CN117142877B - 一种轻质硅砖的制备方法及其所得轻质硅砖 - Google Patents
一种轻质硅砖的制备方法及其所得轻质硅砖 Download PDFInfo
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- ZHJGWYRLJUCMRT-UHFFFAOYSA-N 5-[6-[(4-methylpiperazin-1-yl)methyl]benzimidazol-1-yl]-3-[1-[2-(trifluoromethyl)phenyl]ethoxy]thiophene-2-carboxamide Chemical compound C=1C=CC=C(C(F)(F)F)C=1C(C)OC(=C(S1)C(N)=O)C=C1N(C1=C2)C=NC1=CC=C2CN1CCN(C)CC1 ZHJGWYRLJUCMRT-UHFFFAOYSA-N 0.000 claims abstract description 40
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Abstract
本发明属于轻质硅砖材料领域,尤其涉及一种轻质硅砖的制备方法及其所得轻质硅砖,本发明借助于四水硝酸钙低熔点特性,利用烘烤后液态四水硝酸钙与硅石细粉和锯末的湿法预混合,配合其他步骤,解决了机压可燃法生产轻质硅砖时干法混合造成的可燃物分布不均问题。并且本发明所涉及的轻质硅砖中四水硝酸钙还同时具有矿化剂和造孔剂功能,作为矿化剂和造孔剂四水硝酸钙能够做到分布均匀且高温烧成过程中逐步分解,吸收应力、降低热导率的同时不会对砖体产生破坏。本发明制备方法简单,原料丰富且性价比优,烧成过程易控,砖体不会泛黄,适宜大型硅砖的工业化生产,成品砖具有较高的强度。
Description
技术领域
本发明属于轻质硅砖材料领域,尤其涉及一种轻质硅砖的制备方法及其所得轻质硅砖。
背景技术
轻质硅砖又称硅质隔热砖,是二氧化硅在91wt%以上,体积密度在1.2 g/cm3以下的轻质耐火材料,耐火度和荷重软化温度与成分相同的普通硅砖相差不大。但由于气孔很多,故耐压强度、抗渣性、抗腐蚀性等不如普通硅砖,而抗热震性能却有所提高,且长期使用不收缩等特性,在轻质保温耐火材料体系及窑炉设计中被大量应用。
目前轻质硅砖普遍采用机压可燃法制备,该方法具有工艺简单,成本低等优点。机压可燃法制备轻质硅砖主要在配料时掺加无烟煤、焦炭屑、锯木屑、果壳粉、聚合物轻球等烧失物,然后通过机压成型并烧制而成。但无烟煤含有较高灰分,易使制品的烧成性能变差,并产生黑心、裂纹、松散甚至碎裂等现象;焦炭屑虽灰分含量较低,但其质量和来源不稳定;锯木屑和聚合物轻球具有弹性,机压成型后坯体的弹性后效作用难以解决,易产生开裂现象。此外,机压可燃法的一个明显问题就是原料,尤其是可燃物,在干法混合过程中难以分散均匀,由此造成的烧后成品砖气孔分布非常不均匀,气孔簇团局部集中情况突出。这样不仅影响成品率,还影响硅砖质量的稳定性,从而会影响硅砖性能。
发明内容
为了解决现有技术存在的上述技术问题,本发明提供一种轻质硅砖的制备方法及其所得轻质硅砖。
本发明所采用的技术方案如下:
一种轻质硅砖的制备方法,包括如下步骤:
S1、将四水硝酸钙烘烤至熔融,将熔融的四水硝酸钙与硅石细粉、锯末进行预混合搅拌,获得泥料;
S2、将S1的泥料与骨料、废硅砖和结合剂进行混炼,之后压制成砖坯;
S3、将所述砖坯经干燥、烧结工序后制得成品。
优选地,四水硝酸钙与硅石细粉、锯末的质量之比为1:1.5-5:0.05-0.5、优选1:1.5-4:0.1-0.4。该优选方案,能够实现湿法混炼,更利于制得成分均匀的泥料。
其中优选地,S1中,以原料总量为基准,四水硝酸钙的用量占10.1wt%~20wt%,硅石细粉的用量占30wt%~60wt%,锯末的用量占1wt%~10wt%。
其中优选地,S2中,以原料总量为基准,骨料的用量占5wt%~57.9wt%,废硅砖的用量占1wt%~15wt%;结合剂用量为原料总量的0.5%~5%。
在上述原料的占比优选方案中,能够实现较好的颗粒级配,更利于高性能轻质硅砖的生产。
其中优选地,所述的轻质硅砖的制备方法还包括:S1中,先将锯末提前在水中浸泡腐烂,再与熔融的四水硝酸钙与硅石细粉进行所述预混合。该优选方案,能够避免锯末在泥料中上浮,更利于提升泥料均匀性。
更优选地,所述浸泡腐烂的条件包括:锯末和水的质量比为1:0.1 -0.5,浸泡时间为12 - 72 h,浸泡温度为10 - 40℃。该优选方案,锯末和水的质量比适宜,浸泡参数适宜,能够实现锯末的充分腐烂,更利于泥料的混炼。
其中优选地,S1中,所述预混合搅拌的条件包括:搅拌时间为1 - 10 min,搅拌转速为50 - 500 转/分。
其中优选地,S2中,所述混炼的条件包括:混炼时间为1 -30 min,混炼转速为50 -500 转/分。
其中优选地,所述骨料是硅石或硅砂中的一种或多种。
其中优选地,所述废硅砖由生产的硅砖残品破碎制得。
其中优选地,所述结合剂为纸浆废液或其他本领域常规种类。
其中优选地,所述骨料的粒度 ≤ 2.18 mm,所述硅石细粉的粒度 ≤ 0.088mm,所述废硅砖的粒度≤ 0.5 mm。
其中优选地,锯末的粒度≤ 5 mm。
其中优选地,S3中所述干燥、烧结工序的过程包括:首先将砖坯自然干燥12~48h至残余水分<1.0 wt%,干燥后置入隧道窑或梭式窑中,升温至1450~1510℃保温24~48h烧结,制得成品。该优选方案,能够避免硅砖在烧成过程中开裂,更利于提升成品砖物理性能。
本发明还提供一种轻质硅砖,其通过前面所述的轻质硅砖的制备方法制得。本发明的轻质硅砖的密度、强度、稳定性等性能均较优。
有益效果:
本发明技术方案所生产的含有四水硝酸钙的轻质硅砖具有以下优势:(1)熔融的液态四水硝酸钙与硅石细粉和锯末的预混合搅拌实现了成品轻质硅砖中原料的均匀分布,提升了成品砖各项性能的稳定性;(2)四水硝酸钙的高温分解逐步进行(如下述反应式1-3),作为矿化剂时,相比于传统采用的石灰乳,能够避免某一温度下因气体大量释放而对砖体产生破坏;(3)四水硝酸钙高温下气体释放总量大,因此四水硝酸钙还同时能够起到造孔剂的作用;(4)单独使用钙质矿化剂(即四水硝酸钙)砖体不会泛黄,并且砖中低熔相熔点较高(CaO-SiO2二元系最低共熔点1430℃),有利于提升成品砖高温性能。
Ca(NO3)2·4H2O→Ca(NO3)2 反应式1
Ca(NO3)2→Ca(NO2)2 反应式2
Ca(NO2)2→CaO 反应式3 。
本发明针对目前采用机压可燃法生产轻质硅砖时的不足和缺陷,在轻质硅砖生产原料中添加四水硝酸钙并配合锯末、硅石细粉以及特定的预混合搅拌步骤,产生以下有益效果:
(1)液态四水硝酸钙与硅石细粉和锯末的预混合搅拌实现了成品轻质硅砖中硅石细粉和造孔剂矿化剂的原料的均匀分布,提升了成品砖各项性能的稳定性;之后再与骨料、废硅砖和结合剂进行混炼,使得均匀分布的泥料与骨料、废硅砖和结合剂充分混匀,利于提升烧后砖的性能及成品率;
(2)四水硝酸钙在硅砖的烧成过程中逐步分解为亚硝酸钙和氧化钙,分解过程呈多步进行,不会在砖内产生过大压力;配合锯末,能够在创造均匀微孔的同时避免对砖体结构产生破坏,利于高性能孔隙均匀轻质硅砖的制备;
(3)四水硝酸钙高温分解后体积收缩大,因此四水硝酸钙还能够起到造孔剂的作用;配合锯末,能够在砖内基质部位和骨料接触位置形成均匀的微孔(主要由锯末脱水和烧失产生)和缝隙(主要由四水硝酸钙脱水和分解产生),利于缓解硅砖烧成过程中产生的体积效应以及提升成品砖的孔隙均匀性;
(4)单独使用钙质矿化剂砖体不会泛黄,并且因此砖中低熔相熔点较高,生产的硅砖强度高、高温体积稳定性好、高温抗热震稳定性和高温蠕变性能优异;
(5)本发明制备方法简单,原料丰富且性价比优,烧成过程易控,适宜轻质硅砖的工业化生产,合格率高。
具体实施方式
本发明借助于四水硝酸钙低熔点特性,利用烘烤后液态四水硝酸钙与硅石细粉和锯末的湿法预混合,配合其他步骤,解决了机压可燃法生产轻质硅砖时干法混合造成的可燃物分布不均问题。并且本发明所涉及的轻质硅砖中四水硝酸钙还同时具有矿化剂和造孔剂功能,作为矿化剂和造孔剂四水硝酸钙能够做到分布均匀且高温烧成过程中逐步分解,吸收应力、降低热导率的同时不会对砖体产生破坏。本发明制备方法简单,原料丰富且性价比优,烧成过程易控,砖体不会泛黄,适宜大型硅砖的工业化生产,成品砖具有较高的强度。
下面结合具体实例对本发明进一步阐述。所有实例中,各原料的含量均以质量百分比计,且骨料的粒度 ≤ 2.18 mm,硅石细粉的粒度 ≤ 0.088mm,废硅砖的粒度≤ 0.5mm,锯末的粒度≤ 5 mm。废硅砖由生产的硅砖残品破碎制得,结合剂为纸浆废液,结合剂的用量基准为由骨料、硅石细粉、废硅砖、锯末、四水硝酸钙组成的混合料总量(即结合剂用量为该混合料总量的用量),其他原料的用量基准为占该混合料总量的用量。
实施例1
事先将锯末提前在水中浸泡腐烂,锯末和水的质量比为1:0.2,浸泡时间为24h,浸泡温度为27℃;然后将19%四水硝酸钙烘烤至熔融后加入39%硅石细粉和2%锯末(即浸泡腐烂后的锯末)并预混合搅拌,预混合搅拌的条件包括:搅拌时间为6 min,搅拌转速为100转/分,制成泥料;将泥料与30%硅砂和10%废硅砖混合,外加上述混合料2%的纸浆废液结合剂,混炼均匀,混炼时间为20 min,混炼转速为150 转/分,压制成型;砖坯自然干燥36h至残余水分<1.0 wt%,后置入隧道窑中于1450oC保温30h烧成,制得轻质硅砖。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为1.06 g/cm3,常温耐压强度为12.1 Mpa,荷重软化温度为1578℃,350℃导热系数0.30W/(m·K),1550℃永久线变化+0.0%,尺寸在50-300μm的孔的占比 75 %,产品合格率93%。
实施例2
参照实施例1进行,不同之处在于,12%四水硝酸钙,45%硅石细粉,2%锯末,31%硅砂;干燥24h,于1460oC保温36h烧成,制得轻质硅砖。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为1.08 g/cm3,常温耐压强度为11.8 Mpa,荷重软化温度为1585℃,350℃导热系数0.31W/(m·K),1550℃永久线变化+0.0%,50-300μm孔占比 73 %,产品合格率92%。
实施例3
参照实施例1进行,不同之处在于,40%硅石细粉,4%锯末,32%硅砂,5%废硅砖;干燥48小时,于1460oC保温30小时烧成,制得轻质硅砖。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为0.99 g/cm3,常温耐压强度为10.3 Mpa,荷重软化温度为1595℃,350℃导热系数0.29W/(m·K),1550℃永久线变化+0.0%,50-300μm孔占比 83 %,产品合格率94%。
实施例4
参照实施例1进行,不同之处在于,37%硅石细粉,4%锯末,干燥36小时,于1450oC保温24小时烧成,制得轻质硅砖。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为1.02 g/cm3,常温耐压强度为10.9 Mpa,荷重软化温度为1609℃,平均350℃导热系数0.30W/(m·K),1550℃永久线变化+0.0%,50-300μm孔占比 82 %,产品合格率91%。
实施例5
参照实施例1进行,不同之处在于,12%四水硝酸钙,44%硅石细粉,4%锯末,35%硅石骨料,5%废硅砖;干燥36小时,于1450oC保温36小时烧成,制得轻质硅砖。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为0.97 g/cm3,常温耐压强度为11.4 Mpa,荷重软化温度为1611℃,平均350℃导热系数0.28W/(m·K),1550℃永久线变化+0.0%,50-300μm孔占比 79 %,产品合格率93%。
实施例6
参照实施例1进行,不同之处在于,调整锯末用量使得四水硝酸钙与锯末的质量之比为1:0.5,其他组分不变,相应调整硅石骨料的用量补足混合料的100%。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为0.91 g/cm3,常温耐压强度为9.1 Mpa,荷重软化温度为1569℃,350℃导热系数0.31W/(m·K),1550℃永久线变化+0.0%,50-300μm孔占比 62 %,产品合格率90%。
实施例7
参照实施例1进行,不同之处在于,调整锯末用量使得四水硝酸钙与锯末的质量之比为1:0.05,其他组分不变,相应调整硅石骨料的用量补足混合料的100%。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为1.18 g/cm3,常温耐压强度为12.4 Mpa,荷重软化温度为1595℃,350℃导热系数0.37W/(m·K),1550℃永久线变化+0.0%,50-300μm孔占比 73 %,产品合格率89%。
实施例8
参照实施例1进行,不同之处在于,调整硅石细粉用量使得四水硝酸钙与硅石细粉的质量之比为1:5,其他组分不变,相应调整硅石骨料的用量补足混合料的100%。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为1.16 g/cm3,常温耐压强度为11.8 Mpa,荷重软化温度为1572℃,350℃导热系数0.38W/(m·K),1550℃永久线变化+0.0%,50-300μm孔占比 78 %,产品合格率88%。
实施例9
参照实施例1进行,不同之处在于,锯末不进行事先腐烂,而是将粉末锯末直接参与混合。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为1.08 g/cm3,常温耐压强度为10.1 Mpa,荷重软化温度为1562℃,350℃导热系数0.37W/(m·K),1550℃永久线变化+0.0%,50-300μm孔占比 72 %,产品合格率86%。
对比例1
其采用矿化剂石灰乳,配合常规制备方法制备硅砖,具体如下:
先将35.0 wt%的硅砂、45%硅石细粉、10 wt%的废硅砖、2%锯末和8.0 wt%石灰乳混合,外加上述混合料1.5 wt%的纸浆废液结合剂,混炼均匀,压制成型;砖坯自然干燥24h后置入隧道窑中于1450oC保温36h烧成,制得轻质硅砖。
所得硅砖经检测,体积密度为1.15 g/cm3,常温耐压强度为5.6 Mpa,荷重软化温度为1539℃,350℃导热系数0.38W/(m·K),1550℃永久线变化+0.2%,50-300μm孔占比 69%,产品合格率80%。
可以看出,对比例1,相比于实施例1,其采用常规配方和方法,所得硅砖常温耐压强度和荷重软化温度低,导热系数高,孔径分布均匀性差。
对比例2
其采用矿化剂石灰乳和铁鳞的组合,配合常规制备方法制备硅砖,具体如下:
先将38.0 wt%的硅砂、45%硅石细粉、10 wt%的废硅砖、2%锯末和4.0 wt%石灰乳和1%铁鳞混合,外加上述混合料1.5 wt%的纸浆废液结合剂,混炼均匀,压制成型;砖坯自然干燥36h后置入隧道窑中于1450oC保温24h烧成,制得轻质硅砖。
所得硅砖经检测,体积密度为1.16 g/cm3,常温耐压强度为5.3 Mpa,荷重软化温度为1510℃,350℃导热系数0.38W/(m·K),1550℃永久线变化+0.1%,50-300μm孔占比 62%,产品合格率82%。
可以看出,对比例2,相比于实施例1,其采用常规配方和方法,所得硅砖常温耐压强度和荷重软化温度低,导热系数高,孔径分布均匀性差。
对比例3
参照实施例1进行,不同之处在于,不对四水硝酸钙烘烤至熔融,而是采用四水硝酸钙粉末进行后续预混合等步骤。
所得硅砖无黑心、裂纹、松散甚至碎裂、泛黄等现象,经检测,体积密度为1.06 g/cm3,常温耐压强度为10.9 Mpa,荷重软化温度为1566℃,350℃导热系数0.33W/(m·K),1550℃永久线变化+0.2%,50-300μm孔占比 69 %,产品合格率82%。
对比例4
参照实施例1进行,不同之处在于,不进行烘烤和预混合,而是直接将所有原料进行混炼,以及进行后续压制等步骤。
所得硅砖无黑心、松散甚至碎裂、泛黄等现象,部分砖体出现裂纹,经检测,体积密度为1.06 g/cm3,常温耐压强度为10.1 Mpa,荷重软化温度为1567℃,350℃导热系数0.36W/(m·K),1550℃永久线变化+0.3%,50-300μm孔占比 65 %,产品合格率75%。
Claims (8)
1.一种轻质硅砖的制备方法,其特征在于,包括如下步骤:
S1、将四水硝酸钙烘烤至熔融,将熔融的四水硝酸钙与硅石细粉、锯末进行预混合搅拌,获得泥料;四水硝酸钙与硅石细粉、锯末的质量之比为1:1.5-5:0.05-0.5;S1中,以原料总量为基准,四水硝酸钙的用量占10.1wt%~20wt%,硅石细粉的用量占30wt%~50wt%,锯末的用量占1wt%~10wt%;
S2、将S1的泥料与骨料、废硅砖和结合剂进行混炼,之后压制成砖坯;S2中,以原料总量为基准,骨料的用量占5wt%~57.9wt%,废硅砖的用量占1wt%~15wt%;结合剂用量为原料总量的0.5%~5%;
S3、将所述砖坯经干燥、烧结工序后制得成品。
2.根据权利要求1所述的轻质硅砖的制备方法,其特征在于,所述的轻质硅砖的制备方法还包括:S1中,先将锯末提前在水中浸泡腐烂,再与熔融的四水硝酸钙与硅石细粉进行所述预混合。
3. 根据权利要求2所述的轻质硅砖的制备方法,其特征在于,所述浸泡腐烂的条件包括:锯末和水的质量比为1:0.1 -0.5,浸泡时间为12 - 72h,浸泡温度为10 - 40℃。
4. 根据权利要求1所述的轻质硅砖的制备方法,其特征在于,S1中,所述预混合搅拌的条件包括:搅拌时间为1 - 10 min,搅拌转速为50 - 500 转/分;
S2中,所述混炼的条件包括:混炼时间为1 - 30 min,混炼转速为50 - 500 转/分。
5.根据权利要求1所述的轻质硅砖的制备方法,其特征在于,所述骨料是硅石或硅砂中的一种或多种,所述废硅砖由生产的硅砖残品破碎制得,所述结合剂为纸浆废液。
6. 根据权利要求1所述的轻质硅砖的制备方法,其特征在于,所述骨料的粒度 ≤2.18 mm,所述硅石细粉的粒度 ≤ 0.088mm,所述废硅砖的粒度≤ 0.5 mm,锯末的粒度≤5 mm。
7. 根据权利要求1所述的轻质硅砖的制备方法,其特征在于,S3中所述干燥、烧结工序的过程包括:首先将砖坯自然干燥12~48h至残余水分<1.0 wt%,干燥后置入隧道窑或梭式窑中,升温至1450~1510℃保温24~48h烧结,制得成品。
8.一种轻质硅砖,其特征在于,其通过如权利要求1-7中任一项所述的轻质硅砖的制备方法制得。
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李红霞.《耐火材料手册 第2版》.北京:冶金工业出版社,2021,第609-610页. * |
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