JPH066605B2 - Method for producing vinyl chloride resin - Google Patents
Method for producing vinyl chloride resinInfo
- Publication number
- JPH066605B2 JPH066605B2 JP7984388A JP7984388A JPH066605B2 JP H066605 B2 JPH066605 B2 JP H066605B2 JP 7984388 A JP7984388 A JP 7984388A JP 7984388 A JP7984388 A JP 7984388A JP H066605 B2 JPH066605 B2 JP H066605B2
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- Prior art keywords
- polymerization
- monomer
- machine
- weight
- vinyl chloride
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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は塩化ビニル系樹脂（以下、ＰＶＣと略す）の製
造方法に関し、更に詳しくは、還流凝縮器を付設した重
合機を用いたポロシティー（空隙率）の高いＰＶＣ粒子
の製造方法に関する。本製造方法によるＰＶＣはポロシ
ティーが高いため、いわゆる残存モノマーとして特に衛
生上問題となる未重合単量体の除去が容易で、かつ成形
加工品のフィッシュ・アイが少ないという特長を有す
る。TECHNICAL FIELD The present invention relates to a method for producing a vinyl chloride resin (hereinafter abbreviated as PVC), and more specifically, porosity using a polymerization machine equipped with a reflux condenser. The present invention relates to a method for producing PVC particles having a high (porosity). Since PVC produced by the present production method has a high porosity, it is easy to remove unpolymerized monomer which is a so-called residual monomer, which is particularly problematic in hygiene, and the molded products have few fish eyes.
ＰＶＣの製造において、重合生産性の向上及び省エネル
ギーを図る目的で還流凝縮器がしばしば用いられる。し
かし乍ら、還流凝縮器による冷却を伴う懸濁重合により
得られたＰＶＣ粒子は一般的にポロシティーが低く、そ
のため未重合単量体の除去が容易でなく、かつ成形加工
品のフィッシュ・アイが多いという問題がある。また、
一般的に重合転化率を高くすれば重合生産性やコスト面
に於いては有利となるが、ポロシティーが低下するので
上述と同様の問題を生じる。In the production of PVC, a reflux condenser is often used for the purpose of improving polymerization productivity and saving energy. However, PVC particles obtained by suspension polymerization accompanied by cooling by a reflux condenser generally have low porosity, and therefore it is not easy to remove unpolymerized monomers, and the fish eye of a molded product is not easily removed. There is a problem that there are many. Also,
Generally, increasing the polymerization conversion rate is advantageous in terms of polymerization productivity and cost, but since porosity decreases, the same problem as described above occurs.
一方、ＰＶＣの残存モノマー及びフィッシュ・アイの品
質レベルに対する市場の要求は近年ますます厳しくなる
傾向にあり、後者についてはポリエステル系等の比較的
可塑化能が低く、粘度の高い高分子可塑剤系で特に問題
とされるようになってきている。On the other hand, market demands for residual monomer of PVC and quality level of fish eye tend to become more and more severe in recent years, and for the latter, a polymer plasticizer system having high viscosity and relatively low plasticizing ability such as polyester system. Is becoming a particularly problematic issue.
本発明者らは、このような現状に鑑み、還流凝縮器を使
用し、かつ重合転化率を高めてもポロシティーが高く、
未重合単量体の除去が容易で、かつ成形加工品のフィッ
シュ・アイが少ないＰＶＣの製造方法について鋭意研究
を重ねた結果、還流凝縮器で凝縮した液化単量体を還流
凝縮器と重合機の間に設けた回収槽に重合中一時的に回
収し、その後回収単量体の全量又はその一部を重合機に
還流させ重合することにより所期の目的が達成できるこ
とを見出し、本発明を完成させたものである。In view of such a current situation, the present inventors use a reflux condenser, and the porosity is high even if the polymerization conversion rate is increased,
As a result of extensive research on a method for producing PVC in which unpolymerized monomers can be easily removed and fish-eyes of molded products are small, liquefied monomers condensed in a reflux condenser are combined with a reflux condenser and a polymerization machine. It was found that the intended purpose can be achieved by temporarily collecting during the polymerization in a recovery tank provided between the two, and then refluxing the whole amount or a part of the recovered monomer to the polymerization machine to perform the polymerization, and the present invention. It has been completed.
即ち、本発明は還流凝縮器を機外に付設した重合機を用
いて塩化ビニル単量体又はこれと共重合し得る他の単量
体との混合物を懸濁重合するに際し、還流凝縮器から重
合機へ還流する液化単量体を還流凝縮器と重合機の間に
設けた回収槽に重合中一時的に回収し、その後回収単量
体の全量又はその一部を重合機に還流させ重合すること
を特徴とする塩化ビニル系樹脂の製造方法を内容とする
ものである。That is, the present invention, when the suspension polymerization of a mixture of vinyl chloride monomer or another monomer copolymerizable therewith using a polymerization machine equipped with a reflux condenser outside the machine, from the reflux condenser The liquefied monomer refluxed to the polymerization machine is temporarily collected during the polymerization in a collection tank provided between the reflux condenser and the polymerization machine, and then all or a part of the recovered monomer is refluxed to the polymerization machine to carry out the polymerization. The present invention is directed to a method for producing a vinyl chloride resin, which is characterized in that
本発明において、還流凝縮器で凝縮した液化単量体の回
収槽への回収開始は、ＰＶＣの最終粒子(Grain)の骨格
が形成された後の重合転化率が２０〜６０％に達した時
点が望ましく、３０〜６０％に達した時点が更に好まし
い。重合転化率が２０％に達しない時点で回収を開始す
るとＰＶＣ粒子の粒度分布が異常となり、また重合転化
率が６０％を越えた時点で回収を開始してもポロシティ
ーを高める効果は小さくなる。単量体の回収速度は特に
限定されないが、還流凝縮器の通常の運転条件下で凝縮
した液化単量体をそのまま回収槽へ回収すればよい。In the present invention, the recovery of the liquefied monomer condensed in the reflux condenser into the recovery tank is started when the polymerization conversion rate after the skeleton of the final particles of PVC (Grain) reaches 20 to 60%. Is desirable, and the time point when it reaches 30 to 60% is more preferable. If recovery is started when the polymerization conversion rate does not reach 20%, the particle size distribution of PVC particles becomes abnormal, and even if recovery is started when the polymerization conversion rate exceeds 60%, the effect of increasing porosity becomes small. . The recovery rate of the monomer is not particularly limited, but the liquefied monomer condensed under the normal operating conditions of the reflux condenser may be directly recovered in the recovery tank.
液化単量体の回収量は特に限定されないが、重合開始時
における重合機中の仕込単量体１００重量部に対して５
〜５０重量部、好ましくは１０〜４０重量部である。回
収量が５重量部未満ではポロシティーを高める効果が小
さく、５０重量部を越えると重合速度が極端に低下した
り、粒度分布が異常になったりする。回収した液化単量
体は、その全量又はその一部を重合機に還流させるが、
その量は任意である。その一部のみを還流させるときは
全量を還流させるときに比べ、ポロシティーを高める効
果は大きいが、重合生産性は低い。重合生産性の面から
は液化単量体の全量を還流させるのが好ましいが、この
場合でも実用上十分に高いポロシティーが得られる。The recovery amount of the liquefied monomer is not particularly limited, but it is 5 per 100 parts by weight of the charged monomer in the polymerization machine at the start of the polymerization.
-50 parts by weight, preferably 10-40 parts by weight. If the amount of recovery is less than 5 parts by weight, the effect of increasing porosity is small, and if it exceeds 50 parts by weight, the polymerization rate is extremely reduced or the particle size distribution becomes abnormal. The recovered liquefied monomer, the whole amount or a part thereof is refluxed to the polymerization machine,
The amount is arbitrary. When only part of it is refluxed, the effect of increasing porosity is greater than when all of it is refluxed, but the polymerization productivity is low. From the viewpoint of polymerization productivity, it is preferable to reflux the entire amount of the liquefied monomer, but even in this case, porosity sufficiently high for practical use can be obtained.
液化単量体を重合機に還流させる時期については特に限
定されないが、重合転化率が４０〜７０％の時点で還流
を開始するのが適当である。重合転化率が７０％を越え
た時点で還流を開始すると重合時間が延び、またポロシ
ティーを高める効果が小さくなる。回収槽に回収した液
化単量体を重合機に還流させるには、ポンプを用いても
よいし、回収槽を還流凝縮器と重合機との中間の高さに
設置し、回収槽と重合機の夫々の気相部を均圧管で結
び、ヘッド差を利用して還流させてもよく、方法は特に
限定されない。The timing of refluxing the liquefied monomer to the polymerization machine is not particularly limited, but it is appropriate to start the reflux at the time when the polymerization conversion rate is 40 to 70%. When the reflux is started at the time when the polymerization conversion rate exceeds 70%, the polymerization time is extended and the effect of increasing the porosity becomes small. A pump may be used to return the liquefied monomer recovered in the recovery tank to the polymerization machine, or the recovery tank may be installed at an intermediate height between the reflux condenser and the polymerization machine. Each gas phase part may be connected by a pressure equalizing tube and refluxed by utilizing the head difference, and the method is not particularly limited.
本発明において塩化ビニル単量体と共重合し得る他の単
量体としては、例えばエチレン、プロピレンなどのオレ
フイン類、酢酸ビニル、ステアリン酸ビニルなどのビニ
ルエステル類、アクリル酸メチル、メタクリル酸メチル
などのアクリル酸エステル、マレイン酸またはフマル酸
などの酸のエステル類及び無水物、アクリロニトリルな
どのニトリル化合物、あるいは塩化ビニリデンの如きビ
ニリデン化合物等が挙げられる。In the present invention, other monomers copolymerizable with the vinyl chloride monomer include, for example, olefins such as ethylene and propylene, vinyl acetates such as vinyl acetate and vinyl stearate, methyl acrylate and methyl methacrylate. Examples thereof include acrylic acid esters, acid esters such as maleic acid and fumaric acid, and anhydrides, nitrile compounds such as acrylonitrile, and vinylidene compounds such as vinylidene chloride.
本発明において使用される重合開始剤としては、塩化ビ
ニル懸濁重合で用いられる開始剤、例えばラウロイルパ
ーオキサイド、３，５，５−トリメキルヘキサノイルパ
ーオキサイド、ｔ−ブチルパーオキシピバレート、ｔ−
ブチルパーオキシネオデカノエート、ジイソプロピルパ
ーオキシジカーボネート、ジ−２−エチルヘキシルバー
オキシジカーボネート及びアセチルシクロヘキシルスル
フオニルパーオキサイドなどのような有機過酸化物並び
にα，α′−アゾビスイソブチロニトリル及びα，α′
−アゾビス２，４−ジメチルバレロニトリルなどのアゾ
化合物の一種又は二種以上の混合物が挙げられる。Examples of the polymerization initiator used in the present invention include those used in suspension polymerization of vinyl chloride, such as lauroyl peroxide, 3,5,5-trimethylmethylhexanoyl peroxide, t-butylperoxypivalate, and t. −
Organic peroxides such as butyl peroxy neodecanoate, diisopropyl peroxydicarbonate, di-2-ethylhexyloxydicarbonate and acetylcyclohexylsulphonyl peroxide, and α, α'-azobisisobutyro Nitrile and α, α '
One or a mixture of two or more azo compounds such as azobis2,4-dimethylvaleronitrile.
本発明において使用される懸濁剤は公知の懸濁剤でよ
く、例えば部分ケン化ポリビニルアルコール、酢酸ビニ
ル−無水マレイン酸共重合体、スチレン−無水マレイン
酸共重合体、ポリビニルピロリドン、ゼラチン、デンプ
ン、メチルセルローズ、ヒドロキシプロピルセルローズ
などが挙げられる。The suspending agent used in the present invention may be a known suspending agent, for example, partially saponified polyvinyl alcohol, vinyl acetate-maleic anhydride copolymer, styrene-maleic anhydride copolymer, polyvinylpyrrolidone, gelatin, starch. , Methyl cellulose, hydroxypropyl cellulose and the like.
本発明においては、必要に応じて分子量調整剤を使用す
ることもできる。In the present invention, a molecular weight modifier may be used if necessary.
また重合反応に使用される開始剤、懸濁剤、分子量調節
剤等は最初に一括して重合反応系に添加してもよく、ま
た重合反応中に分割して添加することもできる。Further, the initiator, the suspending agent, the molecular weight modifier and the like used in the polymerization reaction may be added to the polymerization reaction system all at once at the beginning, or may be dividedly added during the polymerization reaction.
本発明における重合反応温度範囲は通常４０〜７５℃で
あるが、特に限定されない。The polymerization reaction temperature range in the present invention is usually 40 to 75 ° C, but is not particularly limited.
本発明の還流凝縮器で凝縮した液化単量体を重合中一時
的に回収槽に回収し、その後回収単量体の全量又はその
一部を重合機に還流させることによりポロシティーが高
くなる理由については明らかではないが、液化単量体を
重合中一時的に回収槽に回収することにより、ＰＶＣ粒
子にある種の「ポップコーン現象」が生じて粒子内の空
隙が大きくなり、これがその後の液化単量体の還流及び
重合によるポロシティー低下を上回るためと推定され
る。The reason why the porosity becomes high by temporarily collecting the liquefied monomer condensed in the reflux condenser of the present invention in the recovery tank during the polymerization and then refluxing the whole amount or a part of the recovered monomer to the polymerization machine. Although it is not clear about the fact that the liquefied monomer is temporarily collected in the collection tank during the polymerization, some kind of "popcorn phenomenon" occurs in the PVC particles and the voids in the particles become large, which causes the liquefaction after that. It is presumed that this is because the decrease in porosity due to the reflux and polymerization of the monomer is exceeded.
本発明によれば、還流凝縮器を付設した重合機を用いて
ＰＶＣを懸濁重合するに際し、転化率を高めてもポロシ
ティーが高く、未重合単量体の除去が容易で、かつ成形
加工品のフィッシュ・アイの少ない樹脂を製造すること
ができるので、本発明の工業的価値は頗る大きいもので
ある。According to the present invention, in suspension polymerization of PVC using a polymerization machine equipped with a reflux condenser, the porosity is high even if the conversion rate is increased, the unpolymerized monomer is easily removed, and the molding process is performed. The industrial value of the present invention is extremely great because a resin having a low fish eye can be produced.
以下、本発明の実施例及び比較例を示すが、これらは何
ら本発明を限定するものではない。Hereinafter, Examples and Comparative Examples of the present invention will be shown, but these do not limit the present invention in any way.
尚、以下において、物性評価は下記の方法に従った； 粒度分布：ＪＩＳ標準ふるいを用いたふるい振とう法に
よった。In the following, the physical properties were evaluated according to the following methods: Particle size distribution: by a sieving shaking method using a JIS standard sieve.
ポロシテイー： 米国AMINCO社製の水銀圧入式ポロシメーター（5-7118
型）を用いて、絶対圧31〜1011psi（口径0.17〜5.8μ
ｍ）の間にＰＶＣ１００ｇ当りに圧入される水銀の容量
を測定してポロシテイーとした。Porosity: Mercury injection porosimeter (5-7118 made by AMINCO, USA)
Type), absolute pressure 31-1011psi (caliber 0.17-5.8μ
The porosity was measured by measuring the volume of mercury injected per 100 g of PVC during m).
残存モノマー： 重合終了後の樹脂懸濁液を遠心脱水機で１分間脱水して
得られる脱水ケーキの１０ｇをシャーレに取り、これを
６５℃の均熱乾燥機に入れて１時間目及び２時間目に取
り出し乾燥樹脂のサンプルを採る。夫々のサンプル１ｇ
を精秤して５０ｍｌ三角フラスコに取り、アセトン２０
ｍｌを加えて１時間振盪した後、アセトン抽出液をサン
プルとしてガスフロマトグラフ（（株）島津製作所製；
ＧＣ−６Ａ）を用いて単量体を定量した。Residual monomer: 10 g of a dehydrated cake obtained by dehydrating the resin suspension after completion of polymerization with a centrifugal dehydrator for 1 minute was put in a petri dish, and this was placed in a soaking dryer at 65 ° C for the first hour and 2 hours. Remove into eyes and take sample of dry resin. 1g of each sample
Accurately weigh it into a 50 ml Erlenmeyer flask, and add acetone 20
After adding ml and shaking for 1 hour, a gas chromatograph (manufactured by Shimadzu Corporation) using the acetone extract as a sample;
The amount of monomer was quantified using GC-6A).
フイツシユ・アイ（ＦＥ）： 重合して得られたＰＶＣ１００重量部、可塑剤〔ＰＮ２
５０（アジピン酸系ポリエステル；分子量約２００
０）、アデカアーガス社製〕４５重量部、トリベース３
重量部、ステアリン酸０．５重量部、二酸化チタン０．
４重量部およびカーボンブラック０．２重量部を混合
し、３時間以上静置した後、１５０℃の８インチロール
で混練し（シート厚さ０．２ｍｍ）、混練開始から５分
目、７分目及び９分目にそれぞれシートを切り出し、シ
ート５cm×５cm中の透明粒子粒をもつて示した。FS (FE): 100 parts by weight of PVC obtained by polymerization, plasticizer [PN2
50 (adipic acid type polyester; molecular weight about 200)
0), manufactured by ADEKA ARGUS] 45 parts by weight, Tribase 3
Parts by weight, 0.5 parts by weight of stearic acid, titanium dioxide 0.
After mixing 4 parts by weight and 0.2 parts by weight of carbon black and allowing to stand for 3 hours or more, kneading with an 8-inch roll at 150 ° C. (sheet thickness 0.2 mm), 5 minutes after starting kneading, 7 minutes Sheets were cut out at the eyes and 9 minutes, respectively, and shown with transparent particles in the sheet 5 cm × 5 cm.
実施例１ 第１図に示す如く、伝熱面積が５m2の還流凝縮器（２）
を付設した内容積が１．７m3の重合機（１）に、水１０
０重量部（６２０kg）に部分鹸化ポリビニルアルコール
０．０７重量部を溶解して仕込み、重合開始剤ｔ−ブチ
ルパーオキシネオデカノエート０．０２５重量部及び
３，５，５−トリメチルヘキサノイルパーオキサイド
０．０３５重量部を添加して脱気し、塩化ビニル単量体
１００重量部（６２０kg）を仕込んだ。昇温して重合温
度を６５℃とし、昇温開始後１時間目に還流凝縮器
（２）の運転を開始し還流凝縮器（２）での除熱速度を
２５，０００kcal／Hrとした。重合転化率が４５％に到
達した時点で、還流凝縮器（２）からの液化単量体の回
収を開始し、総量３０重量部を回収槽（３）に回収し
た。その後、重合転化率が５５％に到達した時に、該液
化単量体の全量をポンプ（４）を用いて、重合機（１）
へ還流させた。重合機内圧力が定常圧より１kg／cm2低
下した時に、未重合単量体をその自圧によって重合系外
へ抜き出して重合を終了させた。重合転化率は７５％で
あった。Example 1 As shown in FIG. 1, a reflux condenser (2) having a heat transfer area of 5 m 2
In a polymerization machine (1) with an internal volume of 1.7 m 3 equipped with a
0.07 part by weight of partially saponified polyvinyl alcohol was dissolved in 0 part by weight (620 kg) and charged, and 0.025 part by weight of a polymerization initiator t-butylperoxy neodecanoate and 3,5,5-trimethylhexanoylper were added. 0.035 parts by weight of oxide was added and degassed, and 100 parts by weight (620 kg) of a vinyl chloride monomer was charged. The temperature was raised to a polymerization temperature of 65 ° C., and the reflux condenser (2) was started 1 hour after the start of the temperature rise, and the heat removal rate in the reflux condenser (2) was set to 25,000 kcal / Hr. When the polymerization conversion rate reached 45%, recovery of the liquefied monomer from the reflux condenser (2) was started, and a total amount of 30 parts by weight was recovered in the recovery tank (3). Then, when the polymerization conversion rate reached 55%, the entire amount of the liquefied monomer was transferred to the polymerization machine (1) using the pump (4).
Refluxed to. When the pressure inside the polymerizer decreased by 1 kg / cm 2 from the steady pressure, the unpolymerized monomer was taken out of the polymerization system by its own pressure to terminate the polymerization. The polymerization conversion rate was 75%.
尚、重合開始時の水／モノマー比は１．０であったが、
重合温度のコントロールを容易にするために、未重合単
量体の重合系外への抜き出し開始時に、これが１．２に
なるように重合期間中定量ポンプを用いて水を等速度で
連続的に追加した。Although the water / monomer ratio at the start of polymerization was 1.0,
In order to facilitate control of the polymerization temperature, at the start of withdrawing the unpolymerized monomer from the polymerization system, water was continuously fed at a constant rate using a metering pump during the polymerization period so that it was 1.2. Added.
得られたＰＶＣの物性を第１表に示す。表から明らかな
如く、得られたＰＶＣはポロシティーが高く、残存モノ
マーが少なく、かつフィッシュ・アイが少ない非常に良
好な品質のものであった。The physical properties of the obtained PVC are shown in Table 1. As is clear from the table, the obtained PVC was of very good quality with high porosity, low residual monomers and low fish eyes.
実施例２ 実施例１において、液化単量体の回収量を１５重量部に
変更した他は、実施例１に準じて重合を行った。Example 2 Polymerization was carried out in the same manner as in Example 1 except that the recovery amount of the liquefied monomer was changed to 15 parts by weight.
得られたＰＶＣは、第１表に示す如く、ポロシティー、
残存モノマー、フィッシュ・アイ共に良好なものであっ
た。The obtained PVC has porosity, as shown in Table 1.
The residual monomer and fish eye were good.
実施例３ 実施例１において、液化単量体の回収槽への回収開始時
点及び回収単量体の重合機への還流開始時点を第１表の
如く変更した他は、実施例１に準じて重合を行った。Example 3 According to Example 1, except that the start point of recovery of the liquefied monomer to the recovery tank and the start point of reflux of the recovered monomer to the polymerization machine were changed as shown in Table 1. Polymerization was carried out.
得られたＰＶＣは、第１表に示した如く、ポロシティ
ー、残存モノマー、フィッシュ・アイ共に良好なもので
あった。As shown in Table 1, the obtained PVC was good in porosity, residual monomer, and fish eye.
比較例１ 実施例１において、液化単量体を回収槽へ回収すること
なく、全重合期間を通じて、重合機へ還流させた他は、
実施例１に準じて重合を行った。Comparative Example 1 In Example 1, except that the liquefied monomer was refluxed to the polymerization machine throughout the entire polymerization period without being recovered in the recovery tank.
Polymerization was carried out according to Example 1.
得られたＰＶＣは、第１表に示す如く、ポロシティーは
低く、残存モノマー、フィッシュ・アイ共に満足できな
いものであった。As shown in Table 1, the obtained PVC had a low porosity, and the residual monomer and fish eyes were unsatisfactory.
第１図は本発明に用いられる重合装置の一例を示す概要
図である。 １・・・重合機 ２・・・還流凝縮器 ３・・・回収槽 ４・・・ポンプFIG. 1 is a schematic diagram showing an example of a polymerization apparatus used in the present invention. 1 ... Polymerizer 2 ... Reflux condenser 3 ... Recovery tank 4 ... Pump
Claims (3)
て塩化ビニル単量体又はこれと共重合し得る他の単量体
との混合物を懸濁重合するに際し、還流凝縮器から重合
機へ還流する液化単量体を還流凝縮器と重合機の間に設
けた回収槽に重合中一時的に回収し、その後回収単量体
の全量又はその一部を重合機に還流させ重合することを
特徴とする塩化ビニル系樹脂の製造方法。1. When carrying out suspension polymerization of a vinyl chloride monomer or a mixture thereof with another monomer copolymerizable with a vinyl chloride monomer using a polymerization machine equipped with a reflux condenser outside the machine, The liquefied monomer refluxed to the polymerization machine is temporarily collected during the polymerization in a collection tank provided between the reflux condenser and the polymerization machine, and then all or a part of the recovered monomer is refluxed to the polymerization machine to carry out the polymerization. A method for producing a vinyl chloride resin, comprising:
化率（仕込単量体に対する生成重合体の重量比率）が２
０〜６０％の時点とし、回収単量体の重合機への還流開
始を重合転化率（仕込単量体に対する生成重合体の重量
比率）が４０〜７０％の時点とする請求項１記載の製造
方法。2. The start of recovery of the liquefied monomer into the recovery tank is set at a polymerization conversion ratio (weight ratio of the produced polymer to the charged monomer) of 2.
The time point of 0 to 60%, and the start of the reflux of the recovered monomer to the polymerization machine is the time point of the polymerization conversion rate (weight ratio of the produced polymer to the charged monomer) of 40 to 70%. Production method.
始時の重合機中の仕込単量体１００重量部に対して、５
〜５０重量部である請求項１記載の製造方法。3. The recovery amount of the liquefied monomer in the recovery tank is 5 with respect to 100 parts by weight of the charged monomer in the polymerization machine at the start of the polymerization.
The manufacturing method according to claim 1, wherein the amount is 50 parts by weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7984388A JPH066605B2 (en) | 1988-03-30 | 1988-03-30 | Method for producing vinyl chloride resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7984388A JPH066605B2 (en) | 1988-03-30 | 1988-03-30 | Method for producing vinyl chloride resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01249813A JPH01249813A (en) | 1989-10-05 |
| JPH066605B2 true JPH066605B2 (en) | 1994-01-26 |
Family
ID=13701486
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7984388A Expired - Lifetime JPH066605B2 (en) | 1988-03-30 | 1988-03-30 | Method for producing vinyl chloride resin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH066605B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5807934A (en) * | 1995-09-19 | 1998-09-15 | Shin-Etsu Chemical Co., Ltd. | Method of removing foam during polymerization of vinyl chloride polymers |
| JP5650915B2 (en) * | 2009-12-18 | 2015-01-07 | 積水化学工業株式会社 | Method for producing vinyl chloride hollow particles, vinyl chloride hollow particles, vinyl chloride resin composition, and vinyl chloride molded article |
| CN116078308B (en) * | 2023-02-20 | 2024-06-21 | 河北国超热力工程有限公司 | Intelligent control method for reflux condenser at top of chloroethylene suspension polymerization kettle |
-
1988
- 1988-03-30 JP JP7984388A patent/JPH066605B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01249813A (en) | 1989-10-05 |
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