JPH057702A - Distillation apparatus equipped with reactor - Google Patents
Distillation apparatus equipped with reactorInfo
- Publication number
- JPH057702A JPH057702A JP16584791A JP16584791A JPH057702A JP H057702 A JPH057702 A JP H057702A JP 16584791 A JP16584791 A JP 16584791A JP 16584791 A JP16584791 A JP 16584791A JP H057702 A JPH057702 A JP H057702A
- Authority
- JP
- Japan
- Prior art keywords
- reactor
- distillation column
- reaction
- distillation
- liquid distributor
- 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
- 238000004821 distillation Methods 0.000 title claims abstract description 57
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000001816 cooling Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000009835 boiling Methods 0.000 claims description 11
- 239000011949 solid catalyst Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 239000000376 reactant Substances 0.000 description 10
- 230000002378 acidificating effect Effects 0.000 description 9
- 239000011521 glass Substances 0.000 description 8
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 description 7
- OBSHSWKHUYGFMF-UHFFFAOYSA-N 3,3-dimethoxy-2-methylprop-1-ene Chemical compound COC(OC)C(C)=C OBSHSWKHUYGFMF-UHFFFAOYSA-N 0.000 description 6
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000003507 refrigerant Substances 0.000 description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- NKDDWNXOKDWJAK-UHFFFAOYSA-N dimethoxymethane Chemical compound COCOC NKDDWNXOKDWJAK-UHFFFAOYSA-N 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- HEWZVZIVELJPQZ-UHFFFAOYSA-N 2,2-dimethoxypropane Chemical compound COC(C)(C)OC HEWZVZIVELJPQZ-UHFFFAOYSA-N 0.000 description 1
- XYJXZLHRRNRNHF-UHFFFAOYSA-N 3,3-diethoxy-2-methylprop-1-ene Chemical compound CCOC(C(C)=C)OCC XYJXZLHRRNRNHF-UHFFFAOYSA-N 0.000 description 1
- MCIPQLOKVXSHTD-UHFFFAOYSA-N 3,3-diethoxyprop-1-ene Chemical compound CCOC(C=C)OCC MCIPQLOKVXSHTD-UHFFFAOYSA-N 0.000 description 1
- OBWGMYALGNDUNM-UHFFFAOYSA-N 3,3-dimethoxyprop-1-ene Chemical compound COC(OC)C=C OBWGMYALGNDUNM-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
(57)【要約】
【目的】 平衡反応を平衡時の反応率より高い反応率で
進行させる反応器付き蒸留装置を提供する。
【構成】 加熱装置，蒸留塔，冷却装置，液分配器，反
応器を備えた蒸留装置であって、加熱装置は蒸留塔の下
部に付けられ、蒸留塔々頂からの留出物が冷却後液分配
器を経て一部は蒸留塔に環流され、一部は反応器へ導か
れ、反応液が蒸留塔へ導かれ、生成物が加熱装置に蓄積
される様にした装置。
(57) [Summary] [Object] To provide a distillation apparatus with a reactor that allows an equilibrium reaction to proceed at a higher reaction rate than that at equilibrium. [Structure] A distillation apparatus equipped with a heating device, a distillation column, a cooling device, a liquid distributor, and a reactor. The heating device is attached to the bottom of the distillation column, and the distillate from the tops of the distillation columns is cooled. An apparatus in which a part is refluxed to a distillation column through a liquid distributor, a part is introduced to a reactor, a reaction liquid is introduced to a distillation column, and a product is accumulated in a heating device.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、反応器を備えた蒸留装
置に関する。詳しくは、平衡反応を平衡時の反応率より
も高い反応率で進行させる、反応器を備えた蒸留装置に
関する。FIELD OF THE INVENTION The present invention relates to a distillation apparatus equipped with a reactor. More specifically, the present invention relates to a distillation apparatus equipped with a reactor that allows an equilibrium reaction to proceed at a higher reaction rate than the equilibrium reaction rate.
【０００２】[0002]
【従来の技術】従来、酸性触媒の存在下で原料物質（以
下、反応物という。）を反応させて、目的とする物質
（以下、目的生成物という。）を得る反応が数多く知ら
れている。一般に、酸性触媒存在下の反応は平衡反応で
あるものが多く、そのままでは反応は途中で止まってし
まい、高反応率で目的生成物を得ることはできない。し
たがって高反応率で目的生成物を得るために、平衡反応
を生成物側へ移動させる種々の方法が検討されており、
代表的な方法としては、（１）反応によりえられる生成
物から、副生する物質（以下、副生成物という。）例え
ばエステル化反応における生成水などを蒸留除去する方
法、（２）目的生成物自体を反応系より除去する方法が
知られている。前者の場合、副生成物が最も低沸点物で
あることが必要であり、通常除去助剤としてベンゼンや
ヘキサンなどの共沸溶剤が使用されている。また後者の
例としては、メチラールの合成法（特開平１−２８７０
５１号公報）が知られており、この場合目的生成物であ
るメチラールが最も低沸点物である。しかしながら、生
成物が原料物質よりも高沸点物である場合について、高
反応率で反応を進行させる方法は知られていない。2. Description of the Related Art Heretofore, many reactions have been known in which a target substance (hereinafter referred to as a target product) is obtained by reacting a raw material (hereinafter referred to as a reactant) in the presence of an acidic catalyst. . In general, many reactions in the presence of an acidic catalyst are equilibrium reactions, and the reaction stops in the middle as it is, and the target product cannot be obtained with a high reaction rate. Therefore, in order to obtain the target product with a high reaction rate, various methods of moving the equilibrium reaction to the product side have been studied,
As a typical method, (1) a method of distilling and removing substances by-produced (hereinafter referred to as by-products) from the product obtained by the reaction, for example, water produced in the esterification reaction, (2) objective production A method of removing the substance itself from the reaction system is known. In the former case, the by-product needs to have the lowest boiling point, and an azeotropic solvent such as benzene or hexane is usually used as a removal aid. Further, as an example of the latter, a method for synthesizing methylal (JP-A-1-2870
No. 51), in which case the target product methylal is the lowest boiling point product. However, in the case where the product has a higher boiling point than that of the raw material, no method is known to allow the reaction to proceed at a high reaction rate.
【０００３】[0003]
【発明が解決しようとする課題】本発明の目的とすると
ころは、生成物の少なくともひとつが反応物よりも高沸
点物である平衡反応であっても、高反応率で目的生成物
を得ることが可能な蒸留装置に関する。The object of the present invention is to obtain a target product with a high reaction rate even in an equilibrium reaction in which at least one of the products has a higher boiling point than the reactant. The present invention relates to a distillation apparatus capable of
【０００４】[0004]
【課題を解決するための手段】本発明は、原料物質より
も生成物の少なくともひとつが高沸点物である反応系に
おいて用いる、加熱装置，蒸留塔，冷却装置，液分配
器，反応器を備えた蒸留装置であって、加熱装置は蒸留
塔下部に付帯し、蒸留塔塔頂部は蒸気流通管によって冷
却装置入側に連結され、冷却装置出側は液分配器の入側
に連結され、液分配器の二つの出側のうちのひとつは蒸
留塔塔頂側部に連結され、液分配器のもう一方の出側は
反応器入側へ連結され、反応器出側は蒸留塔側部へ連結
された蒸留装置であって、反応器内へは反応を進行させ
る固体触媒が充填出来るようになっていることを特徴と
する反応器を備えた蒸留装置にある。The present invention comprises a heating device, a distillation column, a cooling device, a liquid distributor, and a reactor used in a reaction system in which at least one of the products is a high-boiling substance rather than the raw material. In the distillation device, the heating device is attached to the lower part of the distillation column, the top part of the distillation column is connected to the inlet side of the cooling device by a vapor flow pipe, and the outlet side of the cooling device is connected to the inlet side of the liquid distributor. One of the two outlets of the distributor is connected to the top of the distillation column, the other outlet of the liquid distributor is connected to the inlet of the reactor, and the outlet of the reactor is connected to the side of the distillation column. A connected distillation apparatus is provided with a reactor characterized in that a solid catalyst for advancing a reaction can be filled in the reactor.
【０００５】以下、本発明を実施例を用いて説明する。
しかしながら、本発明は実施例によってなんら限定され
るものではない。第１図は本発明の１実施例を示す工程
図である。また第２図及び第３図は、それぞれ本発明に
おける加熱装置及び冷却装置周辺の１態様の概要を示す
部分工程図である。The present invention will be described below with reference to examples.
However, the present invention is not limited to the examples. FIG. 1 is a process drawing showing one embodiment of the present invention. Further, FIG. 2 and FIG. 3 are partial process diagrams showing the outline of one aspect around the heating device and the cooling device in the present invention.
【０００６】まず、加熱装置１内へ反応物を導入し、加
熱を開始する。該加熱装置１は蒸留塔２内温度を所定の
温度に保持するために設置されており、この機能を発揮
できるものであれば装置の種類，計上，能力等について
特に制限されるものではなく、目的に応じて任意に選択
すればよい。また、加熱装置１は第１図に示すように蒸
留塔下部に一体化していても、第２図に示すように蒸留
塔と分離した型であってもいずれでもよい。First, a reactant is introduced into the heating device 1 to start heating. The heating device 1 is installed in order to maintain the temperature inside the distillation column 2 at a predetermined temperature, and the type, cost, capacity, etc. of the device are not particularly limited as long as they can exhibit this function. It may be arbitrarily selected according to the purpose. The heating device 1 may be integrated with the lower part of the distillation column as shown in FIG. 1 or may be of a type separated from the distillation column as shown in FIG.
【０００７】加熱装置１において気化した反応物は、蒸
留塔２を通り蒸留塔頂部に連結された蒸気流通管を通っ
て、冷却装置３の入側へ導かれる。蒸留塔２は、多段式
蒸留塔であっても、充填式蒸留塔であってもよく、目的
に応じて任意に選択すればよい。冷却装置３へ導入され
た反応物の蒸気は、冷却，液化されて液分配器４へ導入
される。冷却装置３は公知の冷却装置を用いることがで
き、特に制限されるものではない。The reactant vaporized in the heating device 1 is guided to the inlet side of the cooling device 3 through the distillation column 2 and the vapor flow pipe connected to the top of the distillation column. The distillation column 2 may be a multistage distillation column or a packed distillation column, and may be arbitrarily selected according to the purpose. The vapor of the reactant introduced into the cooling device 3 is cooled and liquefied and introduced into the liquid distributor 4. A known cooling device can be used as the cooling device 3 and is not particularly limited.
【０００８】液分配器４においては、蒸留塔の性能を維
持するのに必要なだけの液を蒸留塔塔頂側部へ導き、残
りの液を反応器５の入側へ導く。液分配器４は液を所定
量に分配できるものであれば特に制限されるものではな
く、目的に応じて任意に選択することができる。In the liquid distributor 4, as much liquid as necessary to maintain the performance of the distillation column is introduced to the top of the distillation column, and the remaining liquid is introduced to the inlet side of the reactor 5. The liquid distributor 4 is not particularly limited as long as it can distribute the liquid in a predetermined amount, and can be arbitrarily selected according to the purpose.
【０００９】反応器５へ導かれた反応物は反応器内で反
応し、反応器５の出口からは反応物と生成物の混合液が
出てくる。反応器５は、固定床反応器でも流動床反応器
でもいずれでもよく、目的に応じて任意に選択すること
ができる。また、反応器５の温度は特に制限されるもの
ではなく反応液の沸点以下で任意に選べばよいが、反応
速度の遅い反応の場合には反応液の沸点に近い温度であ
ることが望ましく、また、反応速度が早く発熱を伴う反
応の場合には反応器を冷却する方が望ましい。この反応
器５内には反応を進行させる固体触媒を充填する。触媒
は、反応を進行させ、かつ、固体である触媒であれば特
に限定されるものではない。たとえば、酸性触媒下で進
行する反応の場合には従来公知の種々の酸性固体触媒を
用いることができ、具体例としては、強酸性イオン交換
樹脂，ゼオライト，活性アルミノシリケート等が挙げら
れる。The reactant introduced into the reactor 5 reacts in the reactor, and a mixture of the reactant and the product comes out from the outlet of the reactor 5. The reactor 5 may be either a fixed bed reactor or a fluidized bed reactor, and can be arbitrarily selected according to the purpose. The temperature of the reactor 5 is not particularly limited and may be arbitrarily selected below the boiling point of the reaction solution, but in the case of a reaction with a slow reaction rate, it is desirable that the temperature be close to the boiling point of the reaction solution. Further, in the case of a reaction which has a high reaction rate and generates heat, it is desirable to cool the reactor. The reactor 5 is filled with a solid catalyst that advances the reaction. The catalyst is not particularly limited as long as it is a solid catalyst that allows the reaction to proceed. For example, in the case of a reaction that proceeds under an acidic catalyst, various conventionally known acidic solid catalysts can be used, and specific examples thereof include a strongly acidic ion exchange resin, zeolite, activated aluminosilicate and the like.
【００１０】反応器５を通った反応液は、反応物と生成
物に分離するために蒸留塔の最上段から最下段までのい
ずれかの段へ導かれる。その位置は反応液の物理的性質
および反応液の温度、蒸留塔の分離能力により決定され
るが、特に蒸留塔の中央の段から最上段までのいずれか
へ導入するのが好ましい。反応物は蒸留塔頂を経由して
反応器へ循環され、生成物は反応の進行にともない加熱
装置１内に蓄積される。The reaction liquid that has passed through the reactor 5 is introduced to any stage from the uppermost stage to the lowermost stage of the distillation column in order to separate into a reactant and a product. The position thereof is determined by the physical properties of the reaction solution, the temperature of the reaction solution, and the separation capacity of the distillation column, but it is particularly preferable to introduce it at any of the middle stage to the uppermost stage of the distillation column. The reaction product is circulated to the reactor via the top of the distillation column, and the product is accumulated in the heating device 1 as the reaction progresses.
【００１１】本発明の蒸留装置は、反応物よりも生成物
の少なくともひとつが高沸点物である平衡反応に対して
使用することができるが、特にアクロレインジメチルア
セタール，アクロレインジエチルアセタール，メタクロ
レインジメチルアセタール，メタクロレインジエチルア
セタール，アセトンジメチルアセタール等の化合物の合
成のように、全ての反応物よりも全ての生成物の方が高
沸点物である平衡反応に対して好ましい結果を与える。The distillation apparatus of the present invention can be used for equilibrium reactions in which at least one of the products has a higher boiling point than the reaction product, and in particular acrolein dimethyl acetal, acrolein diethyl acetal, methacrolein dimethyl acetal. , Methacrolein diethyl acetal, acetone dimethyl acetal, and the like give better results for equilibrium reactions in which all products have higher boiling points than all reactants.
【００１２】本発明の蒸留装置は、第１図のように密閉
系であっても第３図のように調圧装置６をつけてもよ
く、目的に応じて任意に選択することができる。調圧装
置６を使用する場合には、調圧装置入側は、冷却装置出
側から液分配器入側までのいずれかへ連結される。調圧
装置６は公知の装置を用いることができ、特に制限され
るものではない。たとえば、本発明の蒸留装置内を大気
圧に制御する場合には、冷却装置出側から液分配器入側
までのいずれかへ配管を設置し、大気へ解放すればよ
い。The distillation apparatus of the present invention may be a closed system as shown in FIG. 1 or may have a pressure adjusting device 6 as shown in FIG. 3, and can be arbitrarily selected according to the purpose. When the pressure regulator 6 is used, the pressure regulator inlet side is connected to any of the cooling device outlet side to the liquid distributor inlet side. A known device can be used as the pressure adjusting device 6 and is not particularly limited. For example, when controlling the atmospheric pressure in the distillation apparatus of the present invention, a pipe may be installed anywhere from the outlet side of the cooling device to the inlet side of the liquid distributor, and open to the atmosphere.
【００１３】以下、実施例を示す。Examples will be shown below.
【実施例１】ガラス製３Ｌフラスコにメタノール１１５
４ｇ（３６モル）、メタクロレイン８４２ｇ（１２モ
ル）、ヒドロキノン２ｇ、炭酸水素ナトリウム２ｇをい
れ、蒸留塔，冷却装置，液分配器，反応器を備えた蒸留
装置にとりつけた。蒸留塔は、内径３５ｍｍ，段間隔３
０ｍｍのガラス製２０段オルダーショウ蒸留塔であり、
冷却装置は冷媒として水道水を用いた３０ｃｍガラス製
ビグリュー管である。液分配器は、振子により液を二分
するような型のもので、電磁石およびタイマーにより液
流量を制御する。反応器はガラス製二重管構造になって
おり、内部には酸性固体触媒として強酸性イオン交換樹
脂（Ａｍｂｅｒｌｉｓｔ−１５，ロームアンドハース社
製）を５０ｍｌ充填し、外部には０℃の冷媒を流した。
また反応器を通った反応液は蒸留塔の中央の段に戻るよ
うに装置を組んだ。その後、油浴を用いてフラスコを加
熱し１２時間反応をおこなった。反応終了後フラスコ内
は二層に分離し、上層はメタクロレインジメチルアセタ
ール１１９２ｇを含む８２％メタクロレインジメチルア
セタール溶液であった。この反応におけるメタクロレイ
ンの反応率は９９％であった。Example 1 Methanol 115 in a glass 3 L flask
4 g (36 mol), methacrolein 842 g (12 mol), hydroquinone 2 g, and sodium hydrogencarbonate 2 g were put and attached to a distillation apparatus equipped with a distillation column, a cooling device, a liquid distributor, and a reactor. The distillation column has an inner diameter of 35 mm and a stage interval of 3
It is a 0 mm glass 20-stage Oldershaw distillation column,
The cooling device is a 30 cm glass Vigreux tube using tap water as a refrigerant. The liquid distributor is of a type in which the liquid is divided into two parts by a pendulum, and the liquid flow rate is controlled by an electromagnet and a timer. The reactor has a double-tube structure made of glass, and is filled with 50 ml of a strongly acidic ion exchange resin (Amberlist-15, manufactured by Rohm and Haas Co.) as an acidic solid catalyst, and a 0 ° C. refrigerant outside. Shed
Further, the apparatus was set up so that the reaction liquid passing through the reactor returned to the central stage of the distillation column. Then, the flask was heated using an oil bath and the reaction was carried out for 12 hours. After the reaction was completed, the inside of the flask was separated into two layers, and the upper layer was an 82% methacrolein dimethyl acetal solution containing 1192 g of methacrolein dimethyl acetal. The reaction rate of methacrolein in this reaction was 99%.
【００１４】〔比較例１〕ガラス製２Ｌフラスコにメタ
ノール５１４ｇ（１６モル）、メタクロレイン３０９ｇ
（４モル）、ヒドロキノン２ｇ、強酸性イオン交換樹脂
（Ａｍｂｅｒｌｉｓｔ−１５．ロームアンドハース社
製）５０ｍｌをいれ、反応をおこなった。反応は瞬時に
終了し、濾過により触媒を除去したところ、メタクロレ
インジメチルアセタール１９０ｇを含む２３％メタクロ
レインジメチルアセタール溶液を得た。この反応におけ
るメタクロレインの反応率は４１％であった。[Comparative Example 1] 514 g (16 mol) of methanol and 309 g of methacrolein were placed in a glass 2 L flask.
(4 mol), 2 g of hydroquinone and 50 ml of a strongly acidic ion exchange resin (Amberlist-15, manufactured by Rohm and Haas Co.) were added and the reaction was carried out. The reaction was instantaneously completed, and the catalyst was removed by filtration to obtain a 23% methacrolein dimethyl acetal solution containing 190 g of methacrolein dimethyl acetal. The reaction rate of methacrolein in this reaction was 41%.
【００１５】〔比較例２〕ガラス製２Ｌフラスコにメタ
ノール５１４ｇ（１６モル）、メタクロレイン３０９ｇ
（４モル）、ヒドロキノン２ｇ、強酸性イオン交換樹脂
（Ａｍｂｅｒｌｉｓｔ−１５．ロームアンドハース社
製）５０ｍｌをいれ、蒸留塔，冷却装置，液分配器，留
出タンクを備えた蒸留装置にとりつけた。蒸留塔は、内
径３５ｍｍ，段間隔３０ｍｍのガラス製２０段オルダー
ショウ蒸留塔であり、冷却装置は冷媒として水道水を用
いた３０ｃｍガラス製ビグリュー管である。液分配器
は、振子により液を二分するような型のもので、電磁石
およびタイマーにより液流量を制御する。液分配器の出
側のうち一方は蒸留塔塔頂側部へ、もう一方は留出タン
ク出側へ連結した。その後、油浴を用いてフラスコを加
熱し蒸留をおこなった。その結果、留出液はメタクロレ
イン３０３ｇを含むメタクロレインとメタノールの混合
液であった。またメタクロレインジメチルアセタールは
得られなかった。Comparative Example 2 A glass 2 L flask was charged with 514 g (16 mol) of methanol and 309 g of methacrolein.
(4 mol), 2 g of hydroquinone, and 50 ml of a strongly acidic ion exchange resin (Amberlist-15, manufactured by Rohm and Haas Co.) were placed in a distillation apparatus equipped with a distillation column, a cooling device, a liquid distributor, and a distilling tank. The distillation column is a glass 20-stage Oldershaw distillation column having an inner diameter of 35 mm and a stage interval of 30 mm, and the cooling device is a 30 cm glass Vigreux tube using tap water as a refrigerant. The liquid distributor is of a type in which the liquid is divided into two parts by a pendulum, and the liquid flow rate is controlled by an electromagnet and a timer. One of the outlets of the liquid distributor was connected to the top of the distillation column and the other was connected to the outlet of the distillation tank. Then, the flask was heated using an oil bath for distillation. As a result, the distillate was a mixed solution of methacrolein containing 303 g of methacrolein and methanol. Further, methacrolein dimethyl acetal was not obtained.
【００１６】[0016]
【発明の効果】以上詳述したように、本発明の蒸留装置
を用いることにより、生成物が反応物よりも高沸点物で
ある平衡反応であっても平衡時の反応率よりも高い反応
率で生成物を得ることができることから、高生産性装置
として工業的見地からその効果はきわめて大きいもので
ある。As described in detail above, by using the distillation apparatus of the present invention, even in the equilibrium reaction in which the product has a higher boiling point than the reactant, the reaction rate higher than that at equilibrium is obtained. Since the product can be obtained by the method described above, the effect is extremely large from the industrial viewpoint as a high productivity device.
【図１】本発明の装置の概略を示す工程図FIG. 1 is a process diagram showing an outline of an apparatus of the present invention.
【図２】加熱装置と蒸留塔が分離した型の装置における
装置下部の概略を示す工程図FIG. 2 is a process diagram showing an outline of a lower part of an apparatus of a type in which a heating device and a distillation column are separated.
【図３】本発明の装置に調圧装置をとりつけた場合の装
置上部の概略を示す工程図FIG. 3 is a process diagram showing an outline of an upper part of a device when a pressure adjusting device is attached to the device of the present invention.
Claims (1)
つが高沸点物である反応系において用いる、加熱装置，
蒸留塔，冷却装置，液分配器，反応器を備えた蒸留装置
であって、加熱装置は蒸留塔下部に付帯し、蒸留塔塔頂
部は蒸気流通管によって冷却装置入側に連結され、冷却
装置出側は液分配器の入側に連結され、液分配器の二つ
の出側のうちのひとつは蒸留塔塔頂側部に連結され、液
分配器のもう一方の出側は反応器入側へ連結され、反応
器出側は蒸留塔側部へ連結された蒸留装置であって、反
応器内へは反応を進行させる固体触媒が充填出来るよう
になっていることを特徴とする反応器を備えた蒸留装
置。Claim: What is claimed is: 1. A heating device used in a reaction system in which at least one of the products is a high-boiling substance rather than the raw material,
A distillation apparatus comprising a distillation column, a cooling device, a liquid distributor, and a reactor, wherein a heating device is attached to a lower part of the distillation column, and a top part of the distillation column is connected to an inlet side of the cooling device by a steam distribution pipe. The outlet side is connected to the inlet side of the liquid distributor, one of the two outlet sides of the liquid distributor is connected to the top side of the distillation column, and the other outlet side of the liquid distributor is the reactor inlet side. Is a distillation apparatus connected to the side of the distillation column on the outlet side of the reactor, and a solid catalyst for advancing the reaction can be filled in the reactor. Equipped with distillation equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16584791A JPH057702A (en) | 1991-07-05 | 1991-07-05 | Distillation apparatus equipped with reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16584791A JPH057702A (en) | 1991-07-05 | 1991-07-05 | Distillation apparatus equipped with reactor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH057702A true JPH057702A (en) | 1993-01-19 |
Family
ID=15820133
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16584791A Pending JPH057702A (en) | 1991-07-05 | 1991-07-05 | Distillation apparatus equipped with reactor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH057702A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SG112887A1 (en) * | 2003-08-07 | 2005-07-28 | Cheng Ming Chou | Multi-stage vacuum distilling, cooling and freezing processes and apparatuses for solution separation and seawater desalination. |
-
1991
- 1991-07-05 JP JP16584791A patent/JPH057702A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SG112887A1 (en) * | 2003-08-07 | 2005-07-28 | Cheng Ming Chou | Multi-stage vacuum distilling, cooling and freezing processes and apparatuses for solution separation and seawater desalination. |
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