JPS62168550A - Method for supporting catalytically active metal - Google Patents
Method for supporting catalytically active metalInfo
- Publication number
- JPS62168550A JPS62168550A JP886986A JP886986A JPS62168550A JP S62168550 A JPS62168550 A JP S62168550A JP 886986 A JP886986 A JP 886986A JP 886986 A JP886986 A JP 886986A JP S62168550 A JPS62168550 A JP S62168550A
- Authority
- JP
- Japan
- Prior art keywords
- active metal
- carrier
- catalytically active
- metal compound
- support
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 31
- 239000002184 metal Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 18
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 4
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 3
- 239000012159 carrier gas Substances 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000007792 gaseous phase Substances 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 7
- 238000001947 vapour-phase growth Methods 0.000 description 6
- 150000002739 metals Chemical class 0.000 description 5
- -1 VOCl2 Chemical class 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000011068 loading method Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052776 Thorium Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001845 chromium compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005078 molybdenum compound Substances 0.000 description 1
- 150000002752 molybdenum compounds Chemical class 0.000 description 1
- QLOKAVKWGPPUCM-UHFFFAOYSA-N oxovanadium;dihydrochloride Chemical compound Cl.Cl.[V]=O QLOKAVKWGPPUCM-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 150000003658 tungsten compounds Chemical class 0.000 description 1
- 150000003682 vanadium compounds Chemical class 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Abstract
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は触媒活性金属の担体への担持方法に関する。[Detailed description of the invention] [Industrial application field] The present invention relates to a method for supporting a catalytically active metal on a support.
触媒活性金属の担体への担持方法として、従゛来は直接
、触媒金属化合物を含む水溶液に担体を浸漬する含浸法
が採用されていた。一方、従来の含浸型触媒に対して、
気相蒸着法による触媒金属の担持方法の検討が行われて
おシ、同一触媒組成の場合、気相蒸着法によシ調製した
触媒の方が含浸法よシも高活性であることが判明した。Conventionally, as a method for supporting a catalytically active metal on a carrier, an impregnation method has been adopted in which the carrier is directly immersed in an aqueous solution containing a catalytic metal compound. On the other hand, compared to conventional impregnated catalysts,
Studies have been conducted on how to support catalyst metals using vapor phase deposition, and it has been found that for the same catalyst composition, catalysts prepared using vapor phase deposition have higher activity than those prepared using impregnation. did.
（特願昭６０〜２６１４４５号）この理由として、気相
蒸着法の場合、触媒活性金属化合物と担体を接触反応さ
せて活性金属を担持する際、活性金属と担体との相互作
用が強いだめ、金属と担体間で電子移動が生じ、金属の
表面電子状態が変化するためと考えられている。さらに
気相蒸着法の方が活性金属を担体上に均一な単分子状で
担持させることができ、蒸着した生成粒子の凝縮を防ぐ
ことができるためと考えられている。(Patent Application No. 60-261445) The reason for this is that in the case of vapor phase deposition, when the active metal is supported by a contact reaction between the catalytically active metal compound and the support, the interaction between the active metal and the support is strong; It is thought that this is because electron transfer occurs between the metal and the carrier, changing the surface electronic state of the metal. Furthermore, it is thought that this is because the vapor phase deposition method allows the active metal to be supported on the carrier in a uniform monomolecular form, thereby preventing condensation of the vapor-deposited particles.
ところが、従来の気相蒸着法では、蒸発した原料を流通
式で通送するだけであり、明確な調製方法は提案されて
いなかった。ゆえに、触媒活性金属を所定量担持させる
ためには担持量より多量の活性金属蒸気を通送させる必
要があシ、コスト面、触媒調製効率等の点で多くの問題
点を有していた。However, in the conventional vapor phase deposition method, the evaporated raw material is simply conveyed through a flow system, and no clear preparation method has been proposed. Therefore, in order to support a predetermined amount of catalytically active metal, it is necessary to pass active metal vapor in an amount larger than the supported amount, which poses many problems in terms of cost, catalyst preparation efficiency, etc.
本発明者は上記欠点を克服すべく鋭意研究の結果、比較
的簡単な方法で、より触媒活性金属を担体に均一にかつ
一定に担持てきる極めて優れた気相蒸着法を見出したの
である。As a result of intensive research to overcome the above-mentioned drawbacks, the inventors of the present invention have discovered an extremely superior vapor phase deposition method that allows the catalytically active metal to be more uniformly and constantly deposited on the carrier using a relatively simple method.
本発明は■族あるいは■族からなる金属酸化物に、活性
金属化合物を接触担持させるにあたって循環型触媒担持
装置を使用することを特徴とする触媒活性金属の担持方
法である。The present invention is a method for supporting a catalytically active metal, which is characterized in that a circulating catalyst supporting device is used for contacting and supporting an active metal compound on a metal oxide of group (1) or group (2).
本発明においては、担体としての■族金属酸化物として
アルミニウム、ガリウム、インジウム、タリウムの酸化
物が、捷た■族金属酸化物トシテチタン、ジルコニウム
、ハフニウム、トリウム、シリコン、ゲルマニウム、ス
ズの酸化物が選ばれる。In the present invention, oxides of aluminum, gallium, indium, and thallium are used as group-III metal oxides as carriers, and oxides of group-III metals such as titanium, zirconium, hafnium, thorium, silicon, germanium, and tin are used as carriers. is selected.
又、気相状態の活性金属化合物としては、バナジウム化
合物としてＶＯＣｌ２ 、ＶＯＢｒ３ 、ＶＯｌ、、鉄
化合物としてＦｅＣ／３ 、Ｆｅ（Ｃｏ）、 、スズ化
合物として８ｎＯ／４ 、ＥＩｎＢｒ４．アルミニウム
化合物としてＡ Ｉ ＯＪ３、チタニウム化合物として
Ｔｉｅｌ！いシリカ化合物としてはＥＩｉＯ１！、 、
５ｉＣＩ！３Ｆ、クロム化合物としてＣｒ０２ＣＩ！２
、モリブデン化合物としてＭｏＯ２（ＯＨ）２、タング
ステン化合物としてＷｅ／、が選ばれる。The active metal compounds in the gas phase include vanadium compounds such as VOCl2, VOBr3, and VOl, iron compounds such as FeC/3 and Fe(Co), and tin compounds such as 8nO/4 and EInBr4. A I OJ3 is an aluminum compound, and Tiel! is a titanium compound. EIiO1 as a silica compound! , ,
5iCI! 3F, Cr02CI as a chromium compound! 2
, MoO2(OH)2 is selected as the molybdenum compound, and We/ is selected as the tungsten compound.
本発明において、担体が粉末である場合は、循環型触媒
担持装置内に触媒活性金属化合物の蒸気と粉末担体を流
動させ循環接触させることによシ、活性金属を担体に担
持する。この循環型触媒担持装置を使用することによシ
、これまでに比べ、触媒活性金属化合物と担体との接触
反応を担体のどの部分においても短時間で均一に行うこ
とができる。そのため高活性な触媒を多量に調製するこ
とが可能となった。In the present invention, when the carrier is a powder, the active metal is supported on the carrier by flowing the vapor of the catalytically active metal compound and the powder carrier in a circulating catalyst supporting device to bring them into circulation contact. By using this circulating catalyst supporting device, the catalytic reaction between the catalytically active metal compound and the carrier can be uniformly carried out in any part of the carrier in a shorter time than ever before. Therefore, it has become possible to prepare a large amount of highly active catalyst.
更に、本発明方法では、触媒活性金属の損失を少くする
ことが可能であシ、低コストで調製できるに加えて、廃
液、廃ガス処理等の管理面の煩雑さを緩和させることが
できるようになった。Furthermore, in the method of the present invention, it is possible to reduce the loss of catalytically active metals, and in addition to being able to prepare them at low cost, it is possible to reduce the complexity of management such as waste liquid and waste gas treatment. Became.
なお、本気相担持方法は、担体は粉末状だけとは限らず
、ベレット状、ハニカム状においても担持することが可
能である。この場合担体を担持塔内に固定し、触媒活性
金属化合物の蒸気を流動させ担体と循環接触反応させる
が、触媒性能および触媒担持効率が低減するものでない
。In addition, in the serious gas phase supporting method, the carrier is not limited to powder form, but can also be supported in pellet form or honeycomb form. In this case, the carrier is fixed in a carrier tower, and the vapor of the catalytically active metal compound is caused to flow and undergo a cyclic contact reaction with the carrier, but the catalyst performance and catalyst loading efficiency are not reduced.
本発明の２種の活性金属の循環型触媒担持装置を第１図
、第２図によって説明する。The circulating type catalyst supporting device for two types of active metals of the present invention will be explained with reference to FIGS. 1 and 2.
担体が粉末状の場合、第１図に示す流動床活性金属気相
担持装置を使用する。まず、装置内に粉末担体とキャリ
アーとしてのＮ２をライン１よシ供給し、装置を封入し
、ポンプ２によりＮ２を循環させる。次に活性金属化合
物の蒸気をその供給部３より循環系内に送り、粉末担体
と共に上方に向けて流動させ、気相の活性金属化合物と
担体とを接触反応させることにより、担体に活性金属を
担持させる。未反応の活性金属化合物とキャリアーガス
は循環ライン４を通シ、再び流動床状に運動している担
体と接触反応させる。流動している金属担持担体は触媒
回収部５にて活性金属の担持状態を観察し、担持量が不
十分な場合、さらに循環させて、活性金属化合物の蒸気
と接触させる。適度な担持量を得るまで循環させた後触
媒回収部５にて触媒を回収し、さらに新たな担体を新し
く供給し、気相担持を継続的に行う。When the support is in powder form, a fluidized bed active metal vapor phase support apparatus shown in FIG. 1 is used. First, a powder carrier and N2 as a carrier are supplied into the apparatus through line 1, the apparatus is sealed, and N2 is circulated by pump 2. Next, the vapor of the active metal compound is sent into the circulation system from the supply section 3 and flowed upward together with the powder carrier, causing a contact reaction between the active metal compound in the gas phase and the carrier, thereby injecting the active metal into the carrier. carry it. The unreacted active metal compound and the carrier gas are passed through the circulation line 4 and brought into contact with the carrier moving in a fluidized bed again. The flowing metal-supported carrier is observed in the catalyst recovery section 5 for the state of active metal supported thereon, and if the supported amount is insufficient, it is further circulated and brought into contact with the vapor of the active metal compound. After circulating the catalyst until a suitable amount of support is obtained, the catalyst is recovered in the catalyst recovery section 5, and a new carrier is supplied to continuously carry out gas phase support.
次に触媒担体がハニカム状の場合、第２図に示す固定床
気相担持装置を使用する。この担持装置は、本質的には
第１図の装置と同様であるが、ハニカム担体を担持塔内
の触媒固定板６の上に固定する点が第１図と異なる。気
相の活性金属化合物は、Ｎ２キャリアーにより系内を循
環し、ハニカム担体表面上に均一に担持される。Next, when the catalyst carrier is in the form of a honeycomb, a fixed bed gas phase carrier shown in FIG. 2 is used. This supporting apparatus is essentially the same as the apparatus shown in FIG. 1, but differs from that shown in FIG. 1 in that the honeycomb carrier is fixed on a catalyst fixing plate 6 in a supporting column. The active metal compound in the gas phase is circulated within the system by the N2 carrier and is uniformly supported on the surface of the honeycomb carrier.
〔実施例１〕
ｒ−アルミナを主成分とする粉末状担体を第１図に示す
、流動床式活性金属担持装置に入れる。まず、系内に乾
燥したＮ２を入れ、活性金属蒸気であるＶＯＣｌ３を約
１００℃に保温して蒸発させる。循環ライン内の温度を
２００℃に保ちγ−アルミナ粉体とＶＯＣ／、、蒸気を
循環接触反応させる。３００ ｃａ／ ｍｉｎの流速で
１０分間、循環接触させた後、ｖｏｃ、ｒ、担持させた
粉末担体を取シ出し酸素雰囲気下５００℃、５時間焼成
した。このようにして得られた触媒を触媒Ａとする。粉
末状の触媒Ａに担持されたＶ含有量はＶ２Ｏ５１でγ−
アルミナ担体に対して３．Ｏｗｔ％であり、どの部分の
担体に対しても均一な担持分布を有していた。[Example 1] A powdered carrier containing r-alumina as a main component is placed in a fluidized bed type active metal supporting apparatus shown in FIG. First, dry N2 is introduced into the system, and VOCl3, which is an active metal vapor, is evaporated by keeping the temperature at about 100°C. The temperature in the circulation line was maintained at 200°C, and the γ-alumina powder, VOC, and steam were subjected to a circulation contact reaction. After cyclic contact for 10 minutes at a flow rate of 300 ca/min, the powder carrier supporting voc, r was taken out and calcined at 500° C. for 5 hours in an oxygen atmosphere. The catalyst thus obtained is referred to as catalyst A. The V content supported on powdered catalyst A is V2O51 and γ-
3 for alumina support. Owt%, and had a uniform loading distribution in all parts of the carrier.
〔実施例２〕
Ｔ１０２（アナターゼ型）を主成分とするノ・ニカム状
担体（縦×横×高さ１００謔Ｘ １００ ｍｍ Ｘｓｏ
ｏｍ）９型金第２図に示す装置の担持塔に充填する。ま
ず、ライン内にＮ２を封入し、約１００℃に保温したＶ
ＯＯ／３蒸気を循環させる。[Example 2] A nicum-shaped carrier (length x width x height 100 mm x 100 mm) containing T102 (anatase type) as the main component
om) Fill the support tower of the apparatus shown in FIG. 2 with type 9 metal. First, N2 was sealed in the line and the V
Circulate OO/3 steam.
循環ライン内の温度を１００℃に保ち、１０分循環させ
た。このようにＶＯＯ／３ を担持させたノ・ニカム状
担体を取り出し酸素雰囲気下５００℃にて３時間焼成し
た。このようにして得られた触媒を触媒Ｂとする。The temperature in the circulation line was maintained at 100°C, and circulation was carried out for 10 minutes. The nicum-like carrier supporting VOO/3 in this way was taken out and fired at 500° C. for 3 hours in an oxygen atmosphere. The catalyst thus obtained is referred to as catalyst B.
〔実施例３〕
実施例２と同じ・・ニカム担体に従来の気相担持法によ
り■ＯＣ１！３を通送して■を担持した触媒を触媒Ｃと
する。[Example 3] Same as Example 2... Catalyst C is a catalyst in which ■OC1!3 is passed onto a nicium carrier by a conventional gas phase loading method to support ■.
■担持量ｖ２０．で５０ ｗｔ％を得るために必要なＶ
ＯＯ／３消費量および担持時間を表１に記す。■Carrying amount v20. V required to obtain 50 wt% in
The OO/3 consumption and loading time are listed in Table 1.
表 １
〔発明の効果〕
本発明の循環型触媒担持装置を使用することによシ、活
性金属を担体に均一で担持させることができ、しかも含
浸型触媒に比べ高活性な触媒を多量に調製することがで
きた。Table 1 [Effects of the invention] By using the circulating catalyst supporting device of the present invention, it is possible to uniformly support active metals on the carrier, and moreover, it is possible to prepare a large amount of highly active catalyst compared to impregnated catalysts. We were able to.
第１図、第２図は本発明の触媒の活性金属担持装置を示
す図である。第１図は担体が粉末の場合第２図は担体が
ハニカムである場合である。
復代理人 内 １） 明
復代理人 萩 原 亮 −
復代理人 安 西 篤 夫FIG. 1 and FIG. 2 are diagrams showing an active metal supporting device for the catalyst of the present invention. FIG. 1 shows the case where the carrier is a powder, and FIG. 2 shows the case where the carrier is a honeycomb. Sub-Agents 1) Meifuku Agent Ryo Hagiwara − Sub-Agent Atsuo Anzai
Claims (1)
金属化合物を接触担持させるにあたつて循環型触媒担持
装置を使用することを特徴とする触媒活性金属の担持方
法。(1) A method for supporting a catalytically active metal, which comprises using a circulating catalyst supporting device for contacting and supporting an active metal compound on a group III or group IV metal oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP886986A JPS62168550A (en) | 1986-01-21 | 1986-01-21 | Method for supporting catalytically active metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP886986A JPS62168550A (en) | 1986-01-21 | 1986-01-21 | Method for supporting catalytically active metal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62168550A true JPS62168550A (en) | 1987-07-24 |
Family
ID=11704691
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP886986A Pending JPS62168550A (en) | 1986-01-21 | 1986-01-21 | Method for supporting catalytically active metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62168550A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004534635A (en) * | 2001-04-25 | 2004-11-18 | ユミコア・アクチエンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフト | Method and apparatus for heat treating powdered materials |
-
1986
- 1986-01-21 JP JP886986A patent/JPS62168550A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004534635A (en) * | 2001-04-25 | 2004-11-18 | ユミコア・アクチエンゲゼルシャフト・ウント・コムパニー・コマンディットゲゼルシャフト | Method and apparatus for heat treating powdered materials |
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