CN107935577A - 一种中温催化型蓄热复合陶瓷材料的制备方法 - Google Patents
一种中温催化型蓄热复合陶瓷材料的制备方法 Download PDFInfo
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- CN107935577A CN107935577A CN201711299926.5A CN201711299926A CN107935577A CN 107935577 A CN107935577 A CN 107935577A CN 201711299926 A CN201711299926 A CN 201711299926A CN 107935577 A CN107935577 A CN 107935577A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000009825 accumulation Methods 0.000 title claims abstract description 18
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 17
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 17
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 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 52
- 238000001354 calcination Methods 0.000 claims abstract description 51
- 239000002002 slurry Substances 0.000 claims abstract description 40
- 238000001035 drying Methods 0.000 claims abstract description 33
- 238000001125 extrusion Methods 0.000 claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- 239000000919 ceramic Substances 0.000 claims abstract description 29
- 230000032683 aging Effects 0.000 claims abstract description 26
- 230000001404 mediated effect Effects 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 11
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 11
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 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 abstract description 10
- 238000005470 impregnation Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 35
- 241000264877 Hippospongia communis Species 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 21
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 20
- 239000000908 ammonium hydroxide Substances 0.000 claims description 20
- 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
- 239000011521 glass Substances 0.000 claims description 15
- 229910000831 Steel Inorganic materials 0.000 claims description 14
- 239000010959 steel Substances 0.000 claims description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 12
- 229920000742 Cotton Polymers 0.000 claims description 12
- 235000021355 Stearic acid Nutrition 0.000 claims description 12
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 12
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 12
- -1 phthalic acid ester Chemical class 0.000 claims description 12
- 239000008117 stearic acid Substances 0.000 claims description 12
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 10
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 10
- 229910000838 Al alloy Inorganic materials 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 10
- 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
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- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 10
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 10
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 9
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 9
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- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims description 8
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims description 8
- 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 description 8
- 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 8
- 235000019837 monoammonium phosphate Nutrition 0.000 claims description 8
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- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 6
- 229940063655 aluminum stearate Drugs 0.000 claims description 6
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- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
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- 235000019698 starch Nutrition 0.000 claims description 2
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- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims 3
- 150000001336 alkenes Chemical class 0.000 claims 2
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims 2
- 239000004793 Polystyrene Substances 0.000 claims 1
- 235000006408 oxalic acid Nutrition 0.000 claims 1
- 229920002223 polystyrene Polymers 0.000 claims 1
- 239000002023 wood Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 4
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- 238000010438 heat treatment Methods 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- 244000025254 Cannabis sativa Species 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 229910052681 coesite Inorganic materials 0.000 description 4
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- 239000000377 silicon dioxide Substances 0.000 description 4
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- 229910052682 stishovite Inorganic materials 0.000 description 4
- 229910052905 tridymite Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
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- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-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
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 1
- 230000002742 anti-folding effect Effects 0.000 description 1
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 229910052761 rare earth metal 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
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- 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
- C04B35/18—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 rich in aluminium oxide
- C04B35/19—Alkali metal aluminosilicates, e.g. spodumene
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0006—Honeycomb structures
- C04B38/0009—Honeycomb structures characterised by features relating to the cell walls, e.g. wall thickness or distribution of pores in the walls
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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Abstract
本发明提供一种中温催化型蓄热复合陶瓷材料的制备方法，主要包括：钾长石、纳米SiO2、纳米氧化锆、α氧化铝、羧甲基纤维素、聚氧化乙烯、高岭土，而后经过泥料捏合，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；本发明为绿色清洁无污染生产，产品具有强度高、抗热震性良好、加工能耗低，生产周期短，绿色清洁无污染的生产优势。该蜂窝陶瓷蓄热体的抗折强度为35～42MPa、真密度为2.2～2.4g/cm3、吸水率0.2～0.9％，气孔分布均匀，平均尺寸为10～20μm，蓄热体使用温度1000～1250℃，可满足蓄热式热力焚化炉装置中蓄热材料的性能要求。
Description
技术领域
本发明涉及一种中温催化型蓄热复合陶瓷材料的制备方法，本发明具良好的换热性能、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，耐磨性差，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
本发明提供一种中温催化型蓄热复合陶瓷材料的制备方法，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：一种中温催化型蓄热复合陶瓷材料的制备方法，其特征在于该脱硝催化剂主要由以下组分：钾长石 68～92.8份、纳米SiO2 3～10份、纳米氧化锆2～10份、α氧化铝8～10份、木浆棉2～3份、氯化聚乙烯3～6份、高岭土10～20份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物3～5份、羟丙基甲基纤维素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、莫来石5～10份、磷酸二氢铵5～10份、聚二甲基硅氧烷0.5～2份、硬脂酸铝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。
一种中温催化型蓄热复合陶瓷材料的制备方法的制备方法包括以下步骤：
（1）泥料捏合：
i）称取纳米、纳米SiO2、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物、邻苯二甲酸酯、单乙醇胺、硬脂酸，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棉浆、α氧化铝、纳米氧化锆、高岭土，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）依次添加羟丙基甲基纤维素、氯化聚乙烯，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、莫来石、磷酸二氢铵、聚二甲基硅氧烷、硬脂酸铝；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，制成浆料；将步骤5所得蜂窝陶瓷坯体放入浆料池内，裹上浆料后放入干燥炉，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。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，几何比表面积为360～700m2/m3。
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：本发明为绿色清洁无污染生产，产品具有强度高、抗热震性良好、加工能耗低，生产周期短，绿色清洁无污染的生产优势。该蜂窝陶瓷蓄热体的抗折强度为35～42MPa、真密度为2.2～2.4g/cm3、吸水率0.2～0.9％，气孔分布均匀，平均尺寸为10～20μm；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。
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
一种中温催化型蓄热复合陶瓷材料的制备方法主要由以下组分：钾长石 68份、纳米SiO2 10份、纳米氧化锆2份、α氧化铝8份、高岭土10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、羟丙基甲基纤维素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组成：氧化铝5份、硝酸铁10份、硝酸锰15份、莫来石5份、磷酸二氢铵5份、聚二甲基硅氧烷2份、硬脂酸铝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
一种中温催化型蓄热复合陶瓷材料的制备方法的制备方法包括以下步骤：
（1）泥料捏合：
i）称取钾长石、纳米SiO2、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物、邻苯二甲酸酯、单乙醇胺、硬脂酸，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棉浆、α氧化铝，纳米氧化锆、高岭土，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）依次添加羟丙基甲基纤维素、氯化聚乙烯，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18～22h，得到蜂窝陶瓷坯体；
（6）上浆：称取氧化铝、硝酸铁、硝酸锰、莫来石、磷酸二氢铵、聚二甲基硅氧烷、硬脂酸铝；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，制成浆料；将步骤5所得蜂窝陶瓷坯体放入浆料池内，裹上浆料后放入干燥炉，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。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，几何比表面积为360～700m2/m3。
实施例2
一种中温催化型蓄热复合陶瓷材料的制备方法主要由以下组分：钾长石 82份、纳米SiO2 6份、纳米氧化锆6份、α氧化铝9份、高岭土15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、羟丙基甲基纤维素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组分组成：氧化铝6份、硝酸铁8份、硝酸锰10份、莫来石9份、磷酸二氢铵8份、聚二甲基硅氧烷1.3份、硬脂酸铝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。
一种中温催化型蓄热复合陶瓷材料的制备方法的制备方法包括以下步骤：
（1）泥料捏合：
i）称取钾长石、纳米SiO2、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物、邻苯二甲酸酯、单乙醇胺、硬脂酸，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棉浆、α氧化铝，纳米氧化锆、高岭土，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）依次添加羟丙基甲基纤维素、氯化聚乙烯，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18～22h，得到蜂窝陶瓷坯体；
（6）上浆：称取氧化铝、硝酸铁、硝酸锰、莫来石、磷酸二氢铵、聚二甲基硅氧烷、硬脂酸铝；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，制成浆料；将步骤5所得蜂窝陶瓷坯体放入浆料池内，裹上浆料后放入干燥炉，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。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，几何比表面积为360～700m2/m3。
实施例3
一种中温催化型蓄热复合陶瓷材料的制备方法主要由以下组分：钾长石 92.8份、纳米SiO2 3份、纳米氧化锆10份、α氧化铝10份、高岭土20份、木棉浆2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、羟丙基甲基纤维素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；
称取氧化铝8份、硝酸铁5份、硝酸锰5份、莫来石10份、磷酸二氢铵10份、聚二甲基硅氧烷0.5份、硬脂酸铝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。
一种中温催化型蓄热复合陶瓷材料的制备方法的制备方法包括以下步骤：
（1）泥料捏合：
i）称取钾长石、纳米SiO2、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物、邻苯二甲酸酯、单乙醇胺、硬脂酸，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棉浆、α氧化铝，纳米氧化锆、高岭土，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）依次添加羟丙基甲基纤维素、氯化聚乙烯，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18～22h，得到蜂窝陶瓷坯体；
（6）上浆：称取氧化铝、硝酸铁、硝酸锰、莫来石、磷酸二氢铵、聚二甲基硅氧烷、硬脂酸铝；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，制成浆料；将步骤5所得蜂窝陶瓷坯体放入浆料池内，裹上浆料后放入干燥炉，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。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，几何比表面积为360～700m2/m3。
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 26～29MPa，耐磨损5.9～6.2cm3，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)
1.一种中温催化型蓄热复合陶瓷材料的制备方法，其特征在于该脱硝催化剂主要由以下组分：钾长石 68～92.8份、纳米SiO2 3～10份、纳米氧化锆2～10份、α氧化铝8～10份、木浆棉2～3份、氯化聚乙烯3～6份、高岭土10～20份、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物烯3～5份、羟丙基甲基纤维素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、莫来石5～10份、磷酸二氢铵5～10份、聚二甲基硅氧烷0.5～2份、硬脂酸铝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所述的一种中温催化型蓄热复合陶瓷材料的制备方法，其特征在于其制备方法包括以下步骤：
（1）泥料捏合：
i）称取钾长石、纳米SiO2、甲基丙烯酸甲酯—丁二烯—苯乙烯三元共聚物烯、邻苯二甲酸酯、单乙醇胺、硬脂酸，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棉浆、α氧化铝，纳米氧化锆、高岭土，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）依次添加羟丙基甲基纤维素、氯化聚乙烯，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（5）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：取氧化铝、硝酸铁、硝酸锰、莫来石、磷酸二氢铵、聚二甲基硅氧烷、硬脂酸铝；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，制成浆料；将步骤5所得蜂窝陶瓷坯体放入浆料池内，裹上浆料后放入干燥炉，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；
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，几何比表面积为360～700m2/m3。
3. 根据权利要求2所述的一种中温催化型蓄热复合陶瓷材料的制备方法，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所述的中温催化型蓄热复合陶瓷材料的制备方法，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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