JP6099568B2 - 硫酸チタニル含有の黒液の蒸解残留物からなる担体触媒 - Google Patents
硫酸チタニル含有の黒液の蒸解残留物からなる担体触媒 Download PDFInfo
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- JP6099568B2 JP6099568B2 JP2013534217A JP2013534217A JP6099568B2 JP 6099568 B2 JP6099568 B2 JP 6099568B2 JP 2013534217 A JP2013534217 A JP 2013534217A JP 2013534217 A JP2013534217 A JP 2013534217A JP 6099568 B2 JP6099568 B2 JP 6099568B2
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- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000002638 heterogeneous catalyst Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- JCDAAXRCMMPNBO-UHFFFAOYSA-N iron(3+);oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Ti+4].[Fe+3].[Fe+3] JCDAAXRCMMPNBO-UHFFFAOYSA-N 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 239000005078 molybdenum compound Substances 0.000 description 1
- 150000002752 molybdenum compounds Chemical class 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 150000002816 nickel compounds Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052615 phyllosilicate Inorganic materials 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004094 preconcentration Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- GRWFGVWFFZKLTI-UHFFFAOYSA-N rac-alpha-Pinene Natural products CC1=CCC2C(C)(C)C1C2 GRWFGVWFFZKLTI-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 1
- VLOPEOIIELCUML-UHFFFAOYSA-L vanadium(2+);sulfate Chemical compound [V+2].[O-]S([O-])(=O)=O VLOPEOIIELCUML-UHFFFAOYSA-L 0.000 description 1
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Description
担体触媒は経済的に極めて重要であり、量的に不均一系触媒の最も大きな群である。この担体触媒は、例えば化石原料の処理のため、中間生成物の更なる加工の際、及び化学製品の合成の際に利用される。更に、担体触媒はエミッションコントロール(Emissionsschutz)のために排気ガス浄化の分野でも経済的重要性が明らかに増している。
この背景から、本発明の基礎となる課題は、特に窒素酸化物還元の場合に、良好な活性を示す経済的に製造可能な触媒担体又は触媒を提供することである。
(a) チタン含有の出発物質を硫酸で蒸解して、固体含有の蒸解溶液を得て、
(b) 前記蒸解溶液中に含まれる固体を分離して、蒸解残留物と、主に固体不含の蒸解溶液とを得て、
(c) 場合により中和し及び/又は不純物、特に中性塩を部分的に洗い出し、
(d) 蒸解残留物を、触媒活性である少なくとも他の成分と混合し、かつ
(e) 場合により得られた混合物をか焼する。
図1は、洗浄しかつ乾燥した蒸解残留物のX線回折図を示す。この場合、特に次の不純物を検出することができる:
ルチル、酸化チタンマグネシウム、イルメナイト及びアナターゼ
次に記載された本発明の実施態様は、相互に任意に組み合わせることができ、かつこのようにして特に好ましい実施態様が生じる。
本発明の組成物の成分(I)は、不溶性の蒸解残留物であり、この不溶性の蒸解残留物は、チタン含有出発物質を硫酸で蒸解する際の硫酸法による二酸化チタンの獲得において生じる。
触媒活性成分(II)の添加の前に、この蒸解残留物は、例えば通常では触媒として又は触媒担体として使用される付加的な二酸化チタンと混合することができる。しかしながら、この付加的な二酸化チタンは、触媒活性成分(II)としても使用することができる。
本発明による組成物の製造のために、蒸解残留物単独に又は蒸解残留物と上記の付加的な二酸化チタン、好ましくは上記の酸化チタン水和物とからなる混合物に、触媒活性である他の成分(II)を添加する。
本発明による組成物(つまり触媒活性担体材料)から本発明による形状安定性の固体を製造するために、セラミックペーストを製造するために、この組成物を有機結合剤及び場合により可塑剤及び他の添加剤、ガラス繊維と、好ましくは水の存在で混合する。この場合、この組成物は、このようにして得られた混合物に対して、好ましくは60〜90質量%、特に70〜80質量%の量で使用される。
本発明による組成物及び成形体は、触媒として良好に適している。
2NH3 + NO + NO2 → 2N2 + 3H2O(排気ガス中にNO及びNO2、急速)
8NH3 + 6NO2 → 7N2 + 12H2O(排気ガス中にNO2だけ、比較的緩慢)
触媒活性の評価のために、本発明による蒸解残留物を有する多様な試料TK、TK−V及びTK−V−W(以後、チタン濃縮物又はTKと表す)並びに多様な慣用の二酸化チタンを有する比較試料(Ti−V−W1、Ti−V−W2、Ti−V3、Ti−V4)を触媒粉末として観察した。このため、触媒活性を、固定床反応器中でのアンモニア−SCR反応によるNOの分解において決定した。チタン濃縮物の試料TKの準備のために、硫酸法による二酸化チタンの製造においてチタン含有原料の硫酸による蒸解の際に生じる不溶性の蒸解残留物を苛性ソーダでpH値7〜8にまで中和し、次いで濾過し、濾過ケークの形で実験室用乾燥庫中で120℃で乾燥した。
Ti=二酸化チタン
W=試料の全質量に対して10質量%のWO3
V=試料の全質量に対して1.5質量%のV2O5
Ti−V−W1=実験室用モデル:二酸化チタン成分:350m2/gのBET表面積を有するアナターゼ
Ti−V−W2=市場で入手可能な材料、crenox A−DW−1
Ti−V3=二酸化チタン成分:90m2/gのBET表面積を有するアナターゼ
Ti−V4=二酸化チタン成分:350m2/gのBET表面積を有するアナターゼ
− 比較的純粋な、塩不含に洗浄された蒸解残留物(TK)は60%を越える触媒効率(450〜500℃の温度範囲で)を達成した。その他に、700℃を超える温度でも、不所望なNO生成は生じないことが特徴的であった。
− 1.5質量%のV2O5の添加量を有する比較的純粋な、塩不含に洗浄された蒸解残留物(TK−V)は70%を越える触媒効率(350〜400℃の温度範囲で)を達成した。
− 1.5質量%のV2O5及び10質量%のWO3の添加量を有する比較的純粋な、塩不含に洗浄された蒸解残留物(TK−V−W)は90%を越える触媒効率(350〜450℃)を達成した。
1.5質量%のV2O5並びに10質量%のWO3の添加量を有する本発明による蒸解残留物についての触媒活性を調査し、その際、この蒸解残留物は、V化合物及びW化合物の添加の前に、異なる様式で前処理されていた。
MFP廃棄物150gを、空気循環型乾燥庫中で130℃で乾燥した。次いで乳鉢中で粉砕を行った。100μmより大きな成分割合を篩別した。
収量:119g
MFP廃棄物150gを、脱塩水約500mlと一緒に磁気撹拌機で再分散させた(pH1.3)。生じた懸濁液を、次いで濃苛性ソーダ12.0gでpH値7に調節し、130℃で空気循環型乾燥庫中で乾燥した。引き続き、乳鉢中で粉砕を行った。100μmより大きな成分割合を篩別した。
収量:123g
MFP廃棄物150gを、脱塩水約500mlと一緒に磁気撹拌機で再分散させた(pH1.3)。この懸濁液を、次いで濃苛性ソーダ11.9gでpH値7に調節し、二重のブラックリボンフィルタで濾過した。生じた濾過ケークを空気循環型乾燥庫中で130℃で乾燥した。引き続き、乳鉢中で粉砕を行った。100μmより大きな成分割合を篩別した。
収量:112g
MFP廃棄物150gを、脱塩水約500mlと一緒に磁気撹拌機で再分散させた(pH1.3)。この懸濁液を、次いで濃苛性ソーダ12.3gでpH値7に調節し、二重のブラックリボンフィルタで濾過した。その後、脱塩水2リットルで洗浄した。生じた濾過ケークを空気循環型乾燥庫中で130℃で乾燥した。引き続き、乳鉢中で粉砕を行った。100μmより大きな成分割合を篩別した。
収量:110g
MFP廃棄物を苛性ソーダでpH値8に調節し、噴霧乾燥した。
MFP廃棄物を苛性ソーダでpH値8に調節し、濾過し、新たに水と共に再分散させ、噴霧乾燥した。
Claims (17)
- (I)硫酸法による二酸化チタンの獲得の際のチタン含有出発材料を硫酸で蒸解すること及び蒸解溶液から分離することによって得られる不溶性の蒸解残留物及び
(II)触媒活性であり、かつ1つ又は複数のタングステン化合物及び/又はバナジウム化合物から選択される1種の他の成分(II)
とを有する組成物の形の、選択的接触還元用の触媒において、
前記組成物は、前記組成物の固体含有率に対して、WO3として計算して1.0〜20質量%のタングステン、及び/又はV2O5として計算して0.05〜3.0質量%のバナジウムを含有し、
前記組成物はか焼された形であることを特徴とする前記触媒。 - 請求項1に記載の触媒において、
前記蒸解残留物は部分的に中和された形であることを特徴とする前記触媒。 - 請求項1又は2に記載の触媒において、
前記蒸解残留物は部分的に洗い出された形であることを特徴とする前記触媒。 - 請求項1から3までのいずれか1項に記載の触媒において、
前記蒸解残留物の硫酸塩含有率は、前記蒸解残留物の固体含有率に対して、1.0〜6.0質量%であることを特徴とする前記触媒。 - 請求項1から3までのいずれか1項に記載の触媒において、
前記組成物のpH値は、1〜5であることを特徴とする前記触媒。 - 請求項1から5までのいずれか1項に記載の触媒において、
前記組成物は6〜54質量%のTi含有率を有する前記触媒。 - 請求項1から6までのいずれか1項に記載の触媒において、
前記組成物はか焼後に3〜70m2/gのBET表面積を有する前記触媒。 - 請求項1から7までのいずれか1項に記載の触媒において、
前記組成物は、前記組成物の固体割合に対して、0.1〜10質量%の硫酸塩含有率を有することを特徴とする前記触媒。 - 請求項1から8までのいずれか1項に記載の触媒において、
前記組成物は、X線粉末回折分析により2シータ=27.5°で測定したルチル主反射の強度は、X線粉末回折図の残りの全ての反射のうちの最も強い反射の強度の少なくとも10%であることを特徴とする前記触媒。 - 請求項1から9までのいずれか1項に記載の触媒において、
前記組成物は、前記蒸解残留物中に含まれる二酸化チタンの他にアナターゼ型の付加的な二酸化チタンを含有し、蒸解残留物対付加的な二酸化チタンの質量比は50より大:50であることを特徴とする前記触媒。 - 請求項1から7までのいずれか1項に記載の触媒において、
前記組成物は、モリブデン、鉄及びマンガンからなる群から選択される少なくとも1種の他の金属酸化物を含有することを特徴とする前記触媒。 - 請求項1から11までのいずれか1項に記載の触媒において、
前記組成物は、組成物の固体含有率に対して、WO3として計算して10質量%のタングステン、及びV2O5として計算して1.5質量%のバナジウムを含有することを特徴とする前記触媒。 - 請求項1から12までのいずれか1項に記載の組成物の形の選択的接触還元用の触媒の製造方法において、
前記方法は次の工程:
(a)チタン含有出発材料を硫酸で蒸解して、固体含有の蒸解溶液を得る工程;
(b)前記蒸解溶液中に含まれる固体を分離して、蒸解残留物とほぼ固体不含の蒸解溶液とを得る工程;
(c)蒸解残留物を、触媒活性である1種の他の成分(II)と混合して組成物を得る工程;
(d)前記工程(c)で得られた組成物をか焼する工程;
を有し、
前記1種の他の成分(II)は、1つ又は複数のタングステン化合物及び/又はバナジウム化合物から選択され、かつ前記組成物の固体含有率に対して、WO3として計算して1.0〜20質量%のタングステン、及び/又はV2O5として計算して0.05〜3.0質量%のバナジウムの量で使用される、前記方法。 - 請求項13に記載の触媒の製造方法において、
前記方法は、中和し、及び/又は前記工程(b)で得られた蒸解残留物からの不純物を部分的に洗い出す工程を有する、前記方法。 - 選択的接触還元用の触媒としての、請求項1から12までのいずれか1項に記載の触媒の使用。
- 請求項1から12までのいずれか1項記載の触媒を含有する、成形及びか焼された形の形状安定性の、選択的接触還元の触媒活性の固体。
- 担体材料上に、請求項1から12までのいずれか1項記載の触媒を含有する、か焼された形の形状安定性の、選択的接触還元の触媒活性の固体。
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PCT/EP2011/064727 WO2012052209A1 (de) | 2010-10-22 | 2011-08-26 | Trägerkatalysator aus aufschlussrückständen der titanylsulfathaltigen schwarzlösung |
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DE102013213191A1 (de) * | 2013-07-05 | 2015-01-08 | Volkswagen Ag | Partikelwandstromfilter zur Abgasnachbehandlung und Verfahren zur Herstellung desselben |
DE102015205843A1 (de) * | 2015-03-31 | 2016-10-06 | Johnson Matthey Catalysts (Germany) Gmbh | Katalysator insbesondere zur Abgasreinigung |
TWI615198B (zh) * | 2015-12-16 | 2018-02-21 | 國立交通大學 | 複合型選擇性催化還原觸媒的製備方法 |
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MY193099A (en) * | 2016-07-26 | 2022-09-26 | Basf Corp | Supported catalyst, monolithic selective catalytic reduction (scr) catalyst, preparation method therefor, and method for nitrogen oxides removal |
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