CN115073191A - 一种抗高温氧化还原气氛交替耐火材料的制备方法 - Google Patents
一种抗高温氧化还原气氛交替耐火材料的制备方法 Download PDFInfo
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- 239000011819 refractory material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 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 30
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 30
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011591 potassium Substances 0.000 claims abstract description 16
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 16
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- 239000000654 additive Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000004927 clay Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 230000008021 deposition Effects 0.000 claims abstract description 9
- 230000000996 additive effect Effects 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004939 coking Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- -1 iron ion Chemical class 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- 150000002500 ions Chemical class 0.000 claims abstract description 3
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 25
- 238000010304 firing Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 3
- 235000011151 potassium sulphates Nutrition 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 235000010755 mineral Nutrition 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 239000004323 potassium nitrate Substances 0.000 claims description 2
- 235000010333 potassium nitrate Nutrition 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims 1
- 238000000465 moulding Methods 0.000 abstract description 6
- 239000011449 brick Substances 0.000 abstract description 4
- 238000005245 sintering Methods 0.000 abstract description 3
- 239000011521 glass Substances 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract 1
- 230000033116 oxidation-reduction process Effects 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 12
- 239000007767 bonding agent Substances 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000006356 dehydrogenation reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000000571 coke Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
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Abstract
本发明公开了一种抗高温氧化还原气氛交替的耐火材料。这种材料以低铝莫来石为骨料，低铝莫来石、二氧化硅微粉、结合粘土、含钾添加剂共磨粉为基质，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1100℃‑1300℃。通过引入含钾添加剂来促进SiO2转化为高硅氧玻璃相，大大降低了烧成温度。引入的含钾添加剂还能够促进Fe2+和Fe3+离子参与高硅氧玻璃相的形成，有效的溶解和封闭铁氧化物及单质铁的危害，从源头上避免了还原气氛下铁离子对2CO→CO2+C反应的催化作用，防止碳沉积及结焦现象产生，同时提高了砖的耐磨性。
Description
技术领域
本发明属于耐火材料领域，具体涉及一种抗高温氧化还原气氛交替耐火材料的制备方法。
背景技术
Catofin工艺在一个全循环中（20min左右），要进行烃蒸汽脱氢，反应器内用蒸汽清洗、空气吹扫、预热催化剂并烧掉少量沉积在催化剂上的结焦，然后抽真空、复原，开始另一次循环；具体如下：
1、丙烷脱氢制烯烃反应；该反应是强吸热反应，且反应后体积增大，所以高温低压有助于反应的进行。但温度过高会导致催化剂结焦，所以实际工作中温度不能太高。
2、待将烃类抽走后，用水蒸气对所有残余气体进行吹扫。
3、置换后通入空气，进行催化剂的烧焦，使催化剂再生。
4、抽真空并通入还原气体，消除残留的O2。
常用的耐火材料中均含有Fe2O3，这是一种十分引人注意的氧化物。耐火材料中含有的这种不稳定氧化物超过一定量时，是不宜用于有还原气氛及真空环境的炉衬的。因为Fe2O3会与气氛中的CO和H2发生如下反应，即
Fe2O3 + 3H2 = 2Fe + 3H2O；
Fe2O3+3CO = 2Fe + 3CO2 ；
而经还原生成的铁，又是如下反应的催化剂，即 2CO = CO2 + C加速了CO的分解和碳的沉积过程。
上述反应结果，会导致铁的生成，破坏了砖体的组织结构和砖内颗粒间的牢固结合，使砖体变得疏松，甚至碎裂。
在实际使用中，除了铁造成的体积效应从而产生剥落、碳沉积、还有炉衬整体位移产生的磨损。
发明内容
为了满足Catofin丙烷脱氢反应器的工况条件，改善现有耐火材料容易产生碳沉积和结焦的现象，提高材料耐磨性，本发明提供了一种抗高温氧化还原气氛交替耐火材料的制备方法。
本发明为完成上述目的采用如下技术方案：
一种抗高温氧化还原气氛交替耐火材料的制备方法，所述抗高温氧化还原气氛交替的耐火材料中各原料质量百分比为：
3-1mm低铝莫来石颗粒 40-65%；
1-0.088mm低铝莫来石颗粒 5-30%；
325目低铝莫来石细粉 20-45%；
二氧化硅微粉 1-5%；
325目结合粘土细粉 1-5%；
含钾添加剂 1-12%；
外加结合剂 3-5%。
耐火材料以低铝莫来石为骨料，低铝莫来石、二氧化硅微粉、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1100℃-1300℃；通过引入含钾添加剂来促进SiO2转化为高硅氧玻璃相，大大降低了烧成温度；引入的含钾添加剂还能够促进Fe2+和Fe3+离子参与高硅氧玻璃相的形成，有效的溶解和封闭铁氧化物及单质铁的危害，从源头上避免了还原气氛下铁离子对2CO→CO2+C反应的催化作用，阻止碳沉积及结焦现象。
低铝莫来石Al2O3含量不大于48%。
二氧化硅微粉中SiO2含量大于99且粒度小于1μm。
含钾添加剂为钾长石、钾云母等含钾的天然矿物或碳酸钾、氯化钾、硝酸钾 、硫酸钾 、氢氧化钾、碳酸氢钾的一种或几种组合。
本发明提供的一种抗高温氧化还原气氛交替的耐火材料，与现有技术相比，本发明的有益效果是在满足现有的性能要求前提下，不仅从根本上避免了铁带来的负面效应，铁的固溶同时增强了材料的耐磨性，将不利的因素（避免碳沉积、结焦）转化成有利的因素（提高耐磨性）；同时，还通过原料选择、烧成温度降低等工艺方式降低了生产成本。在实际使用中，有效避免了铁变价造成的体积效应进而剥落、碳沉积，提高了耐磨性。
为了更好的满足实际使用条件，本发明采用低铝莫来石体系，能满足现有的性能要求，不仅从根本上避免了铁带来的负面效应，铁的固溶同时增强了材料的耐磨性，将不利的因素（碳沉积、结焦）转化成有利的因素（耐磨性提高）；同时，还通过原料选择、烧成温度降低等工艺方式降低了生产成本。
具体实施方式
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：
实施例一：
使用本专利技术所制备抗高温氧化还原气氛交替的耐火材料配料为：3-1mm低铝莫来石颗粒50%，1-0.088mm低铝莫来石颗粒 20%，325目低铝莫来石细粉20%，二氧化硅微粉1%，325目结合粘土细粉5%，钾长石微粉4%，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1300℃烧成。
实施例二：
使用本专利技术所制备抗高温氧化还原气氛交替的耐火材料配料为：3-1mm低铝莫来石颗粒60%，1-0.088mm低铝莫来石颗粒 15%，325目低铝莫来石细粉10%，二氧化硅微粉4%，325目结合粘土细粉1%，钾云母微粉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1250℃烧成。
实施例三：
使用本专利技术所制备抗高温氧化还原气氛交替的耐火材料配料为：3-1mm低铝莫来石颗粒45%，1-0.088mm低铝莫来石颗粒 20%，325目低铝莫来石细粉30%，二氧化硅微粉1%，325目结合粘土细粉2%，氯化钾2%，外加树脂结合剂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1100℃烧成。
实施例四：
使用本专利技术所制备抗高温氧化还原气氛交替的耐火材料配料为：3-1mm低铝莫来石颗粒65%，1-0.088mm低铝莫来石颗粒 5%，325目低铝莫来石细粉10%，二氧化硅微粉5%，325目结合粘土细粉4%，钾长石微粉11%，外加糊精溶液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1200℃烧成。
实施例五：
使用本专利技术所制备抗高温氧化还原气氛交替的耐火材料配料为：3-1mm低铝莫来石颗粒40%，1-0.088mm低铝莫来石颗粒 30%，325目低铝莫来石细粉20%，二氧化硅微粉4%，325目结合粘土细粉5%，硫酸钾1%，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1150℃烧成。
Claims (4)
1.一种抗高温氧化还原气氛交替的耐火材料的制备方法，其特征在于：内火材料的原料组成重量百分比为：
3-1mm低铝莫来石颗粒 40-65%；
1-0.088mm低铝莫来石颗粒 5-30%；
325目低铝莫来石细粉 20-45%；
二氧化硅微粉 1-5%；
325目结合粘土细粉 1-5%；
含钾添加剂 1-12%；
外加结合剂 3-5%；
耐火材料以低铝莫来石为骨料，低铝莫来石、二氧化硅微粉、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1100℃-1300℃；通过引入含钾添加剂来促进SiO2转化为高硅氧玻璃相，大大降低了烧成温度；引入的含钾添加剂还能够促进Fe2+和Fe3+离子参与高硅氧玻璃相的形成，有效的溶解和封闭铁氧化物及单质铁的危害，从源头上避免了还原气氛下铁离子对2CO→CO2+C反应的催化作用，阻止碳沉积及结焦现象。
2.根据权利要求1所述的一种抗高温氧化还原气氛交替的耐火材料的制备方法，其特征在于：低铝莫来石Al2O3含量不大于48%。
3.根据权利要求1所述的一种抗高温氧化还原气氛交替的耐火材料的制备方法，其特征在于：二氧化硅微粉中SiO2含量大于99且粒度小于1μm。
4.根据权利要求1所述的一种抗高温氧化还原气氛交替的耐火材料的制备方法，其特征在于：含钾添加剂为钾长石、钾云母等含钾的天然矿物或碳酸钾、氯化钾、硝酸钾 、硫酸钾 、氢氧化钾、碳酸氢钾的一种或几种组合。
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