CN108129142A - 一种丙烷脱氢装置用耐火材料及其制备方法 - Google Patents
一种丙烷脱氢装置用耐火材料及其制备方法 Download PDFInfo
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- CN108129142A CN108129142A CN201711184363.5A CN201711184363A CN108129142A CN 108129142 A CN108129142 A CN 108129142A CN 201711184363 A CN201711184363 A CN 201711184363A CN 108129142 A CN108129142 A CN 108129142A
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- refractory material
- dehydrogenating propane
- mesh
- bonding agent
- propane device
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- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000001294 propane Substances 0.000 title claims abstract description 23
- 239000011819 refractory material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000007767 bonding agent Substances 0.000 claims abstract description 18
- 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 17
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 17
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004411 aluminium Substances 0.000 claims abstract description 10
- 238000000465 moulding Methods 0.000 claims abstract description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052851 sillimanite Inorganic materials 0.000 claims abstract description 3
- 239000003595 mist Substances 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical group O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052594 sapphire Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 claims description 2
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N chromium(III) oxide Inorganic materials O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 claims description 2
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 2
- 230000035939 shock Effects 0.000 abstract description 9
- 238000005260 corrosion Methods 0.000 abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052593 corundum Inorganic materials 0.000 abstract description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 3
- 229910052849 andalusite Inorganic materials 0.000 abstract description 2
- 239000004927 clay Substances 0.000 abstract 1
- 229910052570 clay Inorganic materials 0.000 abstract 1
- 238000010304 firing Methods 0.000 abstract 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 14
- 238000000034 method Methods 0.000 description 10
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 10
- 239000012071 phase Substances 0.000 description 8
- 238000006356 dehydrogenation reaction Methods 0.000 description 7
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- 230000008569 process Effects 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000004230 steam cracking Methods 0.000 description 3
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
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- 238000011160 research Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
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- 150000001336 alkenes Chemical class 0.000 description 1
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- 229910052681 coesite Inorganic materials 0.000 description 1
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- 235000013312 flour Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000003915 liquefied petroleum gas Substances 0.000 description 1
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- 229910052682 stishovite Inorganic materials 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- 229910052905 tridymite Inorganic materials 0.000 description 1
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- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
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Abstract
本发明公开一种丙烷脱氢装置用耐火材料及其制备方法,配方包括莫来石、焦宝石、硅线石、红柱石、α‑Al2O3微粉、苏州泥、金属铝粉、金属硅粉以及TiO2,另外还添加有矿化剂、结合剂和水,通过细粉预混合、骨料混合、成型、干燥和烧成等步骤制备,所得耐火材料具有纯度高、显气孔率率低、体积密度大、抗热震性能好、抗腐性能强、莫来石含量高等优良性能。
Description
技术领域
本发明涉及一种丙烷脱氢装置用耐火材料及其制备方法,属于耐火材料领域。
背景技术
丙烯是一种重要的有机化工原料,其工业用量仅次于乙烯,同时更是一种国家战略原料,除用于生产聚丙烯外,还是生产苯酚、丙酮、丙二醇、丙烯腈、环氧丙烷、 丙烯酸、丁醇、辛醇以及异丙醇等产品的主要原料。随着丙烯下游产品需求量不断增 长,丙烯资源短缺的状况还会进一步加剧,据统计在全球的丙烯需求中,中国市场占 到了15%以上,且消费量还在以每年约5%~6%的速度增长。
丙烷催化脱氢制丙烯比烃类蒸气裂解能产生更多的丙烯,也是当前获得丙烯最先进的技术。当用蒸气裂解生产丙烯时,丙烯收率最多只有33%,而用催化脱氢法生产 丙烯,总收率可达80%以上,催化脱氢的设备投资比烃类蒸气裂解低33%,并且采用 催化脱氢的方法,能有效地利用液化石油气资源使之转变为有用的烯烃。但是国内对 丙烷脱氢技术的研究比较晚,也没有成熟的工业化生产技术,都是从国外购买工艺包, 要付出巨大的成本。因此,近年开发扩大丙烯来源的丙烷脱氢(PDH)制丙烯生产工艺成 为备受关注的热点。
丙烷脱氢工艺流程可主要划分为原料预处理、脱氢反应及催化剂再生、产品分离等三部分。其中脱氢反应(包括催化剂再生)为核心环节,脱氢反应器也成为丙烷脱 氢装置的核心设备之一,一般采用卧式固定床反应器结构,内部砌筑耐火砖。
由于反应器内还原性气氛,温度变化大,且存在结焦情况,对耐火材料腐蚀作用较强,目前国内还没有相关专门的耐火材料研究,因此,针对丙烷脱氢装置的工况条 件,开发一种具有显气孔率低、抗热震性能好、耐腐蚀的丙烷脱氢装置专用耐火材料 尤为必要和迫切。
发明内容
发明目的:本发明所要解决的技术问题是针对现有技术的不足,提供一种纯度高、显气孔率率低、体积密度大、抗热震性能好、抗腐性能强、莫来石含量高的丙烷脱氢 装置用耐火材料,满足该装置日益发展的需求,取代进口材料并实现国产化。
为了解决上述技术问题,本发明公开了一种丙烷脱氢装置用耐火材料,其配方包括如下质量百分比的组份:
上述组份含量为100%,另加以上述组份总质量计的:
矿化剂 0.2~0.8%
结合剂 3~5%
水 3~5%。
进一步的,该丙烷脱氢装置用耐火材料配方优选如下质量百分比的组份:
上述组份含量为100%,另加以上述组份总质量计的:
矿化剂 0.5%
结合剂 4%
水 3%。
其中,所述莫来石是烧结莫来石、电熔莫来石中的一种或两种的组合。
所述矿化剂为ZrO2、B2O、CeO2、Li2O、La2O3和Cr2O3中的一种或多种的组合。
所述结合剂为铝溶胶、硅溶胶和硅铝溶胶中的一种或多种。
本发明还提供该丙烷脱氢装置用耐火材料的制备方法,包括如下步骤:
(1)细粉预混合:将<240目莫来石、<200目焦宝石、<280目红柱石、α-Al2O3微粉、苏州泥、<200目金属铝粉、<400目金属硅粉、<0.5μmTiO2、矿化剂于预混机 中混匀,出料后备用;
(2)骨料混合:将3~5mm莫来石、1~3mm莫来石、1~3mm焦宝石、<1mm焦宝 石、80~100目硅线石一起加入混料机内干混5~8分钟,加入全部的水及2/3配方量的 结合剂继续混合5~10分钟,然后加入步骤(1)预混合后得到的细粉,搅拌3~5分钟, 再加入剩余1/3配方量的结合剂,最后混炼10~20分钟出料;
(3)成型:将步骤(2)得到的物料采用600吨以上压机成型;
(4)干燥:将步骤(3)成型后的物料在80~120℃条件下干燥;
(5)烧成:将步骤(4)干燥后的物料进行烧结既得。
其中,步骤(5)的烧结制度为升温至1200℃保温2~3小时,再升温至1350℃保 温4~6小时,继续升温至1530℃保温3~6小时,最后再升温至1580~1650℃保温8~12 小时。
本发明复合添加金属铝粉和金属硅粉,利用这两者具有良好的塑性,在机压成型过程中发生塑性形变,填充在粗颗粒孔隙之间,使砖坯致密化,降低了显气孔率,提 高体积密度;同时金属铝粉和硅粉熔点较低,能在较低温度下形成液相,其他组分受 到液相的浸润,有利于促进烧结,提高制品致密度和强度;除此之外,金属铝粉和金 属硅粉被氧化后,在高温下相互作用形成晶须状莫来石相,在基质中相互交错,结合 牢固,提高强度;引入<0.5mmTiO2超细粉,一方面促进制品烧结提高抵抗热应力的 能力;另一方面T iO2与Al2O3反应形成钛酸铝,有效降低制品膨胀系数,有利于提高 制品热震稳定性;由于钛酸铝在750-1300℃期间易分解,分解后就达不到预期改善热 震稳定性能的目的,因此引入一部分矿化剂,可以有效抑制钛酸铝受热分解,发挥其 优良性能;结合剂采用铝溶胶、硅溶胶或者硅铝溶胶中的一种,成型过程中利用其优 良的粘结性能,改善成型性能,提高坯体强度;烧成过程中,结合剂脱水形成Al2O3、 SiO2活性粒子,或者两者同时存在,活性极高,可有效促进烧结,提高产品致密度, 同时在基质中形成莫来石晶须网状交错连接,体积稍有膨胀填充孔隙,提高制品强度; 复合引入红柱石和硅线石,利用其高温过程中转变成莫来石相,体积发生膨胀,在制 品内部形成微裂纹,实现微裂纹增韧,提高制品热震稳定性。本发明产品物相组成中, 主晶相为莫来石相,并且直接引入和原位生成莫来石相并存,莫来石本身膨胀系数较 小,具有良好的热震稳定性和抗腐蚀性能。
有益效果:
1、本申请制备的耐火材料具有纯度高、显气孔率率低、体积密度大、抗热震性能好、抗腐性能强、莫来石含量高等优良性能。
2、本申请制备方法,预混合提高粉料均化程度,根据物相变化规律设置不同温度保温区,有利于在煅烧过程中保证各种粉料及矿化剂在基质中均匀分布,促使高温下 物理化学变化更多的向理论设计方向进行,达到理想的性能指标。
具体实施方式
下面结合具体实施方式对本发明做更进一步的具体说明,本发明的上述和/或其他 方面的优点将会变得更加清楚。
实施例1
配方为:
上述组份含量为100%,另加以上述组份总质量计的:
矿化剂 0.2%
结合剂 3%
水 5%。
制备步骤:
(1)细粉预混合:将<240目莫来石、<200目焦宝石、<280目红柱石、α-Al2O3微粉、苏州泥、<200目金属铝粉、<400目金属硅粉、<0.5μmTiO2和矿化剂于预混机 中混匀,出料后备用;
(2)骨料混合:将3~5mm莫来石、1~3mm莫来石、1~3mm焦宝石、<1mm焦宝 石、80~100目硅线石一起加入混料机内干混5~8分钟,加入全部的水以及2/3配方量 的结合剂继续混合5~10分钟,然后加入步骤(1)预混合后得到的细粉,搅拌3~5分 钟,再加入剩余1/3配方量的结合剂,最后混炼10~20分钟出料;
(3)成型:将步骤(2)得到的物料采用1000吨压机成型;
(4)干燥:将步骤(3)成型后的砖坯在80~120℃条件下干燥;
(5)烧成:将步骤(4)干燥后的物料进行烧结,升温至1200℃保温2~3小时,再升温至1350℃保温4~6小时,继续升温至1530℃保温3~6小时,最后再升温至1580~1650℃保温8~12小时。
实施例2
配方为:
上述组份含量为100%,另加以上述组份总质量计的:
矿化剂 0.5%
结合剂 4%
水 3%。
制备步骤同实施例1。
实施例3
配方为:
上述组份含量为100%,另加以上述组份总质量计的:
矿化剂 0.8%
结合剂 5%
水 3%。
制备步骤同实施例1。
将实施例1~3制备得到的耐火材料进行测试,结果见表1:
表1
指标 | 实施例1 | 实施例2 | 实施例3 |
莫来石相占比% | 67 | 66 | 64 |
耐压强度MPa | 85 | 92 | 87 |
体积密度g/cm3 | 2.41 | 2.42 | 2.41 |
显气孔率% | 19.1 | 18.6 | 18.6 |
抗热震性能(1100℃水冷)次 | 17 | 22 | 19 |
抗腐蚀性能 | 优良 | 优良 | 优良 |
本发明提供了一种丙烷脱氢装置用耐火材料及其制备方法的思路及方法,具体实现该技术方案的方法和途径很多,以上所述仅是本发明的优选实施方式,应当指出, 对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若 干改进和润饰,这些改进和润饰也应视为本发明的保护范围。本实施例中未明确的各 组成部分均可用现有技术加以实现。
Claims (7)
1.一种丙烷脱氢装置用耐火材料,其特征在于,配方包括如下质量百分比的组份:
上述组份含量为100%,另加以上述组份总质量计的:
矿化剂 0.2~0.8%
结合剂 3~5%
水 3~5%。
2.一种丙烷脱氢装置用耐火材料,其特征在于,配方包括如下质量百分比的组份:
上述组份含量为100%,另加以上述组份总质量计的:
矿化剂 0.5%
结合剂 4%
水 3%。
3.根据权利要求1或2所述一种丙烷脱氢装置用耐火材料,其特征在于,所述莫来石是烧结莫来石、电熔莫来石中的一种或两种的组合。
4.根据权利要求1或2所述一种丙烷脱氢装置用耐火材料,其特征在于,所述矿化剂为ZrO2、B2O、CeO2、Li2O、La2O3和Cr2O3中的一种或多种的组合。
5.根据权利要求1或2所述一种丙烷脱氢装置用耐火材料,其特征在于,所述结合剂为铝溶胶、硅溶胶和硅铝溶胶中的一种或多种。
6.权利要求1或2所述丙烷脱氢装置用耐火材料的制备方法,其特征在于,包括如下步骤:
(1)细粉预混合:将<240目莫来石、<200目焦宝石、<280目红柱石、α-Al2O3微粉、苏州泥、<200目金属铝粉、<400目金属硅粉、<0.5μmTiO2和矿化剂于预混机中混匀,出料后备用;
(2)骨料混合:将3~5mm莫来石、1~3mm莫来石、1~3mm焦宝石、<1mm焦宝石、80~100目硅线石一起加入混料机内干混5~8分钟,加入全部的水以及2/3配方量的结合剂继续混合5~10分钟,然后加入步骤(1)预混合后得到的细粉,搅拌3~5分钟,再加入剩余1/3配方量的结合剂,最后混炼10~20分钟出料;
(3)成型:将步骤(2)得到的物料采用600吨以上压机成型;
(4)干燥:将步骤(3)成型后的砖坯在80~120℃条件下干燥;
(5)烧成:将步骤(4)干燥后的物料进行烧结既得。
7.根据权利要求6所述丙烷脱氢装置用耐火材料的制备方法,其特征在于,步骤(5)的烧结制度为升温至1200℃保温2~3小时,再升温至1350℃保温4~6小时,继续升温至1530℃保温3~6小时,最后再升温至1580~1650℃保温8~12小时。
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CN108569907A (zh) * | 2018-06-12 | 2018-09-25 | 中钢集团洛阳耐火材料研究院有限公司 | 一种Catofin丙烷脱氢反应器用耐火材料的制备方法 |
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