CN107986766A - 一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体 - Google Patents
一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体 Download PDFInfo
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- CN107986766A CN107986766A CN201711299920.8A CN201711299920A CN107986766A CN 107986766 A CN107986766 A CN 107986766A CN 201711299920 A CN201711299920 A CN 201711299920A CN 107986766 A CN107986766 A CN 107986766A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 43
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 15
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 15
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 14
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 238000003860 storage Methods 0.000 title claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 61
- 238000001354 calcination Methods 0.000 claims abstract description 52
- 239000003054 catalyst Substances 0.000 claims abstract description 37
- 238000001035 drying Methods 0.000 claims abstract description 37
- 239000002002 slurry Substances 0.000 claims abstract description 36
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- -1 phthalic acid ester Chemical class 0.000 claims abstract description 12
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052582 BN Inorganic materials 0.000 claims abstract description 11
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 11
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920001131 Pulp (paper) Polymers 0.000 claims abstract description 11
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- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 11
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 11
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 11
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 11
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 11
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- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 11
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 11
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- 241000264877 Hippospongia communis Species 0.000 claims description 29
- 238000001914 filtration Methods 0.000 claims description 20
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 20
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- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 19
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- 239000000758 substrate Substances 0.000 claims description 19
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- 229920000049 Carbon (fiber) Polymers 0.000 claims description 10
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- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 10
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- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 10
- 239000007822 coupling agent Substances 0.000 claims description 10
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 10
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
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- 150000002148 esters Chemical class 0.000 claims 1
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- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- 230000007797 corrosion Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
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- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 description 1
- WWILHZQYNPQALT-UHFFFAOYSA-N 2-methyl-2-morpholin-4-ylpropanal Chemical compound O=CC(C)(C)N1CCOCC1 WWILHZQYNPQALT-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical class [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
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- 229910052746 lanthanum Inorganic materials 0.000 description 1
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- GFNGCDBZVSLSFT-UHFFFAOYSA-N titanium vanadium Chemical compound [Ti].[V] GFNGCDBZVSLSFT-UHFFFAOYSA-N 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,属于催化技术领域;该脱硝催化剂主要由以下组分:氧化锆35~40份,氧化铝微粉70~80份、氮化硼5~10份、SiO25~8份、蒙脱石为10~15份、木浆棉2~3份、三氧化钨4~5份、氯化聚乙烯3~6份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物3~5份、氰乙基纤维素3~6份、邻苯二甲酸酯2~3份、单乙醇胺2~3份、硬脂酸1~3份经过泥料捏合,陈腐,挤出成型、干燥与煅烧、浸渍催化浆料、再次干燥与煅烧工序制备而成。
Description
技术领域
本发明涉及一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,本发明制备的脱硝催化剂,具备良好的机械强度、抗酸腐蚀能力、抗热震性能,可适应于燃煤锅炉、火电机组的空预器中,以取代空预器中换热原件考登钢,兼具良好的换热性能、脱硝活性和较宽的温度窗口。
背景技术
近年来,能源及与之相关的环境成为全世界各国最为关注的热点。我国由于人均能源资源短缺,环境容量有限,生态脆弱,将极大的制约我国的可持续发展。国内GDP 每年高速发展,能源消耗急骤增加,环境、生态日益恶化。节能降耗成为解决能源问题的一大主攻方向。据统计,国内的工业部门能源消耗量占全国能源总量的70%。其中工业窑炉是我国耗能大户,约占全国总能耗的25%,能源利用率低是造成工业炉耗能大的主要原因之一。
与发达国家的工业炉相比,国内的工业窑炉平均热效率要低20%左右,浪费的能源相当于2亿吨标准煤,可见工业窑炉节能潜力是十分巨大的。
目前工业窑炉中的空气预热器中所用的换热原件材质为考登钢,考登钢具有机械强度高、不易破损、换热速率快、热容大等优点,但是在使用过程中,考登钢表面的搪瓷易脱落,钢材裸漏以后非常容易被硫酸氢铵或结露而成的硫酸腐蚀,尤其是全国燃煤电厂在全面实施超低排放之后。为使脱硝处理后的氮氧化物浓度达到超低排放标准,目前,主流的降低NOx排放方法是,增加一层催化剂,这样会导致系统阻力、空气预热器阻力提高,SO2向SO3的转化率上升,气溶胶排放增加,导致氨逃逸增大、腐蚀及堵塞现象增加等。
空气预热器在使用过程中,换热元件缓慢转动,温度较高的烟气和冷空气交替流经换热元件,进行周期性的换热。在一个换热周期内,换热元件的温度周期性变化,选用稀土元素Ce、La作为活性组分,具有较宽的脱硝活性温度区间。
传统的钒钛系脱硝催化剂,活性温度窗口较窄(320~400℃),运行过程中易受SO2中毒,低温下活性较低,且易产生硫铵,堵塞催化剂孔及空预器及下游设备,造成系统压降较大,增加引风机的用电成本等不利因素。
而且现有稀土基催化剂不具有蓄热功能,并且耐磨性差,活性温度范围窄,强度低,使用寿命短;使得应用范围受到极大局限,因此,我们迫切需要研究一种新型催化剂,以替代上述产品。
发明内容
本发明提供一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,以解决上述技术问题。
为解决上述技术问题,本发明方案采用的技术方案是:一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,其特征在于该脱硝催化剂主要由以下组分:氧化锆35~40份,氧化铝微粉70~80份、氮化硼5~10份、SiO25~8份、蒙脱石为10~15份、木浆棉2~3份、三氧化钨4~5份、氯化聚乙烯3~6份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物3~5份、氰乙基纤维素3~6份、邻苯二甲酸酯2~3份、单乙醇胺2~3份、硬脂酸1~3份经过泥料捏合,陈腐,挤出成型、干燥与煅烧、浸渍催化浆料、再次干燥与煅烧工序制备而成。
所述催化浆料由以下组分组成:氧化铝5~8份、硝酸铁5~10份、硝酸锰5~15份、氧化铝微粉5~10份、磷酸二氢铵5~10份、聚二甲基硅氧烷0.5~2份、碳纤维6~10份;硝酸钇3~5份、偏钨酸铵5~8份、硝酸铈5~8份,硝酸镧2~4份、钛酸酯偶联剂3份。
一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,其制备方法包括以下步骤:
(1)泥料捏合:
i)称取氧化锆,氧化铝微粉、氮化硼、SiO2、蒙脱石为、硬脂酸、单乙醇胺、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物,20%氨水调节泥料pH,去离子水:粉料重量比为0.4~0.6,搅拌捏合20min左右,通过捏合及调节添加的去离子水、氨水调节泥料指标,泥料捏合(i)泥料水分目标值38~45%,pH目标值7.8~9.4;
ii)添加20%氨水0.5~1.5份,盖上搅拌机顶盖,边搅拌边加热升温至95℃以上,然后打开顶盖,蒸发浓缩泥料水分至泥料呈颗粒状,所述泥料水分目标值25~28%,pH目标值7.8~8.5;
iii)边搅拌边依次添加木浆棉,三氧化钨,添加20%氨水,搅拌15min左右,所述泥料水分目标值29~34%,pH目标值8.1~9.2;
iv)依次添加氯化聚乙烯、氰乙基纤维素,搅拌10min以上,所述泥料水分目标值28~32%,pH目标值8.1~9.0;
(2)陈腐:将混炼好的泥料,用保鲜膜密封保存,陈腐,陈腐3-4h;
(3)预过滤挤出:将陈腐好的泥料,在预过滤挤出机上,挤出力塑性1700~2200N,过滤挤出成泥条;
(4)成型挤出:在前端装有SCR成型模具的真空挤出机上进行挤出成型,得到催化剂湿坯;
(5)干燥-煅烧:将步骤(4)得到的催化剂湿坯,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,干燥温度为90℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期5h;将干燥后的催化剂坯料进行煅烧,煅烧温度1100℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为18~22h,得到蜂窝陶瓷坯体;
(6)上浆:称取氧化铝、硝酸铁、硝酸锰、氧化铝微粉、磷酸二氢铵、聚二甲基硅氧烷、碳纤维、硝酸钇、偏钨酸铵、硝酸铈、硝酸镧、钛酸酯偶联剂,在70~95℃溶于含有1.2~3.5份草酸的水溶液,浆液比1:3,加升温至80℃并保温,用超声波震荡搅拌1~2小时,制成催化浆料;将步骤5所得蜂窝陶瓷坯体放入催化浆料池内,裹上催化浆料后放入干燥炉,干燥温度为70℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期20~30分钟,刮除蜂窝陶瓷坯体外侧的催化浆料并清理干净后,重新放入干燥炉,干燥温度为90℃,干燥周期1h;
(7)干燥-煅烧:将步骤(6)得到的蜂窝陶瓷坯体,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,进行煅烧,煅烧温度550℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为7~9h,得到中温蜂窝陶瓷。
作为优选,所述步骤(3)预过滤挤出,滤网采用网孔规格为1.0x4mm 或0.8x3mm的不锈钢滤网。
作为优选,所述步骤(4)成型挤出,挤出机控制条件为,挤出压力7MPa,挤出温度<35℃,真空度-0.094MPa左右。
本发明具有如下优点:本发明先经过高温烧制蜂窝陶瓷胚体,再将蜂窝陶瓷坯体上浆,最后经过中温烧制而成。本发明提高催化剂抗烧结能力,有利于提高催化剂热稳定性;可适应于燃煤锅炉、火电机组的空预器中;氧化铝微粉作为蓄热材料已经得到广泛应用,在蓄热材料使用过程中温度变化的幅度也很大,也没有发现蓄热材料破裂,因此可完全满足作为催化剂载体的要求。因此,如果选择低成本的氧化铝微粉蜂窝陶瓷载体,可明显降低催化剂的成本,同时,由于整体式催化剂是轴向传热,可利用氧化铝微粉蜂窝陶瓷载体的蓄热功能,提高催化剂温度的均匀性,改善催化性能。本发明在中温的环境下的脱硝率极高,反应条件温和,对环境无任何污染。
具体实施方式
为了便于理解本发明,下面将实施例对本发明进行更全面的描述。但是本发明可以以不同的形式来实现,并不限于本文所描述的实施例。相反的,提供这些实施例的目的是使对本发明的公开内容更加透彻全面。
实施例1
一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体主要由以下组分:氧化锆35份,氧化铝微粉80份、氮化硼5份、SiO28份、蒙脱石为10份、木浆棉2份、三氧化钨4份、氯化聚乙烯3份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物5份、氰乙基纤维素3份、邻苯二甲酸酯3份、单乙醇胺2份、硬脂酸3份经过泥料捏合,陈腐,挤出成型、干燥与煅烧、浸渍催化浆料、再次干燥与煅烧工序制备而成。
所述催化浆料由以下组分构成:氧化铝5份、硝酸铁10份、硝酸锰15份、氧化铝微粉5份、磷酸二氢铵5份、聚二甲基硅氧烷2份、碳纤维10份、硝酸钇5份、偏钨酸铵8份、硝酸铈5份、硝酸镧4份、钛酸酯偶联剂3份。
其制备方法包括以下步骤:
(1)泥料捏合:
i)称取氧化锆,氧化铝微粉、氮化硼、SiO2、蒙脱石、硬脂酸、单乙醇胺、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物,20%氨水调节泥料pH,去离子水:粉料重量比为0.4~0.6,搅拌捏合20min左右,通过捏合及调节添加的去离子水、氨水调节泥料指标,泥料捏合(i)泥料水分目标值38~45%,pH目标值7.8~9.4;
ii)添加20%氨水0.5份,盖上搅拌机顶盖,边搅拌边加热升温至95℃以上,然后打开顶盖,蒸发浓缩泥料水分至泥料呈颗粒状,所述泥料水分目标值25~28%,pH目标值7.8~8.5;
iii)边搅拌边依次添加木浆棉,三氧化钨,添加20%氨水,搅拌15min左右,所述泥料水分目标值29~34%,pH目标值8.1~9.2;
iv)依次添加氯化聚乙烯、氰乙基纤维素,搅拌10min以上,所述泥料水分目标值28~32%,pH目标值8.1~9.0。
(2)陈腐:将混炼好的泥料,用保鲜膜密封保存,陈腐,陈腐4h;
(3)预过滤挤出:将陈腐好的泥料,在预过滤挤出机上,挤出力塑性1700~2200N,滤网采用网孔规格为1.0x4mm 或0.8x3mm的不锈钢滤网,过滤挤出成泥条;
(4)成型挤出:在前端装有SCR成型模具的真空挤出机上进行挤出成型,挤出机控制条件为,挤出压力7MPa,挤出温度<35℃,真空度-0.094MPa左右,得到催化剂湿坯;
(5)干燥-煅烧:将步骤(4)得到的催化剂湿坯,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,干燥温度为90℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期5h;将干燥后的催化剂坯料进行煅烧,煅烧温度1100℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为18h,得到蜂窝陶瓷坯体。
(6)上浆:称取氧化铝、硝酸铁、硝酸锰、氧化铝微粉、磷酸二氢铵、聚二甲基硅氧烷、碳纤维、硝酸钇、偏钨酸铵、硝酸铈,硝酸镧、钛酸酯偶联剂,在70℃溶于含有1.2份草酸的水溶液,浆液比1:3,加升温至80℃并保温,用超声波震荡搅拌1小时,制成催化浆料;将步骤5所得蜂窝陶瓷坯体放入催化浆料池内,裹上催化浆料后放入干燥炉,干燥温度为70℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期20分钟,刮除蜂窝陶瓷坯体外侧的催化浆料并清理干净后,重新放入干燥炉,干燥温度为90℃,干燥周期1h;
(7)干燥-煅烧:将步骤(6)得到的蜂窝陶瓷坯体,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,进行煅烧,煅烧温度550℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为9h,得到中温蜂窝陶瓷。所得产品几何尺寸为150x150x(500~1250)mm,孔径为5~8mm,内壁厚0.7~1.2mm。
实施例2
一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体主要由以下组分:氧化锆38份,氧化铝微粉75份、氮化硼7份、SiO26份、蒙脱石为14份、木浆棉3份、三氧化钨5份、氯化聚乙烯5份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物4份、氰乙基纤维素5份、邻苯二甲酸酯2份、单乙醇胺3份、硬脂酸2份经过泥料捏合,陈腐,挤出成型、干燥与煅烧、浸渍催化浆料、再次干燥与煅烧工序制备而成。
所述催化浆料由以下成分组成:氧化铝6份、硝酸铁8份、硝酸锰10份、氧化铝微粉9份、磷酸二氢铵8份、聚二甲基硅氧烷1.3份、碳纤维7份、硝酸钇4份、偏钨酸铵7份、硝酸铈6份、硝酸镧3份、钛酸酯偶联剂3份。
其制备方法包括以下步骤:
(1)泥料捏合:
i)称取氧化锆38份,氧化铝微粉75份、氮化硼7份、SiO26份、蒙脱石为14份、硬脂酸2份、单乙醇胺3份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物4份,20%氨水调节泥料pH,去离子水:粉料重量比为0.4~0.6,搅拌捏合20min左右,通过捏合及调节添加的去离子水、氨水调节泥料指标,泥料捏合(i)泥料水分目标值38~45%,pH目标值7.8~9.4;
ii)添加20%氨水1份,盖上搅拌机顶盖,边搅拌边加热升温至95℃以上,然后打开顶盖,蒸发浓缩泥料水分至泥料呈颗粒状,所述泥料水分目标值25~28%,pH目标值7.8~8.5;
iii)边搅拌边依次添加木浆棉3份,三氧化钨5份,添加20%氨水,搅拌15min左右,所述泥料水分目标值29~34%,pH目标值8.1~9.2;
iv)依次添加氯化聚乙烯5份、氰乙基纤维素5份,搅拌10min以上,所述泥料水分目标值28~32%,pH目标值8.1~9.0。
(2)陈腐:将混炼好的泥料,用保鲜膜密封保存,陈腐,陈腐3h;
(3)预过滤挤出:将陈腐好的泥料,在预过滤挤出机上,挤出力塑性1700~2200N,滤网采用网孔规格为1.0x4mm 或0.8x3mm的不锈钢滤网,过滤挤出成泥条;
(4)成型挤出:在前端装有SCR成型模具的真空挤出机上进行挤出成型,挤出机控制条件为,挤出压力7MPa,挤出温度<35℃,真空度-0.094MPa左右,得到催化剂湿坯;
(5)干燥-煅烧:将步骤(4)得到的催化剂湿坯,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,干燥温度为90℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期5h;将干燥后的催化剂坯料进行煅烧,煅烧温度1100℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为21h,得到蜂窝陶瓷坯体。
(6)上浆:称取氧化铝、硝酸铁、硝酸锰、氧化铝微粉、磷酸二氢铵、聚二甲基硅氧烷、碳纤维、硝酸钇、偏钨酸铵、硝酸铈、硝酸镧、钛酸酯偶联剂,在85℃溶于含有2.2份草酸的水溶液,浆液比1:3,加升温至80℃并保温,用超声波震荡搅拌1.5小时,制成催化浆料;将步骤5所得蜂窝陶瓷坯体放入催化浆料池内,裹上催化浆料后放入干燥炉,干燥温度为70℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期25分钟,刮除蜂窝陶瓷坯体外侧的催化浆料并清理干净后,重新放入干燥炉,干燥温度为90℃,干燥周期1h;
(7)干燥-煅烧:将步骤(6)得到的蜂窝陶瓷坯体,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,进行煅烧,煅烧温度550℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为8h,得到中温蜂窝陶瓷。所得产品几何尺寸为150x150x(500~1250)mm,孔径为5~8mm,内壁厚0.7~1.2mm。
实施例3
一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体主要由以下组分:氧化锆40份,氧化铝微粉70份、氮化硼10份、SiO25份、蒙脱石为15份、木浆棉3份、三氧化钨5份、氯化聚乙烯6份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物3份、氰乙基纤维素6份、邻苯二甲酸酯2份、单乙醇胺2份、硬脂酸1份经过泥料捏合,陈腐,挤出成型、干燥与煅烧、浸渍催化浆料、再次干燥与煅烧工序制备而成。
所述催化浆料由以下成分组成:氧化铝8份、硝酸铁5份、硝酸锰5份、氧化铝微粉10份、磷酸二氢铵10份、聚二甲基硅氧烷0.5份、碳纤维6份、硝酸钇3份、偏钨酸铵5份、硝酸铈8份,硝酸镧2份、钛酸酯偶联剂3份。
(1)泥料捏合:
i)称取氧化锆40份,氧化铝微粉80份、氮化硼10份、SiO25份、蒙脱石为15份、硬脂酸1份、单乙醇胺2份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物3份,20%氨水调节泥料pH,去离子水:粉料重量比为0.4~0.6,搅拌捏合20min左右,通过捏合及调节添加的去离子水、氨水调节泥料指标,泥料捏合(i)泥料水分目标值38~45%,pH目标值7.8~9.4;
ii)添加20%氨水1.5份,盖上搅拌机顶盖,边搅拌边加热升温至95℃以上,然后打开顶盖,蒸发浓缩泥料水分至泥料呈颗粒状,所述泥料水分目标值25~28%,pH目标值7.8~8.5;
iii)边搅拌边依次添加木浆棉3份,三氧化钨5份,添加20%氨水,搅拌15min左右,所述泥料水分目标值29~34%,pH目标值8.1~9.2;
iv)依次添加氯化聚乙烯6份、氰乙基纤维素3份,搅拌10min以上,所述泥料水分目标值28~32%,pH目标值8.1~9.0。
(2)陈腐:将混炼好的泥料,用保鲜膜密封保存,陈腐,陈腐3h;
(3)预过滤挤出:将陈腐好的泥料,在预过滤挤出机上,挤出力塑性1700~2200N,滤网采用网孔规格为1.0x4mm 或0.8x3mm的不锈钢滤网,过滤挤出成泥条;
(4)成型挤出:在前端装有SCR成型模具的真空挤出机上进行挤出成型,挤出机控制条件为,挤出压力7MPa,挤出温度<35℃,真空度-0.094MPa左右,得到催化剂湿坯;
(5)干燥-煅烧:将步骤(4)得到的催化剂湿坯,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,干燥温度为90℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期5h;将干燥后的催化剂坯料进行煅烧,煅烧温度1100℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为22h,得到蜂窝陶瓷坯体。
(6)上浆:称取氧化铝、硝酸铁、硝酸锰、氧化铝微粉、磷酸二氢铵、聚二甲基硅氧烷、碳纤维、硝酸钇、偏钨酸铵、硝酸铈,硝酸镧、钛酸酯偶联剂,在95℃溶于含有1.2~3.5份草酸的水溶液,浆液比1:3,加升温至80℃并保温,用超声波震荡搅拌2小时,制成催化浆料;将步骤5所得蜂窝陶瓷坯体放入催化浆料池内,裹上催化浆料后放入干燥炉,干燥温度为70℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期30分钟,刮除蜂窝陶瓷坯体外侧的催化浆料并清理干净后,重新放入干燥炉,干燥温度为90℃,干燥周期1h;
(7)干燥-煅烧:将步骤(6)得到的蜂窝陶瓷坯体,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,进行煅烧,煅烧温度550℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为7h,得到中温蜂窝陶瓷。所得产品几何尺寸为150x150x(500~1250)mm,孔径为5~8mm,内壁厚0.7~1.2mm。
将本发明实施例1-3所得产品与从市场上买到的其他公司产品进行对比,得到以下检测指标:
经测试,本发明催化剂的抗压强度轴向为 45~48MPa,耐磨损2.7~3.0cm3,催化剂的使用寿命在5~6年,具有较高的强度和导热系数,因此具有广泛的社会和经济价值。
本发明所述的实施例仅仅是对本发明的优选实施方式进行的描述,并非对本发明构思和范围进行限定,在不脱离本发明涉及思想的前提下,本领域中工程技术人员对本发明的技术方案作出的各种变形和改进,均应落入本发明的保护范围,本发明请求保护的技术内用,已经全部记载在权利要求书中。
Claims (4)
1.一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,其特征在于该脱硝催化剂主要由以下组分:该脱硝催化剂主要由以下组分:氧化锆35~40份,氧化铝微粉70~80份、氮化硼5~10份、SiO25~8份、蒙脱石为10~15份、木浆棉2~3份、三氧化钨4~5份、氯化聚乙烯3~6份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物3~5份、氰乙基纤维素3~6份、邻苯二甲酸酯2~3份、单乙醇胺2~3份、硬脂酸1~3份经过泥料捏合,陈腐,挤出成型、干燥与煅烧、浸渍催化浆料、再次干燥与煅烧工序制备而成;
所述催化浆料由以下组分组成:氧化铝5~8份、硝酸铁5~10份、硝酸锰5~15份、氧化铝微粉5~10份、磷酸二氢铵5~10份、聚二甲基硅氧烷0.5~2份、碳纤维6~10份;硝酸钇3~5份、偏钨酸铵5~8份、硝酸铈5~8份,硝酸镧2~4份、钛酸酯偶联剂3份。
2.根据权利要求1所述的一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,其特征在于其制备方法包括以下步骤:
(1)泥料捏合:
i)称取氧化锆,氧化铝微粉、氮化硼、SiO2、蒙脱石为、硬脂酸、单乙醇胺、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物,20%氨水调节泥料pH,去离子水:粉料重量比为0.4~0.6,搅拌捏合20min左右,通过捏合及调节添加的去离子水、氨水调节泥料指标,泥料捏合(i)泥料水分目标值38~45%,pH目标值7.8~9.4;
ii)添加20%氨水0.5~1.5份,盖上搅拌机顶盖,边搅拌边加热升温至95℃以上,然后打开顶盖,蒸发浓缩泥料水分至泥料呈颗粒状,所述泥料水分目标值25~28%,pH目标值7.8~8.5;
iii)边搅拌边依次添加木浆棉,三氧化钨,添加20%氨水,搅拌15min左右,所述泥料水分目标值29~34%,pH目标值8.1~9.2;
iv)依次添加氯化聚乙烯、氰乙基纤维素,搅拌10min以上,所述泥料水分目标值28~32%,pH目标值8.1~9.0;
(2)陈腐:将混炼好的泥料,用保鲜膜密封保存,陈腐,陈腐3-4h;
(3)预过滤挤出:将陈腐好的泥料,在预过滤挤出机上,挤出力塑性1700~2200N,过滤挤出成泥条;
(4)成型挤出:在前端装有SCR成型模具的真空挤出机上进行挤出成型,得到催化剂湿坯;
(5)干燥-煅烧:将步骤(4)得到的催化剂湿坯,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,干燥温度为90℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期5h;将干燥后的催化剂坯料进行煅烧,煅烧温度1100℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为18~22h,得到蜂窝陶瓷坯体;
(6)上浆:称取氧化铝、硝酸铁、硝酸锰、氧化铝微粉、磷酸二氢铵、聚二甲基硅氧烷、碳纤维、硝酸钇、偏钨酸铵、硝酸铈、硝酸镧、钛酸酯偶联剂,在70~95℃溶于含有1.2~3.5份草酸的水溶液,浆液比1:3,加升温至80℃并保温,用超声波震荡搅拌1~2小时,制成催化浆料;将步骤5所得蜂窝陶瓷坯体放入催化浆料池内,裹上催化浆料后放入干燥炉,干燥温度为70℃,控制温度从30℃起,按5℃/小时梯度递增,干燥周期20~30分钟,刮除蜂窝陶瓷坯体外侧的催化浆料并清理干净后,重新放入干燥炉,干燥温度为90℃,干燥周期1h;
(7)干燥-煅烧:将步骤(6)得到的蜂窝陶瓷坯体,转移至铝合金托盘上,用带保温棉的玻璃钢材质的盒盖包装好,进行煅烧,煅烧温度550℃,煅烧过程中,控制温度从100℃起,按100℃/小时梯度递增,煅烧时间为7~9h,得到中温蜂窝陶瓷。
3. 根据权利要求2所述的一种复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,其特征在于:步骤(3)预过滤挤出,滤网采用网孔规格为1.0x4mm 或0.8x3mm的不锈钢滤网。
4.根据权利要求2所述的复合中温稀土脱硝陶瓷材料的蓄热陶瓷体,其特征在于:步骤(4)成型挤出,挤出机控制条件为,挤出压力7MPa,挤出温度<35℃,真空度-0.094MPa左右。
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