CN107108378A - 具有高光谱发射率的成型烧结耐火材料及其生产方法及提高耐火成型体光谱发射率的方法 - Google Patents

具有高光谱发射率的成型烧结耐火材料及其生产方法及提高耐火成型体光谱发射率的方法 Download PDF

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CN107108378A
CN107108378A CN201580041666.4A CN201580041666A CN107108378A CN 107108378 A CN107108378 A CN 107108378A CN 201580041666 A CN201580041666 A CN 201580041666A CN 107108378 A CN107108378 A CN 107108378A
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weight
sio
matrix
emissivity
brick
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F·布伦克
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P-D Refractory Co Ltd
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Abstract

本发明涉及尤其用于玻璃熔窑的烧制耐火成型体，其含有SiO2、SiC以及粘合剂或粘合剂混合物作为主要组分，其中所述材料具有高的光谱发射率，其中在基质中分布有在1μm至5μm的光谱范围内在高于1000℃的温度下具有高于基质光谱发射能力的光谱发射能力的物质，其中所述物质含有碳化硅，所述材料中的碳化硅含量为0.2至20重量％，优选为0.3至15重量％，所述材料的二氧化硅含量为至少78重量％并且具有最多6重量％的其他物质，总和为100重量％。本发明还涉及生产耐火成型体的方法以及提高耐火成型体的光谱发射率的方法。

Description

具有高光谱发射率的成型烧结耐火材料及其生产方法及提高 耐火成型体光谱发射率的方法
技术领域
本发明涉及尤其用于玻璃熔窑的烧结耐火成型体。本发明还涉及生产耐火成型体的方法以及提高耐火成型体的光谱发射率的方法。
背景技术
燃烧燃料的玻璃熔窑均为非常耗能的高温加工设备，需要利用燃烧器从上方将生产玻璃所需的原料加热到1450℃以上的温度，若为钠钙玻璃，则要加热到1550℃，使其熔化成为液态玻璃熔体。几乎仅仅通过辐射将热量传递给玻璃熔体，不仅从燃烧器火焰或燃烧气体直接传热，而且也通过上部结构(熔窑拱顶和侧壁)中玻璃熔体液面上方起到二次加热面作用的耐火衬里高温侧表面间接传热。这种情况下必然也会在拱顶和池壁之间发生相互辐射和多重反射。传热的决定性因素是参与辐射交换的炉膛主要部件随波长和温度变化的辐射特性，也就是炉内气氛、耐火材料和玻璃熔体。例如在W.Trier所著的“玻璃熔炉”(ISBN3-540-12494-2)中可找到玻璃熔炉的描述。
因为耐火材料具有选择性的辐射特性，因此随波长和温度变化的发射率就是其辐射特性的特征值，必须通过测量技术手段予以确定。出于能量上的考虑，例如进行传热计算，需要此外按照所有波长求平均的取决于温度的总发射率。这种情况下关键是大约1至5μm的波长范围，因为根据维恩位移定律和普朗克辐射定律，在玻璃熔窑中的当前温度下大部分通过辐射传递的能量均落在该范围。光谱发射率首先取决于耐火材料的化学和矿物成分。发射率可以具有0与1之间的值，后者是一种物理理想状态(所谓的黑体)。
使用致密的硅砖在熔窑上部结构尤其在熔窑拱顶中给钠钙玻璃生产熔窑砌衬，玻璃总产量的绝大部分是钠钙玻璃。由于在温度约为1500至1600℃的拱顶中使用，需要有极好的热机械材料特性，因此仅可使用不含助溶剂的、SiO2含量至少为93％通常高于95％的优质硅砖。决定其使用的另一个技术原因是硅砖成分与玻璃熔体接触有良性的溶解特性。在机械负荷明显很小的池壁区域中，也可使用比较耐腐蚀的铝锆硅耐火砖(熔铸AZS砖)，这些砖除了具有主要成分Al2O3和ZrO2之外，也含有大约12至16％少量的SiO2。然而这种情况下要注意玻璃相从砖材料中析出的危险，玻璃相在玻璃熔体中难以溶解，并且会导致形成纹影或者其他玻璃缺陷。关于硅砖和AZS材料的概况，例如可参阅书籍″Handbook ofRefractory Materials″，Hrsg.G.Routsohka u.H.Wuthnow(ISBN 978-3-8027-3162-4)。
US 4,183,761公开了具有很少气孔率的高导热硅砖的生产方法，使用粒径小于0.074mm的0.5至10重量％氮化硅(Si3N4，也含有Si2ON2)或者碳化硅(SiC)或者两者的混合物作为混合料组分，在1200至1400℃之间的烧结过程中要进行非常复杂的温度控制，并且要保持非常特殊的炉内气氛。以此保证在耐火砖烧制过程中晶粒极细的氮化物和/或者碳化物完全转变为SiO2，并且体积增大将基质孔隙填满，从而形成比较致密的耐火砖组织结构。按照该专利生产的耐火砖的化学矿物成分和辐射特性相当于传统硅砖。当然从热工学角度观察，在玻璃熔窑中尤其在拱顶中使用高导热硅砖特别不利于生产，因为在拱顶绝热层结构保持不变的情况下，热损失将会因此而增加，并且使用这样的砖无法实现辐射特性改善。
当然如果使用硅石和AZS耐火材料，从热传递角度来看有很大缺点，众所周知其总发射率会随着温度上升而急剧减小。显而易见，改善上部结构中耐火衬里的辐射特性能强化对玻璃熔体的辐射传热，从而可以节省能源和/或者提高生产效率。
因此已有人建议对朝向炉膛(使用过程中高温侧)的耐火材料表面进行涂层处理，前提条件是涂层具有比耐火基材更高的发射率。这些涂层剂(所谓的高发射率涂料)主要由一种粉末状耐火填料(或填料混合物)、至少一种粘合剂和至少一种具有高发射率的粉剂(高发射率添加剂)构成。在启动玻璃熔窑之前在耐火基材上喷涂或者刷涂薄薄一层颜色近似一致的涂层剂。
例如在专利说明书US 6,007,873中推荐了用于1000℃以上工作温度的高发射率涂层，该涂层由一种含磷酸铝的粘合剂和一种铈和铽族稀土氧化物含量为5至75重量％的高发射率添加剂构成。此类涂层一般具有10至250μm的厚度。与氧化铈(CeO2和/或者Ce2O3)相比，高发射率添加剂氧化铬(Cr2O3)和碳化硅(SiC)在使用1400至1500℃工作温度进行比较性评估的时候会因为反应引起失效。没有提供关于含氧化铈涂层的实际辐射特性以及关于基材的信息，仅仅陈述了所取得的效果，间接认为改善了熔炉的总效率。
US 6,921,431 B2公开了一种主要用于耐火材料的热保护涂层(ThermalProtective Coating)，该涂层尤其也能提高涂层基材的发射率，并且以干物质为参考主要具有大约2至20重量％一种或多种高发射率添加剂，例如六硼化硅(SiB6)、碳化硼(B4C)、四硼化硅(SiB4)、碳化硅(SiC)、二硅化钼(MoSi2)、二硅化钨(WSi2)、二硼化锆(ZrB2)、亚铬酸铜(Cr2Ce2O5)和金属氧化物。粘合剂是胶体氧化硅和/或者氧化铝，含量约为1.5至5重量％的陶土矿类稳定剂添加剂应可提高预备涂层溶液的储存性能(固体物质含量约为40至70％)。为了避免剥落，建议干燥状态下的最大涂层厚度约为25.4至254μm；提出将每m2基材表面积150至200克干物质作为最佳层厚。涂层应可在最高3500°F(1926℃)使用温度下反射热量。然而没有提出关于辐射特性的验证信息或者至少关于功能的证明。
窑炉使用寿命约为8至14年，在使用过程中尤其因为与炉料成分和蒸发产物进行反应而产生的炉气会引起强烈的热负荷及腐蚀负荷，玻璃熔窑上部结构中的耐火衬里或多或少被强烈腐蚀，主要特征表现为逐渐剥蚀材料。例如拱顶中硅砖的材料剥蚀量可能有几厘米的总厚度。很薄、晶粒极细并且因此不太耐腐蚀的涂层的使用寿命非常有限。涂层的机械特性不够充分、在基材上的附着力很差和/或者所使用的高发射率添加剂缺乏耐氧化性，以及使用过程中在涂层和耐火基材之间引起的反应，同样对使用寿命有很大的不利影响。尤其要注意，如果涂层的化学成分与玻璃的成分偏差很大，那么即使进入玻璃熔体中的涂层材料很少，也会造成玻璃缺陷。
DE 28 14 250 C2公开了改善玻璃熔窑中辐射热传递的另一种方法，按照该方法所述，使得上部结构中耐火砖的炉膛侧表面形成特殊的廓形，即可增大热辐射面。为此设计了棱锥或者截锥状凹进部分，其最大的横断面指向炉膛侧表面。较高的辐射面尤其是凹进部分如同将辐射热能集束的反射镜一样的情况可使得更多的热辐射从上部结构发射到炉膛之中。然而在该实施方式中，绝大部分指向炉膛内部的耐火衬里表面依然是光滑均匀的设计，因此按照热辐射传递的一般原理可知，理论上最多只能略微改善总辐射能力。也正是基于这个原因，在专业界依然对这种表面轮廓的效率争论不休。
发明内容
本发明的目的在于提供具有改善的热辐射能力的、用于玻璃熔窑上部结构的耐火成型材料。本发明的目的还在于给出生产所述材料的方法，以及可以提高耐火成型体的光谱发射率的方法。
可以通过权利要求1、4和11实现这些目的。相应从属权利要求所述均为本发明的有益改进实施方案。
示例性地依据附图阐述本发明。将根据本发明的成型体(1)的辐射特性与用于玻璃熔窑上部结构的常见材料、硅砖(2)和熔铸AZS材料(3)的辐射特性进行对比。
附图说明
图1所示为光谱发射率(测量温度1200℃)，
图2所示为相应的随温度变化的总发射率。
具体实施方式
在此以及在本说明书的实施例中用来测定光谱发射率的测量原理基于在相同温度和相同光学几何条件下样品材料的光谱辐射热流密度与黑体的光谱辐射热流密度的比较(所谓的静态辐射对比原理)。由在某一温度下测定的光谱发射率计算出按照波长求平均的对应于该温度的总发射率。
本发明基于出人意料的认识，若具有高发射率的物质分散存在于成型体的基质中，其中该物质与基质相容，则能够以可测量的方式显著改善烧结耐火成型体的热辐射能力。与单面涂覆的涂层相比，在根据本发明的材料中高发射率添加剂已经是材料组织的成分，因此整个成型体具有改善的辐射能力，并且由于当前主要的腐蚀性负荷引起的取决于应用的材料剥蚀不会导致改善的辐射能力的损失，如同薄涂覆的材料表面的情况。此外还可以如同通常在熔窑上部结构中使用的耐火砖一样砌衬根据本发明的材料。
本发明使用碳化硅作为耐高温的非氧化物高发射率添加剂。通常根据所谓的Acheson法在2000℃至2400℃下通过高纯石英砂(SiO2)的碳热还原和渗碳来制备碳化硅(SiC)。在最高约1600℃的温度下的高温应用中SiC的特性是，由于与来自炉内气氛的空气氧的反应(所谓的钝化氧化)而形成二氧化硅钝化层。在生产根据本发明的材料时，该过程已经在传统的烧制过程中发生。出人意料的是，围绕剩余的SiC核心即高发射率添加剂形成的SiO2保护层通过在基质中根据本发明的至少90％、优选至少94重量％的高SiO2含量决定性地增强，或者防止腐蚀(相容性)。这尤其也适用于最终在以后的应用中决定辐射特性的成型体的表面或者与表面相邻的组织。被证明有利的是，使用粒径小于1.5mm、优选小于1mm的SiC。
在本发明的范畴内认识到SiO2的积极作用之后，本发明的一个特别实施方案的有利方面在于，使用已经具有SiO2保护层的SiC颗粒，优选通过使用诸如窑具(Brennhilfsmitteln)的回收材料。
由于基质中的SiO2含量高，根据本发明的材料获得高温应用所需的热机械特性，尤其是压力流变特性。这通过传统的生产烧制得以确保，其中从所用的SiO2原料基本上在基质中形成鳞石英和/或方石英晶体SiO2成分。
用于形成根据本发明的材料的基质的基础原料是无定形SiO2或晶体SiO2或两者的混合物。对于耐火粗陶瓷材料常见的粒度为0至6mm，优选为0至4mm。例如使用透明石英玻璃(Kieselgut)或者不透明熔融石英(石英料Quarzgut，Kieselgut)或者两者的混合物作为无定形SiO2，其SiO2含量大于99重量％。在烧制砖时，在约1150℃的温度以上会转变为方石英。优选单独地或作为混合物使用由β-石英组成的天然矿物性石英岩、石英砂和石英粉作为晶体原料，其SiO2含量大于96重量％。在富含石英的原料比例高时，需要适当加入矿化剂，该矿化剂在烧制成型体时以经济的方式促使石英按需要基本上转变成方石英和鳞石英，并且不会因为与高发射率添加剂反应而破坏其辐射特性。例如氢氧化钙Ca(OH)2满足这些条件，并且被证明是特别合适的，因为额外地还发挥粘合剂的作用。
根据本发明，将含碳化硅的高发射率添加剂与至少一种粒状SiO2原料及与合适的粘合剂或粘合剂混合物任选连同水混合，从而产生可以压制的坯料。例如可以使用木质素磺酸盐(亚硫酸盐废液)、糊精、氢氧化钙和磷酸盐作为粘合剂。在此合并具有SiO2的原料，使得在干坯料中存在至少78重量％的SiO2，其中考虑到随后成型的干燥和烧成材料的基质具有至少90重量％、优选至少94重量％的SiO2。以如下方式安排含碳化物的物质在混合物中的比例，使得基于烧成材料的含量为0.2至20重量％，优选为0.3至15重量％。
制备的坯料例如形成砖块，并将砖块干燥。随后在一般对于富含SiO2的耐火材料常见的条件下在高于1200℃、优选在1300℃与1550℃之间的烧结温度下烧制砖块。以此方式处理的砖块形成针对性地基本上为晶体的基质，即具有方石英或鳞石英或两者的混合物，其中石英含量尽可能小，优选小于1重量％。
以下实施例用于说明，并非意在限制本发明的保护范围。
实施例1至3：粒状原料组分为具有4mm最大颗粒和典型粒径分布的X射线无定形熔融石英和不同量的粒径为0-1的SiC，在加入额外的1重量％亚硫酸盐废液和3.5重量％水的情况下，将它们一起作为100重量％均匀混合。SiC含量为0重量％(实施例1)、5重量％(实施例2)和15重量％(实施例3)，其中在加入0重量％和5重量％时，将各自凑足15重量％SiC缺少的部分替换成相应粒度的熔融石英。将如此获得的混合物在约80MPa的压制压力下压制成为成型体。在110℃下干燥至重量恒定之后，在约1450℃的烧结温度下烧制生坯。烧成的成型体通过X射线衍射分析测得的晶体SiO2(方石英)的含量大于50重量％。
实施例4至6：与实施例1至3相比，使用具有3mm最大颗粒的晶体SiO2作为SiO2原料组分，并且粒度为0至1mm的SiC的含量为0重量％(实施例4)、0.5重量％(实施例5)和5重量％(实施例6)。将各自凑足5重量％SiC缺少的部分替换成相应粒度的晶体SiO2。额外地加入0.5重量％亚硫酸盐废液、4重量％水和约3重量％氢氧化钙，并且混合至均匀。将在约80MPa的压制压力下压制并且随后在110℃下干燥至重量恒定的成型体在约1450℃的烧结温度下进行烧制。烧成的成型体中未转化的石英的含量低于1重量％。
测得的基本性质列于下表。给出在1600℃下按照所有波长求平均的总发射率作为辐射特性的特征值。
(*)根据DIN EN ISO 21068-1/2
来自实施例1和4的非本发明的烧制成型体的辐射特性对应于传统硅砖的辐射特性，其中来自实施例4的成型体在其他特性方面也与玻璃熔窑上部结构中使用的传统硅砖材料是可比较的。从这些实施例毫无疑问地看出，通过根据本发明在成型体基质中掺入高发射率添加剂，以可测量的方式非常有效地改善了辐射特性。出人意料的是，由实施例4和5在1600℃下的总发射率的比较可以看出，在基质中非常少的高发射率添加剂用量就已经引起显著的改善。
所有根据本发明的烧制成型体(实施例2、3、5和6)均显示出根据EN 993-9与传统硅砖相当的、优异的压力流变特性，其特征在于，在1600℃的试验温度和0.2MPa的负荷下，在5与25小时的保持时间之间流变小于0.2％。
根据实施例3制成的根据本发明的成型体在电加热炉中以1600℃的温度经历100小时。随后测定的辐射特性相当于原始成型体的辐射特性。此外，根据实施例2和6制成的根据本发明的成型体在真实条件下在钠钙玻璃熔窑上部结构中使用大致多于一个月。随后测定的暴露于热的炉内气氛的成型体表面的辐射特性同样相当于未使用的原始材料的辐射特性。
从这些实施例毫无疑问地看出，本发明以简单的方式实现了不同寻常并且完全出人意料的改进。

Claims (20)

1.用于玻璃熔窑上部结构中的成型烧制耐火材料，其含有SiO2、SiC以及粘合剂或粘合剂混合物作为主要组分，其特征在于，所述材料具有高的光谱发射率，其中在基质中分布有在1μm至5μm的光谱范围内在高于1000℃的温度下具有高于基质光谱发射能力的光谱发射能力的物质，其中所述物质含有碳化硅，所述材料中的碳化硅含量为0.2至20重量％，优选为0.3至15重量％，所述材料的二氧化硅含量为至少78重量％并且具有最多6重量％的其他物质，总和为100重量％。
2.根据权利要求1所述的材料，其特征在于，所述基质的SiO2含量为至少90重量％，优选为至少94重量％。
3.根据权利要求1和2所述的材料，其特征在于，所述其他物质包括粘合剂成分和/或杂质，如CaO、Fe2O3、P2O5、Al2O3、碱。
4.用于生产根据权利要求1至3中任一项或多项所述的用于玻璃熔窑上部结构中的耐火材料的方法，其特征在于，将在1μm至5μm的光谱范围内在高于1000℃的温度下的光谱发射能力高于耐火材料的基质的光谱发射能力的粒状物质掺入耐火材料的基质中。
5.根据权利要求4所述的方法，其特征在于，所述粒状物质含有碳化硅，并且与至少一种粒状SiO2原料和粘合剂或粘合剂混合物混合成能够压制的坯料，成型成砖块，将砖块干燥，随后进行烧制。
6.根据权利要求4和5所述的方法，其特征在于，混入粒径＜1.5mm、优选＜1mm的SiC作为含碳化硅的物质，所述材料中碳化硅的含量为0.2至20重量％，优选为0.3至15重量％，并且以在组合物中最多6重量％的含量混入木质素磺酸盐、糊精、氢氧化钙、磷酸盐或等效添加剂作为粘合剂或粘合剂混合物。
7.根据权利要求4至6所述的方法，其特征在于，所述含碳化硅的物质具有SiO2层。
8.根据上述权利要求中任一项所述的方法，其特征在于，使用回收材料尤其是窑具作为含碳化硅的物质。
9.根据权利要求4至8中任一项或多项所述的方法，其特征在于，以至少78重量％的量使用SiO2含量为至少96重量％、粒度为0至6mm、优选为0至4mm的无定形或晶体SiO2或两者的混合物作为SiO2原料。
10.根据权利要求4至9中任一项或多项所述的方法，其特征在于，在高于1200℃、优选在1300℃与1550℃之间的温度下烧制砖块。
11.用于提高成型烧制耐火材料的光谱发射率的方法，其特征在于，在耐火材料的基质中嵌入具有在高于1000℃的温度范围内比耐火材料的基质的发射率高出至少15％的总发射率的物质。
12.根据权利要求11所述的方法，其特征在于，所述耐火材料是在玻璃熔窑的上部结构和侧壁中使用的硅砖。
13.根据权利要求11和12所述的方法，其特征在于，所述耐火材料的二氧化硅含量为至少78重量％，将含碳化硅的粒状物质分布于耐火材料的基质中，所述材料中碳化硅的含量为0.2至20重量％，优选为0.3至15重量％，并且具有最多6重量％的其他物质，总和为100重量％。
14.根据权利要求11至13所述的方法，其特征在于，所述基质的SiO2含量为至少90重量％，优选为至少94重量％。
15.根据权利要求11至13所述的方法，其特征在于，将含碳化硅的物质与至少一种粒状SiO2原料和粘合剂或粘合剂混合物如木质素磺酸盐、糊精、氢氧化钙、磷酸盐或等效添加剂在加入水的情况下混合成能够压制的坯料，成型成砖块，将砖块干燥，随后在高于1200℃的温度下烧制。
16.根据权利要求15所述的方法，其特征在于，优选在1300与1550℃之间的温度下烧制砖块。
17.根据权利要求11至16至少一项所述的方法，其特征在于，使用SiC作为含碳化硅的物质。
18.根据权利要求11至17至少一项所述的方法，其特征在于，使用具有SiO2表面层的SiC(碳化硅)作为含碳化硅的物质。
19.根据权利要求11至18至少一项所述的方法，其特征在于，使用优选由窑具组成的回收材料作为含碳化硅的物质。
20.根据权利要求11至19任一项或多项所述的方法，其特征在于，以至少78重量％的量混入无定形或晶体SiO2或两者的混合物作为SiO2原料。
CN201580041666.4A 2014-08-01 2015-07-29 具有高光谱发射率的成型烧结耐火材料及其生产方法及提高耐火成型体光谱发射率的方法 Pending CN107108378A (zh)

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