,由包括组分a和树脂结合剂的原料制备得到;所述组分a包括颗粒料和细粉;
所述颗粒料为刚玉颗粒;
所述颗粒料包括3~5mm、1~3mm和0~1mm三种颗粒级别;
所述细粉按重量份数计包括:
所述细粉的粒度≤0.074mm。
在本发明的某些实施例中,所述刚玉颗粒的材质包括棕刚玉、致密刚玉、白刚玉、板状刚玉和高铝刚玉中的至少一种。
本发明中,所述颗粒料包括3~5mm、1~3mm和0~1mm三种颗粒级别;所述颗粒料的粒径为3~5mm时,不包括3mm;所述颗粒料的粒径为1~3mm时,不包括1mm。
在本发明的某些实施例中,所述颗粒料和细粉的质量比为55~65:35~45;比如60:40、59:41。具体的,所述3~5mm的颗粒料、1~3mm的颗粒料和0~1mm的颗粒料的质量比为15~21:25~35:9~15;比如18:30:12、20:29:11、21:25:14、15:35:9。
在本发明的某些实施例中,所述细粉中,氮化硅铁的粒度为≤0.074mm,结合粘土的粒度为≤0.074mm,刚玉细粉的粒度为≤0.045mm,金属硅粉的粒度为≤0.045mm,氧化铝微粉的粒度为≤5μm,炭黑的粒度为≤10nm。
在本发明的某些实施例中,所述刚玉细粉的材质包括棕刚玉、致密刚玉、白刚玉、板状刚玉和高铝刚玉中的至少一种。在某些实施例中,所述刚玉细粉的重量份数为18份、16份、15份、20份。
在本发明的某些实施例中,所述氧化铝微粉为α氧化铝微粉。在某些实施例中,所述α氧化铝微粉的重量份数为6份、8份、9份、4份。
在某些实施例中,所述金属硅粉的重量份数为5份、4份、5.5份、7份。
在本发明的某些实施例中,所述炭黑为纳米级炭黑,具体为炭黑N220。在某些实施例中,所述炭黑的重量份数为4份、5份、2份、6份。
在本发明的某些实施例中,所述结合粘土为维罗泥,具体为广西维罗泥。在某些实施例中,所述结合粘土的重量份数为2份、3份、1.5份、1份。
在本发明的某些实施例中,所述树脂结合剂为热固性酚醛树脂,具体为PF5321酚醛树脂。所述组分a和树脂结合剂的质量比为100:3.5~4;比如100:4、100:3.5、100:3.8。
本发明还提供了一种上文所述的微孔刚玉砖的制备方法,包括以下步骤:
A)将细粉预混,得到预混粉;
B)将颗粒料干混后,与部分树脂结合剂混碾,再与所述预混粉混碾,然后与剩余树脂结合剂净混,制得泥料;
C)将所述泥料进行困料、筛分,然后机压成型,干燥,得到砖坯;
D)将所述砖坯在还原气气氛下1470~1480℃烧成,得到微孔刚玉砖。
所述微孔刚玉砖的制备方法中采用的原料组分同上,在此不再赘述。
步骤A)中:
将细粉预混,得到预混粉。
在本发明的某些实施例中,所述预混的转速为60~65rpm,时间为15~20min。所述预混设备可以为双螺杆混合机。
步骤B)中:
将颗粒料干混后,与部分树脂结合剂混碾,再与所述预混粉混碾,然后与剩余树脂结合剂净混,制得泥料。
在本发明的某些实施例中,所述干混的时间为1~2min。
在本发明的某些实施例中,所述部分树脂结合剂占全部树脂结合剂质量的70%~80%。与部分树脂结合剂混碾的时间为10~12min。
在本发明的某些实施例中,再与所述预混粉混碾的时间为4~5min。
在本发明的某些实施例中,所述净混的时间为20~25min。
在本发明的某些实施例中,所述干混、混碾和净混均在带碾轮的混练机中进行。
步骤C)中:
将所述泥料进行困料、筛分,然后机压成型,干燥,得到砖坯。
在本发明的某些实施例中,所述困料的温度为20~25℃,比如25℃、20℃、24℃、21℃;湿度为80%~85%,比如85%、80%、82%、83%;时间为18~24h,比如24h、18h、22h、23h。所述困料在困料室内进行。
在本发明的某些实施例中,所述筛分采用的筛子孔径为7~9mm,比如8mm。
在本发明的某些实施例中,所述机压成型后的成型体密度≥3.25g/cm3,显气孔率≤5%。所述机压成型在1250吨以上电动双螺旋压机上,双面加压成型。
在本发明的某些实施例中,所述干燥包括:
先自然干燥24~36h后,再在天然气干燥窑内、200~250℃干燥24~36h。
步骤D)中:
将所述砖坯在还原气气氛下1470~1480℃烧成,得到微孔刚玉砖。
在本发明的某些实施例中,所述烧成的温度为1480℃或1470℃;时间为35~40h,比如40h、38h、35h或39h。
具体的,所述烧成包括:
将所述砖坯装入窑车密封匣钵内,以焦炭作为介质,推入125.4m隧道窑,当温度上升到1470~1480℃时,进入保温过程,保温烧成35~40h。
在本发明的某些实施例中,所述烧成后,还包括:冷却。具体的,包括:离开隧道窑烧成带,进入冷却带,冷却后即可出窑。
在本发明的某些实施例中,所述冷却后,还包括:
进行切、磨工序,达到尺寸要求后,得到微孔刚玉砖。
本发明对上文采用的原料来源并无特殊的限制,可以为一般市售。
本发明通过调整制品的配方,引入金属硅粉、氮化硅铁、纳米级炭黑、氧化铝微粉和结合粘土,改善了制品基质组成,优化了基质部分各级粒度相互填充及微孔形成机理及工艺,获得了比较理想的微孔结构。制品获得了良好的抗渣、抗碱、抗铁水侵蚀性能,抗热震性能得到了大大提高。
本发明获得的微孔刚玉砖微孔化结构较优,平均孔径不超过0.3μm,小于1μm孔容积率高于83%,透气度小于0.3mDa;具有较低的显气孔率,显气孔率不超过9.2%;较高的体积密度,体积密度不小于3.16g/cm3;较高的耐压强度,耐压强度不小于140MPa;抗渣性测试中,溶蚀率不超过4.5%;抗碱性测试中,强度下降率小于5.5%;铁水熔蚀指数不超过0.5%;1100℃水冷热震的次数不低于4次。因而本发明微孔刚玉砖具有良好的抗渣、抗碱、抗铁水侵蚀性能,而且具有较好的抗热震性能。
本发明制备得到的微孔刚玉砖特别适用于高炉炉缸区域,包括高炉炉底、炉壁以及风口、铁口、渣口。
为了进一步说明本发明,以下结合实施例对本发明提供的一种微孔刚玉砖及其制备方法进行详细描述,但不能将其理解为对本发明保护范围的限定。
实施例1
1)细粉预混:将白刚玉细粉≤0.045mm 18重量份、α氧化铝微粉≤5μm 6重量份、炭黑N220≤10nm 4重量份、氮化硅铁≤0.074mm 5重量份、广西维罗泥≤0.074mm 2重量份、金属硅粉≤0.045mm 5重量份一起加入到双螺杆混合机中强力预混(预混的转速为60rpm)15min,制得预混粉。
2)将棕刚玉3~5mm(不包括3mm)18重量份、棕刚玉1~3mm(不包括1mm)30重量份、棕刚玉0~1mm 12重量份加入到混练机内干混2min,加入3.2重量份PF5321酚醛树脂混碾10min后,加入所述预混粉混碾5min,加入0.8份PF5321酚醛树脂,净混25min后出料,制得泥料。
3)将所述泥料推入困料室内进行困料,困料室内温度控制在25℃,湿度控制在85%,困料24h,经过8mm筛网筛分后,机压成型,成型在1250吨电动双螺旋压机上进行,采取双面加压方式,得到的成型体密度≥3.25g/cm3,显气孔率≤5%。成型后,先自然干燥24h,再进天然气干燥窑内、200℃干燥36h,得到砖坯。
4)将所述砖坯装入窑车密封匣钵内,以焦炭作为介质,推入125.4m隧道窑,当温度上升到1480℃时,进入保温过程,保温烧成40h后,离开隧道窑烧成带,进入冷却带,冷却后即可出窑;
加工:将烧制后的单块砖进行切、磨工序,达到尺寸要求后,即为成品砖。
实施例2
1)细粉预混:将板状刚玉细粉≤0.045mm 16重量份、α氧化铝微粉≤5μm 8重量份、炭黑N220≤10nm 5重量份、氮化硅铁≤0.074mm 4重量份、广西维罗泥≤0.074mm 3重量份、金属硅粉≤0.045mm 4重量份一起加入到双螺杆混合机预混设备中强力预混(预混的转速为60rpm)20min,制得预混粉。
2)将致密刚玉3~5mm(不包括3mm)20重量份、致密刚玉1~3mm(不包括1mm)29重量份、致密刚玉0~1mm 11重量份加入到混练机内干混1min,加入2.8重量份PF5321酚醛树脂混碾12min后,加入所述预混粉混碾4min,加入0.7份PF5321酚醛树脂,净混20min后出料,制得泥料。
3)将所述泥料推入困料室内进行困料,困料室内温度控制在20℃,湿度控制在80%,困料18h,经过8mm筛网筛分后,机压成型,成型在1250吨电动双螺旋压机上进行,采取双面加压方式,得到的成型体密度≥3.25g/cm3,显气孔率≤5%。成型后,先自然干燥36h,再进天然气干燥窑内、250℃干燥30h,得到砖坯。
4)将所述砖坯装入窑车密封匣钵内,以焦炭作为介质,推入125.4m隧道窑,当温度上升到1470℃时,进入保温过程,保温烧成38h后,离开隧道窑烧成带,进入冷却带,冷却后即可出窑;
加工:将烧制后的单块砖进行切、磨工序,达到尺寸要求后,即为成品砖。
实施例3
1)细粉预混:将白刚玉细粉≤0.045mm 15重量份、α氧化铝微粉≤5μm 9重量份、炭黑N220≤10nm 2重量份、氮化硅铁≤0.074mm 7重量份、广西维罗泥≤0.074mm 1.5重量份、金属硅粉≤0.045mm 5.5重量份一起加入到双螺杆混合机预混设备中强力预混(预混的转速为60rpm)18min,制得预混粉。
2)将致密刚玉3~5mm(不包括3mm)21重量份、致密刚玉1~3mm(不包括1mm)25重量份、致密刚玉0~1mm 14重量份加入到混练机内干混1.5min,加入3重量份PF5321酚醛树脂混碾11min后,加入所述预混粉混碾4.5min,加入1份PF5321酚醛树脂,净混22min后出料,制得泥料。
3)将所述泥料推入困料室内进行困料,困料室内温度控制在24℃,湿度控制在82%,困料22h,经过8mm筛网筛分后,机压成型,成型在1250吨电动双螺旋压机上进行,采取双面加压方式,得到的成型体密度≥3.25g/cm3,显气孔率≤5%。成型后,先自然干燥32h,再进天然气干燥窑内、240℃干燥28h,得到砖坯。
4)将所述砖坯装入窑车密封匣钵内,以焦炭作为介质,推入125.4m隧道窑,当温度上升到1480℃时,进入保温过程,保温烧成35h后,离开隧道窑烧成带,进入冷却带,冷却后即可出窑;
加工:将烧制后的单块砖进行切、磨工序,达到尺寸要求后,即为成品砖。
实施例4
1)细粉预混:将板状刚玉细粉≤0.045mm 20重量份、α氧化铝微粉≤5μm 4重量份、炭黑N220≤10nm 6重量份、氮化硅铁≤0.074mm 3重量份、广西维罗泥≤0.074mm 1重量份、金属硅粉≤0.045mm 7重量份一起加入到双螺杆混合机预混设备中强力预混(预混的转速为60rpm)16min,制得预混粉。
2)将棕刚玉3~5mm(不包括3mm)15重量份、棕刚玉1~3mm(不包括1mm)35重量份、致密刚玉0~1mm 9重量份加入到混练机内干混1.8min,加入2.66重量份PF5321酚醛树脂混碾10min后,加入所述预混粉混碾5min,加入1.14份PF5321酚醛树脂,净混23min后出料,制得泥料。
3)将所述泥料推入困料室内进行困料,困料室内温度控制在21℃,湿度控制在83%,困料23h,经过8mm筛网筛分后,机压成型,成型在1250吨电动双螺旋压机上进行,采取双面加压方式,得到的成型体密度≥3.25g/cm3,显气孔率≤5%。成型后,先自然干燥35h,再进天然气干燥窑内、210℃干燥34h,得到砖坯。
4)将所述砖坯装入窑车密封匣钵内,以焦炭作为介质,推入125.4m隧道窑,当温度上升到1470℃时,进入保温过程,保温烧成39h后,离开隧道窑烧成带,进入冷却带,冷却后即可出窑;
加工:将烧制后的单块砖进行切、磨工序,达到尺寸要求后,即为成品砖。
对比例1
1)细粉预混:将白刚玉细粉≤0.045mm 21.5重量份、α氧化铝微粉≤5μm 6重量份、氮化硅细粉≤0.088mm 4.5重量份、广西维罗泥≤0.074mm 2重量份、金属硅粉≤0.045mm 6重量份一起加入到双螺杆混合机预混设备中强力预混(预混的转速为60rpm)15min,制得预混粉。
2)将棕刚玉3~5mm(不包括3mm)20重量份、棕刚玉1~3mm(不包括1mm)30重量份、棕刚玉0~1mm 10重量份加入到混练机内干混1min,加入4重量份PF5321酚醛树脂混碾10min后,加入所述预混粉净混25min后出料,制得泥料。
3)将所述泥料推入困料室内进行困料,困料室内温度控制在25℃,湿度控制在85%,困料24h,经过8mm筛网筛分后,机压成型,成型在1250吨电动双螺旋压机上进行,采取双面加压方式,得到的成型体密度≥3.25g/cm3,显气孔率≤12%。成型后,先自然干燥24h,再进天然气干燥窑内、200℃干燥36h,得到砖坯。
4)将所述砖坯装入窑车密封匣钵内,以焦炭作为介质,推入125.4m隧道窑,当温度上升到1500℃时,进入保温过程,保温烧成50h后,离开隧道窑烧成带,进入冷却带,冷却后即可出窑;
加工:将烧制后的单块砖进行切、磨工序,达到尺寸要求后,即为成品砖。
对比例2
1)细粉预混:将白刚玉细粉≤0.045mm 21.5重量份、α氧化铝微粉≤5μm 6重量份、碳化硅细粉≤0.045mm 4.5重量份、广西维罗泥≤0.074mm 2重量份、金属硅粉≤0.045mm 6重量份一起加入到双螺杆混合机预混设备中强力预混(预混的转速为60rpm)15min,制得预混粉。
2)将棕刚玉3~5mm(不包括3mm)20重量份、棕刚玉1~3mm(不包括1mm)30重量份、棕刚玉0~1mm 10重量份加入到混练机内干混1min,加入4重量份PF5321酚醛树脂混碾10min后,加入所述预混粉,净混25min后出料,制得泥料。
3)将所述泥料推入困料室内进行困料,困料室内温度控制在25℃,湿度控制在85%,困料24h,经过8mm筛网筛分后,机压成型,成型在1250吨电动双螺旋压机上进行,采取双面加压方式,得到的成型体密度≥3.25g/cm3,显气孔率≤12%。成型后,先自然干燥24h,再进天然气干燥窑内、200℃干燥36h,得到砖坯。
4)将所述砖坯装入窑车密封匣钵内,以焦炭作为介质,推入125.4m隧道窑,当温度上升到1500℃时,进入保温过程,保温烧成50h后,离开隧道窑烧成带,进入冷却带,冷却后即可出窑;
加工:将烧制后的单块砖进行切、磨工序,达到尺寸要求后,即为成品砖。
对比例3
与实施例3的区别在于:
步骤2)中,将致密刚玉3~5mm(不包括3mm)40重量份、致密刚玉0~1mm 20重量份加入到混练机内干混1.5min,加入3重量份PF5321酚醛树脂混碾11min后,加入所述预混粉混碾4.5min,加入1份PF5321酚醛树脂,净混22min后出料,制得泥料。
性能测试
对实施例1~4和对比例1~3所得成品砖进行化学成分(Al2O3、Fe2O3、C总)、显气孔率、体积密度、常温耐压、铁水熔蚀指数、抗渣性、抗碱性、透气度、平均孔径、小于1μm孔容积率和抗热震性进行测试:
砖的制样按GB/T 7321的规定进行。
按照GB/T 6900-2006铝硅系耐火材料化学分析方法中的乙酸锌返滴定EDTA容量法(9.1)测定氧化铝量。
按照GB/T 6900-2006铝硅系耐火材料化学分析方法中的(10)氧化铁的测定测定氧化铁量。
按照GB/T 16555-2008含碳、碳化硅、氮化物耐火材料化学分析方法中的燃烧气体容量法(10.1)测定总碳量。
按照GB/T 2997-2000中致密定形耐火制品体积密度、显气孔率和真气孔率试验方法测试砖的显气孔率和体积密度。
按照GB/T 5072-2008耐火材料常温耐压强度试验方法测试砖的耐压强度。
按照YB/T 4036高炉炭块铁水熔蚀指数试验方法测试砖的抗铁水熔蚀指数。
按照YB/T 117高炉用耐火材料抗渣性试验方法测试砖的抗渣性(溶蚀率)。
按照GB/T 14983耐火材料抗碱性试验方法测试砖的抗碱性(强度下降率)。
按照GB/T 3000致密定形耐火制品透气度试验方法测试砖的透气度。
按照YB/T 118耐火材料气孔孔径分布试验方法测试砖的平均孔径和小于1μm孔容积率。
按照YB/T 376.1-1995耐火制品抗热震性试验方法(水急冷法)测试砖的热震稳定性。
测试结果参见表1。
表1实施例1~4和对比例1~3所得成品砖的性能测试结果
从表1可知,本发明获得的微孔刚玉砖微孔化结构较优,平均孔径不超过0.3μm,小于1μm孔容积率高于83%,透气度小于0.3mDa;具有较低的显气孔率,显气孔率不超过9.2%;较高的体积密度,体积密度不小于3.16g/cm3;较高的耐压强度,耐压强度不小于140MPa;抗渣性测试中,溶蚀率不超过4.5%;抗碱性测试中,强度下降率小于5.5%;铁水熔蚀指数不超过0.5%;1100℃水冷热震的次数不低于4次。因而本发明微孔刚玉砖具有良好的抗渣、抗碱、抗铁水侵蚀性能,而且具有较好的抗热震性能。
对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下,在其它实施例中实现。因此,本发明将不会被限制于本文所示的这些实施例,而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。
Claims (10)
1.一种微孔刚玉砖,由包括组分a和树脂结合剂的原料制备得到;所述组分a包括颗粒料和细粉;
所述颗粒料为刚玉颗粒;
所述颗粒料包括3~5mm、1~3mm和0~1mm三种颗粒级别;
所述细粉按重量份数计包括:
所述细粉的粒度≤0.074mm。
2.根据权利要求1所述的微孔刚玉砖,其特征在于,所述刚玉颗粒的材质包括棕刚玉、致密刚玉、白刚玉、板状刚玉和高铝刚玉中的至少一种。
3.根据权利要求1所述的微孔刚玉砖,其特征在于,所述颗粒料和细粉的质量比为55~65:35~45;
所述3~5mm的颗粒料、1~3mm的颗粒料和0~1mm的颗粒料的质量比为15~21:25~35:9~15。
4.根据权利要求1所述的微孔刚玉砖,其特征在于,所述细粉中,氮化硅铁和结合粘土的粒度为≤0.074mm,刚玉细粉和金属硅粉的粒度为≤0.045mm,氧化铝微粉的粒度为≤5μm,炭黑的粒度为≤10nm。
5.根据权利要求1所述的微孔刚玉砖,其特征在于,所述刚玉细粉的材质包括棕刚玉、致密刚玉、白刚玉、板状刚玉和高铝刚玉中的至少一种;
所述氧化铝微粉为α氧化铝微粉;
所述炭黑为纳米级炭黑;
所述结合粘土为维罗泥;
所述树脂结合剂为热固性酚醛树脂;
所述组分a和树脂结合剂的质量比为100:3.5~4。
6.一种权利要求1~5任意一项所述的微孔刚玉砖的制备方法,包括以下步骤:
A)将细粉预混,得到预混粉;
B)将颗粒料干混后,与部分树脂结合剂混碾,再与所述预混粉混碾,然后与剩余树脂结合剂净混,制得泥料;
C)将所述泥料进行困料、筛分,然后机压成型,干燥,得到砖坯;
D)将所述砖坯在还原气气氛下1470~1480℃烧成,得到微孔刚玉砖。
7.根据权利要求1所述的制备方法,其特征在于,步骤A)中,所述预混的转速为60~65rpm,时间为15~20min。
8.根据权利要求1所述的制备方法,其特征在于,步骤B)中,
所述干混的时间为1~2min;
所述部分树脂结合剂占全部树脂结合剂质量的70%~80%;
与部分树脂结合剂混碾的时间为10~12min;
再与所述预混粉混碾的时间为4~5min;
所述净混的时间为20~25min。
9.根据权利要求1所述的制备方法,其特征在于,步骤C)中,所述困料的温度为20~25℃,湿度为80%~85%,时间为18~24h;
所述筛分采用的筛子孔径为7~9mm;
所述机压成型后的成型体密度≥3.25g/cm3,显气孔率≤5%;
所述干燥包括:
先自然干燥24~36h后,再在天然气干燥窑内、200~250℃干燥24~36h。
10.根据权利要求1所述的制备方法,其特征在于,步骤D)中,所述烧成的时间为35~40h。
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