CN116253574A - 一种低铝超低气孔氯化炉用耐火材料的制备方法 - Google Patents
一种低铝超低气孔氯化炉用耐火材料的制备方法 Download PDFInfo
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 62
- 238000005660 chlorination reaction Methods 0.000 title claims abstract description 35
- 239000011819 refractory material Substances 0.000 title claims abstract description 22
- 239000011148 porous material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 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 claims abstract description 34
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 15
- 239000011591 potassium Substances 0.000 claims abstract description 15
- 239000005350 fused silica glass Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 13
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- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 3
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 12
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 229910052903 pyrophyllite Inorganic materials 0.000 claims 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims 1
- 238000001354 calcination Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 14
- 239000011159 matrix material Substances 0.000 abstract description 8
- 229910052906 cristobalite Inorganic materials 0.000 abstract description 5
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- 239000012071 phase Substances 0.000 abstract description 4
- 239000007791 liquid phase Substances 0.000 abstract description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
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- 230000001737 promoting effect Effects 0.000 abstract description 2
- 238000010304 firing Methods 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- 238000009835 boiling Methods 0.000 description 11
- 239000011449 brick Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 239000000460 chlorine Substances 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
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- 239000000126 substance Substances 0.000 description 2
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
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- 230000003628 erosive effect Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
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- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
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- 230000009467 reduction Effects 0.000 description 1
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- 230000035939 shock Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
本发明公开了一种低铝超低气孔氯化炉用耐火材料的制备方法，以高钾低铝莫来石、普通低铝莫来石、熔融石英为骨料，325目低铝原料、结合粘土为基质，经轮碾机混合，睏料后机压成型；坯体经干燥后，在高温窑炉内氧化气氛下进行烧成，最高烧成温度为1380℃‑1480℃高温烧成。由于含钾液相环带的存在，熔融石英细颗粒表面在高温时继续溶解，避免方石英化，促进整体烧结。基质中低铝原料由于经过高温煅烧，使得方石英相存在于莫来石晶间，高温烧成相变引起的体积效应得到有效缓解。通过特制低铝原料的引入可以使得基质中氧化铝含量降低，满足氯化炉中使用条件，同时避免了烧成时方石英化引起的体积膨胀效应，降低了整体气孔率。
Description
技术领域
本发明属于耐火材料领域，具体涉及一种低铝超低气孔氯化炉用耐火材料的制备方法。
背景技术
钛冶金通常采用氯化冶金的方式从钛铁矿或富钛料中将钛元素以四氯化钛形式提取出来，再根据下游产品选择还原或是氧化来生产金属钛或者氧化钛；而钛的氯化冶金根据其反应体系的不同主要分为熔盐氯化和沸腾氯化两种；沸腾氯化由于其具有产能大、不产生废盐等优势，是近年来四氯化钛生产的主流工艺，尤其是国际上先进的氯化法钛白粉生产技术均是采用沸腾氯化法生产工艺；钛冶金过程的沸腾氯化主要在沸腾氯化炉内进行，而内衬材料则是沸腾氯化炉最为重要的组成部分，是关系到其能否正常使用和运行的关键；整个沸腾氯化炉内衬的主要作用是形成气流边界，形成撞击流的约束，使得物料合理流态化，并在高温反应下起到隔热、绝热的作用；在整个运行过程中，氯化炉内成分十分复杂，主要成分为：高钛渣颗粒，TiCl4、Cl2、O2、CO、CO2、N2等；沸腾氯化炉主要分为以下几个部分：由于沸腾氯化炉的特殊结构，氯气进气口主要安装在该段，均匀的分布在四周；在通入气体后，形成撞击流，在炉底和四周内衬的约束下，形成向上的流态化反应床层；炉底和反应段内衬正常工作温度为900～1000℃，这一区域主要承受炉料在撞击流作用下的直接冲击和摩擦作用；该部位因承受物料的冲击、上升的磨损气体侵入、碳沉积发生反应而容易发生内衬材料的损坏；其损坏原因主要有：a．热的作用: 即热负荷、热冲击；b．化学作用：由于氯气、碱金属、渣等化学元素的侵入，造成内衬材料渣化和损坏，以及氯气与耐火材料的化学作用；c．机械作用：由于物料颗粒的摩擦和含尘烟气磨损造成内衬材料的受损。
专利CN103086724B“氯化炉用莫来石陶瓷釉化复合大砖的制备方法”公开了一种氯化法钛白粉生产中高温氯化炉炉衬用莫来石陶瓷釉化复合耐火材料的制备方法；该方法将釉料混合液采用人工涂刷或喷涂设备在砖面涂刷或喷2～5mm低温釉化的高温釉，在随后的烘炉过程中使砖体表面产生一层1～3mm厚的抗氯气和四氯化钛以及强酸腐蚀的高温釉化层，避免高温氯气和高温四氯化钛及强酸和氯化杂质的渗漏和腐蚀；这种方法实施起来较为困难，且在高温烘烤过程中容易出现起皮掉落等问题，对砖很难起到保护作用。
在实际运行过程中，由于温度梯度和氯气的渗透作用，热面砖后部极易发生侵蚀，造成热面砖后部慢慢被掏空；氯化炉热面砖寿命往往在8个月左右，而且容易出现突然窜气或坍塌等现象，对企业安全生产、稳定运行带来一系列问题。
对残砖进行扫描电子显微镜分析后，发现残砖中的反应区域基质中的Al2O3已经反应挥发殆尽，只剩下SiO2，而骨料中也出现了反应环带，表面Al2O3也出现反应和挥发。
发明内容
本发明的目的是提供一种低铝超低气孔氯化炉用耐火材料的制备方法，从降低砖的气孔率和提高基质中SiO2含量来着手，提高沸腾氯化炉的使用寿命。
本发明的目的采用如下技术方案实现：
一种低铝超低气孔氯化炉用耐火材料的制备方法，耐火材料的原料组成及质量百分比为：
3-1mm高钾低铝莫来石颗粒 10-30%，
3-1mm普通低铝莫来石颗粒 10-30%，
1-0.088mm普通低铝莫来石颗粒 15-30%，
0.2-0.1mm熔融石英颗粒 5-15%，
325目低铝原料细粉 15-30%，
325目结合粘土细粉 6-10%，
外加结合剂 3-5%；
以高钾低铝莫来石、普通低铝莫来石、熔融石英为骨料，325目低铝原料、结合粘土为基质，经轮碾机混合，睏料后机压成型；坯体经干燥后，在高温窑炉内氧化气氛下进行烧成，最高烧成温度为1380℃-1480℃。
所得到的低铝超低气孔氯化炉用耐火材料的制备方法中Al2O3含量为32%～43%，气孔率＜8%。
本发明提供的一种低铝超低气孔氯化炉用耐火材料的制备方法，采用上述技术方案，通过引入粗颗粒高钾低铝莫来石，高温烧成时形成不连续的局部液相环带，促进烧结；由于含钾液相环带的存在，熔融石英细颗粒表面在高温时继续溶解，避免方石英化，促进整体烧结。基质中低铝原料由于经过高温煅烧，使得方石英相存在于莫来石晶间，高温烧成相变引起的体积效应得到有效缓解；通过粗颗粒高钾低铝莫来石、细颗粒熔融石英和特质低铝原料细粉的配合作用，有效降低了整砖特别是基质中Al2O3含量，同时还大大降低了整砖气孔率；不仅避免了基质中SiO2含量过高引起的方石英化体积膨胀效应，还能够增加基质中SiO2整体含量，提高抗侵蚀性。
实施方式
为了充分说明本发明的特点，现对本发明举例加以说明，但本发明的具体实施方式不局限于以下实例，可以在允许范围内根据实际情况进行适当的方案调整：
结合具体实施例对本发明进行说明：
实施例
低铝超低气孔氯化炉用耐火材料的配料为：3-1mm高钾低铝莫来石颗粒10%，3-1mm普通低铝莫来石颗粒30%，1-0.088mm普通低铝莫来石颗粒30%，0.2-0.1mm熔融石英颗粒5%，325目低铝原料细粉15%，325目结合粘土细粉10%，外加纸浆液5%；先将结合剂加入混合均匀的骨料中，再加入预混合好的细粉部分，经轮碾机混合，睏料后机压成型；坯体经干燥后，经过1480℃烧成，烧成得到Al2O3含量为42.7%，显气孔率为7.8%。
实施例
低铝超低气孔氯化炉用耐火材料配料为：3-1mm高钾低铝莫来石颗粒10%，3-1mm普通低铝莫来石颗粒15%，1-0.088mm普通低铝莫来石颗粒25%，0.2-0.1mm熔融石英颗粒15%，325目低铝原料细粉29%，325目结合粘土细粉6%，外加纸浆液4%；先将结合剂加入混合均匀的骨料中，再加入预混合好的细粉部分，经轮碾机混合，睏料后机压成型。坯体经干燥后，经过1380℃烧成，烧成得到Al2O3含量为32.5%，显气孔率为6.6%。
实施例
低铝超低气孔氯化炉用耐火材料配料为：3-1mm高钾低铝莫来石颗粒15%，3-1mm普通低铝莫来石颗粒25%，1-0.088mm普通低铝莫来石颗粒20%，0.2-0.1mm熔融石英颗粒10%，325目低铝原料细粉24%，325目结合粘土细粉6%，外加纸浆液3%；先将结合剂加入混合均匀的骨料中，再加入预混合好的细粉部分，经轮碾机混合，睏料后机压成型。坯体经干燥后，经过1400℃烧成，烧成得到Al2O3含量为35.7%，显气孔率为7.6%。
实施例
低铝超低气孔氯化炉用耐火材料配料为：3-1mm高钾低铝莫来石颗粒20%，3-1mm普通低铝莫来石颗粒25%，1-0.088mm普通低铝莫来石颗粒25%，0.2-0.1mm熔融石英颗粒5%，325目低铝原料细粉20%，325目结合粘土细粉10%，外加纸浆液5%；先将结合剂加入混合均匀的骨料中，再加入预混合好的细粉部分，经轮碾机混合，睏料后机压成型。坯体经干燥后，经过1480℃烧成，烧成得到Al2O3含量为41.9%，显气孔率为7.4%。
实施例
低铝超低气孔氯化炉用耐火材料配料为：3-1mm高钾低铝莫来石颗粒30%，3-1mm普通低铝莫来石颗粒20%，1-0.088mm普通低铝莫来石颗粒15%，0.2-0.1mm熔融石英颗粒5%，325目低铝原料细粉20%，325目结合粘土细粉10%，外加纸浆液5%；先将结合剂加入混合均匀的骨料中，再加入预混合好的细粉部分，经轮碾机混合，睏料后机压成型。坯体经干燥后，经过1380℃烧成，烧成得到Al2O3含量为39.6%，显气孔率为7.2%。
Claims (5)
1.一种低铝超低气孔氯化炉用耐火材料的制备方法，耐火材料的原料组成及质量百分比为：
3-1mm高钾低铝莫来石颗粒 10-30%，
3-1mm普通低铝莫来石颗粒 10-30%，
1-0.088mm普通低铝莫来石颗粒 15-30%，
0.2-0.1mm熔融石英颗粒 5-15%，
325目低铝原料细粉 15-30%，
325目结合粘土细粉 6-10%，
外加结合剂 3-5%；
以高钾低铝莫来石、普通低铝莫来石、熔融石英为骨料，325目低铝原料、结合粘土为基质，经轮碾机混合，睏料后机压成型；坯体经干燥后，在高温窑炉内氧化气氛下进行烧成，最高烧成温度为1380℃-1480℃。
2.根据权利要求1所述的一种低铝超低气孔氯化炉用耐火材料的制备方法，其特征在于：高钾低铝莫来石中，Al2O3含量为44～45%，K2O含量为1.0～2.0%。
3.根据权利要求1所述的一种低铝超低气孔氯化炉用耐火材料的制备方法，其特征在于：普通低铝莫来石中，Al2O3含量为45～50%，K2O含量＜0.15%。
4.根据权利要求1所述的一种低铝超低气孔氯化炉用耐火材料的制备方法，其特征在于：低铝原料细粉 是由精选后的叶腊石原矿经过高温煅烧后破碎制成，叶腊石煅烧温度不低于1550℃，不高于1600℃，煅烧后Al2O3含量为27%～30%，Al2O3+SiO2合量≥96%。
5.根据权利要求1所述的一种低铝超低气孔氯化炉用耐火材料的制备方法，其特征在于：超低气孔低铝耐火材料中Al2O3含量为32%～43%，气孔率＜8%。
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