JPH0987392A - Continuous polycondensation polymer manufacturing apparatus and manufacturing method - Google Patents
Continuous polycondensation polymer manufacturing apparatus and manufacturing methodInfo
- Publication number
- JPH0987392A JPH0987392A JP24125495A JP24125495A JPH0987392A JP H0987392 A JPH0987392 A JP H0987392A JP 24125495 A JP24125495 A JP 24125495A JP 24125495 A JP24125495 A JP 24125495A JP H0987392 A JPH0987392 A JP H0987392A
- Authority
- JP
- Japan
- Prior art keywords
- stirring
- tower
- manufacturing apparatus
- polycondensation
- transesterification
- 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
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- Physical Or Chemical Processes And Apparatus (AREA)
- Polyesters Or Polycarbonates (AREA)
- Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)
Abstract
Description
【発明の詳細な説明】Detailed Description of the Invention
【0001】[0001]
【産業上の利用分野】本発明は高分子樹脂の製造装置及
び方法に関するもので、特にポリエチレンテレフタレー
ト、ポリカーボネート等の重縮合系高分子の重合に好適
な装置及び方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus and method for producing polymer resins, and more particularly to an apparatus and method suitable for polymerizing polycondensation polymers such as polyethylene terephthalate and polycarbonate.
【0002】[0002]
【従来の技術】従来ポリエチレンテレフタレート(PE
T)の重合方法は社団法人化学工学協会編プロセス集成
(1970)P892にあるようにエステル交換槽、初
期重合槽、重合槽から構成される製造プロセスが使用さ
れている。実際のプロセスではエステル交換槽が数台に
分割され、また初期重合槽も2分割されて使用されるの
が一般的である。2. Description of the Related Art Conventional polyethylene terephthalate (PE
As the polymerization method of T), a manufacturing process including a transesterification tank, an initial polymerization tank, and a polymerization tank is used as described in Process Compilation (1970) P892 edited by Japan Chemical Engineering Association. In an actual process, it is general that the transesterification tank is divided into several units, and the initial polymerization tank is also divided into two and used.
【0003】[0003]
【発明が解決しようとする課題】本発明の目的はエステ
ル交換槽と初期重合槽の一部を一体化して第1製造装
置、初期重合槽の残りと最終重合工程を一体化して第2
製造装置とし、反応槽の数を低減することにより各撹拌
槽の駆動部品や配管点数、シール部品等の全体部品点数
の低減を図るものであるAn object of the present invention is to integrate a part of the transesterification tank and the initial polymerization tank into a first production apparatus, and integrate the rest of the initial polymerization tank and the final polymerization step into a second one.
As a manufacturing device, by reducing the number of reaction tanks, the number of drive parts, piping points, seal parts, etc. of each stirring tank is reduced.
【0004】[0004]
【課題を解決するための手段】上記の課題や目的はエス
テル交換槽を上塔に設置し、初期重合槽を下塔に設置し
て一体化した第1製造装置と中間重合槽と最終重合槽を
一体化した横型の第2製造装置とで重縮合系高分子の連
続製造装置を構成することにより、製造装置の構成部品
点数及び材料の低減、装置の組立配管工数の削減、保温
据付けコストの低減を図ることにより達成される。[Means for Solving the Problems] The above problems and objectives are to install a transesterification tank in an upper tower and an initial polymerization tank in a lower tower to integrate them into a first manufacturing apparatus, an intermediate polymerization tank and a final polymerization tank. By configuring a continuous polycondensation polymer manufacturing device with a horizontal second manufacturing device that integrates the above, the number of components and materials of the manufacturing device can be reduced, the number of man-hours for assembling and piping the device can be reduced, and the heat insulation and installation cost can be reduced. This is achieved by reducing the amount.
【0005】[0005]
【作用】第1製造装置の入口ノズルより連続供給された
原料は上塔でエステル交換された後、オリゴマーを生成
し、下塔へ供給され下塔内の各撹拌室で、揮発物を蒸発
させながら、下塔下部側へ流動し、効率良く重縮合反応
が進み、重合度が高められる。さらに第2製造装置に供
給され、横型の撹拌室内で撹拌部材により撹拌及び表面
更新作用を受け、順次下流側へ移動して効率良く反応が
進み目的の重合度まで高められる。The raw material continuously supplied from the inlet nozzle of the first manufacturing apparatus undergoes transesterification in the upper tower to form an oligomer, which is then supplied to the lower tower to evaporate volatile matter in each stirring chamber in the lower tower. However, it flows to the lower side of the lower tower, the polycondensation reaction proceeds efficiently, and the degree of polymerization is increased. Further, it is supplied to the second manufacturing apparatus, and subjected to stirring and surface renewal action by the stirring member in the horizontal stirring chamber, sequentially moving to the downstream side, and the reaction proceeds efficiently to increase the degree of polymerization to the target.
【0006】[0006]
【実施例】図1に本発明の一実施例を示す。図におい
て、左側は竪型の第1製造装置、右側は横型の第2製造
装置を示しており、1は竪長円筒状の第1製造装置本体
で外周を熱媒ジャケット(図示せず)で覆われており、
容器本体は内部で2分割され、上塔側はエステル交換槽
2、下塔側は初期重合槽3が形成されている。原料13
はエステル交換槽2の下部に設けた供給ノズル4より入
り、低粘度用撹拌翼6により撹拌混合され、エステル化
反応が促進される。エステル交換槽2の上部にはエステ
ル交換反応によって生成される副生物12を除去するノ
ズル11が取り付けられており、下流側にあるコンデン
サーにより分離回収される。エステル交換槽2と初期重
合槽3は連結管7で結合されており、その上端側はエス
テル交換槽2上部の液表面まで立ち上げられ、下端側は
初期重合槽3の槽内上部に設けたトレイ8aの液溜りの
中に設置されており、該連結管7の途中にはトレイ8a
の液面高さを調整する流量調整バルブ9が設けてあり、
トレイ8a上の液面が所定の高さになるように制御され
ている。初期重合槽3の気相部には各トレイの液表面か
ら重合反応によって生成し、気化した副生物等は揮発物
14を取り除くための揮発物取り出しノズル10が設け
られている。揮発物取り出しノズル10の下流側には槽
内の圧力を減圧雰囲気にするために真空ポンプ(図示せ
ず)や副生物を捕集するためのコンデンサー(図示せ
ず)等が設けられる。図に示したように本実施例では初
期重合槽3の内部に撹拌翼部材を持たない構成となって
いる。この撹拌翼の代わりに流下式トレイを多段に設置
して大きな表面更新作用を得る構造となっている。初期
重合槽3の内部にはリング状のトレイ8aと円筒状のト
レイ8bとが交互に配置されており、リング状のトレイ
8aの内周上面側と円筒状のトレイ8bの外周上面側と
には1個所あるいは複数個所の切欠き部が設けられ、処
理液は下流側のトレイへと流れて行き初期重合槽3の底
部へと到達し、抜き出しノズル5から初期重合物15が
取り出され、さらに次の第2製造装置へと進んで行く。
図において、30は概略円形断面を有する横長の円筒状
の第2製造装置本体で外周を熱媒ジャケット(図示せ
ず)で覆われており、内部長手方向に2本の回転軸31
が取り付けられている。回転軸31には例えば特許第1
024745に示すような掻き取り板と円板で形成され
る撹拌翼32が設置されている。それぞれの撹拌翼32
は本体容器30の内壁表面と撹拌軸及び翼の表面をかき
とって回転する。さらに、本体30の最上部には揮発物
の出口ノズルが設けられ反応副生物40を取りだすため
に配管で凝縮器及び真空ポンプ(図示せず)に接続され
る。また、処理液の最終重合物41は入口と反対側に設
けた出口より取りだされる。FIG. 1 shows an embodiment of the present invention. In the figure, the left side shows a vertical first manufacturing apparatus, the right side shows a horizontal second manufacturing apparatus, 1 is a vertically long cylindrical first manufacturing apparatus main body and a heat medium jacket (not shown) on the outer periphery. Covered,
The container body is divided into two inside, the transesterification tank 2 is formed on the upper tower side, and the initial polymerization tank 3 is formed on the lower tower side. Raw material 13
Enters through a supply nozzle 4 provided in the lower part of the transesterification tank 2 and is agitated and mixed by a low-viscosity agitating blade 6 to accelerate the esterification reaction. A nozzle 11 for removing a by-product 12 produced by a transesterification reaction is attached to the upper part of the transesterification tank 2, and is separated and recovered by a condenser on the downstream side. The transesterification tank 2 and the initial polymerization tank 3 are connected by a connecting pipe 7. The upper end side of the transesterification tank 2 is raised to the liquid surface above the transesterification tank 2, and the lower end side thereof is provided in the upper part of the initial polymerization tank 3. The tray 8a is installed in the liquid pool, and the tray 8a is provided in the middle of the connecting pipe 7.
A flow rate adjusting valve 9 for adjusting the liquid level height of
The liquid level on the tray 8a is controlled to have a predetermined height. The vapor phase portion of the initial polymerization tank 3 is provided with a volatile matter extraction nozzle 10 for removing the volatile matter 14 generated by the polymerization reaction from the liquid surface of each tray and evaporated. A vacuum pump (not shown), a condenser (not shown) for collecting by-products, and the like are provided on the downstream side of the volatile matter removal nozzle 10 in order to reduce the pressure in the tank to a reduced pressure atmosphere. As shown in the figure, in this embodiment, the initial polymerization tank 3 has no stirring blade member inside. Instead of this agitating blade, downflow trays are installed in multiple stages to obtain a large surface renewal action. Inside the initial polymerization tank 3, ring-shaped trays 8a and cylindrical trays 8b are alternately arranged. On the inner peripheral upper surface side of the ring-shaped tray 8a and the outer peripheral upper surface side of the cylindrical tray 8b. Is provided with one or a plurality of notches, the processing liquid flows to the tray on the downstream side, reaches the bottom of the initial polymerization tank 3, and the initial polymerization product 15 is taken out from the extraction nozzle 5, Proceed to the next second manufacturing equipment.
In the figure, reference numeral 30 denotes a horizontally long cylindrical second manufacturing apparatus main body having a substantially circular cross section, the outer periphery of which is covered with a heat medium jacket (not shown), and two rotary shafts 31 extending in the inner longitudinal direction.
Is attached. For the rotary shaft 31, for example, the first patent
A stirring blade 32 formed of a scraping plate and a disc as shown in 024745 is installed. Each stirring blade 32
Rotates by scraping off the inner wall surface of the main body container 30, the stirring shaft, and the surfaces of the blades. Further, a volatile matter outlet nozzle is provided at the top of the main body 30 and is connected to a condenser and a vacuum pump (not shown) by piping to take out the reaction by-product 40. Further, the final polymerized product 41 of the treatment liquid is taken out from the outlet provided on the side opposite to the inlet.
【0007】以上の構成においてポリエチレンテレフタ
レートを製造する場合について説明する。ポリエチレン
テレフタレートの原料についてはテレフタル酸とエチレ
ングリコールの混合物またはジメチルテレフタレートと
エチレングリコールの混合物が一般的である。これらの
原料を第1製造装置1の入口ノズル4からエステル交換
槽2へ供給する。本発明の推奨される運転条件としては
エステル交換槽は撹拌翼の回転数100から200rp
m、温度240℃から260℃、圧力は大気圧下または
加圧条件下でエステル交換反応を行なう。エステル交換
反応によって生成する副生物(水とエチレングリコール
あるいはメタノールとエチレングリコール)は副生物除
去ノズル11より上流側に設置された副生物の捕集コン
デンサー(図示せず)により回収される。一方、エステ
ル交換により生成したビスベータヒドロキシエチルテレ
フタレート(重合度4から8)は処理液表面に設けた連
結管7の上端から下塔側の上部のトレイに供給される。
この時、下塔の操作圧力は1.3kPaから133Pa
であるために連結管7の途中に設けた流量調整バルブ9
によりトレイ8aの液高さが常に一定となるように流量
調整されている。処理液は最上部のリング状のトレイ8
aから円筒状のトレイ8bさらにリング状のトレイ8a
へと順次流下していく。この時、処理液は減圧雰囲気に
あるために重合反応によって生成される副生物が気化す
るために激しい発泡が起こり、これによって処理液は混
合されると同時に表面更新作用を強く受け重合反応が促
進されていく。このようなトレイの構造を複数段設置す
ることにより反応に必要な滞留時間を確保することがで
き目的の重合度(10から30)を得ることができる。
さらに、初期重合物15は第2製造装置30の入口ノズ
ルより連続供給し、2本の撹拌軸31に取り付けた撹拌
翼32で撹拌し処理液の表面を更新して、重合反応で生
じるエチレングリコール等の揮発物を蒸発除去し、重縮
合反応が進み高粘度の最終重合物(重合度90から11
0)41となる。この間に分離したエチレングリコール
等の揮発物40は出口ノズルより排出される。この時の
操作条件は例えば温度260〜300℃、圧力0.01
〜10kPa、回転数3〜30rpmの範囲で行われ
る。撹拌室内の処理液は撹拌翼によって薄膜状になり、
良好な表面更新を受けるので、滞留による劣化もなく品
質の良い製品重合物を効率良く得ることができる。The case of producing polyethylene terephthalate with the above constitution will be described. As a raw material of polyethylene terephthalate, a mixture of terephthalic acid and ethylene glycol or a mixture of dimethyl terephthalate and ethylene glycol is generally used. These raw materials are supplied to the transesterification tank 2 from the inlet nozzle 4 of the first manufacturing apparatus 1. The recommended operating condition of the present invention is that the transesterification tank has a stirring blade rotation speed of 100 to 200 rp.
m, temperature 240 ° C. to 260 ° C., pressure is atmospheric pressure or under elevated pressure to carry out the transesterification reaction. By-products (water and ethylene glycol or methanol and ethylene glycol) produced by the transesterification reaction are collected by a by-product collection condenser (not shown) installed upstream of the by-product removal nozzle 11. On the other hand, bis beta hydroxyethyl terephthalate (polymerization degree 4 to 8) produced by transesterification is supplied from the upper end of the connecting pipe 7 provided on the surface of the treatment liquid to the upper tray on the lower tower side.
At this time, the operating pressure of the lower tower is from 1.3 kPa to 133 Pa
Therefore, the flow rate adjusting valve 9 provided in the middle of the connecting pipe 7
The flow rate is adjusted so that the liquid height of the tray 8a is always constant. The processing liquid is the uppermost ring-shaped tray 8.
a to cylindrical tray 8b and ring-shaped tray 8a
It flows down to sequentially. At this time, since the treatment liquid is in a reduced pressure atmosphere, a by-product generated by the polymerization reaction is vaporized and vigorous foaming occurs. As a result, the treatment liquid is mixed and at the same time strongly receives a surface renewal action to accelerate the polymerization reaction. Will be done. By installing such a tray structure in a plurality of stages, it is possible to secure a residence time necessary for the reaction and obtain a desired degree of polymerization (10 to 30).
Further, the initial polymerization product 15 is continuously supplied from the inlet nozzle of the second manufacturing apparatus 30, and is stirred by the stirring blades 32 attached to the two stirring shafts 31 to renew the surface of the treatment liquid, so that ethylene glycol generated by the polymerization reaction is generated. And other volatile substances are removed by evaporation, the polycondensation reaction proceeds, and the highly viscous final polymer (degree of polymerization 90 to 11
0) 41. The volatile matter 40 such as ethylene glycol separated during this period is discharged from the outlet nozzle. The operating conditions at this time are, for example, a temperature of 260 to 300 ° C. and a pressure of 0.01.
It is performed in the range of 10 to 10 kPa and the rotation speed of 3 to 30 rpm. The processing liquid in the stirring chamber becomes a thin film by the stirring blades,
Since it undergoes a good surface renewal, it is possible to efficiently obtain a product polymer of good quality without deterioration due to retention.
【0008】同様にして本発明は、ポリアミド、ポリカ
ーボネート等の重縮合系樹脂の連続塊状重合に適用でき
る。Similarly, the present invention can be applied to continuous bulk polymerization of polycondensation resins such as polyamide and polycarbonate.
【0009】本発明の推奨される他の実施例を図2に示
す。図の第1製造装置のエステル交換槽2と第2製造装
置30の構成及び動作は同一であるために説明は省略す
る。本発明の初期重合槽3は上塔のエステル交換槽2と
連結管7で結合されその間に流量調整バルブ9を設け、
下塔上部に設けた液トレイ24上の液面が所定の高さに
なるように制御されている。該液トレイは中央部が空間
となったリング状になっており下流側と同一雰囲気にな
るように構成している。その下流側にはリング状の液溜
りを形成する撹拌室20が多段に設置され、該撹拌室2
0の内部をくまなく撹拌する撹拌部材22が各撹拌室ご
とに設けられ、初期重合室の中心部に設置された撹拌軸
23に結合されている。また各々の撹拌室20はそれぞ
れの上側のトレイの上部側液面とその撹拌室の底部側面
部とを連結する連結管21が設置され、処理液は必ず撹
拌室の液表面から流れ出し、撹拌室の底部側から供給さ
れる流れとなる。Another preferred embodiment of the present invention is shown in FIG. Since the configurations and operations of the transesterification tank 2 of the first manufacturing apparatus and the second manufacturing apparatus 30 in the figure are the same, description thereof will be omitted. The initial polymerization tank 3 of the present invention is connected to the transesterification tank 2 of the upper tower by a connecting pipe 7, and a flow rate adjusting valve 9 is provided between them.
The liquid level on the liquid tray 24 provided at the upper part of the lower tower is controlled so as to have a predetermined height. The liquid tray has a ring shape with a space in the center and is configured to have the same atmosphere as the downstream side. On the downstream side thereof, stirring chambers 20 forming a ring-shaped liquid pool are installed in multiple stages.
A stirring member 22 that stirs the inside of 0 is provided for each stirring chamber, and is connected to a stirring shaft 23 installed at the center of the initial polymerization chamber. Further, each stirring chamber 20 is provided with a connecting pipe 21 that connects the upper side liquid surface of each upper tray and the bottom side surface portion of the stirring chamber, so that the processing liquid always flows out from the liquid surface of the stirring chamber, The flow is supplied from the bottom side of the.
【0010】以上の構成においてポリエチレンテレフタ
レートを製造する場合について説明する。ポリエチレン
テレフタレートの原料についてはテレフタル酸とエチレ
ングリコールの混合物またはジメチルテレフタレートと
エチレングリコールの混合物が一般的である。これらの
原料を入口ノズル4からエステル交換槽2へ供給する。
エステル交換槽は撹拌翼の回転数100から200rp
m、温度240℃から260℃、圧力は大気圧下または
加圧条件下でエステル交換反応を行なう。エステル交換
反応によって生成する副生物(水とエチレングリコール
あるいはメタノールとエチレングリコール)は副生物除
去ノズル11より上流側に設置された副生物の捕集コン
デンサー(図示せず)により回収される。一方、エステ
ル交換により生成したビスベータヒドロキシエチルテレ
フタレートは処理液表面に設けた連結管7の上端から下
塔側の上部のトレイに供給される。この時、下塔の操作
圧力は13kPaから133Paであるために連結管7
の途中に設けた流量調整バルブ9によりトレイ24の液
高さが常に一定となるように流量調整されている。最上
部のトレイ上にある処理液は連結管21によりすぐ下流
の撹拌室20へと流れて行く。撹拌室20に供給された
処理液は撹拌部材22により撹拌され重合反応が促進さ
れる。また、撹拌翼による撹拌作用で表面更新作用が活
発となり反応が一段と進んでいく。この時発生する反応
副生物は揮発物14を取り除くための揮発物取り出しノ
ズル10より除去される。初期重合槽内で所定の滞留時
間経過した処理液は槽下部へ集まり抜き出しノズル5か
ら初期重合物15が取り出され、さらにつぎの竪型最終
重合槽(第2製造装置)へと進んでいき重合度が高めら
れる。The case of producing polyethylene terephthalate with the above constitution will be described. As a raw material of polyethylene terephthalate, a mixture of terephthalic acid and ethylene glycol or a mixture of dimethyl terephthalate and ethylene glycol is generally used. These raw materials are supplied from the inlet nozzle 4 to the transesterification tank 2.
The transesterification tank has a stirring blade rotation speed of 100 to 200 rp
m, temperature 240 ° C. to 260 ° C., pressure is atmospheric pressure or under elevated pressure to carry out the transesterification reaction. By-products (water and ethylene glycol or methanol and ethylene glycol) produced by the transesterification reaction are collected by a by-product collection condenser (not shown) installed upstream of the by-product removal nozzle 11. On the other hand, bisbetahydroxyethyl terephthalate produced by transesterification is supplied from the upper end of the connecting pipe 7 provided on the surface of the treatment liquid to the upper tray on the lower tower side. At this time, since the operating pressure of the lower tower is 13 kPa to 133 Pa, the connecting pipe 7
The flow rate is adjusted by the flow rate adjusting valve 9 provided in the middle of the process so that the liquid height of the tray 24 is always constant. The treatment liquid on the uppermost tray flows to the stirring chamber 20 immediately downstream through the connecting pipe 21. The treatment liquid supplied to the stirring chamber 20 is stirred by the stirring member 22 to accelerate the polymerization reaction. In addition, the stirring action by the stirring blade activates the surface renewal action, and the reaction proceeds further. The reaction by-product generated at this time is removed from the volatile matter extraction nozzle 10 for removing the volatile matter 14. The treatment liquid after a predetermined residence time has elapsed in the initial polymerization tank is collected in the lower portion of the tank, the initial polymerization product 15 is taken out from the withdrawing nozzle 5, and further proceeds to the next vertical final polymerization tank (second manufacturing apparatus) for polymerization. The degree is increased.
【0011】本発明の推奨される他の実施例を図3に示
す。図の第1製造装置の初期重合槽3と第2製造装置3
0の構成及び動作は同一であるために説明は省略する。
原料13はエステル交換槽2の下部に設けた供給ノズル
4より入る。このとき原料13は外部熱交17によりエ
ステル交換反応温度まで加熱されて供給される。また、
供給ノズル4には上塔上部の循環ノズル16から循環ポ
ンプ6により循環する循環液18が原料13と合流して
供給される。この循環ポンプ6による循環作用によって
上塔内の処理液は撹拌混合され、エステル化反応が促進
される。エステル交換槽2の上部にはエステル交換反応
によって生成される副生物12を除去するノズル11が
取り付けられており、下流側にあるコンデンサーにより
分離回収される。エステル交換槽2と初期重合槽3は連
結管7で結合されており、その上端側はエステル交換槽
2上部の液表面まで立ち上げられ、下端側は初期重合槽
3の槽内上部に設けたトレイ8aの液溜りの中に設置さ
れており、該連結管7の途中にはトレイ8aの液面高さ
を調整する流量調整バルブ9が設けてあり、トレイ8a
上の液面が所定の高さになるように制御されている。初
期重合槽3の気相部には各トレイの液表面から重合反応
によって生成し、気化した副生物等は揮発物14を取り
除くための揮発物取り出しノズル10が設けられてい
る。揮発物取り出しノズル10の下流側には槽内の圧力
を減圧雰囲気にするために真空ポンプ(図示せず)や副
生物を捕集するためのコンデンサー(図示せず)等が設
けられる。図に示したように本実施例では初期重合槽3
の内部に撹拌翼部材を持たない構成となっている。この
撹拌翼の代わりに流下式トレイを多段に設置して大きな
表面更新作用を得る構造となっている。初期重合槽3の
内部にはリング状のトレイ8aと円筒状のトレイ8bと
が交互に配置されており、リング状のトレイ8aの内周
上面側と円筒状のトレイ8bの外周上面側とには1個所
あるいは複数個所の切欠き部が設けられ処理液を下流側
のトレイへと流れて行き初期重合槽3の底部へと到達
し、抜き出しノズル5から初期重合物15が取り出さ
れ、さらに次の重合槽30(第2製造装置)へと進んで
行き、さらに重合度が高められる。Another preferred embodiment of the present invention is shown in FIG. The initial polymerization tank 3 and the second manufacturing apparatus 3 of the first manufacturing apparatus in the figure
Since the configuration and operation of 0 are the same, description thereof will be omitted.
The raw material 13 enters from a supply nozzle 4 provided at the bottom of the transesterification tank 2. At this time, the raw material 13 is heated to the transesterification reaction temperature by the external heat exchange 17 and supplied. Also,
The circulation liquid 18 circulated by the circulation pump 6 is supplied to the supply nozzle 4 from the circulation nozzle 16 in the upper part of the upper tower by merging with the material 13. The treatment liquid in the upper tower is agitated and mixed by the circulation action of the circulation pump 6, and the esterification reaction is promoted. A nozzle 11 for removing a by-product 12 produced by a transesterification reaction is attached to the upper part of the transesterification tank 2, and is separated and recovered by a condenser on the downstream side. The transesterification tank 2 and the initial polymerization tank 3 are connected by a connecting pipe 7. The upper end side of the transesterification tank 2 is raised to the liquid surface above the transesterification tank 2, and the lower end side thereof is provided in the upper part of the initial polymerization tank 3. It is installed in the liquid pool of the tray 8a, and a flow rate adjusting valve 9 for adjusting the liquid level height of the tray 8a is provided in the middle of the connecting pipe 7,
The upper liquid surface is controlled so as to have a predetermined height. The vapor phase portion of the initial polymerization tank 3 is provided with a volatile matter extraction nozzle 10 for removing the volatile matter 14 generated by the polymerization reaction from the liquid surface of each tray and evaporated. A vacuum pump (not shown), a condenser (not shown) for collecting by-products, and the like are provided on the downstream side of the volatile matter removal nozzle 10 in order to reduce the pressure in the tank to a reduced pressure atmosphere. As shown in the figure, in this embodiment, the initial polymerization tank 3
It does not have a stirring blade member inside. Instead of this agitating blade, downflow trays are installed in multiple stages to obtain a large surface renewal action. Inside the initial polymerization tank 3, ring-shaped trays 8a and cylindrical trays 8b are alternately arranged. On the inner peripheral upper surface side of the ring-shaped tray 8a and the outer peripheral upper surface side of the cylindrical tray 8b. Is provided with one or a plurality of notches, the processing solution flows to the tray on the downstream side, reaches the bottom of the initial polymerization tank 3, and the initial polymerization product 15 is taken out from the extraction nozzle 5, To the polymerization tank 30 (second manufacturing apparatus), and the degree of polymerization is further increased.
【0012】本発明の他の実施例を図4に示す。本実施
例では図3の実施例の第1製造装置の下塔の初期重合槽
を多段の撹拌室20と撹拌部材22で構成したものであ
る。Another embodiment of the present invention is shown in FIG. In this embodiment, the initial polymerization tank of the lower tower of the first manufacturing apparatus of the embodiment shown in FIG. 3 is composed of a multi-stage stirring chamber 20 and a stirring member 22.
【0013】本発明の初期重合槽3は上塔のエステル交
換槽2と連結管7で結合されその間に流量調整バルブ9
を設け、下塔上部に設けた液トレイ24上の液面が所定
の高さになるように制御されている。該液トレイは中央
部が空間となったリング状になっており下流側と同一雰
囲気になるように構成している。その下流側にはリング
状の液溜りを形成する撹拌室20が多段に設置され、該
撹拌室20の内部をくまなく撹拌する撹拌部材22が各
撹拌室ごとに設けられ、初期重合室の中心部に設置され
た撹拌軸23に結合されている。また各々の撹拌室20
はそれぞれの上側のトレイの上部側液面とその撹拌室の
底部側面部とを連結する連結管21が設置され、処理液
は必ず撹拌室の液表面から流れ出し、撹拌室の底部側か
ら供給される流れとなる。The initial polymerization tank 3 of the present invention is connected to the transesterification tank 2 of the upper tower by a connecting pipe 7, and a flow rate adjusting valve 9 is provided therebetween.
Is provided so that the liquid level on the liquid tray 24 provided at the upper part of the lower tower is controlled to a predetermined height. The liquid tray has a ring shape with a space in the center and is configured to have the same atmosphere as the downstream side. On the downstream side thereof, stirring chambers 20 forming a ring-shaped liquid pool are installed in multiple stages, and a stirring member 22 for thoroughly stirring the inside of the stirring chamber 20 is provided for each stirring chamber, and the center of the initial polymerization chamber is provided. It is connected to a stirring shaft 23 installed in the section. In addition, each stirring chamber 20
Is provided with a connecting pipe 21 that connects the upper liquid surface of each upper tray to the bottom side surface of the stirring chamber, and the processing liquid always flows out from the liquid surface of the stirring chamber and is supplied from the bottom side of the stirring chamber. It becomes a flow.
【0014】以上の構成においてポリエチレンテレフタ
レートを製造する場合について説明する。ポリエチレン
テレフタレートの原料についてはテレフタル酸とエチレ
ングリコールの混合物またはジメチルテレフタレートと
エチレングリコールの混合物が一般的である。これらの
原料13は外部熱交17を経由して加熱され、入口ノズ
ル4からエステル交換槽2へ供給される。エステル交換
槽は上部に設けた循環ノズル16からポンプ6により循
環液18を循環し、槽内を均一に撹拌する。槽内は温度
240℃から260℃、圧力は大気圧下または加圧条件
下でエステル交換反応を行なう。エステル交換反応によ
って生成する副生物(水とエチレングリコールあるいは
メタノールとエチレングリコール)は副生物除去ノズル
11より上流側に設置された副生物の捕集コンデンサー
(図示せず)により回収される。一方、エステル交換に
より生成したビスベータヒドロキシエチルテレフタレー
トは処理液表面に設けた連結管7の上端から下塔側の上
部のトレイに供給される。この時、下塔の操作圧力は1
3000Paから133Paであるために連結管7の途
中に設けた流量調整バルブ9によりトレイ24の液高さ
が常に一定となるように流量調整されている。最上部の
トレイ上にある処理液は連結管21によりすぐ下流の撹
拌室20へと流れて行く。撹拌室20に供給された処理
液は撹拌部材22により撹拌され重合反応が促進され
る。また、撹拌翼による撹拌作用で表面更新作用が活発
となり反応が一段と進んでいく。この時発生する反応副
生物は揮発物14を取り除くための揮発物取り出しノズ
ル10より除去される。初期重合槽内で所定の滞留時間
経過した処理液は槽下部へ集まり抜き出しノズル5から
初期重合物15が取り出され、第2製造装置30へと進
んでいき装置内で表面更新作用を受け重合度が高められ
る。The case of producing polyethylene terephthalate with the above constitution will be described. As a raw material of polyethylene terephthalate, a mixture of terephthalic acid and ethylene glycol or a mixture of dimethyl terephthalate and ethylene glycol is generally used. These raw materials 13 are heated via the external heat exchanger 17 and supplied from the inlet nozzle 4 to the transesterification tank 2. In the transesterification tank, the circulating liquid 16 is circulated by the pump 6 from the circulation nozzle 16 provided at the upper part to uniformly stir the inside of the tank. The temperature in the tank is 240 ° C. to 260 ° C., and the transesterification reaction is carried out under atmospheric pressure or under pressure. By-products (water and ethylene glycol or methanol and ethylene glycol) produced by the transesterification reaction are collected by a by-product collection condenser (not shown) installed upstream of the by-product removal nozzle 11. On the other hand, bisbetahydroxyethyl terephthalate produced by transesterification is supplied from the upper end of the connecting pipe 7 provided on the surface of the treatment liquid to the upper tray on the lower tower side. At this time, the operating pressure of the lower tower is 1
Since the pressure is 3000 Pa to 133 Pa, the flow rate is adjusted by the flow rate adjusting valve 9 provided in the middle of the connecting pipe 7 so that the liquid height of the tray 24 is always constant. The treatment liquid on the uppermost tray flows to the stirring chamber 20 immediately downstream through the connecting pipe 21. The treatment liquid supplied to the stirring chamber 20 is stirred by the stirring member 22 to accelerate the polymerization reaction. In addition, the stirring action by the stirring blade activates the surface renewal action, and the reaction proceeds further. The reaction by-product generated at this time is removed from the volatile matter extraction nozzle 10 for removing the volatile matter 14. The treatment liquid after a lapse of a predetermined residence time in the initial polymerization tank collects in the lower part of the tank and the initial polymerization product 15 is taken out from the withdrawing nozzle 5 and proceeds to the second manufacturing apparatus 30 to undergo a surface renewal action in the apparatus to obtain a polymerization degree. Is increased.
【0015】本発明の他の実施例を図5に示す。本発明
は他の実施例図1の第1製造装置と同様の構成作用であ
るので詳細説明は省略する。本実施例では第2製造装置
に1軸式の横型装置を使用した場合である。図におい
て、35は概略円形断面を有する横長の円筒状の第2製
造装置本体で外周を熱媒ジャケット(図示せず)で覆わ
れており、内部長手方向に1本の回転軸33が取り付け
られている。回転軸33には例えば車輪型の円板と掻き
取り板とで形成される撹拌翼34が設置されている。そ
れぞれの撹拌翼34は本体容器35の内壁表面と撹拌軸
及び翼の表面をかきとって回転する。さらに、本体35
の最上部には揮発物の出口ノズルが設けられ反応副生物
40を取りだすために配管で凝縮器及び真空ポンプ(図
示せず)に接続される。第1製造装置から供給される初
期重合物15は本体容器35内で表面更新作用を受け重
合度が高められ、処理液の最終重合物41は入口と反対
側に設けた出口より取りだされる。Another embodiment of the present invention is shown in FIG. Since the present invention has the same construction and operation as the first manufacturing apparatus of FIG. 1 of another embodiment, detailed description thereof will be omitted. In this embodiment, a uniaxial horizontal device is used as the second manufacturing device. In the figure, reference numeral 35 denotes a horizontally long cylindrical second manufacturing apparatus main body having a substantially circular cross section, the outer periphery of which is covered with a heat medium jacket (not shown), and one rotary shaft 33 is attached in the inner longitudinal direction. Has been. The rotating shaft 33 is provided with a stirring blade 34 formed of, for example, a wheel-shaped disc and a scraping plate. Each stirring blade 34 scrapes against the inner wall surface of the main body container 35, the stirring shaft, and the surface of the blade to rotate. Further, the main body 35
An outlet nozzle for volatile matter is provided at the top of the pipe, and is connected to a condenser and a vacuum pump (not shown) by piping to take out the reaction by-product 40. The initial polymerization product 15 supplied from the first manufacturing apparatus undergoes a surface renewal action in the main body container 35 to increase the degree of polymerization, and the final polymerization product 41 of the treatment liquid is taken out from the outlet provided on the side opposite to the inlet. .
【0016】本発明の他の実施例を図6に示す。本発明
は他の実施例の図2の第1製造装置と同様の構成作用で
あるので詳細説明は省略する。本実施例では第2製造装
置に1軸式の横型装置を使用した場合である。さらに本
発明の他の実施例として、図3または図4に示した第1
製造装置と第2製造装置として1軸式の横型装置を使用
した場合も同様の作用、効果が得られるが詳細説明は省
略する。Another embodiment of the present invention is shown in FIG. Since the present invention has the same construction and operation as the first manufacturing apparatus of FIG. 2 of another embodiment, detailed description thereof will be omitted. In this embodiment, a uniaxial horizontal device is used as the second manufacturing device. Furthermore, as another embodiment of the present invention, the first embodiment shown in FIG. 3 or FIG.
The same operation and effect can be obtained when a uniaxial horizontal device is used as the manufacturing device and the second manufacturing device, but detailed description thereof will be omitted.
【0017】[0017]
【発明の効果】本発明によれば、エステル交換槽と初期
重合槽を一体構造とした第1製造装置と横型の最終重合
槽である第2製造装置とを連結することにより重縮合系
樹脂の連続製造装置の装置価格を安価にすることがで
き、しかも装置の設置スペースも大幅に少なくてすむ利
点がある。According to the present invention, a polycondensation resin of a polycondensation system can be produced by connecting a first manufacturing apparatus having an integrated structure of a transesterification tank and an initial polymerization tank to a second manufacturing apparatus which is a horizontal final polymerization tank. There is an advantage that the device price of the continuous manufacturing device can be reduced and the installation space of the device can be significantly reduced.
【図1】本発明の一実施例を示す装置構成図である。FIG. 1 is a device configuration diagram showing an embodiment of the present invention.
【図2】本発明の他の実施例を示す装置構成図である。FIG. 2 is a device configuration diagram showing another embodiment of the present invention.
【図3】本発明の他の実施例を示す装置構成図である。FIG. 3 is a device configuration diagram showing another embodiment of the present invention.
【図4】本発明の他の実施例を示す装置構成図である。FIG. 4 is a device configuration diagram showing another embodiment of the present invention.
【図5】本発明の他の実施例を示す装置構成図である。FIG. 5 is a device configuration diagram showing another embodiment of the present invention.
【図6】本発明の他の実施例を示す装置構成図である。FIG. 6 is a device configuration diagram showing another embodiment of the present invention.
1…第一製造装置本体、2…エステル交換槽、3…初期
重合槽、4…供給ノズル、5…抜き出しノズル、6…低
粘度撹拌翼、7…連結管、8a…リング状トレイ、8b
…円筒状トレイ、9…流量調整バルブ、10…揮発物取
り出しノズル、11…副生物除去ノズル、12…副生
物、13…原料、14…揮発物、15…初期重合物、1
6…循環ノズル、17…外部熱交、18…循環液、20
…撹拌室、21…連結管、22…撹拌翼、23…撹拌
軸、24…トレイ、30…第2製造装置本体、31…回
転軸、32…撹拌翼、33…撹拌軸、34…撹拌翼、3
5…第2製造装置本体、40…副生物、41…最終重合
物。DESCRIPTION OF SYMBOLS 1 ... Main body of a manufacturing apparatus, 2 ... Transesterification tank, 3 ... Initial polymerization tank, 4 ... Supply nozzle, 5 ... Extraction nozzle, 6 ... Low viscosity stirring blade, 7 ... Connection pipe, 8a ... Ring tray, 8b
... Cylindrical tray, 9 ... Flow rate adjusting valve, 10 ... Volatile substance taking-out nozzle, 11 ... By-product removing nozzle, 12 ... By-product, 13 ... Raw material, 14 ... Volatile substance, 15 ... Prepolymer, 1
6 ... Circulation nozzle, 17 ... External heat exchange, 18 ... Circulating liquid, 20
... stirring chamber, 21 ... connecting pipe, 22 ... stirring blade, 23 ... stirring shaft, 24 ... tray, 30 ... second manufacturing apparatus body, 31 ... rotating shaft, 32 ... stirring blade, 33 ... stirring shaft, 34 ... stirring blade Three
5 ... 2nd manufacturing apparatus main body, 40 ... By-product, 41 ... Final polymer.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 木下 高年 山口県下松市大字東豊井794番地 株式会 社日立製作所笠戸工場内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Takatoshi Kinoshita 794 Higashi-Toyoi, Kudamatsu City, Yamaguchi Prefecture Stock company Hitachi Ltd. Kasado Plant
Claims (15)
置において原料の混合物からエステル交換反応によりオ
リゴマーを生成するエステル交換槽と該オリゴマーを重
縮合反応させて中間重合物を生成する初期重合槽とを鉛
直方向に直列に配置し、上塔のエステル交換塔と下塔の
初期重合塔とを結合し一体構造物となるように形成した
竪型の第1製造装置と重縮合反応により中間重合物から
最終重合物を製造する横型の第2製造装置とにより構成
したことを特徴とする重縮合系高分子の連続製造装置。1. A transesterification tank for producing an oligomer by a transesterification reaction from a mixture of raw materials in a production apparatus for continuously producing a polycondensation polymer, and a polycondensation reaction between the oligomer and an initial stage of producing an intermediate polymer. By vertically arranging a polymerization tank in series and connecting a transesterification tower of an upper tower and an initial polymerization tower of a lower tower so as to form an integrated structure, a vertical type first manufacturing apparatus and a polycondensation reaction An apparatus for continuously producing a polycondensation polymer, comprising a horizontal second production apparatus for producing a final polymer from an intermediate polymer.
1製造装置の上塔の原料入口部は上塔の底部側に設け、
上塔と下塔の連結管を上塔の上部液表面まで立ち上げ、
下塔の連結管端部は下塔の上部に設けた液溜りの液中に
設け、下塔の底部に処理液の抜き出し口を設けた構造と
することを特徴とする重縮合系高分子の連続製造装置。2. The continuous manufacturing apparatus according to claim 1, wherein the raw material inlet of the upper tower of the first manufacturing apparatus is provided on the bottom side of the upper tower,
Raise the connecting pipe of the upper tower and the lower tower to the upper liquid surface of the upper tower,
The end of the connecting pipe of the lower tower is provided in the liquid in the liquid pool provided at the upper part of the lower tower, and the outlet of the processing liquid is provided at the bottom of the lower tower. Continuous manufacturing equipment.
塔と下塔を連結する連結管に流量調整バルブを設け、上
塔と下塔の圧力差がある場合でも所定の流量に制御する
ことを特徴とする重縮合系高分子の連続製造装置。3. The continuous production apparatus according to claim 2, wherein a flow rate adjusting valve is provided in a connecting pipe connecting the upper tower and the lower tower to control the flow rate to a predetermined value even when there is a pressure difference between the upper tower and the lower tower. An apparatus for continuously producing a polycondensation polymer, which is characterized in that
塔には槽内を均一に撹拌混合する低粘度用の撹拌翼を設
け、下塔には複数段の液溜りを有するトレイを配置し、
撹拌翼を設置しない構造とすることを特徴とする重縮合
系高分子の連続製造装置。4. The continuous production apparatus according to claim 2, wherein the upper tower is provided with a low-viscosity stirring blade for uniformly stirring and mixing the inside of the tank, and the lower tower is provided with a tray having a plurality of liquid pools. Then
An apparatus for continuously producing a polycondensation polymer, which has a structure without a stirring blade.
塔に設置する複数段のトレイは断面形状がL型のリング
状のトレイとリング状の中空部の径より大きな直径を有
する円形状のトレイを交互に複数段設置することを特徴
とする重縮合系高分子の連続製造装置。5. The continuous manufacturing apparatus according to claim 4, wherein a plurality of trays installed in the lower tower have a circular shape having a cross-sectional shape of an L-shaped ring-shaped tray and a diameter larger than the diameter of the ring-shaped hollow portion. An apparatus for continuous production of polycondensation polymer, characterized in that a plurality of trays are alternately installed.
塔に設置したL型のリング状のトレイの内径側及び円形
状のトレイの外径側のそれぞれを一部又は複数個所切欠
きトレイ内の処理液を流下させる構造とすることを特徴
とする重縮合系高分子の連続製造装置。6. The continuous manufacturing apparatus according to claim 5, wherein a part or a plurality of cutout trays are provided on each of the inner diameter side of the L-shaped ring tray and the outer diameter side of the circular tray installed in the lower tower. An apparatus for continuously producing a polycondensation polymer, characterized in that the treatment liquid in the inside is made to flow down.
塔には槽内を均一に撹拌混合する低粘度用の撹拌翼を設
け、下塔には本体内部の長手方向を複数段に分割してそ
れぞれL型形状の断面を有するリング状部材で中心部に
空間を有する撹拌室を形成しそれぞれの撹拌室内をくま
なく撹拌する撹拌部材を下塔中心部に設けた撹拌軸に取
り付け、たことを特徴とする重縮合系高分子の連続製造
装置。7. The continuous manufacturing apparatus according to claim 2, wherein the upper tower is provided with a low-viscosity stirring blade for uniformly stirring and mixing the inside of the tank, and the lower tower is divided into a plurality of stages in the longitudinal direction inside the main body. Then, each of the ring-shaped members having an L-shaped cross section forms a stirring chamber having a space in the center, and the stirring members for thoroughly stirring the respective stirring chambers are attached to a stirring shaft provided in the center of the lower tower. An apparatus for continuously producing a polycondensation polymer, which is characterized in that
塔に設けた上下の撹拌室を連結する連結管を上部の撹拌
室側は液表面側とし、下部の撹拌室側は撹拌室底部に連
結する構造としたことを特徴とする重縮合系高分子の連
続製造装置。8. The continuous production apparatus according to claim 7, wherein a connecting pipe for connecting the upper and lower stirring chambers provided in the lower tower is the liquid surface side on the upper stirring chamber side and the stirring chamber bottom is on the lower stirring chamber side. An apparatus for continuously producing a polycondensation polymer, which has a structure of connecting to a polycondensation polymer.
て、上塔には槽内を均一に撹拌混合するために外部循環
式の撹拌機構を備え、撹拌翼を設置しない構造とするこ
とを特徴とする重縮合系高分子の連続製造装置。9. The continuous production apparatus according to claim 2 or 3, wherein the upper tower is provided with an external circulation type stirring mechanism for uniformly stirring and mixing the inside of the tank, and has a structure without stirring blades. The continuous production equipment of the characteristic polycondensation polymer.
第2製造装置は実質的に横型の概略円筒状容器本体長手
方向の両端部の下部にそれぞれ被処理液の入口及び出口
を有し、本体内部の長手方向に設けた回転軸に撹拌部材
を取り付けて本体の内側に近接して回転する装置とし、
本体上部に揮発物の出口を設けたことを特徴とする重縮
合系高分子の連続製造装置。10. The continuous manufacturing apparatus according to claim 1,
The second manufacturing apparatus has an inlet and an outlet for the liquid to be treated at the lower portions of both ends in the longitudinal direction of the substantially horizontal substantially cylindrical container body, and a stirring member is attached to a rotary shaft provided in the longitudinal direction inside the body. And a device that rotates close to the inside of the main body,
An apparatus for continuous production of polycondensation polymers, characterized in that a volatile matter outlet is provided at the top of the main body.
て、第2製造装置は2軸式の撹拌翼構成とし、それぞれ
の撹拌翼間及び撹拌軸表面、撹拌室の内壁面をくまなく
掻き取る掻き取り板を具備した概略円板状の撹拌部材を
回転軸に取り付けたことを特徴とする重縮合系高分子の
連続製造装置。11. The continuous manufacturing apparatus according to claim 10, wherein the second manufacturing apparatus has a biaxial stirring blade structure, and scrapes between the respective stirring blades, the surface of the stirring shaft, and the inner wall surface of the stirring chamber. An apparatus for continuously producing a polycondensation polymer, wherein a substantially disk-shaped stirring member having a take-up plate is attached to a rotary shaft.
て、第2製造装置は1軸式の撹拌翼構成とし、撹拌翼に
は撹拌室の内壁面をくまなく掻き取る掻き取り板を具備
した概略円板状の撹拌部材を回転軸に取り付けたことを
特徴とする重縮合系高分子の連続製造装置。12. The continuous manufacturing apparatus according to claim 10, wherein the second manufacturing apparatus has a uniaxial stirring blade structure, and the stirring blade is equipped with a scraping plate for scraping all over the inner wall surface of the stirring chamber. An apparatus for continuously producing a polycondensation polymer, wherein a disc-shaped stirring member is attached to a rotary shaft.
て、横型の第2製造装置は本体長手方向に複数個のを仕
切板を設置し、内部の処理液の粘度に応じて仕切板の高
さを調節し、それぞれの仕切板間で保持する処理液量を
最適な量に保つことを特徴とする重縮合系高分子の連続
製造装置。13. The continuous manufacturing apparatus according to claim 10, wherein the horizontal second manufacturing apparatus is provided with a plurality of partition plates in the longitudinal direction of the main body, and the height of the partition plates is adjusted according to the viscosity of the processing liquid inside. The continuous production apparatus for polycondensation polymer, characterized in that the amount of treatment liquid held between the respective partition plates is adjusted to an optimum amount.
製造装置記載の装置により、重縮合系高分子の原料を第
1製造装置に供給し、上塔においては概略大気圧下でエ
ステル交換反応を行ないオリゴマーを生成し、下塔にお
いては減圧雰囲気中で重縮合反応操作を行ない低重合度
から中重合度の初期重合反応物あるいは中間重合反応物
を得、さらに該反応物を第2製造装置に供給し、減圧雰
囲気中で重縮合反応操作を行ない高重合度の反応物を得
ることを特徴とする重縮合系高分子の連続製造方法。14. A continuous production apparatus according to any one of claims 1 to 13, wherein a raw material for a polycondensation polymer is supplied to the first production apparatus, and transesterification is carried out in the upper column under substantially atmospheric pressure. The reaction is carried out to form an oligomer, and the polycondensation reaction is carried out in a lower column in a reduced pressure atmosphere to obtain an initial polymerization reaction product or an intermediate polymerization reaction product having a low to medium polymerization degree, and further producing the reaction product in the second production. A continuous production method of a polycondensation polymer, which comprises supplying a reactor and performing a polycondensation reaction operation in a reduced pressure atmosphere to obtain a reaction product having a high degree of polymerization.
製造装置記載の装置によりテレフタル酸とエチレングリ
コールの混合物またはジメチルテレフタレートとエチレ
ングリコールの混合物を原料として第1製造装置に供給
し、上塔で温度200℃から270℃、圧力は大気圧あ
るいは加圧条件下でエステル交換反応を行ないビスベー
タヒドロキシエチルテレフタレートを生成し、下塔へ流
下し、温度200℃から300℃、圧力は10kPaか
ら0.1kPaの範囲で、エチレングリコール等の揮発
物を蒸発させ順次下流側の撹拌室へ移動しながら重合度
を高め、さらに第2製造装置へ供給し、温度260℃か
ら300℃、圧力は10kPaから0.01kPaの範
囲で重縮合反応を行ない重合度を上げるポリエチレンテ
レフタレートの連続重縮合方法。15. A continuous production apparatus according to any one of claims 1 to 13, wherein a mixture of terephthalic acid and ethylene glycol or a mixture of dimethyl terephthalate and ethylene glycol is supplied as a raw material to the first production apparatus, and the upper tower is provided. At a temperature of 200 ° C to 270 ° C at a pressure of atmospheric pressure or under pressure to perform a transesterification reaction to produce bisbetahydroxyethyl terephthalate, which is flowed down to a lower column at a temperature of 200 ° C to 300 ° C and a pressure of 10 kPa to 0 Within the range of 1 kPa, volatile substances such as ethylene glycol are evaporated and sequentially moved to the stirring chamber on the downstream side to increase the degree of polymerization, and then supplied to the second manufacturing apparatus, and the temperature is from 260 ° C to 300 ° C and the pressure is from 10 kPa. A polyethylene terephthalate series that increases the degree of polymerization by performing a polycondensation reaction in the range of 0.01 kPa Polycondensation method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24125495A JPH0987392A (en) | 1995-09-20 | 1995-09-20 | Continuous polycondensation polymer manufacturing apparatus and manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24125495A JPH0987392A (en) | 1995-09-20 | 1995-09-20 | Continuous polycondensation polymer manufacturing apparatus and manufacturing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0987392A true JPH0987392A (en) | 1997-03-31 |
Family
ID=17071511
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24125495A Pending JPH0987392A (en) | 1995-09-20 | 1995-09-20 | Continuous polycondensation polymer manufacturing apparatus and manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0987392A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002114840A (en) * | 2000-07-31 | 2002-04-16 | Mitsui Takeda Chemicals Inc | Method for producing polyester polyol, apparatus for producing polyester polyol, polyester polyol and polyurethane foam |
| JP2006507377A (en) * | 2002-10-02 | 2006-03-02 | ツィマー アーゲー | Method and apparatus for continuous production of polyester |
| WO2017179327A1 (en) * | 2016-04-13 | 2017-10-19 | 株式会社クレハ | Device for continuously producing poly(arylene sulfide) and process for continuously producing poly(arylene sulfide) |
| US10807062B2 (en) | 2017-10-12 | 2020-10-20 | Kureha Corporation | Continuous production apparatus and continuous production method for polymer |
-
1995
- 1995-09-20 JP JP24125495A patent/JPH0987392A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002114840A (en) * | 2000-07-31 | 2002-04-16 | Mitsui Takeda Chemicals Inc | Method for producing polyester polyol, apparatus for producing polyester polyol, polyester polyol and polyurethane foam |
| JP2006507377A (en) * | 2002-10-02 | 2006-03-02 | ツィマー アーゲー | Method and apparatus for continuous production of polyester |
| WO2017179327A1 (en) * | 2016-04-13 | 2017-10-19 | 株式会社クレハ | Device for continuously producing poly(arylene sulfide) and process for continuously producing poly(arylene sulfide) |
| JPWO2017179327A1 (en) * | 2016-04-13 | 2018-10-18 | 株式会社クレハ | Continuous production apparatus for polyarylene sulfide and continuous production method for polyarylene sulfide |
| US10538629B2 (en) | 2016-04-13 | 2020-01-21 | Kureha Corporation | Device for continuously producing poly(arylene sulfide) and method for continuously producing poly(arylene sulfide) |
| US10807062B2 (en) | 2017-10-12 | 2020-10-20 | Kureha Corporation | Continuous production apparatus and continuous production method for polymer |
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