JPH10113551A - Continuous reaction apparatus and production method using thereof - Google Patents
Continuous reaction apparatus and production method using thereofInfo
- Publication number
- JPH10113551A JPH10113551A JP8272251A JP27225196A JPH10113551A JP H10113551 A JPH10113551 A JP H10113551A JP 8272251 A JP8272251 A JP 8272251A JP 27225196 A JP27225196 A JP 27225196A JP H10113551 A JPH10113551 A JP H10113551A
- Authority
- JP
- Japan
- Prior art keywords
- reaction
- liquid
- solid catalyst
- catalyst
- reaction vessel
- 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
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、連続反応装置及びそれ
を用いた生産方法に関する。さらに詳しくは、少なくと
も、液状原料供給口を備えた反応容器、反応混合物を循
環するための循環ポンプ及び液体サイクロンから構成さ
れる連続反応装置、及びそれを用いた生産方法に関す
る。The present invention relates to a continuous reactor and a production method using the same. More specifically, the present invention relates to at least a reaction vessel having a liquid material supply port, a continuous reaction apparatus including a circulation pump for circulating a reaction mixture and a liquid cyclone, and a production method using the same.
【０００２】[0002]
【従来の技術】従来、固体触媒を用いて行う液−固反応
あるいは気−液−固反応が多く知られている。これらの
反応において、反応混合物と触媒は通常濾過機又は遠心
分離機などで分離され、分離された触媒は溶媒で逆洗あ
るいは調整して循環再使用される。しかしながら、この
ような操作は極めて煩雑であり、とくに、反応系が高圧
で行われる場合、上述したような既存の分離装置で触媒
を分離しようとすると、分離する前に系を常圧又は常圧
付近にして実施する必要があり、しかも分離後の触媒を
高圧の反応容器にもどすには特殊な供給装置が必要であ
る。2. Description of the Related Art Conventionally, a liquid-solid reaction or a gas-liquid-solid reaction performed using a solid catalyst has been widely known. In these reactions, the reaction mixture and the catalyst are usually separated by a filter or a centrifuge, and the separated catalyst is back-washed or adjusted with a solvent and reused by circulation. However, such an operation is extremely complicated, and in particular, when the reaction system is performed at a high pressure, when the catalyst is to be separated by the existing separation device as described above, the system is set to normal pressure or normal pressure before separation. It needs to be carried out in the vicinity, and a special supply device is required to return the separated catalyst to the high-pressure reaction vessel.
【０００３】[0003]
【発明が解決しようとする課題】煩雑な操作を必要とし
ない合理的なプロセスを構築することは、工業的規模で
生産を実施する場合、不可欠な技術課題であり、本発明
の目的は、従来のように、触媒を分離するのに濾過機又
は遠心分離機などの回分式の分離手段によらず、固体触
媒を含む反応混合物から触媒を連続的に分離でき、分離
した触媒はそのまま再使用可能な連続反応装置を提供す
ること及びそれを用いた生産方法を提供することにあ
る。The construction of a rational process that does not require complicated operations is an indispensable technical problem when carrying out production on an industrial scale. The catalyst can be continuously separated from the reaction mixture containing the solid catalyst without using a batch type separation means such as a filter or a centrifugal separator to separate the catalyst, and the separated catalyst can be reused as it is And a production method using the same.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、上記課題
を解決するため鋭意検討し、反応系に液体サイクロンを
設けることにより、上記課題が解決されることを見出
し、本発明を完成させるに至った。すなわち、本発明
は、少なくとも、液状原料供給口を備えた反応容器、反
応混合物を循環するための循環ポンプ及び液体サイクロ
ンから構成されることを特徴とする連続反応装置であ
る。Means for Solving the Problems The present inventors diligently studied to solve the above problems, and found that the above problems could be solved by providing a liquid cyclone in the reaction system, and completed the present invention. Reached. That is, the present invention is a continuous reaction apparatus comprising at least a reaction vessel provided with a liquid material supply port, a circulation pump for circulating a reaction mixture, and a liquid cyclone.
【０００５】本発明のもう一つの発明は、液状原料を固
体触媒の存在下に液相で反応させて反応生成物を得る生
産方法において、反応混合物の一部は反応容器へ循環さ
せつつ、一部を液体サイクロンへ導き、液体サイクロン
で液状の反応混合物と固体触媒を分離し、該固体触媒は
反応容器へリサイクルし、該液状の反応混合物は反応系
外へ抜き出すことを特徴とする連続生産方法である。Another invention of the present invention relates to a production method for producing a reaction product by reacting a liquid raw material in a liquid phase in the presence of a solid catalyst. A continuous reaction method, wherein a liquid reaction mixture and a solid catalyst are separated by a liquid cyclone, the solid catalyst is recycled to a reaction vessel, and the liquid reaction mixture is withdrawn out of the reaction system. It is.
【０００６】本発明の反応装置において、反応器として
液状原料供給口を備えた反応容器が使用される。反応容
器は液状原料供給口を備えていれば如何なる形状のもの
でもよく、水添反応、還元アミノ化反応などガスを使用
する場合は、別途ガスの供給口を設ければよい。[0006] In the reaction apparatus of the present invention, a reaction vessel provided with a liquid material supply port is used as a reactor. The reaction vessel may have any shape as long as it has a liquid material supply port. When a gas such as a hydrogenation reaction or a reductive amination reaction is used, a separate gas supply port may be provided.
【０００７】ガスを液状原料によく溶解させるために、
また混合状態を良好にするために反応容器に撹拌機を備
えるのが好ましい。また、液状原料供給口を備えた反応
容器にエゼクタを設けるとガスの分散が良好となり、好
ましい。反応容器は環状の反応容器であってもよい。In order to dissolve the gas in the liquid material well,
Further, it is preferable to provide a stirrer in the reaction vessel in order to improve the mixing state. Further, it is preferable to provide an ejector in a reaction vessel provided with a liquid material supply port, since the gas can be dispersed well. The reaction vessel may be an annular reaction vessel.
【０００８】本発明の連続反応装置は、少なくとも、液
状原料供給口を備えた反応容器、反応混合物を循環する
ための循環ポンプ及び液体サイクロンから構成され、所
定の操作条件下において反応を行い、反応容器から抜き
出された反応混合物の一部を反応容器へ循環させつつ、
一部を液体サイクロンへ導き、液体サイクロンで液状の
反応混合物と固体触媒を分離し、該固体触媒は反応容器
へリサイクルし、該液状の反応混合物は反応系外へ抜き
出すことによって連続生産が実施される。反応容器にお
ける液面は適宜調節すればよいが、通常は容器の６０％
〜８０％で実施することが多い。[0008] The continuous reaction apparatus of the present invention comprises at least a reaction vessel provided with a liquid material supply port, a circulation pump for circulating a reaction mixture, and a liquid cyclone. While circulating a part of the reaction mixture extracted from the vessel to the reaction vessel,
A part of the reaction mixture is led to a liquid cyclone, the liquid reaction mixture is separated from the solid catalyst by the liquid cyclone, and the solid catalyst is recycled to the reaction vessel. You. The liquid level in the reaction vessel may be appropriately adjusted, but is usually 60% of the vessel.
It is often performed at ~ 80%.
【０００９】液体サイクロンは液体と固体触媒を分離す
るためのものであり、分離された固体触媒は反応容器に
もどされる。液体サイクロンの効率をあげるためには、
サイクロンの円筒部の直径を小さくするのが望ましく、
スリム状のサイクロンを必要に応じて複数個使用するの
がよい。[0009] The hydrocyclone is for separating a liquid and a solid catalyst, and the separated solid catalyst is returned to a reaction vessel. To increase the efficiency of the hydrocyclone,
It is desirable to reduce the diameter of the cylindrical part of the cyclone,
It is preferable to use a plurality of slim cyclones as necessary.
【００１０】本発明において、反応圧力及び反応温度は
とくに限定されず、圧力は常圧〜高圧まで幅広く適用す
ることができ、温度も低温から高温まで幅広く適用され
る。分離された液状の反応混合物は、反応生成物、未反
応液状原料及び若干の触媒からなっており、フィルタ−
を通して次の工程へ供給される。In the present invention, the reaction pressure and the reaction temperature are not particularly limited, and the pressure can be widely applied from normal pressure to high pressure, and the temperature is also widely applied from low to high temperature. The separated liquid reaction mixture is composed of the reaction product, unreacted liquid raw material and some catalyst.
Through to the next step.
【００１１】[0011]
【発明の実施の形態】以下、本発明を図により具体的に
説明する。図１は本発明の連続反応装置を示すフローチ
ャートである。１は液状原料供給ラインであり、２は反
応容器、３は撹拌機、４はガスの分散機である。まず、
一次仕込みとして、１から液状原料及び溶媒に溶解され
たスラリ−状の固体触媒を反応容器２に仕込む。所定の
液面に達したら撹拌機３を回転し、所定の圧力及び温度
に達したら、循環ポンプ５で液状原料及びスラリ−状の
固体触媒からなる液状物を冷却器６を通して全量循環さ
せる。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be specifically described below with reference to the drawings. FIG. 1 is a flowchart showing the continuous reaction apparatus of the present invention. 1 is a liquid raw material supply line, 2 is a reaction vessel, 3 is a stirrer, and 4 is a gas disperser. First,
As a primary charge, a slurry-like solid catalyst dissolved in a liquid raw material and a solvent is charged from 1 into the reaction vessel 2. When the liquid level reaches a predetermined level, the stirrer 3 is rotated. When the pressure and the temperature reach a predetermined level, the circulating pump 5 circulates the whole liquid material composed of the liquid raw material and the slurry-like solid catalyst through the cooler 6.
【００１２】所定の操作条件に達したら、水素などのガ
スをガス供給ライン４から仕込み、反応を開始する。冷
却器は図１又は図２のように、反応容器の外部に設けて
もよいが、ジャケット形式で反応容器に直接設置しても
よい。冷却器６は必要に応じて加熱器として使用され
る。冷却器又は加熱器は他の媒体と熱交換を行うように
するのが熱的に効率がよい。When predetermined operating conditions are reached, a gas such as hydrogen is charged from the gas supply line 4 to start the reaction. The cooler may be provided outside the reaction vessel as shown in FIG. 1 or FIG. 2, or may be provided directly in the reaction vessel in a jacket form. The cooler 6 is used as a heater as needed. Coolers or heaters are thermally efficient to exchange heat with other media.
【００１３】図２は反応容器２にエゼクタ９を設けたも
のであり、このようなエゼクタ−によれば、循環された
液状反応混合物の速度をあげて反応容器内へ吹き込むこ
とができ、供給されるガスとともに反応容器内の流動状
態をさらによくし、ガスの吸収効率を高くすることがで
きる。FIG. 2 shows an example in which an ejector 9 is provided in the reaction vessel 2. According to such an ejector, the circulated liquid reaction mixture can be blown into the reaction vessel at an increased speed and supplied. The flow state in the reaction vessel together with the gas can be further improved, and the gas absorption efficiency can be increased.
【００１４】所定の反応率に達したら、液状原料及びガ
スを連続的に供給しながら、反応混合物の一部を液体サ
イクロン７に導き、反応混合物を液体と固体に分離す
る。分離された固体触媒は反応容器２へリサイクルさ
れ、再使用される。また、分離された液体は、反応生成
物及び未反応物の他、若干の固体触媒が含まれることが
あるので、必要に応じフィルタ８を通して次の工程へ供
給する。When a predetermined reaction rate is reached, a part of the reaction mixture is introduced into a liquid cyclone 7 while continuously supplying a liquid raw material and a gas, and the reaction mixture is separated into a liquid and a solid. The separated solid catalyst is recycled to the reaction vessel 2 and reused. The separated liquid may contain a small amount of a solid catalyst in addition to a reaction product and an unreacted product, and is supplied to the next step through the filter 8 as necessary.
【００１５】本発明が対象とする反応はとくに限定され
るものではなく、水素添加反応、アミノ化反応、アルキ
ル化反応、ニトリル化反応、酸化反応、塩素化反応、カ
ルボニル化反応などに適用することができる。反応に用
いられる液状原料としては、医薬、農薬、香料、染料な
どの化学反応に用いられる有機化合物があげられる。一
例をあげれば、ヘキセン、ブタジエン、アセトン、メチ
ルエチルケトン、ベンゼン、ジクロロベンゼン、トルイ
ジン、フェノール、アニリン、ニトロベンゼン、ニトロ
ベンゼンスルホン酸、ニトロＴ酸、ｐーアミノジフェニ
ルアミン、ｐーニトロフェノール、ゲラニオール、脂肪
酸、脂肪酸ニトリル、ラウリルアルコール、ｐーキシレ
ン、イソプロパノール、ブタノール、２，３ーブチレン
グリコール、１，９ーノナンジアール、２ーメチルー
１，８ーオクタンジアール、又はこれらの混合物を例示
することができる。The reaction of the present invention is not particularly limited, and is applicable to hydrogenation, amination, alkylation, nitrilation, oxidation, chlorination, carbonylation, etc. Can be. Examples of the liquid raw material used for the reaction include organic compounds used for chemical reactions such as medicines, agricultural chemicals, flavors, and dyes. For example, hexene, butadiene, acetone, methyl ethyl ketone, benzene, dichlorobenzene, toluidine, phenol, aniline, nitrobenzene, nitrobenzenesulfonic acid, nitro T acid, p-aminodiphenylamine, p-nitrophenol, geraniol, fatty acid, fatty acid nitrile , Lauryl alcohol, p-xylene, isopropanol, butanol, 2,3-butylene glycol, 1,9-nonandial, 2-methyl-1,8-octanedial, or a mixture thereof.
【００１６】なかでも、１，９ーノナンジアール、２ー
メチルー１，８ーオクタンジアール、又はこれらの混合
物のようなジアルデヒド類は不安定であり、閉鎖系で行
うのが望ましいので本発明の連続反応装置に好適であ
る。In particular, dialdehydes such as 1,9-nonandial, 2-methyl-1,8-octanedial, and mixtures thereof are unstable, and it is desirable to carry out the reaction in a closed system. Suitable for the device.
【００１７】本発明に使用される固体触媒は液状原料に
応じて決められるものであるが、液状原料と混合した場
合、スラリ−状になるものが好ましい。これらの固体触
媒を例示すると、ニッケル、コバルト、銅、銀、白金、
クロム、パラジウム、マンガン、鉄、チタン、トリウ
ム、マグネシウム、亜鉛、タングステン、モリブデン、
レニウム及びジルコニウムなどの金属のうち少なくとも
一種以上の金属触媒またはその変性触媒、ラネ−触媒及
びシリカ、アルミナ、ケイソウ土、マグネシウム、酸化
亜鉛などに担持させた触媒をあげることができる。The solid catalyst used in the present invention is determined according to the liquid raw material, but is preferably in the form of a slurry when mixed with the liquid raw material. Illustrative of these solid catalysts are nickel, cobalt, copper, silver, platinum,
Chromium, palladium, manganese, iron, titanium, thorium, magnesium, zinc, tungsten, molybdenum,
Examples thereof include at least one metal catalyst such as rhenium and zirconium or a modified catalyst thereof, a Raney catalyst, and a catalyst supported on silica, alumina, diatomaceous earth, magnesium, zinc oxide and the like.
【００１８】反応を実施するにあたって、適宜溶媒を使
用してもよい。溶媒は通常種々の反応に一般的に使用さ
れる溶媒であるが、このような例としては、メタノ−
ル、エタノ−ル、ブタノ−ル、ヘキサノ−ル、２−エチ
ルヘキサノ−ル、オクタノ−ル、エチレングリコ−ルな
どのアルコ−ル類、ヘキサン、オクタン、デカン、流動
パラフィン、シクロヘキサンなどの脂肪族炭化水素類な
どをあげることができる。触媒調製に用いる溶媒と反応
に用いる溶媒とが同じ種類のものであるのが好ましいこ
とはもちろんである。In carrying out the reaction, a solvent may be used as appropriate. The solvent is generally a solvent generally used for various reactions. Examples of such a solvent include methano-
Alcohols such as ethanol, ethanol, butanol, hexanole, 2-ethylhexanol, octanol and ethylene glycol, and aliphatic carbons such as hexane, octane, decane, liquid paraffin and cyclohexane. Hydrogens and the like can be given. It is needless to say that the solvent used for preparing the catalyst and the solvent used for the reaction are preferably of the same type.
【００１９】本発明の反応装置は、常圧でも勿論使用で
きるが、高圧になるとさらに効果を発揮する。すなわ
ち、反応系が高圧であると、従来法の場合、一旦常圧近
辺の圧力にもどして固体触媒の分離を行う必要があり、
しかも再使用のために再度昇圧して特殊な供給装置で反
応系へもどす必要があったが、本発明の反応装置はその
ような煩わしさはなく、液体サイクロンで反応混合物と
固体触媒を連続的に効率よく分離し、分離された固体触
媒を連続的に再使用しながら反応を実施することができ
る。若干の触媒の損失は反応液の状態をチェックするこ
とにより、適宜補給すればよい。連続反応は、系内の圧
力、温度、液面レベルなど所定の条件になるように適宜
制御しながら実施される。The reactor of the present invention can of course be used at normal pressure, but it is more effective at higher pressure. That is, when the reaction system is at a high pressure, in the case of the conventional method, it is necessary to once return to a pressure near normal pressure to separate the solid catalyst,
In addition, it was necessary to increase the pressure again for reuse and return it to the reaction system with a special supply device.However, the reaction device of the present invention does not have such a troublesomeness. And the reaction can be carried out while continuously reusing the separated solid catalyst. A slight loss of the catalyst may be appropriately replenished by checking the state of the reaction solution. The continuous reaction is carried out while appropriately controlling the pressure, temperature, liquid level and the like in the system so as to satisfy predetermined conditions.
【００２０】[0020]
【実施例】以下、実施例により本発明をさらに具体的に
説明する。 実施例１ 図１に示す２枚のタ−ビン翼を有する撹拌槽を反応容器
とし、図１に示す反応装置により、固体触媒としてニッ
ケルーケイソウ土触媒を使用して１，９ーノナンジアー
ル及び２ーメチルー１，８ーオクタンジアールの連続還
元アミノ化反応を行った。反応原料として、１，９ーノ
ナンジアール及び２ーメチルー１，８ーオクタンジアー
ルの８：２の混合物、溶媒としてメタノ−ル及び上記固
体触媒を反応容器に仕込み、定常時の反応容器内液状混
合物１２００ｋｇ、触媒濃度１ｗｔ％、反応圧力５０ａ
ｔｍ、温度１５０℃になるように、１，９ーノナンジア
ール及び２ーメチルー１，８ーオクタンジアールの混合
物を２１７ｋｇ／ｈｒ、メタノ−ルを６１６ｋｇ／ｈ
ｒ、液体アンモニアを３５５ｋｇ／ｈｒ及び水素を６３
Ｎｍ3 ／ｈｒで連続的に供給して反応を行い、循環反応
液のうち３０ｋｇ／ｍｉｎを直径１ｃｍ、高さ１０ｃｍ
の液体サイクロン素子１２本からなる液体サイクロン装
置に供給し、残りを１４０℃に設定した冷却器を通して
反応容器に循環した。The present invention will be described more specifically with reference to the following examples. Example 1 A stirring vessel having two turbine blades as shown in FIG. 1 was used as a reaction vessel, and a 1,9-nonandial and 2-methyl-methyl diatomaceous earth catalyst was used as a solid catalyst by the reactor shown in FIG. A continuous reductive amination reaction of 1,8-octanedial was performed. As a reaction raw material, an 8: 2 mixture of 1,9-nonandial and 2-methyl-1,8-octanedial, methanol and a solid catalyst as a solvent were charged into a reaction vessel, and 1200 kg of a liquid mixture in the reaction vessel at a steady state was charged. Catalyst concentration 1 wt%, reaction pressure 50a
217 kg / hr of a mixture of 1,9-nonandial and 2-methyl-1,8-octanedial and 616 kg / h of methanol so that the temperature is 150 ° C.
r, 355 kg / hr of liquid ammonia and 63 of hydrogen
The reaction is carried out by continuously supplying Nm 3 / hr, and 30 kg / min of the circulating reaction solution is 1 cm in diameter and 10 cm in height.
Was supplied to a liquid cyclone device consisting of 12 liquid cyclone elements, and the remainder was circulated to a reaction vessel through a cooler set at 140 ° C.
【００２１】液体サイクロンからは、メタノ−ル５２ｗ
ｔ％、アンモニア２６ｗｔ％、Ｈ2Ｏ４ｗｔ％と、０．
０５ｗｔ％の触媒を含む１，９−ノナンジアミン及び２
−メチル−１，８−オクタンジアミン混合物１７ｗｔ％
からなる清澄な液が２０ｋｇ／ｍｉｎで得られた。清澄
液には、１，９ーノナンジアール及び２ーメチルー１，
８ーオクタンジアールは検出されなかった。該清澄液を
２ｍ2 のフィルタ−に通してさらに触媒を分離したが、
反応系外へ流出した触媒はわずかであった。From the hydrocyclone, methanol 52w
%, ammonia 26 wt%, H 2 O 4 wt%, and 0.1 wt%.
1,9-nonanediamine containing 05 wt% of catalyst and 2
-Methyl-1,8-octanediamine mixture 17wt%
Was obtained at 20 kg / min. The clarified liquid contained 1,9-nonandial and 2-methyl-1,
8-octanedial was not detected. The clarified liquid was passed through a 2 m 2 filter to further separate the catalyst.
A small amount of the catalyst flowed out of the reaction system.
【００２２】実施例２ 図２に示すエゼクタを備えた反応容器を使用した以外は
実施例１と同様に操作したところ、液体サイクロンから
０．０１ｗｔ％の触媒を含む清澄な液が得られた。Example 2 The same operation as in Example 1 was carried out except that the reaction vessel equipped with an ejector shown in FIG. 2 was used. As a result, a clear liquid containing 0.01% by weight of a catalyst was obtained from the hydrocyclone.
【００２３】比較例１ 液体サイクロンを有さない従来の反応装置を用いて、実
施例１と同様の反応を行った。反応液は常圧にもどし、
濾過機で固体触媒の濾過を行い、固体触媒は溶媒で再調
製した後、加圧ポンプにより反応容器にリサイクル使用
した。Comparative Example 1 The same reaction as in Example 1 was carried out using a conventional reactor having no hydrocyclone. The reaction solution is returned to normal pressure,
The solid catalyst was filtered by a filter, and the solid catalyst was re-prepared with a solvent and then recycled to the reaction vessel by a pressure pump.
【００２４】比較例２ 液体サイクロンを有さない従来の反応装置を用いて、実
施例１と同様の反応を行った。反応液は常圧にもどし、
遠心分離機で固体触媒の分離を行い、固体触媒は溶媒で
再調製した後、加圧ポンプにより反応容器にリサイクル
使用した。Comparative Example 2 The same reaction as in Example 1 was carried out using a conventional reactor having no hydrocyclone. The reaction solution is returned to normal pressure,
The solid catalyst was separated by a centrifugal separator, and the solid catalyst was re-prepared with a solvent and then recycled to the reaction vessel by a pressure pump.
【００２５】比較例１及び比較例２では煩雑な触媒分離
回収操作及び触媒の調製再使用操作を必要とするのに対
し、実施例１及び実施例２ではこのような操作を必要と
せず、安定に連続運転可能であった。以上の結果から、
本発明の効果は明らかである。In Comparative Examples 1 and 2, complicated operation for separating and recovering the catalyst and operation for preparing and reusing the catalyst are required, whereas in Examples 1 and 2, such operation is not required and the operation is stable. Could be operated continuously. From the above results,
The effects of the present invention are clear.
【００２６】[0026]
【発明の効果】本発明によれば、反応系に液体サイクロ
ンを設けることにより、液状の反応混合物と固体触媒を
連続的に分離することができるので、煩雑な触媒分離回
収操作を必要とせず、連続的に効率よく生産を実施する
ことができる。According to the present invention, by providing a liquid cyclone in a reaction system, a liquid reaction mixture and a solid catalyst can be continuously separated, so that a complicated catalyst separation and recovery operation is not required. Production can be continuously and efficiently performed.
【図１】本発明の連続反応装置の一例である。FIG. 1 is an example of the continuous reaction apparatus of the present invention.
【図２】本発明の連続反応装置の別の例である。FIG. 2 is another example of the continuous reaction apparatus of the present invention.
１ 液状原料供給ライン ２ 反応容器 ３ 撹拌機 ４ ガス供給ライン ５ 循環ポンプ ６ 加熱器又は冷却器 ７ 液体サイクロン ８ フィルタ− ９ エゼクタ Reference Signs List 1 liquid raw material supply line 2 reaction vessel 3 stirrer 4 gas supply line 5 circulation pump 6 heater or cooler 7 liquid cyclone 8 filter 9 ejector
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ // Ｃ０７Ｂ 61/00 ３００ Ｂ０１Ｊ 23/74 ３２１Ｘ ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 6 Identification symbol FI // C07B 61/00 300 B01J 23/74 321X
Claims (6)
応容器、反応混合物を循環するための循環ポンプ及び液
体サイクロンから構成されることを特徴とする連続反応
装置。1. A continuous reaction apparatus comprising at least a reaction vessel having a liquid material supply port, a circulation pump for circulating a reaction mixture, and a liquid cyclone.
反応容器が撹拌機を備えた反応容器である連続反応装
置。2. The continuous reactor according to claim 1, wherein
A continuous reactor in which the reaction vessel is a reaction vessel equipped with a stirrer.
反応容器がエゼクタを備えた反応容器である連続反応装
置。3. The continuous reactor according to claim 1, wherein
A continuous reactor in which the reaction vessel is a reaction vessel provided with an ejector.
反応容器が環状の反応容器である連続反応装置。4. The continuous reactor according to claim 1, wherein
A continuous reactor in which the reaction vessel is an annular reaction vessel.
応させて反応生成物を得る生産方法において、反応混合
物の一部は反応容器へ循環させつつ、一部を液体サイク
ロンへ導き、液体サイクロンで液状の反応混合物と固体
触媒を分離し、該固体触媒は反応容器へリサイクルし、
該液状の反応混合物は反応系外へ抜き出すことを特徴と
する連続生産方法。5. A method for producing a reaction product by reacting a liquid raw material in a liquid phase in the presence of a solid catalyst, wherein a part of the reaction mixture is circulated to a reaction vessel while a part is guided to a liquid cyclone. Separate the liquid reaction mixture and the solid catalyst in the hydrocyclone, the solid catalyst is recycled to the reaction vessel,
A continuous production method, wherein the liquid reaction mixture is withdrawn outside the reaction system.
原料が１，９ーノナンジアール及び／又は２ーメチルー
１，８ーオクタンジアールである連続生産方法。6. The continuous production method according to claim 5, wherein the liquid raw material is 1,9-nonandial and / or 2-methyl-1,8-octanedial.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8272251A JPH10113551A (en) | 1996-10-15 | 1996-10-15 | Continuous reaction apparatus and production method using thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8272251A JPH10113551A (en) | 1996-10-15 | 1996-10-15 | Continuous reaction apparatus and production method using thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH10113551A true JPH10113551A (en) | 1998-05-06 |
Family
ID=17511248
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8272251A Pending JPH10113551A (en) | 1996-10-15 | 1996-10-15 | Continuous reaction apparatus and production method using thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH10113551A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000066255A1 (en) * | 1999-04-30 | 2000-11-09 | Slowik Guenter | Method and device for processing a substance or substance mixture which is situated in a container and rotates about the container axis, notably because of a mixing or stirring action |
| WO2003035258A1 (en) * | 2001-10-24 | 2003-05-01 | Daikin Industries, Ltd. | Method and system for the recovery of catalysts and process and unit for the production of perfluoroalkyl iodide telomers |
| JP2006199685A (en) * | 2004-12-22 | 2006-08-03 | Sumitomo Chemical Co Ltd | Method for producing cyclohexanone oxime |
| JP2014028368A (en) * | 2001-03-22 | 2014-02-13 | Ceramic Fuel Cells Ltd | Liquid phase reactor |
-
1996
- 1996-10-15 JP JP8272251A patent/JPH10113551A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000066255A1 (en) * | 1999-04-30 | 2000-11-09 | Slowik Guenter | Method and device for processing a substance or substance mixture which is situated in a container and rotates about the container axis, notably because of a mixing or stirring action |
| JP2014028368A (en) * | 2001-03-22 | 2014-02-13 | Ceramic Fuel Cells Ltd | Liquid phase reactor |
| JP2015083303A (en) * | 2001-03-22 | 2015-04-30 | ビーケイ・ギウリニ・ゲゼルシャフト・ミット・ベシュレンクテル・ハフツングＢｋ Ｇｉｕｌｉｎｉ Ｇｍｂｈ | Liquid phase reactor |
| WO2003035258A1 (en) * | 2001-10-24 | 2003-05-01 | Daikin Industries, Ltd. | Method and system for the recovery of catalysts and process and unit for the production of perfluoroalkyl iodide telomers |
| US7601878B2 (en) | 2001-10-24 | 2009-10-13 | Daikin Industries, Ltd. | Process and unit for production of perfluoroalkyl iodide telomers |
| JP2006199685A (en) * | 2004-12-22 | 2006-08-03 | Sumitomo Chemical Co Ltd | Method for producing cyclohexanone oxime |
| JP4577205B2 (en) * | 2004-12-22 | 2010-11-10 | 住友化学株式会社 | Method for producing cyclohexanone oxime |
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