JPH08193102A - Production of vinyl chloride polymer - Google Patents

Production of vinyl chloride polymer

Info

Publication number
JPH08193102A
JPH08193102A JP7006635A JP663595A JPH08193102A JP H08193102 A JPH08193102 A JP H08193102A JP 7006635 A JP7006635 A JP 7006635A JP 663595 A JP663595 A JP 663595A JP H08193102 A JPH08193102 A JP H08193102A
Authority
JP
Japan
Prior art keywords
vinyl chloride
temperature control
control element
tank container
polymerization
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.)
Granted
Application number
JP7006635A
Other languages
Japanese (ja)
Other versions
JP3156535B2 (en
Inventor
Hideto Iizawa
英人 飯澤
Susumu Kato
進 加藤
Shuichi Sakakibara
秀一 榊原
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 Chemical Corp
Original Assignee
Mitsubishi Chemical Corp
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 Chemical Corp filed Critical Mitsubishi Chemical Corp
Priority to JP00663595A priority Critical patent/JP3156535B2/en
Publication of JPH08193102A publication Critical patent/JPH08193102A/en
Application granted granted Critical
Publication of JP3156535B2 publication Critical patent/JP3156535B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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  • Physical Or Chemical Processes And Apparatus (AREA)
  • Polymerisation Methods In General (AREA)

Abstract

PURPOSE: To enable a high-quality vinyl chloride polymer to be produced at high efficiency by using a vessel comprising a main body having a thermostat element disposed over a bottom end plate of the main body and tilting toward the bottom center. CONSTITUTION: Vinyl chloride or a mixture thereof with a minor proportion of one or more copolymerizable monomers is polymerized using a thermostatic vessel comprising a main body 1, a thermostat element 5 disposed inside the straight part of the main body, and a thermostat element 5a connected to the element 5 and disposed over a bottom end plate 3 so as to tilt toward the center of the bottom. Thus, high cooling efficiency, high production efficiency, and high polymer product quality, which are effects of the use of a thermostat polymerizer, can be ensured over long. Further, since there is no space between the bottom end plate and the lower end of the thermostat element and/or the partition for fixing the thermostat element, there is no fear of scale deposition or erosion in the bottom part. Hence, higher product quality is attained and equipment maintenance is facilitated.

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、塩化ビニル系重合体の
製造方法に関し、特に高品質の塩化ビニル系重合体を、
高い生産性で製造することができる塩化ビニル系重合体
の製造方法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a vinyl chloride polymer, and in particular to a high quality vinyl chloride polymer,
The present invention relates to a method for producing a vinyl chloride polymer that can be produced with high productivity.

【0002】[0002]

【従来の技術】一般に、塩化ビニル又は塩化ビニルを主
体とする共重合可能な単量体の混合物(以下まとめて
「塩化ビニル系単量体」という)の重合反応に用いられ
る槽容器は、容器本体1′を円筒形胴部の両端に皿形鏡
板を溶接した耐圧密閉容器で形成すると共に、発熱の除
去や内容物の加熱のためのジャケット16をこの容器本
体1′の外部に付設した外部ジャケット方式の槽容器
(図6)が用いられる。
2. Description of the Related Art Generally, a tank container used for a polymerization reaction of vinyl chloride or a mixture of vinyl chloride-based copolymerizable monomers (hereinafter collectively referred to as "vinyl chloride-based monomer") is a container. The main body 1'is formed of a pressure-tight sealed container in which dish-shaped end plates are welded to both ends of a cylindrical body, and a jacket 16 for removing heat generation and heating contents is attached to the outside of the container main body 1 '. A jacket-type tank container (Fig. 6) is used.

【0003】この方式の槽容器は容器本体で耐圧強度を
保持するため、一般に容器の板厚が大きくなり、容器本
体の壁を通しての伝熱係数が低く、発熱反応である塩化
ビニル系単量体の重合においては、高い生産性を得るこ
とが困難であった。また、槽容器を大型化する場合、強
度面の必要性から容器本体の壁の板厚を大きくする必要
があり、更に伝熱係数の低下を招くという不都合があっ
た。
In this type of tank container, since the container body maintains pressure resistance, the plate thickness of the container is generally large, the coefficient of heat transfer through the wall of the container body is low, and the vinyl chloride monomer which is an exothermic reaction. In the polymerization of, it was difficult to obtain high productivity. Further, in the case of enlarging the tank container, it is necessary to increase the plate thickness of the wall of the container body due to the necessity of strength, and there is a disadvantage that the heat transfer coefficient is further lowered.

【0004】そこで、この熱伝導での不利を解決すべ
く、図7に示すように容器本体1′の円筒形胴部の内面
と直角に仕切板17を間隔をおいて並設し、仕切板17
の先端間に内ストリップ18を跨設することによって、
該内ストリップ18と前記容器本体1′の内面との間に
仕切板17により仕切られた螺旋状の熱媒流路19を形
成した内部ジャケット方式(特開昭57−147502
号)の槽容器が提案されている。該方式の槽容器におい
ては、容器本体1’の内径に比べて仕切板17の間隔を
小さくすることにより耐圧強度を高め、内ストリップ1
8の肉厚を薄くし、伝熱係数を高くすることができる。
Therefore, in order to solve the disadvantage of heat conduction, partition plates 17 are arranged side by side at a right angle to the inner surface of the cylindrical body of the container body 1 ', as shown in FIG. 17
By straddling the inner strip 18 between the tips of the
An internal jacket method in which a spiral heating medium flow passage 19 partitioned by a partition plate 17 is formed between the inner strip 18 and the inner surface of the container body 1 '(JP-A-57-147502).
No.) tank container is proposed. In the tank container of this system, the pressure resistance strength is increased by making the interval between the partition plates 17 smaller than the inner diameter of the container body 1 ', and the inner strip 1
It is possible to reduce the thickness of No. 8 and increase the heat transfer coefficient.

【0005】しかしながら内部ジャケット方式の槽容器
は熱伝導性に優れる反面、塩化ビニル系単量体の重合反
応時に内容物が接する槽容器内面に、多数存在する内ス
トリップ18相互間の溶接部が表面に露出していること
による不都合な点がある。即ち、溶接部はその施工上表
面粗度が粗く、溶接欠陥部分が存在するが、塩化ビニル
系単量体の重合反応では、反応混合物の接する部分(以
下、「接液部」という)の表面粗度が粗いと、重合体ス
ケールが付着しやすく、また付着・生成したスケールが
剥離し製品中に混入すると、品質の悪化(特に、フィル
ム等に加工したときに、フィルム中に未溶融物が残る、
いわゆるフィッシュアイ(FE))を引き起こす。この
ような品質悪化を招く重合体スケールの付着を防ごうと
する場合、多数存在する溶接線を極度に平滑にしたり、
特別な付着防止・除去技術を導入する必要があるなど、
設備の製作・維持のコストが大きくなる不都合がある。
However, while the inner jacket type vessel container has excellent thermal conductivity, a large number of inner strips 18 are welded to each other on the inner surface of the vessel vessel where the contents come into contact during the polymerization reaction of the vinyl chloride monomer. There is a disadvantage due to being exposed to. That is, the welded portion has a rough surface roughness due to its construction, and a welding defect portion exists, but in the polymerization reaction of the vinyl chloride-based monomer, the surface of the contacting portion of the reaction mixture (hereinafter referred to as "wetted portion") If the roughness is rough, polymer scale tends to adhere, and if the adhered / generated scale peels off and is mixed in the product, the quality deteriorates (especially when processed into a film, unmelted matter is left in the film. Remain,
Causes so-called fish eye (FE). When trying to prevent the adhesion of polymer scale that causes such deterioration of quality, extremely smooth the welding lines that exist in large numbers,
It is necessary to introduce special anti-adhesion / removal technology.
There is an inconvenience that the cost of manufacturing and maintaining the equipment increases.

【0006】また、塩化ビニル系単量体の重合反応で
は、反応の進行に伴い発生する塩化水素による腐食を防
ぐため、槽容器内面の材質としてステンレス材を用いる
例が多いが、ステンレス材の溶接部は溶接による残留応
力が集中している。このため、容器内面に溶接線が隣接
して多数存在する内部ジャケット方式の槽容器を用いて
塩化ビニル系単量体の重合反応を行う場合、この塩化水
素(塩素イオン)による応力腐食割れの懸念があるの
で、溶接線の劣化程度の検査を入念にかつ継続的に行う
必要があり、メンテナンスが煩雑で検査費用が嵩むとい
う不都合もある。
In addition, in the polymerization reaction of vinyl chloride-based monomers, in order to prevent corrosion due to hydrogen chloride generated as the reaction progresses, stainless steel is often used as the material for the inner surface of the vessel. The residual stress due to welding is concentrated in the area. For this reason, when a vinyl chloride-based monomer polymerization reaction is carried out using a tank container of the internal jacket method in which many welding lines are adjacent to the inner surface of the container, there is concern about stress corrosion cracking due to this hydrogen chloride (chlorine ion). Therefore, it is necessary to carefully and continuously inspect the degree of deterioration of the welding line, and maintenance is complicated and inspection costs increase.

【0007】この内部ジャケット方式の槽容器の不利を
解決すべく、本発明者らは、先にかかる問題のない水性
媒体中における塩化ビニル系重合体の製造方法として、
内板の外面に直角に仕切板を間隔をおいて並設し、該仕
切板の先端間に外ストリップを跨設することによって、
前記内板と外ストリップとの間に仕切板により仕切られ
た熱媒の流路を有する流路壁(以下「温調エレメント」
という)を形成し、この温調エレメントを容器本体内に
外ストリップ側を容器本体の内面に対向させて間隔をお
いて固定した構造の槽容器(以下「温調エレメント方式
の槽容器」という)中で塩化ビニル系単量体の重合反応
を行う方法を提案した。
[0007] In order to solve the disadvantage of this inner jacket type tank container, the present inventors have proposed a method for producing a vinyl chloride polymer in an aqueous medium, which does not have the above problems.
Partition plates are arranged side by side at a right angle to the outer surface of the inner plate, and by straddling an outer strip between the tips of the partition plates,
A flow path wall having a flow path of a heat medium partitioned by a partition plate between the inner plate and the outer strip (hereinafter referred to as "temperature control element").
) Is formed, and the temperature control element is fixed inside the container body with the outer strip side facing the inner surface of the container body at a distance (hereinafter referred to as "temperature control element type tank container"). In this paper, we proposed a method to carry out the polymerization reaction of vinyl chloride monomer.

【0008】[0008]

【発明が解決しようとする課題】本発明の目的は、温調
エレメント方式の槽容器中で塩化ビニル系重合体を製造
する際に、温調エレメントの下部の形状を改良すること
により、高品質の塩化ビニル系重合体を製造する方法を
提供することにある。
SUMMARY OF THE INVENTION An object of the present invention is to improve the quality of the lower part of the temperature control element by improving the shape of the lower part of the temperature control element when producing a vinyl chloride polymer in a temperature control element type vessel. Another object of the present invention is to provide a method for producing the vinyl chloride polymer.

【0009】[0009]

【課題を解決するための手段】即ち、本発明の要旨は、
塩化ビニル系単量体の水性媒体中における重合を、内板
の外面に直角に仕切板を間隔をおいて並設し、該仕切板
の先端間に外ストリップを跨設することによって、前記
内板と外ストリップとの間に仕切板により仕切られた熱
媒の流路を有する流路壁(温調エレメント)を形成し、
この温調エレメントを容器本体内に外ストリップ側を容
器本体の内面に対向させて間隔をおいて固定した槽容器
中で行うに際し、槽容器本体の円筒形胴部の温調エレメ
ントに接続して、該槽容器本体の底部鏡板部分に槽容器
底部中心側に向かって傾斜した形状の温調エレメントが
設けられた槽容器を用いることを特徴とする塩化ビニル
系重合体の製造方法、に存する。以下、本発明について
詳細に説明する。
That is, the gist of the present invention is as follows.
Polymerization of vinyl chloride-based monomer in an aqueous medium is carried out by arranging partition plates side by side at a right angle to the outer surface of the inner plate, and straddling an outer strip between the tips of the partition plates. A flow path wall (temperature control element) having a flow path of a heat medium partitioned by a partition plate is formed between the plate and the outer strip,
When performing this temperature control element in a vessel body in which the outer strip side is opposed to the inner surface of the vessel body inside the vessel body and fixed at intervals, connect it to the temperature control element of the cylindrical body of the vessel body. A method for producing a vinyl chloride polymer, characterized in that a tank container in which a temperature control element having a shape inclined toward the center of the bottom of the tank container is provided on the bottom end plate portion of the tank container body is used. Hereinafter, the present invention will be described in detail.

【0010】〈槽容器〉槽容器本体 本発明方法に使用される温調エレメント方式の槽容器
(以下「重合槽」ということもある)は次のような構造
のものである。
<Tank Container> Tank container main body The temperature control element type tank container (hereinafter sometimes referred to as “polymerization tank”) used in the method of the present invention has the following structure.

【0011】即ち、図1〜図4に示すように、内板6の
外面に直角に仕切板7を間隔をおいて並設し、仕切板7
の先端間に外ストリップ8を跨設することにより、前記
内板6と外ストリップ8との間に仕切板7により仕切ら
れた熱媒の流路9を有する温調エレメント5を形成す
る。この温調エレメント5の外径を槽容器の内径より小
さく製作し、その外ストリップ8側を容器本体1の内面
に対向させて間隔をおいて固定して温調エレメント方式
の槽容器を構成する。この時、容器の円筒形胴部(以下
「直胴部」ということもある)については円筒状の温調
エレメントを用い、また容器の底部鏡板部分には、この
直胴部の温調エレメントに接続して、該槽容器底部中心
側に向かって傾斜した形状の温調エレメント(以下、こ
のような容器の底部鏡板部分に設けられた温調エレメン
トを「底部温調エレメント」という。)を設置する。
That is, as shown in FIGS. 1 to 4, the partition plates 7 are arranged side by side at right angles to the outer surface of the inner plate 6 to form the partition plates 7.
By arranging the outer strip 8 between the tips of the above, the temperature control element 5 having the flow path 9 for the heat medium partitioned by the partition plate 7 is formed between the inner plate 6 and the outer strip 8. The outer diameter of the temperature control element 5 is made smaller than the inner diameter of the tank container, and the outer strip 8 side of the temperature control element 5 is opposed to the inner surface of the container body 1 and fixed at intervals to form a temperature control element type tank container. . At this time, a cylindrical temperature control element is used for the cylindrical body part of the container (hereinafter also referred to as “straight body part”), and the temperature control element of the straight body part is used for the bottom end plate part of the container. A temperature control element having a shape inclined toward the center side of the bottom of the vessel container is connected (hereinafter, the temperature control element provided on the bottom end plate portion of such a vessel is referred to as "bottom temperature control element"). To do.

【0012】この底部温調エレメントの形状は、例えば
槽容器の底部中心に向かって円錐形もしくは円錐台状5
a(図1)、皿形状5b(図3)あるいは半球状5c
(図4)等に形成するのが良く、かつ槽容器本体の底部
鏡板と相似形となっているのがより好ましい。また、塩
化ビニル系単量体の重合には通常円筒形の直胴部の上下
部に皿形鏡板を溶接した形式の槽容器が多く用いられて
おり、撹拌強度等に関し従来の知識を活かした設計を容
易に行えることから、図3に示すような皿形状の底部形
状が特に好ましい。
The shape of the bottom temperature control element is, for example, a conical shape or a truncated cone shape 5 toward the center of the bottom of the tank container.
a (Fig. 1), dish shape 5b (Fig. 3) or hemispherical 5c
(FIG. 4) and the like, and more preferably, it has a shape similar to the bottom end plate of the tank container body. In addition, for the polymerization of vinyl chloride-based monomers, a tank container in which a dish-shaped end plate is welded to the upper and lower parts of a cylindrical straight body is usually used, and conventional knowledge on stirring strength was utilized. The dish-shaped bottom shape as shown in FIG. 3 is particularly preferable because it can be easily designed.

【0013】また、この底部温調エレメントと直胴部の
温調エレメントとの接続部は、連続溶接や接続板を用い
る等の方法で、両方の温調エレメントの内板面同士が隙
間なく接合されたものであるのが好ましい。このような
形状を取ることにより、図5に示すような直胴部に円筒
形の温調エレメント5のみが設置された槽容器において
生じる温調エレメント下端部及び/またはこれを固定す
る隔壁13と底部鏡板3とに挟まれた空間がなくなるの
で、反応時の反応混合物の滞留が少なくなり、かつ洗浄
を容易に行うことができ、スケール付着の可能性が低く
なる。
Further, at the connecting portion between the bottom temperature control element and the straight body temperature control element, the inner plate surfaces of both temperature control elements are joined together without a gap by a method such as continuous welding or using a connecting plate. It is preferable that the By adopting such a shape, the lower end of the temperature control element generated in the tank container in which only the cylindrical temperature control element 5 is installed in the straight body portion as shown in FIG. 5 and / or the partition wall 13 for fixing the same. Since the space sandwiched between the bottom end plate 3 and the bottom end plate 3 is eliminated, the amount of the reaction mixture retained during the reaction is reduced, the cleaning can be easily performed, and the possibility of scale adhesion is reduced.

【0014】上記の温調エレメントの固定は、その中心
線と容器の中心線とがほぼ一致するように行うのが良
く、このとき容器本体の内面と温調エレメントの外面
(即ち外ストリップ側)との間には両者の大きさの差に
相当する間隙ができる。この間隙に重合反応中に反応混
合物が侵入してスケールを形成するのを防止するため、
その上下の開口部を封止しておくことがより好ましい。
The temperature control element is preferably fixed so that the center line of the temperature control element and the center line of the container substantially coincide with each other. At this time, the inner surface of the container body and the outer surface of the temperature control element (that is, the outer strip side). A gap corresponding to the size difference between the two is formed. To prevent the reaction mixture from penetrating into this gap during the polymerization reaction to form scale,
It is more preferable to seal the upper and lower openings.

【0015】この開口部を封止するためには、底部温調
エレメントの下端部については図1に示すように槽容器
ノズル12の周囲の底部鏡板3に連続溶接等により直接
封止しても、また図3及び図4に示すように隔壁を介し
て封止してもよい。また温調エレメントの上端部につい
ては、通常、容器の直胴部2または頂部鏡板4に隔壁1
3を取り付け封止する。
In order to seal this opening, the lower end of the bottom temperature control element may be directly sealed to the bottom end plate 3 around the tank container nozzle 12 by continuous welding or the like as shown in FIG. Alternatively, as shown in FIGS. 3 and 4, sealing may be performed via a partition wall. Regarding the upper end of the temperature control element, the partition wall 1 is usually attached to the straight body part 2 or the top end plate 4 of the container.
Attach 3 and seal.

【0016】このようにして容器本体1の内部に固定さ
れた温調エレメント5の外面と容器本体1の内面との間
には間隙室が形成された構造となり、反応混合物の上記
間隙への侵入と、これに伴うスケール付着の生成とが防
止できる。この間隙の上部及び/又は下部を封止するた
めの隔壁等には、温調エレメントの熱による膨張・収縮
を吸収できるような伸縮吸収部を設けておくのが良く、
また塩化ビニル系単量体の重合の際に通常用いられる温
度や圧力に耐え得るような強度を持たせておく必要があ
る。
In this way, a gap chamber is formed between the outer surface of the temperature control element 5 fixed inside the container body 1 and the inner surface of the container body 1, and the reaction mixture enters the gap. It is possible to prevent the generation of scale adhesion accompanying this. A partition for sealing the upper part and / or the lower part of this gap is preferably provided with an expansion and contraction absorbing part capable of absorbing expansion and contraction due to heat of the temperature control element,
Further, it is necessary to have a strength that can withstand the temperature and pressure normally used in the polymerization of vinyl chloride-based monomers.

【0017】また、温調エレメント及びこれと容器本体
との間隙の上下部を封止するための溶接や隔壁が反応圧
等により破壊されるのを防ぐため、容器本体の内面(主
に頂部鏡板の部分)と温調エレメントの内板とで囲まれ
た空間(以下「本体室」という)の内圧と間隙室の内圧
とを実質的に同じになるようにするのが保安上好まし
く、このときは上記したほどの隔壁の耐圧強度は必要が
なくなる。この場合、本体室の内圧と間隙室の内圧との
差が3Kg/cm2以下、好ましくは1Kg/cm2以下、より好ま
しくは0.7Kg/cm2以下となるようにするのがよい。
Further, in order to prevent the temperature control element and the welding for sealing the upper and lower portions of the gap between the temperature control element and the container body and the partition wall from being destroyed by the reaction pressure, etc., the inner surface of the container body (mainly the top end plate). (Part) and the inner plate of the temperature control element (hereinafter referred to as "main body chamber") and the internal pressure of the gap chamber are preferably substantially the same from the viewpoint of safety. Does not require the pressure resistance of the partition wall as described above. In this case, the difference between the internal pressure of the inner pressure and the gap chamber body chamber 3 Kg / cm 2 or less, preferably 1Kg / cm 2 or less, and more preferably to such a 0.7 Kg / cm 2 or less.

【0018】本体室と間隙室とを実質的に同圧とするた
めの方法としては、例えば図1に示すような連通管を用
いて両室を連通させて均圧を確保する方法、隔壁に開口
部を設ける方法、あるいは本体室及び間隙室の内圧を検
出し、間隙室内の圧力を本体室の内圧と実質的に同じに
なるように別途設置した加圧・減圧装置により調節する
方法等があるが、特に限定されるものではなく、またこ
れらを組み合せて用いてもよい。
As a method for making the main chamber and the gap chamber substantially at the same pressure, for example, a method of connecting both chambers by using a communication pipe as shown in FIG. A method of providing an opening or a method of detecting the internal pressure of the main body chamber and the gap chamber and adjusting the pressure in the gap chamber by a separately installed pressurization / decompression device so that the pressure is substantially the same as the internal pressure of the main body chamber, etc. However, it is not particularly limited, and these may be used in combination.

【0019】また、空気シリンダー方式や封液加圧用の
シリンダー方式等のバランスピストン方式の均圧器や、
ベローズやダイヤフラム等の隔膜方式の均圧器を介して
本体室と間隙室を連結して両室の内圧の差を小さくして
もよい。このような連通管等の均圧設備を用いた場合、
その槽容器側の開口部を介して水等の液体を本体室へ注
入することにより、この開口部及びその周辺へのスケー
ル付着や閉塞を防止する処置を講じておくことが好まし
い。
Further, a balance piston type pressure equalizer such as an air cylinder type or a cylinder type for pressurizing the sealing liquid,
The main chamber and the gap chamber may be connected via a diaphragm type pressure equalizer such as a bellows or a diaphragm to reduce the difference in internal pressure between the two chambers. When using a pressure equalizing equipment such as such a communication pipe,
It is preferable to inject a liquid such as water into the main chamber through the opening on the side of the tank container to prevent the scale from adhering to or clogging the opening and its surroundings.

【0020】温調エレメント5内での熱媒の流路は、図
1に示すように単一の螺旋状としてもよいし、底部鏡板
部は螺旋状、容器本体胴部は周方向は蛇行状とするなど
複数の流路で形成してもよく、また流路を複数に区分し
てもよい。流路に供給する熱媒としては、加熱用には蒸
気、温水等が用いられ、冷却用には、工業用水等の常温
水、別途冷水塔や冷凍機で冷却された水、エチレングリ
コール等の冷媒、フロン等の低温沸点冷媒等が使用でき
るが、いずれも特に限定されない。
The flow path of the heat medium in the temperature control element 5 may be a single spiral as shown in FIG. 1, the bottom end plate may be spiral, and the body of the container may be serpentine in the circumferential direction. May be formed by a plurality of flow paths, or the flow paths may be divided into a plurality of flow paths. As the heat medium supplied to the flow path, steam, hot water or the like is used for heating, normal temperature water such as industrial water is used for cooling, water separately cooled by a cold water tower or a refrigerator, ethylene glycol or the like. A low-temperature boiling point refrigerant such as a refrigerant or chlorofluorocarbon can be used, but is not particularly limited.

【0021】内板6の板厚は、必要とされる強度と仕切
板7の間隔とに依存するが、容器本体1の胴長に比べて
仕切板7の間隔は小さいので、内板6の厚さを薄くし
て、高い伝熱係数を得ることができる。内板6の材質
は、前述したように接液部の耐食性を考慮して、ステン
レス材(ステンレス無垢材、ステンレス・炭素鋼クラッ
ド材など、特にSUS316Lが好ましい)やガラスラ
イニング材等が用いられるが、塩素イオンによる応力腐
食割れに耐性のある材質であれば、特に限定されるもの
ではない。
The plate thickness of the inner plate 6 depends on the required strength and the space between the partition plates 7, but since the space between the partition plates 7 is smaller than the body length of the container body 1, The thickness can be reduced to obtain a high heat transfer coefficient. As the material of the inner plate 6, a stainless steel material (pure stainless steel material, stainless steel / carbon steel clad material, etc., especially SUS316L is preferable) or a glass lining material is used in consideration of the corrosion resistance of the liquid contact part as described above. The material is not particularly limited as long as it is a material resistant to stress corrosion cracking due to chlorine ions.

【0022】スケール付着防止の観点から内板6の表面
は平滑であるのが好ましい。該表面を平滑にするために
は、工業的に通常実施されるバフ仕上げ、電解研磨等の
方法を特に限定することなく用いることができる。ま
た、その表面粗度としては、Rmaxで通常10μm以
下、好ましくは3μm以下、より好ましくは1μm以下
がよい。Rmaxの測定は、JIS B 0601にて
規定された方法を用いればよい。
From the viewpoint of preventing scale adhesion, it is preferable that the surface of the inner plate 6 is smooth. In order to make the surface smooth, methods such as buffing and electropolishing that are commonly used in industry can be used without particular limitation. The surface roughness of Rmax is usually 10 μm or less, preferably 3 μm or less, and more preferably 1 μm or less. The Rmax may be measured by using the method specified in JIS B0601.

【0023】このように製作された槽容器の本体室側の
内容面に溶接部が占める割合は、内部ジャケット方式の
槽容器より著しく少ないので、重合体スケールの付着や
生成が少なく、得られる製品の品質も良好であり、また
応力腐食割れの懸念も少ないので、保守・点検(いわゆ
るメンテナンス)の程度も通常の外部ジャケット方式の
槽容器並のものでよい。
The welded portion occupies the content surface of the main body chamber side of the tank container manufactured as described above in a remarkably smaller proportion than that of the tank container of the inner jacket type, so that adhesion and formation of polymer scale are less and the obtained product is obtained. Since the quality is good and there is little concern about stress corrosion cracking, the degree of maintenance / inspection (so-called maintenance) may be the same as that of a normal outer jacket type vessel container.

【0024】槽容器付帯設備 本発明方法においては、付加的な冷却装置として還流冷
却器を設置してもよい。還流冷却器の形式、材質は特に
限定されるものではなく、ステンレス鋼を接液部の材質
とする多管式熱交換器等の、一般に塩化ビニル系単量体
の重合に使用される還流冷却器を使用すればよい。伝熱
面積は生産品種の要求品質、除熱負荷の程度、負荷制御
の方式に応じて決定すればよい。負荷制御の方式として
は、一般に用いられている方法でよく、還流冷却器に供
給する冷却媒体の量やその温度で制御する方法などが用
いられる。
Equipment attached to tank container In the method of the present invention, a reflux condenser may be installed as an additional cooling device. The type and material of the reflux condenser are not particularly limited, and the reflux cooling generally used for polymerization of vinyl chloride-based monomers, such as a multi-tube heat exchanger with stainless steel as the material of the liquid contact part, is used. You can use a vessel. The heat transfer area may be determined according to the required quality of the product type, the degree of heat removal load, and the load control method. The load control method may be a generally used method, such as a method of controlling the amount of cooling medium supplied to the reflux condenser or its temperature.

【0025】また、この還流冷却器は槽容器の気相部に
設置するが、槽容器本体の頂部鏡板に接続配管を介して
竪型に設置するのが、飛散した重合体の滞留や固着を防
ぐ上で好適である。その他の槽容器(重合槽)の付帯機
器である撹拌翼やバッフルなどの形状は、特に限定され
るものではなく、従来の懸濁重合法、乳化重合法又は微
細懸濁重合法で、一般的に使用されている設備・機器を
使用することができる。
Further, this reflux condenser is installed in the gas phase part of the tank container, but is installed vertically on the top end plate of the tank container body through a connecting pipe so that retention and sticking of scattered polymer is prevented. It is suitable for prevention. The shape of the stirring blades, baffles, etc., which are the auxiliary equipment of the other tank container (polymerization tank), is not particularly limited, and it is a conventional suspension polymerization method, emulsion polymerization method or fine suspension polymerization method, You can use the equipment and equipment used in.

【0026】〈重合処方〉本発明にいう塩化ビニル系重
合体とは、塩化ビニル系単量体を水性媒体中で重合して
得られる、塩化ビニルを主な構成単位とする重合体のこ
とをいう。塩化ビニル系単量体の水性媒体中での重合方
法には、一般に懸濁重合法と乳化重合法ならびに微細懸
濁重合法とがある。塩化ビニル系単量体の懸濁重合は、
通常、塩化ビニル系単量体を分散剤を含有する水性媒体
中で、油溶性重合開始剤の存在下に重合させることによ
って実施される。
<Polymerization Prescription> The vinyl chloride polymer as referred to in the present invention means a polymer having vinyl chloride as a main constituent unit, which is obtained by polymerizing a vinyl chloride monomer in an aqueous medium. Say. As a polymerization method of the vinyl chloride-based monomer in an aqueous medium, there are generally a suspension polymerization method, an emulsion polymerization method and a fine suspension polymerization method. Suspension polymerization of vinyl chloride monomer
Usually, it is carried out by polymerizing a vinyl chloride-based monomer in an aqueous medium containing a dispersant in the presence of an oil-soluble polymerization initiator.

【0027】塩化ビニル系単量体の乳化重合は、塩化ビ
ニル系単量体を水性媒体中で、乳化剤及び水溶性重合開
始剤の存在下に、また、微細懸濁重合は、塩化ビニル系
単量体を水性媒体中で、乳化剤及び油溶性重合開始剤の
存在下に、均質化処理の上重合させることによって実施
される。
Emulsion polymerization of a vinyl chloride monomer is carried out in an aqueous medium in the presence of an emulsifier and a water-soluble polymerization initiator, and fine suspension polymerization is carried out by a vinyl chloride monomer. It is carried out by polymerizing the monomer in an aqueous medium in the presence of an emulsifier and an oil-soluble polymerization initiator, followed by homogenization treatment.

【0028】単量体 本発明方法において使用される塩化ビニル系単量体と
は、塩化ビニル単量体単独及び塩化ビニル単量体を主体
とする共重合可能な単量体の混合物を含む。塩化ビニル
単量体と共重合可能な他の単量体としては、従来一般的
に用いられているものを使用することができ、特に限定
されない。上記の他の単量体としては、例えば、酢酸ビ
ニル、プロピオン酸ビニル、ステアリン酸ビニル等のビ
ニルエステル類、メチルビニルエーテル、エチルビニル
エーテル、オクチルビニルエーテル、ラウリルビニルエ
ーテル、セチルビニルエーテル等のアルキルビニルエー
テル類、エチレン等のα−オレフィン類、アクリル酸、
メタクリル酸等の一価不飽和酸、これらの一価不飽和酸
のメチルエステル、エチルエステル等のアルキルエステ
ル類、マレイン酸、フマル酸、イタコン酸等の二価不飽
和酸、これらの二価不飽和酸のメチルエステル、エチル
エステル等のアルキルエステル類、塩化ビニリデン等の
ビニリデン化合物、アクリロニトリル等の不飽和ニトリ
ルなどの一種又は二種以上の混合物が挙げられる。これ
らの他の単量体は、塩化ビニル単量体に対し、通常、3
0重量%以下、好ましくは20重量%以下の割合で使用
されるが、特に制限はない。
Monomer The vinyl chloride-based monomer used in the method of the present invention includes vinyl chloride monomer alone and a mixture of copolymerizable monomers mainly composed of vinyl chloride monomer. As the other monomer copolymerizable with the vinyl chloride monomer, those generally used in the related art can be used and are not particularly limited. Examples of the above-mentioned other monomers include vinyl acetates such as vinyl acetate, vinyl propionate and vinyl stearate, alkyl vinyl ethers such as methyl vinyl ether, ethyl vinyl ether, octyl vinyl ether, lauryl vinyl ether and cetyl vinyl ether, ethylene and the like. Α-olefins, acrylic acid,
Mono-unsaturated acids such as methacrylic acid, alkyl esters of these mono-unsaturated acids such as methyl ester and ethyl ester, di-unsaturated acids such as maleic acid, fumaric acid, itaconic acid, etc. One or a mixture of two or more of alkyl esters such as methyl ester and ethyl ester of saturated acid, vinylidene compound such as vinylidene chloride, unsaturated nitrile such as acrylonitrile and the like can be mentioned. These other monomers are usually 3
It is used in an amount of 0% by weight or less, preferably 20% by weight or less, but there is no particular limitation.

【0029】分散剤 本発明方法において使用できる分散剤は、塩化ビニル系
単量体の懸濁重合法で従来一般的に使用されているもの
でよく、特に限定されない。上記分散剤としては、例え
ば部分ケン化ポリ酢酸ビニル(いわゆるポリビニルアル
コール)、ヒドロキシプロピルメチルセルロースなどの
セルロース誘導体、ゼラチンなどの水溶性ポリマー等が
挙げられる。また、分散助剤としてラウリル硫酸ナトリ
ウムなどのアニオン性界面活性剤、ソルビタン脂肪酸エ
ステル類やグリセリン脂肪酸エステル類などの非イオン
性界面活性剤等を使用しても差し支えない。これらの分
散剤あるいは分散助剤は単独で又は2種類以上の組合せ
で用いることができる。また、これらの分散剤の使用量
には特に制限はなく、その種類、撹拌強度、重合温度、
塩化ビニル単量体と共重合させる他の単量体の種類と組
成、目的とする塩化ビニル系重合体の粒径等によって多
少異なるが、一般には塩化ビニル系単量体の総量に対し
て通常0.001〜2重量%、好ましくは0.03〜1
重量%の範囲内で用いられる。
Dispersant The dispersant that can be used in the method of the present invention is not particularly limited, and may be one that has been commonly used in the suspension polymerization method of vinyl chloride monomers. Examples of the dispersant include partially saponified polyvinyl acetate (so-called polyvinyl alcohol), cellulose derivatives such as hydroxypropylmethyl cellulose, and water-soluble polymers such as gelatin. In addition, anionic surfactants such as sodium lauryl sulfate and nonionic surfactants such as sorbitan fatty acid esters and glycerin fatty acid esters may be used as a dispersion aid. These dispersants or dispersion aids can be used alone or in combination of two or more. The amount of these dispersants used is not particularly limited, and its type, stirring strength, polymerization temperature,
Depending on the type and composition of other monomers to be copolymerized with the vinyl chloride monomer and the particle size of the intended vinyl chloride polymer, etc. 0.001-2% by weight, preferably 0.03-1
Used in the range of wt%.

【0030】乳化剤 乳化重合法及び微細懸濁重合法に用いられる乳化剤とし
ては、例えば、高級アルコール硫酸エステル塩(アルカ
リ金属塩、アンモニウム塩)、アルキルベンゼンスルホ
ン酸塩(アルカリ金属塩、アンモニウム塩)、高級脂肪
酸塩(アルカリ金属塩、アンモニウム塩)その他のアニ
オン界面活性剤、ノニオン界面活性剤、及び/またはカ
チオン界面活性剤が挙げられる。これらの界面活性剤
は、1種類を用いてもよいし、2種類以上の併用も可能
である。乳化剤の使用量は、塩化ビニル系単量体に対
し、通常0.1〜3重量%(好ましくは0.3〜1重量
%)の範囲であるが、特に限定されない。また、これら
の乳化剤を加工時の発泡性等の調整用に追加して用いて
もよく、この時は重合用乳化剤とは別に、重合反応終了
後に添加してもよい。
Emulsifiers Examples of emulsifiers used in the emulsion polymerization method and the fine suspension polymerization method include higher alcohol sulfate ester salts (alkali metal salts and ammonium salts), alkylbenzene sulfonates (alkali metal salts and ammonium salts), higher salts. Examples include fatty acid salts (alkali metal salts, ammonium salts) and other anionic surfactants, nonionic surfactants, and / or cationic surfactants. These surfactants may be used alone or in combination of two or more. The amount of the emulsifier used is usually 0.1 to 3% by weight (preferably 0.3 to 1% by weight) based on the vinyl chloride-based monomer, but is not particularly limited. Further, these emulsifiers may be additionally used for adjusting the foaming property during processing, and at this time, separately from the emulsifier for polymerization, they may be added after the completion of the polymerization reaction.

【0031】重合開始剤 本発明方法において使用される重合開始剤は、塩化ビニ
ル系単量体の各重合法で、従来一般的に使用されるもの
でよく、特に限定されない。
Polymerization Initiator The polymerization initiator used in the method of the present invention may be any conventionally used one in each polymerization method of vinyl chloride type monomers and is not particularly limited.

【0032】懸濁重合法で使用される重合開始剤として
は、例えばt−ブチルペルオキシピバレート、t−ブチ
ルペルオキシネオデカノエート、t−ヘキシルペルオキ
シピバレート、t−ヘキシルペルオキシネオデカノエー
ト、α−クミルペルオキシネオデカノエートなどのペル
エステル化合物、ジラウロイルペルオキシドなどのジア
シル又はジアルキルペルオキシド化合物、ジイソプロピ
ルペルオキシジカーボネート、ジ−2−エチルヘキシル
ペルオキシジカーボネートなどのペルカーボネート化合
物、アゾビス(2,4−ジメチルバレロニトリル)、ア
ゾビスイソブチロニトリルなどのアゾ化合物等が挙げら
れる。これらの重合開始剤は、単独で又は2種類以上の
組合せで使用することができる。重合開始剤の使用量
は、開始剤の種類や重合温度、所望の反応時間等によっ
ても異なるが、一般に塩化ビニル系単量体の総量に対し
0.01〜1重量%の範囲である。 乳化重合法で使用
される重合開始剤としては、過硫酸塩(ナトリウム塩、
カリウム塩、アンモニウム塩)、過酸化水素等の水溶性
過酸化物、または、これらの水溶性過酸化物と水溶性還
元剤(例えば、亜硫酸ナトリウム、ピロ亜硫酸ナトリウ
ム、亜硫酸水素ナトリウム、アスコルビン酸、ナトリウ
ムホルムアルデヒドスルホキシレート等)との組合せか
らなる水溶性レドックス系開始剤が例示される。
The polymerization initiator used in the suspension polymerization method is, for example, t-butylperoxypivalate, t-butylperoxyneodecanoate, t-hexylperoxypivalate, t-hexylperoxyneodecanoate, Perester compounds such as α-cumyl peroxy neodecanoate, diacyl or dialkyl peroxide compounds such as dilauroyl peroxide, percarbonate compounds such as diisopropyl peroxydicarbonate, di-2-ethylhexyl peroxydicarbonate, azobis (2,4 -Dimethylvaleronitrile), azo compounds such as azobisisobutyronitrile, and the like. These polymerization initiators can be used alone or in combination of two or more. Although the amount of the polymerization initiator used varies depending on the type of the initiator, the polymerization temperature, the desired reaction time, etc., it is generally in the range of 0.01 to 1% by weight based on the total amount of the vinyl chloride monomer. As the polymerization initiator used in the emulsion polymerization method, persulfate (sodium salt,
Water-soluble peroxides such as potassium salt, ammonium salt) and hydrogen peroxide, or water-soluble peroxides and water-soluble reducing agents (for example, sodium sulfite, sodium pyrosulfite, sodium hydrogen sulfite, ascorbic acid, sodium). Examples of the water-soluble redox initiator include a combination with formaldehyde sulfoxylate and the like).

【0033】微細懸濁重合法で用いられる重合開始剤
は、アゾビスイソブチロニトリル、アゾビス(2,4−
ジメチルバレロニトリル)、ラウロイルペルオキシド、
t−ブチルペルオキシピバレート等の単量体可溶性(油
溶性)開始剤、または、これらの油溶性開始剤と前記の
水溶性還元剤との組合せからなるレドックス系開始剤が
例示される。
The polymerization initiator used in the fine suspension polymerization method is azobisisobutyronitrile or azobis (2,4-
Dimethyl valeronitrile), lauroyl peroxide,
Examples thereof include a monomer-soluble (oil-soluble) initiator such as t-butylperoxypivalate, or a redox-based initiator composed of a combination of these oil-soluble initiators and the above water-soluble reducing agent.

【0034】その他の助剤 更に本発明方法においては、必要に応じて塩化ビニル系
単量体の重合に使用される重合度調整剤(連鎖移動剤、
架橋剤)、酸化防止剤、pH調整剤、レドックス系開始
剤の活性化剤等の各種重合助剤を適宜添加することがで
き、これらの各成分の仕込量等は、従来塩化ビニル系単
量体の重合で実施されている一般的な条件で差し支えな
い。
Other Auxiliary Agents Further, in the method of the present invention, a polymerization degree adjusting agent (a chain transfer agent, a chain transfer agent, or
Cross-linking agent), antioxidant, pH adjuster, various polymerization aids such as activators of redox-based initiators can be added as appropriate. The general conditions used for body polymerization can be used.

【0035】なお、塩化ビニル系単量体の重合に用いら
れる重合度調整剤としては、トリクロルエチレン、四塩
化炭素、2−メルカプトエタノール、オクチルメルカプ
タン等の連鎖移動剤、フタル酸ジアリル、イソシアヌル
酸トリアリル、エチレングリコールジアクリレート、ト
リメチロールプロパントリメタクリレート等の架橋剤が
例示できる。
As the polymerization degree regulator used for the polymerization of vinyl chloride type monomers, trichlorethylene, carbon tetrachloride, chain transfer agents such as 2-mercaptoethanol and octyl mercaptan, diallyl phthalate and triallyl isocyanurate. Examples thereof include cross-linking agents such as ethylene glycol diacrylate and trimethylolpropane trimethacrylate.

【0036】〈重合方法〉仕込方法 本発明方法を実施するに際して、槽容器への水性媒体、
塩化ビニル系単量体、重合開始剤、懸濁重合法の分散
剤、乳化重合法及び微細懸濁重合法の乳化剤、その他各
種重合助剤の仕込割合及び仕込方法は、特に限定されな
い。
<Polymerization Method> Preparation Method In carrying out the method of the present invention, an aqueous medium to be filled in a vessel,
The charging ratio and charging method of the vinyl chloride monomer, the polymerization initiator, the dispersant of the suspension polymerization method, the emulsifier of the emulsion polymerization method and the fine suspension polymerization method, and other various polymerization aids are not particularly limited.

【0037】重合温度 本発明方法において採用される重合温度は、用いる重合
開始剤の種類、重合方法、重合度調整剤の使用の有無、
目標とする重合度等によっても異なるが、一般に、0〜
90℃、特に40〜70℃の範囲を用いることが多い。
また、反応に際しては、一定温度で重合を行わせても、
或いは重合の途中で重合温度を変化させてもよい。
Polymerization temperature : The polymerization temperature employed in the method of the present invention includes the type of polymerization initiator used, the polymerization method, the presence or absence of a polymerization degree modifier,
Generally, it varies from 0 to, although it varies depending on the target degree of polymerization and the like.
90 ° C., especially 40 to 70 ° C. is often used.
Further, in the reaction, even if the polymerization is carried out at a constant temperature,
Alternatively, the polymerization temperature may be changed during the polymerization.

【0038】重合停止方法 本発明方法において、重合反応を停止させる方法として
は、いわゆる重合禁止剤や重合停止剤を添加したり、重
合槽から未反応単量体を回収する方法等が例示される。
Polymerization Termination Method In the method of the present invention, examples of the method for terminating the polymerization reaction include a method of adding a so-called polymerization inhibitor or a polymerization terminator, a method of recovering unreacted monomers from a polymerization tank, and the like. .

【0039】〈後処理方法〉懸濁重合法で生成した塩化
ビニル系重合体のスラリーの脱水・乾燥等の操作として
は、一般に行われている遠心脱水・流動乾燥等の脱水・
乾燥手段でよく、特に限定はされない。乳化重合法及び
微細懸濁重合法で生成した塩化ビニル系重合体のラテッ
クスの乾燥等の操作は、従来から行われている回転円盤
や、二流体ノズル等の噴霧ノズルなどを用いる噴霧乾燥
等の手段を用いればよく、特に限定されない。また、乾
燥処理前にラテックス中の水分の一部を予め取り除き、
ラテックス中の塩化ビニル系重合体の濃度を上げる濃縮
操作をしてもよいし、乾燥後の製品を、分級・粉砕する
操作を行ってもよい。
<Post-Treatment Method> The operations such as dehydration and drying of the slurry of the vinyl chloride polymer produced by the suspension polymerization method are generally performed such as centrifugal dehydration and fluidized drying.
Drying means may be used without any particular limitation. Operations such as drying of the latex of the vinyl chloride polymer produced by the emulsion polymerization method and the fine suspension polymerization method can be performed by spray drying using a conventionally used rotating disk or a spray nozzle such as a two-fluid nozzle. Means may be used and there is no particular limitation. Also, before the drying treatment, some of the water content in the latex is removed in advance,
A concentration operation for increasing the concentration of the vinyl chloride polymer in the latex may be performed, or a product after drying may be classified and pulverized.

【0040】[0040]

【実施例】次に、本発明方法の具体的態様を実施例を用
いて説明するが、本発明は、その要旨を越えない限り、
以下の実施例によって限定されるものではない。なお、
得られた塩化ビニル系重合体のフィッシュアイ(以下、
「FE」と略称する)の評価は下記の方法により行い、
FE個数が少ないほど高品質の塩化ビニル系重合体であ
る、と判定した
EXAMPLES Next, specific embodiments of the method of the present invention will be described with reference to Examples, but the present invention is not limited as long as the gist thereof is not exceeded.
The present invention is not limited to the examples below. In addition,
The fish eye of the obtained vinyl chloride polymer (hereinafter,
“FE” is abbreviated) is evaluated by the following method,
It was judged that the smaller the number of FE, the higher the quality of the vinyl chloride polymer.

【0041】フィッシュ・アイ評価方法 塩化ビニル系重合体100重量部、可塑剤(DOP)5
0重量部、鉛系粉末安定剤3重量部を、塩化ビニル系重
合体100gをベースとして採取し、ビーカーで予備混
合した後、155℃のロールでそれぞれ4分間、5分
間、7分間混練し、厚さ0.4mmのロールシートを作
成した。得られたロール・シートの一辺5cmの正方形
(面積25cm2 )中に認められるFEの数をそれぞれ
計数して、FE個数とした。
Fish eye evaluation method 100 parts by weight of vinyl chloride polymer, plasticizer (DOP) 5
0 parts by weight and 3 parts by weight of a lead-based powder stabilizer were sampled on the basis of 100 g of a vinyl chloride polymer, premixed in a beaker, and then kneaded with a roll at 155 ° C. for 4 minutes, 5 minutes, and 7 minutes, respectively, A roll sheet having a thickness of 0.4 mm was created. The number of FEs observed in a square (area: 25 cm 2 ) having a side of 5 cm on each side of the obtained roll sheet was counted to obtain the FE number.

【0042】<実施例1>内容積400リットルで、撹
拌器を備え、槽容器内壁(及び温調エレメントの内筒の
表面)を電解研磨処理によりRmax1.2μm程度と
し、間隙室と本体室とに区分されたステンレス製の温調
エレメント方式の槽容器に、図3に示すような底部温調
エレメント及び図1に示すような連通管を設置した。
<Example 1> An internal volume of 400 liters was provided with a stirrer, and the inner wall of the tank (and the surface of the inner cylinder of the temperature control element) was electrolytically polished to have a Rmax of about 1.2 μm. The bottom temperature control element as shown in FIG. 3 and the communicating pipe as shown in FIG. 1 were installed in the stainless steel temperature control element type vessel container divided into.

【0043】この槽容器に塩化ビニル単量体100k
g、脱イオン水150kg、分散剤として部分ケン化ポ
リ酢酸ビニル60g、及び開始剤としてジオクチルペル
オキシジカーボネートを40g仕込んだ後、温調エレメ
ントに温水を循環し、57℃まで加温し重合を開始し
た。所定の重合率に達するまで57℃の反応温度を保持
して重合を実施した後、未反応の塩化ビニル単量体を回
収し、生成スラリーを抜き出し、換気した上、槽容器を
開放して槽容器内壁(溶接部、その他の部位、温調エレ
メント下端隔壁下部)へのスケール付着状況を観察し
た。
In this tank container, vinyl chloride monomer 100 k
g, 150 kg of deionized water, 60 g of partially saponified polyvinyl acetate as a dispersant, and 40 g of dioctyl peroxydicarbonate as an initiator, and then warm water is circulated through the temperature control element to heat up to 57 ° C. to start polymerization. did. After carrying out the polymerization while maintaining the reaction temperature of 57 ° C until the predetermined polymerization rate is reached, the unreacted vinyl chloride monomer is recovered, the produced slurry is extracted, ventilated, and the tank container is opened to open the tank. The state of scale adhesion to the inner wall of the container (welded part, other parts, lower part of the temperature control element lower end partition wall) was observed.

【0044】スケール付着状況の観察後、槽容器内壁を
低圧のイオン交換水で洗浄した上で、同条件で次バッチ
のテストを繰り返した。スケール付着状況の観察結果を
表−1に示す。各バッチで得られたスラリーを乾燥して
得た塩化ビニル系重合体について、前記の方法でFEの
評価を行った。結果を表−2に示す。
After observing the scale adhesion state, the inner wall of the vessel was washed with low-pressure ion-exchanged water, and the test of the next batch was repeated under the same conditions. Table 1 shows the results of observation of the scale adhesion state. The vinyl chloride polymer obtained by drying the slurry obtained in each batch was evaluated for FE by the method described above. Table 2 shows the results.

【0045】<比較例1>槽容器として図5に示すよう
な底部温調エレメントを有しない温調エレメント方式の
槽容器を用いたこと以外は全て実施例1と同じ条件で塩
化ビニル単量体の重合反応を行い、同様の評価を実施し
た。結果を表−1、表−2に併せて示す。
Comparative Example 1 Vinyl chloride monomer was used under the same conditions as in Example 1 except that a temperature control element type tank container having no bottom temperature control element as shown in FIG. 5 was used as the tank container. Polymerization reaction was performed and the same evaluation was performed. The results are also shown in Table-1 and Table-2.

【0046】[0046]

【表1】 判定基準:○ … 全表面積の10%未満の内壁に付着が生成 △ … 全表面積の10%以上、50%未満の内壁に付着が生成 × … 全表面積の50%以上の内壁に付着が生成[Table 1] Criteria: ○ ... Adhesion is generated on the inner wall of less than 10% of the total surface area. △ ... Adhesion is generated on the inner wall of 10% or more and less than 50% of the total surface area .. × Adhesion is generated on the inner wall of 50% or more of the total surface area.

【0047】[0047]

【表2】 [Table 2]

【0048】[0048]

【発明の効果】温調エレメント方式の槽容器を用いて塩
化ビニル系単量体の重合を行う際に、、該槽容器本体直
胴部の温調エレメントに接続して容器本体の底部鏡板部
分に槽容器底部中心側に向かって傾斜した形状の温調エ
レメントが設けられた槽容器を用いるという本発明の方
法を採ることにより、(1)除熱効率が高く生産性が良
い、及び溶接線の露出が少なく、製品重合体の品質も良
い、という温調エレメント方式の重合槽を用いる効果の
維持・確保、及び(2)温調エレメント下端部及び/ま
たはこれを固定する隔壁と底部鏡板とに挟まれた空間が
なくなり、この部分でのスケール付着や腐食の恐れが少
なくなるので、製品品質が向上し、機器の保守も容易に
なる、という効果を得ることができた。
[Effects of the Invention] When polymerizing a vinyl chloride monomer using a temperature control element type tank container, the bottom end plate portion of the container body is connected to the temperature control element of the body of the tank container body. By adopting the method of the present invention in which the temperature control element having a shape inclined toward the center of the bottom of the tank container is used, (1) heat removal efficiency is high and productivity is good, and welding line Maintaining and securing the effect of using a temperature control element type polymerization tank, which is less exposed and the quality of the product polymer is good, and (2) for the lower end of the temperature control element and / or the partition wall and bottom end plate for fixing this Since there is no space between them, the risk of scale adhesion and corrosion at this part is reduced, so that the product quality is improved and the maintenance of the equipment is facilitated.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明方法の実施に使用できる温調エレメント
方式の槽容器の一例を示す縦断面図
FIG. 1 is a vertical sectional view showing an example of a temperature control element type vessel container that can be used for carrying out the method of the present invention.

【図2】図1の要部拡大図FIG. 2 is an enlarged view of a main part of FIG.

【図3】本発明方法の実施に使用できる温調エレメント
方式の槽容器の他の例を示す要部縦断面図
FIG. 3 is a longitudinal cross-sectional view of a main part showing another example of a temperature control element type tank container that can be used for carrying out the method of the present invention.

【図4】本発明方法の実施に使用できる温調エレメント
方式の槽容器の他の例を示す要部縦断面図
FIG. 4 is a vertical cross-sectional view of a main part showing another example of a temperature control element type tank container that can be used for carrying out the method of the present invention.

【図5】本発明方法の範囲外の温調エレメント方式の槽
容器の一例を示す縦断面図
FIG. 5 is a longitudinal sectional view showing an example of a temperature control element type tank container outside the scope of the method of the present invention.

【図6】従来の槽容器の例を示す縦断面図FIG. 6 is a vertical sectional view showing an example of a conventional tank container.

【図7】従来の槽容器の他の例を示す要部拡大縦断面図FIG. 7 is an enlarged vertical sectional view of an essential part showing another example of a conventional tank container.

【符号の説明】[Explanation of symbols]

1、1’ 容器本体 2 直胴部 3 底部鏡板 4 頂部鏡板 5 温調エレメント(5a,5b,5c 底部温調
エレメント) 6 内板 7、17 仕切板 8 外ストリップ 9、19 熱媒流路 10 熱媒流路入口 11 熱媒流路出口 12 槽容器ノズル 13 隔壁 14 間隙室 15 連通管 16 (外部)ジャケット 18 内ストリップ H 間隙
1, 1'Container main body 2 Straight body part 3 Bottom mirror plate 4 Top mirror plate 5 Temperature control element (5a, 5b, 5c Bottom temperature control element) 6 Inner plate 7, 17 Partition plate 8 Outer strip 9, 19 Heat transfer channel 10 Heat medium flow path inlet 11 Heat medium flow path outlet 12 Tank container nozzle 13 Partition wall 14 Gap chamber 15 Communication pipe 16 (External) jacket 18 Inner strip H Gap

Claims (6)

【特許請求の範囲】[Claims] 【請求項1】 塩化ビニルまたは塩化ビニルを主体とす
る共重合可能な単量体の混合物の水性媒体中における重
合を、内板の外面に直角に仕切板を間隔をおいて並設
し、該仕切板の先端間に外ストリップを跨設することに
よって、前記内板と外ストリップとの間に仕切板により
仕切られた熱媒の流路を有する流路壁(以下「温調エレ
メント」という)を形成し、この温調エレメントを容器
本体内に外ストリップ側を容器本体の内面に対向させて
間隔をおいて固定した槽容器中で行うに際し、槽容器本
体の円筒形胴部の温調エレメントに接続して、槽容器本
体の底部鏡板部分に槽容器底部中心側に向かって傾斜し
た形状の温調エレメントが設けられた槽容器を用いるこ
とを特徴とする塩化ビニル系重合体の製造方法。
1. Polymerization of vinyl chloride or a mixture of vinyl chloride-based copolymerizable monomers in an aqueous medium is carried out by arranging partition plates side by side at right angles to the outer surface of the inner plate, A flow path wall (hereinafter referred to as a "temperature control element") having a flow path of a heat medium partitioned by the partition plate between the inner plate and the outer strip by straddling an outer strip between the ends of the partition plate. When the temperature control element is formed in a tank container in which the outer strip side is opposed to the inner surface of the container body and fixed at a distance, the temperature control element of the cylindrical body of the tank container body is formed. A method for producing a vinyl chloride polymer, characterized in that a tank container in which a temperature control element having a shape inclined toward the center of the bottom of the tank container is provided on the bottom end plate portion of the tank container body is used.
【請求項2】 槽容器本体の底部鏡板部分に設けられた
温調エレメントの形状が円錐形または円錐台形となって
いる請求項1に記載の塩化ビニル系重合体の製造方法。
2. The method for producing a vinyl chloride polymer according to claim 1, wherein the temperature control element provided on the bottom end plate portion of the tank container body has a conical shape or a truncated cone shape.
【請求項3】 槽容器本体の底部鏡板部分に設けられた
温調エレメントの形状が皿形状となっている請求項1に
記載の塩化ビニル系重合体の製造方法
3. The method for producing a vinyl chloride polymer according to claim 1, wherein the temperature control element provided on the bottom end plate portion of the tank container body has a dish shape.
【請求項4】 槽容器本体の底部鏡板部分に設けられた
温調エレメントの形状が半球状となっている請求項1に
記載の塩化ビニル系重合体の製造方法
4. The method for producing a vinyl chloride polymer according to claim 1, wherein the temperature control element provided on the bottom end plate portion of the tank container body has a hemispherical shape.
【請求項5】 温調エレメントの形状が槽容器の底部鏡
板と相似形となっている請求項1〜4のいずれか1項に
記載の塩化ビニル系重合体の製造方法
5. The method for producing a vinyl chloride polymer according to claim 1, wherein the temperature control element has a shape similar to that of the bottom end plate of the tank container.
【請求項6】 温調エレメントの外ストリップ側と槽容
器本体の内面との間の間隙の上下部を封止して間隙室を
形成した構造を有し、かつこの槽容器本体の内面と温調
エレメントの内板とで囲まれた空間と間隙室とを実質的
に同圧とした槽容器を用いる請求項1〜5のいずれか1
項に記載の塩化ビニル系重合体の製造方法。
6. A structure having a gap chamber formed by sealing the upper and lower portions of the gap between the outer strip side of the temperature control element and the inner surface of the tank container body, and the inner surface of the tank container body and the temperature The tank container in which the space surrounded by the inner plate of the adjusting element and the gap chamber have substantially the same pressure is used.
Item 8. A method for producing a vinyl chloride polymer according to the item.
JP00663595A 1995-01-19 1995-01-19 Method for producing vinyl chloride polymer Expired - Fee Related JP3156535B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP00663595A JP3156535B2 (en) 1995-01-19 1995-01-19 Method for producing vinyl chloride polymer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP00663595A JP3156535B2 (en) 1995-01-19 1995-01-19 Method for producing vinyl chloride polymer

Publications (2)

Publication Number Publication Date
JPH08193102A true JPH08193102A (en) 1996-07-30
JP3156535B2 JP3156535B2 (en) 2001-04-16

Family

ID=11643834

Family Applications (1)

Application Number Title Priority Date Filing Date
JP00663595A Expired - Fee Related JP3156535B2 (en) 1995-01-19 1995-01-19 Method for producing vinyl chloride polymer

Country Status (1)

Country Link
JP (1) JP3156535B2 (en)

Also Published As

Publication number Publication date
JP3156535B2 (en) 2001-04-16

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