CN108975900A - 水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法 - Google Patents

水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法 Download PDF

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CN108975900A
CN108975900A CN201810935271.4A CN201810935271A CN108975900A CN 108975900 A CN108975900 A CN 108975900A CN 201810935271 A CN201810935271 A CN 201810935271A CN 108975900 A CN108975900 A CN 108975900A
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magnesium aluminate
aluminate spinel
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赵世贤
李红霞
孙红刚
蔡斌利
王岚
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Sinosteel Luoyang Institute of Refractories Research Co Ltd
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Abstract

本发明属于耐火材料技术领域，公开一种水煤浆气化炉用镁铝尖晶石‑碳化硅耐火材料的制备方法。公开的一种水煤浆气化炉用镁铝尖晶石‑碳化硅耐火材料的制备方法以能够固溶煤渣中FeO的烧结镁铝尖晶石颗粒作为骨料，以SiC粉和Si粉作为基质，将烧结镁铝尖晶石颗粒与聚碳硅烷结合剂混碾6～10分钟，混合均匀的烧结镁铝尖晶石颗粒与结合剂内加入基质，然后混碾25～30分钟，将混合料困料12~24h后压成生坯，最后在埋碳或氮气气氛下烧成得到镁铝尖晶石‑碳化硅耐火材料。本发明显著提高了耐火材料的抗渗透性，降低了煤渣的侵蚀速率；在一定程度上减小了煤渣中FeO对碳化硅的氧化作用；聚碳硅烷原位形成碳化硅结合相提高了材料强度。

Description

水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法
技术领域
本发明属于耐火材料技术领域，主要涉及一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法。
背景技术
水煤浆气化技术是目前国内外应用的主流煤气化技术；水煤浆气化炉工作环境苛刻，同时存在高温、高压、还原气体以及侵蚀性熔渣等，要求内衬材料具有高抗侵蚀性和抗热震性；目前所用材料为抗侵蚀性能优异的高铬耐火材料(Cr2O3含量80～95%)；但随着煤气化技术的发展以及气化煤种的多样化，现有高铬材料面临着诸多问题：首先，高铬耐火材料在气化炉中由于熔渣的渗透在热震过程中易导致剥落、损毁，其使用寿命为3～24个月，由于材料价格昂贵更换频繁，造成维修成本极高；其次，对于生物质灰渣或碱金属含量高的煤渣，由于其熔点低、粘度小，会加剧高铬材料的渗透，同时碱金属氧化物会与Cr2O3发生反应形成低熔物，进一步加剧高铬材料的剥落和损毁；最后，含铬耐火材料存在六价铬的污染，国外许多国家已经明令禁止或限制含铬耐火材料的使用，新型绿色-环境友好耐火材料的开发和应用将是发展趋势。
近些年，国内外相关研究者已经开展了水煤浆气化炉用无铬耐火材料的研发，其中对尖晶石基耐火材料的研究较多；另外，也先后报道了氧化铝基、氧化镁基和碳化硅基耐火材料的相关结果，包括Al2O3-CaO、Al2O3-SiC-C、MgO-MA、非氧化物结合SiC等体系，但这些材料在煤气化特殊环境下均没有表现出较好的抗煤渣侵蚀性。
尖晶石质耐火材料具有优异的高温强度和高抗侵蚀性，并且该材料已在钢包内衬、水泥窑、玻璃窑炉和黑液气化等领域得到广泛的应用；碳化硅材料同样具有优异的抗煤渣渗透性，作为水冷壁气化炉内衬材料已得到很好的应用。笔者的前期研究结果表明，尖晶石和碳化硅耐火材料在实验室模拟煤气化工作环境下的抗侵蚀和抗渗透性相比其它材料更加优异。因此，将尖晶石和碳化硅复合，制备一种氧化物-非氧化物复合耐火材料，能够发挥两种材料的各自优势，显著提高其抗煤渣侵蚀性能。
发明内容
本发明的目的在于提出一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，通过该方法制备的尖晶石-碳化硅耐火材料能够发挥尖晶石和碳化硅各自的优势，制备的耐火材料具有优异的抗煤渣侵蚀性。
为实现以上目的，本发明采用如下技术方案：
一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，所述的制备方法以能够固溶煤渣中FeO的烧结镁铝尖晶石颗粒作为骨料，以SiC粉和Si粉作为基质，所述骨料与基质的组成和加入量分别为：烧结镁铝尖晶石60～75%，SiC粉20～40%，Si粉0～5%；所述基质与骨料的总质量为100%；将烧结镁铝尖晶石颗粒与结合剂混碾6～10分钟，混合均匀的烧结镁铝尖晶石颗粒与结合剂内加入基质，然后混碾25～30分钟，将混合料困料12~24h后，在摩擦压力机或液压压机上经150～200MPa压成生坯；生坯经60oC干燥5h，100oC干燥4h，最后在埋碳或氮气气氛下经1350～1600oC烧成得到镁铝尖晶石-碳化硅耐火材料；所述的结合剂为外加，加入量为骨料和基质总质量的3～10%；所述的结合剂为碳化硅前驱体；所述的碳化硅前驱体为聚碳硅烷；所述的聚碳硅烷在压制生坯的过程中起到结合剂的作用，使坯体具有强度，聚碳硅烷在烧结过程中原位转变为碳化硅，将基质粉体和颗粒结合为一体。
所述骨料与基质的组成和加入量分别为烧结镁铝尖晶石65～72%，SiC粉24～34%，Si粉1～4%。
所述结合剂的加入量为骨料和基质总质量的4～8%。
所述结合剂的加入量为骨料和基质总质量的5～7%。
所述烧结镁铝尖晶石颗粒为富铝尖晶石，由1～3mm和0.5～1mm两种粒度组成。
所述的基质中SiC粉的为200目、325目和2000目三种粒度组成。
所述的基质中Si粉的粒度为≤5μm。
所述的聚碳硅烷由汽油、二氯乙烷、甲苯、二甲苯、四氢呋喃、正己烷中的一种作溶剂或稀释剂。
本发明提出的一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，采用上述技术方案，具有如下有益效果：
1、将尖晶石和碳化硅复合后，尖晶石作为骨料，碳化硅作为基质，一方面碳化硅基质对煤渣的不润湿性能够显著提高复合材料的抗渗透性，另一方面，尖晶石颗粒较细粉能够显著降低煤渣的侵蚀速率；另外，渣中FeO会固溶到镁铝尖晶石中形成复合尖晶石，从而在一定程度上减小了FeO对碳化硅的氧化作用；因此，尖晶石和碳化硅复合后，可充分发挥其互补作用从而有效提高材料的抗侵蚀性能。
2、聚碳硅烷在压制过程中能够起到结合剂的作用，使坯体具有一定的强度，同时在烧结过程中原位转变为碳化硅，起到结合粉体和颗粒的作用，提高了制品的性能。
3、选择性的加入Si粉在埋碳气氛下原位生成碳化硅，进一步提高制品性能，另外，在氮气气氛下生成Si3N4结合相，同样提高了制品的性能。
具体实施方式
参照以下实施例对本发明作进一步说明，但本发明不局限于下述实施例。
实施例1：一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料，其原料按重量百分比组成为：1～3mm烧结镁铝尖晶石颗粒55%，0.5～1mm烧结镁铝尖晶石颗粒10%，200目碳化硅粉7%，325目碳化硅粉23%，2000目碳化硅粉3%， 粒度≤5μm的Si粉2%，外加6%结合剂。将烧结镁铝尖晶石颗粒与聚碳硅烷结合剂混碾8分钟，然后加入碳化硅粉和Si粉，继续混碾30分钟，将混合料困料12h后，在摩擦压力机或液压压机上经150MPa压成生坯；生坯在60oC干燥5h，100oC干燥4h，最后在氮气气氛下经1450oC烧成得到镁铝尖晶石-碳化硅耐火材料。
实施例2：一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料，其原料按重量百分比组成为：1～3mm烧结镁铝尖晶石颗粒60%，0.5～1mm烧结镁铝尖晶石颗粒8%，200目碳化硅粉9%，325目碳化硅粉20%，2000目碳化硅粉2%， 粒度≤5μm的Si粉1%，外加7%聚碳硅烷结合剂；将烧结镁铝尖晶石颗粒与聚碳硅烷结合剂混碾10分钟，然后加入碳化硅粉和Si粉，继续混碾30分钟，将混合料困料20h后，在摩擦压力机或液压压机上经180MPa压成生坯；生坯在60oC干燥5h，100oC干燥4h，最后在氮气气氛下经1400oC烧成得到镁铝尖晶石-碳化硅耐火材料。
实施例3：一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料，其原料按重量百分比组成为：1～3mm烧结镁铝尖晶石颗粒58%，0.5～1mm烧结镁铝尖晶石颗粒7%，200目碳化硅粉7%，325目碳化硅粉20%，2000目碳化硅粉5%， 粒度≤5μm的Si粉3%，外加5%聚碳硅烷结合剂。将烧结镁铝尖晶石颗粒与聚碳硅烷结合剂混碾10分钟，然后加入碳化硅粉和Si粉，继续混碾28分钟，将混合料困料24h后，在摩擦压力机或液压压机上经200MPa压成生坯；生坯在60oC干燥5h，100oC干燥4h，最后在埋碳气氛下经1500oC烧成得到镁铝尖晶石-碳化硅耐火材料。
实施例4：一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料，其原料按重量百分比组成为：1～3mm烧结镁铝尖晶石颗粒62%，0.5～1mm烧结镁铝尖晶石颗粒10%，200目碳化硅粉6%，325目碳化硅粉17%，2000目碳化硅粉1%， 粒度≤5μm的Si粉4%，外加5%聚碳硅烷结合剂；将烧结镁铝尖晶石颗粒与聚碳硅烷结合剂混碾6分钟，然后加入碳化硅粉和Si粉，继续混碾25分钟，将混合料困料18h后，在摩擦压力机或液压压机上经180MPa压成生坯；生坯在60oC干燥5h，100oC干燥4h，最后在埋碳气氛下经1600oC烧成得到镁铝尖晶石-碳化硅耐火材料。

Claims (8)

1.一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述的制备方法以能够固溶煤渣中FeO的烧结镁铝尖晶石颗粒作为骨料，以SiC粉和Si粉作为基质，所述骨料与基质的组成和加入量分别为：烧结镁铝尖晶石60～75%，SiC粉20～40%，Si粉0～5%；所述基质与骨料的总质量为100%；将烧结镁铝尖晶石颗粒与结合剂混碾6～10分钟，混合均匀的烧结镁铝尖晶石颗粒与结合剂内加入基质，然后混碾25～30分钟，将混合料困料12~24h后，在摩擦压力机或液压压机上经150～200MPa压成生坯；生坯经60oC干燥5h，100oC干燥4h，最后在埋碳或氮气气氛下经1350～1600oC烧成得到镁铝尖晶石-碳化硅耐火材料；所述的结合剂为外加，加入量为骨料和基质总质量的3～10%；所述的结合剂为碳化硅前驱体；所述的碳化硅前驱体为聚碳硅烷；所述的聚碳硅烷在压制生坯的过程中起到结合剂的作用，使坯体具有强度，聚碳硅烷在烧结过程中原位转变为碳化硅，将基质粉体和颗粒结合为一体。
2.如权利要求1所述的一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述骨料与基质的组成和加入量分别为烧结镁铝尖晶石65～72%，SiC粉24～34%，Si粉1～4%。
3.如权利要求1所述的一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述结合剂的加入量为骨料和基质总质量的4～8%。
4.如权利要求1所述的一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述结合剂的加入量为骨料和基质总质量的5～7%。
5.如权利要求1所述的一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述烧结镁铝尖晶石颗粒为富铝尖晶石，由1～3mm和0.5～1mm两种粒度组成。
6.如权利要求1所述的一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述的基质中SiC粉的为200目、325目和2000目三种粒度组成。
7.如权利要求1所述的一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述的基质中Si粉的粒度为≤5μm。
8.如权利要求1所述的一种水煤浆气化炉用镁铝尖晶石-碳化硅耐火材料的制备方法，其特征在于：所述的聚碳硅烷由汽油、二氯乙烷、甲苯、二甲苯、四氢呋喃、正己烷中的一种作溶剂或稀释剂。
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CN109763204A (zh) * 2019-01-28 2019-05-17 江西嘉捷信达新材料科技有限公司 含MgAl2O4碳化硅纤维及其制备方法
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