JP6407278B2 - アルケンを気相酸化して不飽和アルデヒド及び/又は不飽和カルボン酸にするための、機械的に安定な中空円筒形触媒成形体 - Google Patents
アルケンを気相酸化して不飽和アルデヒド及び/又は不飽和カルボン酸にするための、機械的に安定な中空円筒形触媒成形体 Download PDFInfo
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- JP6407278B2 JP6407278B2 JP2016529945A JP2016529945A JP6407278B2 JP 6407278 B2 JP6407278 B2 JP 6407278B2 JP 2016529945 A JP2016529945 A JP 2016529945A JP 2016529945 A JP2016529945 A JP 2016529945A JP 6407278 B2 JP6407278 B2 JP 6407278B2
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Classifications
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
- B01J23/8885—Tungsten containing also molybdenum
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
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- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Description
(i)ADは、3.5〜4.5mmの範囲にあり、
(ii)下記等式による比率q:
かつ
下記等式による比率p:
X1は、ニッケル及び/又はコバルトであり、
X2は、タリウム、アルカリ金属、及び/又はアルカリ土類金属であり、
X3は、亜鉛、リン、ヒ素、ホウ素、アンチモン、スズ、セリウム、鉛、バナジウム、クロム、及び/又はタングステンであり、
X4は、ケイ素、アルミニウム、チタン、及び/又はジルコニウムであり、
aは、0.2〜5の範囲の数であり、
bは、0.01〜10の範囲の数であり、
cは、0〜10の範囲の数であり、
dは、0〜2の範囲の数であり、
eは、0〜8の範囲の数であり、
fは、0〜10の範囲の数であり、かつ
nは、式(I)中の酸素とは異なる元素の価数と頻度によって特定される数であり、
又は式(II)に相当し得る:
Y2は、モリブデン若しくはタングステン、又はモリブデン及びタングステンであり、
Y3は、アルカリ金属、タリウム、及び/又はサマリウムであり、
Y4は、アルカリ土類金属、ニッケル、コバルト、マンガン、亜鉛、スズ、カドミウム、及び/又は水銀であり、
Y5は、鉄、又は鉄とバナジウム、クロム、及びセリウムの元素のうち少なくとも1種であり、
Y6は、リン、ヒ素、ホウ素、アンチモン、及び/又はビスマスであり、
Y7は、希土類金属、チタン、ジルコニウム、ニオブ、タンタル、レニウム、ルテニウム、ロジウム、銅、銀、金、アルミニウム、ガリウム、インジウム、ケイ素、ゲルマニウム、鉛、トリウム、及び/又はウランであり、
Y8は、モリブデン若しくはタングステン、又はモリブデン及びタングステンであり、
a’は、0.01〜8の範囲の数であり、
b’は、0.1〜30の範囲の数であり、
c’は、0〜4の範囲の数であり、
d’は、0〜20の範囲の数であり、
e’は、0〜20の範囲にある0より大きい数であり、
f’は、0〜6の範囲の数であり、
g’は、0〜15の範囲の数であり、
h’は、8〜16の範囲の数であり、
x’及びy’は、式(II)中の酸素とは異なる元素の価数と頻度によって特定される数であり、かつ
p及びqは、その比率p/qが、0.1〜10である数である。
X1は、Co及び/又はNiであり、
X2はアルカリ金属であり、
X4は、Si及び/又はAlであり、
aは、0.3〜1の範囲の数であり、
bは、0.5〜10の範囲の数であり、
cは、2〜10の範囲の数であり、
dは、0〜0.5の範囲の数であり、
fは、0〜10の範囲の数であり、かつ
nは、式(Ia)中の酸素とは異なる元素の価数と頻度によって特定される数である。
条件1:12−c−1.5×b=A、ここでAは、0.5〜1.5の範囲の数であり、
条件2:商a/Aが、0.2〜1.3の範囲の数であり、
条件3:商c/bが、2.5〜9の範囲の数である。
Y2は、モリブデン若しくはタングステン、又はモリブデン及びタングステンであり、
Y3は、アルカリ金属及び/又はタリウム、好適にはK、Csであり、
Y4は、アルカリ土類金属、ニッケル、コバルト、及び/又はスズであり、
Y6は、リン、ヒ素、ホウ素、アンチモン、及び/又はビスマスであり、
Y7は、チタン、ジルコニウム、アルミニウム、ケイ素、銅、銀、及び/又は金であり、好適にはSiであり、
Y8は、モリブデン若しくはタングステン、又はモリブデン及びタングステンであり、
a’は、0.1〜2の範囲の数であり、
b’は、0.2〜4の範囲の数であり、
c’は、0.02〜2の範囲の数であり、
d’は、3〜10の範囲の数であり、
e’は、0.01〜5、好適には0.1〜4の範囲の数であり、
f’は、0〜5の範囲の数であり、
g’は、0〜10の範囲の数であり、好適には0〜10の範囲にある0より大きい数であり、特に好ましくは0.2〜10の範囲にある数であり、極めて特に好ましくは0.4〜3の範囲にある数であり、
x’及びy’は、式(IIa)中の酸素とは異なる元素の価数と頻度によって特定される数であり、かつ
p及びqは、その比率p/qが、0.1〜5、好適には0.4〜2である数である。
(i)複合金属酸化物の元素の構成成分の供給源から、密接な乾燥混合物を作成する工程、
(ii)密接な乾燥混合物を圧縮して、中空円筒形成形体の前駆体にする工程、
(iii)350〜650℃の範囲の温度でか焼する工程。
アルケンを気相酸化して不飽和アルデヒド及び/又は不飽和カルボン酸にするための、機械的に安定な中空円筒形触媒成形体
I)以下のような活性物質の化学量論を有する、中空円筒形非担持型触媒成形体の製造:
[Bi2W2O9・2WO3]0.50[Mo12Co5.4Fe3.1Si1.5K0.08Ox]1
a)出発材料1の製造(Bi1W2O7.5=1/2Bi2W2O9・1WO3)
1.75m3の特殊鋼製ダブルジャケット式容器(ジャケットの間に温度調整用の水を貫流させたもの、十字型撹拌機付)内で、硝酸水溶液に入れた25℃の硝酸ビスマス溶液(Bi:11.2質量%、遊離硝酸3〜5質量%;ベルギー国、Tilly 1495在のSidech S.A.社製のビスマス金属から硝酸で製造、その純度は、Biが99.997質量%超、Pbが7mg/kg未満、Ni、Ag、Feがそれぞれ5mg/kg未満、Cu、Sbが3mg/kg未満、Cd、Znは1mg/kg未満)780kg中に、25℃で20分以内に、何回かに分けて25℃のタングステン酸(Wが74.1質量%、平均粒度0.4〜0.8μm(ASTM B 330により製造者が測定)、強熱減量(750℃で2時間、空気中)6〜8質量%、Goslar D-38615在のH. C. Starck社製)214.7kgを入れて撹拌した(70回転/分)。続いて、生成した水性混合物をさらに3時間、25℃で撹拌し、それから噴霧乾燥した。噴霧乾燥は、Niro社製のFS 15型回転ディスク式噴霧塔で、熱した並流の空気で、ガス取り入れ温度300±10℃、ガス排出温度100±10℃、ディスク回転数18000回転/分、処理量200l/h、空気量1900Nm3/hで行った。生じた噴霧粉末は、強熱損失が12.8質量%(900℃で質量が一定になるまで強熱した陶器製るつぼ内で、600℃で3時間、空気下で強熱)であり、(絶対圧1.1barの分散圧で)d50が28.0μm(d10=9.1μm、d90=55.2μm)であった。
以下のようにして溶液Aを作製した:水で温度調整した1.75m3の特殊鋼製ダブルジャケット式容器(十字型撹拌機付)で、60℃で撹拌しながら(70回転/分)、温度60℃の水660lに、1分以内で、温度60℃の水酸化カリウム水溶液(KOH47.5質量%)1.075kg、及び引き続き供給速度600kg/hで差動供給秤量によって、温度が25℃のアンモニウムヘプタモリブデート四水和物(粒度dが1mm未満の白色結晶、MoO381.5質量%、NH37.0〜8.5質量%、アルカリ金属最大150mg/kg、Goslar D-38642在、H.C. Starck社製)237.1kgを供給し、生成した溶液を、60℃で60分間撹拌した(70回転/分)。
出発材料2を134kg、混合翼と切断翼(混合翼の回転数:39回転/分、切断翼の回転数3000回転/分)を備える傾斜配置型混合機(VIL型、充填体積200l、Aachener Misch- und Knetmaschinenfabrik社製)に初充填し、1分間、事前混合した。これに対して10分以内にさらなる混合で、セルホイール式ゲートを介して、出発材料1を下記化学量論の複合金属酸化物:
[Bi2W2Og・2WO3]0.50[MO12CO5.4Fe3.1Si1.5K0.08Ox]1
に必要な量を10分以内に計量供給した。それから、混合工程をさらに15分間続け、両方の出発材料を強力かつ完全に均質化した(存在する場合にはアグロメレートの粉砕を含む)。上記材料全体に対して、さらに2分以内に、Timcal AG製の黒鉛であるTIMREX T44を混ぜた。
4×3×2
4×2×2
5×3×2
ロータリープレス機の回転速度は、35〜45回転/分であった。
反応管(V2A鋼製、外形21mm、肉厚3mm、内径15mm、長さ120cm)を、上方から下方へと流れ方向で、以下のように充填した:
・区間1:長さ約30cm
事前充填物として、直径1.5〜2.0mmのステアタイトビーズ40g
・区間2:長さ約70cm
I)で作製し、か焼した中空円筒形成形体40gと、ステアタイトの中空円筒形(寸法5mm×3mm×2mm、外径×高さ×内径)60gとの均質な混合物で触媒を充填。
プロペン5体積%、
酸素9.5体積%、及び
100体積%になる残量としてのN2。
触媒50gを、長さ3m、内径23mmの垂直管を通じて、落下させた。触媒は、管の真下にある陶器製のシャーレに落とし、衝突の際に生じる粉塵と破断物から分離した。粉塵から分離された無傷の触媒成形体を秤量した。無傷の触媒成形体の割合は、この際に測定した質量を、落下試験に使用した触媒成形体の質量と比較することによって特定した(表1における「落下試験」の欄を参照)。無傷の触媒成形体の割合は、触媒成形体の機械的な耐久性についての基準である。その結果が、以下の表1にまとめてある。
Claims (15)
- ADが、3.7〜4.3mmの範囲で選択されている、請求項1に記載の中空円筒形触媒成形体。
- qが、0.45〜0.55mmの範囲で選択されている、請求項1又は2に記載の中空円筒形触媒成形体。
- pが、0.65〜0.9の範囲で選択されている、請求項1から3までのいずれか1項に記載の中空円筒形触媒成形体。
- 触媒成形体の形状体積が、22〜34mm3である、請求項1から4までのいずれか1項に記載の中空円筒形触媒成形体。
- 触媒成形体の形状面積対、触媒成形体の形状体積の比率が、22〜32cm-1である、請求項1から5までのいずれか1項に記載の中空円筒形触媒成形体。
- 触媒成形体の密度が、1.2〜2.0g/cm3である、請求項1から6までのいずれか1項に記載の中空円筒形触媒成形体。
- ADが3.7〜4.3mmの範囲で、Hが2.8〜3.2mmの範囲で、かつIDが1.8〜2.2mmの範囲で選択されている、請求項1から8までのいずれか1項に記載の中空円筒形触媒成形体。
- 前記複合金属酸化物が、少なくともモリブデン、鉄、及びビスマスの元素を有する、請求項1から9までのいずれか1項に記載の中空円筒形触媒成形体。
- 以下の工程:
(i)複合金属酸化物の元素構成成分の供給源から、密接な乾燥混合物を作製する工程、
(ii)前記密接な乾燥混合物を圧縮して、中空円筒形成形体の前駆体にする工程、及び
(iii)350〜650℃の範囲の温度でか焼する工程
によって得られる、請求項1から10までのいずれか1項に記載の中空円筒形触媒成形体の製造方法。 - 前記密接な乾燥混合物を、タブレット化によって圧縮して、中空円筒形成形体の前駆体にする、請求項11に記載の中空円筒形触媒成形体の製造方法。
- か焼の前に、触媒成形体の前駆体の最大相対質量低減率が1分あたり1%という値を超えない条件下で、前記中空円筒形成形体の前駆体を熱により前処理することによって得られる、請求項11又は12に記載の中空円筒形触媒成形体の製造方法。
- アルケンを分子状酸素とともに、充填物が請求項1から10までのいずれか1項に記載の中空円筒形触媒成形体を有する触媒固定床に通す、α,β−不飽和アルデヒド及び/又はα,β−不飽和カルボン酸を製造するための方法。
- プロペンの気相酸化によってアクロレインを製造するための、請求項14に記載の方法。
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US9700876B2 (en) | 2017-07-11 |
JP2016538120A (ja) | 2016-12-08 |
US20150133686A1 (en) | 2015-05-14 |
CN105899480B (zh) | 2018-11-13 |
BR112016010410B1 (pt) | 2021-12-28 |
WO2015067659A1 (de) | 2015-05-14 |
BR112016010410A2 (pt) | 2017-08-08 |
MY173267A (en) | 2020-01-09 |
EP3068753A1 (de) | 2016-09-21 |
CN105899480A (zh) | 2016-08-24 |
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