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JPH0238401A - Continuous polymerization apparatus - Google Patents

Continuous polymerization apparatus

Info

Publication number
JPH0238401A
JPH0238401A JP63188275A JP18827588A JPH0238401A JP H0238401 A JPH0238401 A JP H0238401A JP 63188275 A JP63188275 A JP 63188275A JP 18827588 A JP18827588 A JP 18827588A JP H0238401 A JPH0238401 A JP H0238401A
Authority
JP
Japan
Prior art keywords
rotating shaft
liq
shaft
container
blades
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
Application number
JP63188275A
Other languages
Japanese (ja)
Inventor
Takahiro Oshida
押田 孝博
Takeyo Kajiwara
梶原 健世
Etsuro Matsumoto
松本 悦郎
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Mitsubishi Kasei Polytec Co
Original Assignee
Mitsubishi Monsanto Chemical Co
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Mitsubishi Monsanto Chemical Co filed Critical Mitsubishi Monsanto Chemical Co
Priority to JP63188275A priority Critical patent/JPH0238401A/en
Publication of JPH0238401A publication Critical patent/JPH0238401A/en
Pending legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05Stirrers
    • B01F27/11Stirrers characterised by the configuration of the stirrers
    • B01F27/112Stirrers characterised by the configuration of the stirrers with arms, paddles, vanes or blades
    • B01F27/1125Stirrers characterised by the configuration of the stirrers with arms, paddles, vanes or blades with vanes or blades extending parallel or oblique to the stirrer axis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F27/00Mixers with rotary stirring devices in fixed receptacles; Kneaders
    • B01F27/05Stirrers
    • B01F27/11Stirrers characterised by the configuration of the stirrers
    • B01F27/114Helically shaped stirrers, i.e. stirrers comprising a helically shaped band or helically shaped band sections
    • B01F27/1145Helically shaped stirrers, i.e. stirrers comprising a helically shaped band or helically shaped band sections ribbon shaped with an open space between the helical ribbon flight and the rotating axis

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mixers Of The Rotary Stirring Type (AREA)
  • Polymerisation Methods In General (AREA)
  • Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)

Abstract

PURPOSE:To improve mixing efficiency with less stirring power by installing a rotatable shaft, equipped with specific flat blades, horizontally at the center of a horizontal cylindrical vessel which has a liq.-supplying port and a liq.- discharging port. CONSTITUTION:A rotatable shaft 7 penetrating through sealing parts 5, 6 at the both ends of the wall is installed in a horizontal cylindrical vessel 1 which has a liq.-supplying port 3 at the center part of the top, a liq.-discharging port 4 at the center of the bottom and an outer wall covered by a jacket 2. The shaft is equipped with uniformly perforated flat blades 8, 9 which, extending outwards radially from the shaft 7, are arranged at regular intervals and have many small holes 13 of which the sum of the areas is 1/3-1/2 of the area of the blades.

Description

【発明の詳細な説明】 〈産業上の利用分野〉 本発明は、高分子重合体を連続的に製造するための重合
反応装置に関するものである。
DETAILED DESCRIPTION OF THE INVENTION <Industrial Application Field> The present invention relates to a polymerization reaction apparatus for continuously producing a high molecular weight polymer.

〈従来の技術〉 高分子重合体を製造するための方法としては、溶液重合
法及び塊状重合法が多用されるが、この溶液重合法及び
塊状重合法においては、重合体が単量体や溶剤に溶解す
る場合、均一液相系となり、重合反応の進行に伴い、高
粘度流体となる。
<Prior art> Solution polymerization and bulk polymerization are often used as methods for producing high molecular weight polymers. When dissolved in , it becomes a homogeneous liquid phase system, and as the polymerization reaction progresses, it becomes a highly viscous fluid.

このような高粘度化する均一液相系の溶液重合及び塊状
重合には、連続重合反応装置が用いられる。
A continuous polymerization reaction apparatus is used for such solution polymerization and bulk polymerization of a homogeneous liquid phase system that increases viscosity.

従来知られている重合反応装置としては、縦型円筒状も
のも(例えば、特公昭55−29725号公報等参照)
と、横型円筒状のもの(例えば、特公昭54−1274
89号公報等参照)があった。このうち横型円筒状のも
のとしては、パドル型の撹拌翼を装備した1軸、2軸ま
たは多軸の撹拌軸を有するものが知られている。
Conventionally known polymerization reactors include vertical cylindrical ones (see, for example, Japanese Patent Publication No. 55-29725, etc.)
and horizontal cylindrical ones (e.g., 1974-1274
(See Publication No. 89, etc.). Among these, horizontal cylindrical ones are known that have one, two, or multiple stirring shafts equipped with paddle-shaped stirring blades.

〈発明が解決しようとする課題) 高分子重合体の製造プロセスでは、一般に、反応混合物
は重合反応初期では粘度が低く、重合反応の中期から終
期にかけては粘度が高くなる。高粘度の反応混合物は均
一混合が困難になり、その重合反応装置の選定如何によ
り製品品質に影響を与えるので、その構造の決定の際に
は、慎重に検討する必要がある。また、高粘度液を均一
に混合するには、撹拌翼の構造によっては、極めて大き
い撹拌力が必要となることもあり、撹拌翼の材質、撹拌
動力等の観点からも、効率の良い混合性能をもった反応
装置を選定することが必要である。
<Problems to be Solved by the Invention> In the production process of high molecular weight polymers, the viscosity of the reaction mixture is generally low at the beginning of the polymerization reaction, and the viscosity increases from the middle to the end of the polymerization reaction. Highly viscous reaction mixtures are difficult to mix uniformly, and product quality is affected by the selection of the polymerization reactor, so careful consideration is required when determining the structure. In addition, to uniformly mix high viscosity liquids, depending on the structure of the stirring blade, an extremely large stirring force may be required, and from the viewpoint of the material of the stirring blade, stirring power, etc., it is necessary to achieve efficient mixing performance. It is necessary to select a reactor with

しかしながら、従来の1軸の重合反応装置にあっては、
粘度の高い反応物に対する混合作用が悪く、反応物が撹
拌軸及び撹拌翼と共回りする現象が認められ、デッドス
ペースを生じるという欠点があった。
However, in the conventional uniaxial polymerization reactor,
The mixing effect for highly viscous reactants was poor, and a phenomenon in which the reactants rotated together with the stirring shaft and stirring blades was observed, creating a dead space.

そこで、1軸の重合反応装置の欠点を改良するために、
種々の研究がなされている。例えば、反応容器の壁面に
固定の邪魔板を架設したもの(特開昭41−64571
号公報参照)、あるいは撹拌軸近傍のデッドスペースを
解消するために中心軸をなくしたいわゆる置型の重合反
応装置(特公昭45−20282号公報参照)等が提案
されている。
Therefore, in order to improve the drawbacks of the uniaxial polymerization reactor,
Various studies have been conducted. For example, one in which a fixed baffle plate is installed on the wall of a reaction vessel (Japanese Patent Laid-Open No. 41-64571
(see Japanese Patent Publication No. 45-20282), or a so-called stationary polymerization reactor without a central shaft in order to eliminate the dead space near the stirring shaft (see Japanese Patent Publication No. 45-20282).

しかし、これらは、構造が非常に複雑になったり、効果
が不充分であるという問題点があった。
However, these have problems in that their structures are extremely complex and their effects are insufficient.

本発明は、上記の問題点に鑑みて、比較的簡単な構造で
、しかも、従来の連続重合反応装置がもっでいたような
欠点を排除し、次のような長所をもった見掛は上1軸の
回転軸を有する連続重合反応装置を提供することを目的
とする。
In view of the above-mentioned problems, the present invention has a relatively simple structure, eliminates the drawbacks of conventional continuous polymerization reactors, and has the following advantages and a superior appearance. An object of the present invention is to provide a continuous polymerization reaction apparatus having a single rotating shaft.

(1)構造が簡単である。(1) The structure is simple.

(2)撹拌混合効率が良い。(2) Good stirring and mixing efficiency.

(3)撹拌動力が小さくてもよい。(3) The stirring power may be small.

(4)デッドスペースが生じない。(4) No dead space occurs.

〈課題を解決するための手段〉 上記の目的達成のため、本発明では、液供給口と液排出
口とを有する横型円筒状の容器と、容器の中心に水平方
向に設けられた回転軸と、回転軸周りにほぼ等間隔で配
置され、それぞれ回転軸から放射状に外方に向かって延
在し、且つ面上にほぼ一様に分布した多数の小孔を有す
る複数の平板翼と、を備えた構成とする。
<Means for Solving the Problems> In order to achieve the above object, the present invention provides a horizontal cylindrical container having a liquid supply port and a liquid discharge port, a rotating shaft provided horizontally at the center of the container, , a plurality of flat plate blades arranged at approximately equal intervals around the rotation axis, each extending radially outward from the rotation axis, and having a large number of small holes distributed approximately uniformly on the surface; The structure shall be equipped with the following.

また、平板翼に形成された小孔の合計面積が平板翼面積
の1/3〜1/2の範囲になるようにする。
Further, the total area of the small holes formed in the flat blade is set to be in the range of 1/3 to 1/2 of the area of the flat blade.

く作用〉 上記の構成では、内容物は、各平板翼の回転と共に上方
あるいは下方に移動させられると同時に、一部は平板翼
面上に設けられた多数の小孔をすり抜け、平板翼の裏側
にて乱流気味に再混合される。
In the above configuration, the contents are moved upward or downward as each flat blade rotates, and at the same time, some of the contents slip through the many small holes provided on the flat blade surface and reach the back side of the flat blade. The mixture is remixed in a somewhat turbulent manner.

これによると、1軸で構造が簡単な上、共回りを生じる
こともなく、滞留現象も防止できるため、効率良く撹拌
させ、重合させることが可能となる。
According to this, the structure is simple because it is uniaxial, there is no co-rotation, and the phenomenon of retention can be prevented, so that it is possible to efficiently stir and polymerize.

尚、本発明に係る連続重合反応装置に適用可能な重合反
応は、例えば、ポリスチレンの溶液重合及び塊状重合、
ポリメチルメタアクリレートの塊状重合、アクリロニト
リル・スチレン樹脂の溶液重合及び塊状重合、アクリロ
ニトリル・ブタジェン・スチレン(ABS)樹脂の溶液
重合、ポリブタジェンの溶液重合、スチレンブタジェン
ゴム(SBR)の溶液重合、ε−カプロラクタムを原料
とする6−ナイロンの重縮合、アジピン酸とへキサメチ
レンジアミンを原料とする6、6−ナイロンの重縮合、
ポリビニルアセテートの溶液重合、等である。このよう
な重合反応は、重合反応の終期に反応混合物が高粘度化
するが、本発明に係る連続重合反応装置を用いると、混
合効率がよく、均一を重合系が得られる。
Polymerization reactions applicable to the continuous polymerization reaction apparatus according to the present invention include, for example, solution polymerization and bulk polymerization of polystyrene;
Bulk polymerization of polymethyl methacrylate, solution polymerization and bulk polymerization of acrylonitrile styrene resin, solution polymerization of acrylonitrile butadiene styrene (ABS) resin, solution polymerization of polybutadiene, solution polymerization of styrene butadiene rubber (SBR), ε- Polycondensation of 6-nylon using caprolactam as a raw material, polycondensation of 6,6-nylon using adipic acid and hexamethylene diamine as raw materials,
Solution polymerization of polyvinyl acetate, etc. In such a polymerization reaction, the reaction mixture becomes highly viscous at the end of the polymerization reaction, but when the continuous polymerization reaction apparatus according to the present invention is used, mixing efficiency is good and a uniform polymerization system can be obtained.

〈実施例〉 以下に、本発明の一実施例を図面に基づいて説明するが
、本発明は、その要旨を超えない限り、以下の例に限定
されるものではない。
<Example> An example of the present invention will be described below based on the drawings, but the present invention is not limited to the following example unless it exceeds the gist thereof.

第1図は、本発明の一実施例を示す概略断面図である。FIG. 1 is a schematic cross-sectional view showing one embodiment of the present invention.

横型円筒状の容器1は、その外周壁を温度調節のための
ジャケット2で囲まれており、頂部中央域に液供給口3
を形成し、また、底部中央域には、液排出口4を形成し
ている。
A horizontal cylindrical container 1 has its outer peripheral wall surrounded by a jacket 2 for temperature control, and has a liquid supply port 3 in the center area of the top.
A liquid discharge port 4 is formed in the center area of the bottom.

容器1内には、容器1両端壁を軸封部5,6を介して回
転可能に貫通する回転軸7が設けられ、この回転軸7周
りに放射状に1対の平板翼8,9を取付けて、パドル族
N10を構成している。尚、この例では、平板翼を1対
としたが、複数の平板翼を回転軸周りにほぼ等間隔に配
置し、それぞれ回転軸から放射状に真っ直ぐ外方に向か
って延在させてもよい。
Inside the container 1, there is provided a rotating shaft 7 that rotatably penetrates both end walls of the container 1 via shaft seals 5 and 6, and a pair of flat blades 8 and 9 are attached radially around this rotating shaft 7. They constitute the paddle group N10. In this example, there is one pair of flat plate blades, but a plurality of flat plate blades may be arranged at approximately equal intervals around the rotation axis, and each may extend radially straight outward from the rotation axis.

平板翼8.9は、それらの端縁が容器1内周壁に近接し
ており、それぞれ斜めに対向する部分に欠損部11.1
2を形成しである。欠損部面積の大きさと位置は広範囲
に変えることができる。また、平板翼8.9面上には多
数の小孔13が形成されており、小孔13の合計面積及
び位置も広範囲に変えることができるが、合計面積は平
板翼8,9面積の1/3〜1/2の範囲にあるのが好ま
しい。
The flat blades 8.9 have their edges close to the inner circumferential wall of the container 1, and have defective parts 11.1 at diagonally opposing parts.
2 is formed. The size and location of the defect area can vary widely. In addition, a large number of small holes 13 are formed on the plane of the flat blades 8.9, and the total area and position of the small holes 13 can be changed over a wide range, but the total area is 1 of the area of the flat blades 8.9. It is preferably in the range of /3 to 1/2.

ここで、回転軸7を図示しない駆動装置により回転させ
た場合、内容物は各平板翼8.9の動きと共に上方ある
いは下方に移動させられると同時に、一部は平板翼8,
9に設けられた多数の小孔13をすり抜け、平板翼8.
9の裏側にて乱流気味に再混合される。よって、平板H
8,9表面付近はもとより、容器1内全体にわたって、
内容物の強力且つ、複雑な流れが形成されることになる
Here, when the rotating shaft 7 is rotated by a drive device (not shown), the contents are moved upward or downward with the movement of each flat plate blade 8.9, and at the same time, some of the contents are
It passes through a large number of small holes 13 provided in the flat blade 8.9.
The mixture is remixed in a slightly turbulent manner on the back side of 9. Therefore, the flat plate H
8, 9 not only near the surface but also throughout the inside of the container 1,
A powerful and complex flow of contents will be formed.

これにより、内容物の共周りや滞留現象を回避すること
ができ、撹拌効果2反応効果を大幅に向上させることが
できる。即ち、この装置においては、従来の1軸の反応
装置に比して、反応物を撹拌混合する機能が優れている
ので、効率良く重合反応を進めることができ、得られる
重合物の品質も安定して優れたものとなる。
This makes it possible to avoid co-circulation and stagnation of the contents, and to significantly improve the stirring effect and the reaction effect. In other words, this device has a better ability to stir and mix the reactants than conventional single-screw reactors, so the polymerization reaction can proceed efficiently and the quality of the resulting polymer is stable. and become excellent.

以下に、従来装置に対する本発明装置の効果を実験によ
り示す。
The effects of the device of the present invention over the conventional device will be shown below through experiments.

比較例 内径300mm 、槽長400mmの透明アクリル類の
横型円筒状容器内に、翼幅100mm、翼径294mm
の置型翼(第2図参照)を設置した撹拌装置を比較例と
して用いた。
Comparative Example In a transparent acrylic horizontal cylindrical container with an inner diameter of 300 mm and a tank length of 400 mm, a blade with a blade width of 100 mm and a blade diameter of 294 mm was placed.
A stirring device equipped with a stationary blade (see Figure 2) was used as a comparative example.

容器内に200ポイズの粘度を有する水飴水溶液にヨウ
素(I2)とチオ硫酸ナトリウム(NazSzO:+)
を各々溶解させた2液を別々に供給した後に、撹拌翼を
n=16rpmの速度で回転させ、I2の茶色がNaz
SzO3により脱色するまでの時間t (min )を
計測することにより、混合完了するまでの所要回転数N
=n −tを求めた。また、撹拌トルクも測定した。
Iodine (I2) and sodium thiosulfate (NazSzO:+) are added to a starch syrup aqueous solution with a viscosity of 200 poise in a container.
After separately supplying the two solutions in which each of
By measuring the time t (min) until decolorization with SzO3, the number of revolutions N required to complete mixing can be determined.
= n - t was calculated. The stirring torque was also measured.

結果は、N=100で容器内容物全体の8割程度が脱色
したが容器中央部の内容物が着色したまま残有し、N=
200でやっと全体が脱色した。撹拌トルクは0.75
Kgf−mであった(表1参照)。
The results showed that when N=100, about 80% of the entire contents of the container were decolored, but the contents in the center of the container remained colored, and N=
At 200, the color was finally completely bleached. Stirring torque is 0.75
Kgf-m (see Table 1).

実施例 比較例に用いたのと同一の容器内に第1図に示したパド
ル装置を設置し、比較例におけると同様の方法で実験を
行い、混合完了までの所要回転数Nを求めた。その結果
、N=35で容器内容物全体が脱色した。撹拌トルクは
0.75Kgf−mであった(表1参照)。
The paddle device shown in FIG. 1 was installed in the same container as used in the comparative example, and an experiment was conducted in the same manner as in the comparative example to determine the number of rotations N required to complete mixing. As a result, the entire contents of the container were decolored at N=35. The stirring torque was 0.75 Kgf-m (see Table 1).

従って、本発明に係る装置は、比較例に用いた装置に比
べ、混合完了までの所要回転数が少なくて済むことが確
認された。
Therefore, it was confirmed that the apparatus according to the present invention requires fewer rotations to complete mixing than the apparatus used in the comparative example.

表1 〈発明の効果〉 以上説明したように、本発明装置によると、装置の構造
が簡単な上、従来の1軸の反応装置にみられる撹拌軸及
び撹拌翼近傍での反応物の共周りや滞留現象も防止でき
、反応物を撹拌混合する機能が優れているので、効率良
く重合反応を進めることができ、得られる重合物の品質
も安定して優れたものとなるという効果を奏し、本発明
の工業上の利用価値は極めて大である。
Table 1 <Effects of the Invention> As explained above, according to the apparatus of the present invention, the structure of the apparatus is simple, and the co-circulation of reactants near the stirring shaft and stirring blades, which is seen in conventional single-shaft reactors, is avoided. It also prevents stagnation and stagnation phenomena, and has an excellent ability to stir and mix reactants, allowing the polymerization reaction to proceed efficiently and resulting in stable and excellent quality of the resulting polymer. The industrial utility value of the present invention is extremely large.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明の一実施例を示す概略断面図、第2図は
比較例に用いた装置の要部図である。 ■・・・容器 3・・・液供給口 4・・・液排出口 5゜ 6・・・軸封部 7・・・回転軸 8゜ 9・・・平板 翼 10・・・パドル装置 12・・・欠損部 13・・・ 小孔
FIG. 1 is a schematic sectional view showing one embodiment of the present invention, and FIG. 2 is a diagram of main parts of an apparatus used in a comparative example. ■ Container 3 Liquid supply port 4 Liquid discharge port 5° 6 Shaft seal 7 Rotating shaft 8° 9 Flat blade 10 Paddle device 12 ... Defect part 13 ... Small hole

Claims (2)

【特許請求の範囲】[Claims] (1)液供給口と液排出口とを有する横型円筒状の容器
と、容器の中心に水平方向に設けられた回転軸と、回転
軸周りにほぼ等間隔で配置され、それぞれ回転軸から放
射状に外方に向かって延在し、且つ面上にほぼ一様に分
布した多数の小孔を有する複数の平板翼と、を備えたこ
とを特徴とする連続重合反応装置。
(1) A horizontal cylindrical container having a liquid supply port and a liquid discharge port, a rotating shaft provided horizontally at the center of the container, and a rotating shaft arranged at approximately equal intervals around the rotating shaft, each radially extending from the rotating shaft. 1. A continuous polymerization reaction apparatus, comprising: a plurality of flat plate blades extending outward from each other and having a large number of small holes substantially uniformly distributed on a surface thereof.
(2)平板翼に形成された小孔の合計面積が平板翼面積
の1/3〜1/2の範囲にあることを特徴とする請求項
1記載の連続重合反応装置。
(2) The continuous polymerization reaction apparatus according to claim 1, wherein the total area of the small holes formed in the flat blade is in the range of 1/3 to 1/2 of the area of the flat blade.
JP63188275A 1988-07-29 1988-07-29 Continuous polymerization apparatus Pending JPH0238401A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP63188275A JPH0238401A (en) 1988-07-29 1988-07-29 Continuous polymerization apparatus

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP63188275A JPH0238401A (en) 1988-07-29 1988-07-29 Continuous polymerization apparatus

Publications (1)

Publication Number Publication Date
JPH0238401A true JPH0238401A (en) 1990-02-07

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Family Applications (1)

Application Number Title Priority Date Filing Date
JP63188275A Pending JPH0238401A (en) 1988-07-29 1988-07-29 Continuous polymerization apparatus

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09108566A (en) * 1995-10-23 1997-04-28 Teijin Ltd Horizontal uniaxial reactor
WO2007011027A1 (en) * 2005-07-22 2007-01-25 Daikin Industries, Ltd. Agitator for horizontal polymerization apparatus and process for producing fluoropolymer
JP2014111229A (en) * 2012-12-05 2014-06-19 Hitachi Zosen Corp Powder dissolving device and powder dissolving method therefor

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09108566A (en) * 1995-10-23 1997-04-28 Teijin Ltd Horizontal uniaxial reactor
WO2007011027A1 (en) * 2005-07-22 2007-01-25 Daikin Industries, Ltd. Agitator for horizontal polymerization apparatus and process for producing fluoropolymer
JP2014111229A (en) * 2012-12-05 2014-06-19 Hitachi Zosen Corp Powder dissolving device and powder dissolving method therefor

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