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JPS6020404B2 - Method for removing vinyl chloride monomer remaining in polymer - Google Patents
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JPS6020404B2 - Method for removing vinyl chloride monomer remaining in polymer - Google Patents

Method for removing vinyl chloride monomer remaining in polymer

Info

Publication number
JPS6020404B2
JPS6020404B2 JP13845874A JP13845874A JPS6020404B2 JP S6020404 B2 JPS6020404 B2 JP S6020404B2 JP 13845874 A JP13845874 A JP 13845874A JP 13845874 A JP13845874 A JP 13845874A JP S6020404 B2 JPS6020404 B2 JP S6020404B2
Authority
JP
Japan
Prior art keywords
polymer
vinyl chloride
vcm
slurry
chloride monomer
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.)
Expired
Application number
JP13845874A
Other languages
Japanese (ja)
Other versions
JPS5165188A (en
Inventor
峰雄 永野
道生 斉藤
広 金子
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.)
Tosoh Corp
Original Assignee
Toyo Soda Manufacturing Co Ltd
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 Toyo Soda Manufacturing Co Ltd filed Critical Toyo Soda Manufacturing Co Ltd
Priority to JP13845874A priority Critical patent/JPS6020404B2/en
Publication of JPS5165188A publication Critical patent/JPS5165188A/en
Publication of JPS6020404B2 publication Critical patent/JPS6020404B2/en
Expired legal-status Critical Current

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  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Description

【発明の詳細な説明】 本発明は塩化ピニル単量体(以下VCMと云う)の除去
回収方法に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for removing and recovering pinyl chloride monomer (hereinafter referred to as VCM).

さらに詳しくは重合後の塩化ビニル重合体または塩化ビ
ニル系共重合体(以下重合体と云う)に付着残存するV
CMを重合体から除去し回収する方法に関する。
More specifically, V remaining attached to vinyl chloride polymer or vinyl chloride copolymer (hereinafter referred to as polymer) after polymerization
The present invention relates to a method for removing and recovering CM from a polymer.

近年VCMの毒性が問題となりつつある。In recent years, the toxicity of VCM has become a problem.

したがって塩化ビニルを取扱う場所等での環境汚染を防
止する上から工程を密閉系として、工程から排出される
VCMの大気中への逸散を極力少なくしたり、また重合
体中へのVCMの残存を可能なかぎり少なくする努力が
なされている。しかしながら従来、重合後未反応VCM
を回収した後なおかつ重合体に付着残存するVCMを、
効率良く除去回収することは困難であった。このような
VCMの除去回収方法として、重合体を加熱しこれに付
着残存するVCMの蒸気圧を高め樽散しやすくして除去
する方法がある。
Therefore, in order to prevent environmental pollution in places where vinyl chloride is handled, the process should be made into a closed system to minimize the escape of VCM emitted from the process into the atmosphere, and to prevent VCM from remaining in the polymer. Efforts are being made to reduce this as much as possible. However, conventionally, unreacted VCM after polymerization
VCM that still remains attached to the polymer after being collected is
It has been difficult to remove and recover efficiently. As a method for removing and recovering such VCM, there is a method in which the polymer is heated to increase the vapor pressure of the VCM remaining attached to the polymer, thereby making it easier to disperse the VCM and removing it.

しかしこの方法は加熱による重合体の変質をもたらし、
この重合体を加工するさし、初期着色、熱安定性、フィ
ッシュアィ特性等諸特性を低下させるので好ましくない
。また重合体を減圧系に保ってVCMを除去回収する方
法がある。
However, this method results in deterioration of the polymer due to heating,
This is not preferable since it deteriorates various properties such as initial coloration, thermal stability, and fish eye properties during processing of this polymer. There is also a method of removing and recovering VCM by keeping the polymer in a reduced pressure system.

この方法も必要充分な減圧度を保つには装置上限界があ
り、また、例えば懸濁重合法で得た重合体スラリ−を処
理する場合は共存する水分をも同時に蒸発させるので効
率が悪い。本発明者らは重合体に付着するVCMを除去
回収する方法につき種々検討した結果、重合後の重合体
スラリーを減圧系内で薄膜状に又は飛沫状に飛散させる
ことにより効率よく重合体に付着したVCMを除去でき
ることを見出し本発明を完成した。すなわち本発明は重
合体スラリーを常圧又は減圧下の分散槽内の回転翼に接
触させて薄膜状および/又は飛沫状に分散させることを
特徴とする重合体中に残存する塩化ビニル単量体の除去
方法を要旨とするものである。
This method also has equipment limitations in maintaining a necessary and sufficient degree of vacuum, and when treating a polymer slurry obtained by suspension polymerization, for example, coexisting water is evaporated at the same time, making it inefficient. The present inventors investigated various methods for removing and recovering VCM adhering to polymers, and found that by scattering the polymer slurry after polymerization in a reduced pressure system in the form of a thin film or in the form of droplets, VCM adheres to the polymer efficiently. The present invention was completed by discovering that VCM can be removed. That is, the present invention is characterized in that the vinyl chloride monomer remaining in the polymer is dispersed in the form of a thin film and/or droplets by bringing the polymer slurry into contact with a rotary blade in a dispersion tank under normal pressure or reduced pressure. The purpose of this article is to explain how to remove .

本発明の一実施例態様を図面により詳述する。An embodiment of the present invention will be explained in detail with reference to the drawings.

第1図においてスラリー取入口1から減圧系に保たれた
分散槽4に重合体スラリーを導入しモーター3によって
回転する回転翼を介して、その遠心力によりスラリ−を
回転翼面および回転翼間に移行させ、スラリーを薄膜状
および/又は飛沫状として飛散させる。回転翼はスラリ
ーが充分薄膜状となるか又は飛沫分散するに充分な遠心
力を与える程度に回転させる。通常500〜2000R
pmの速度で回転させることが好ましい。薄膜状又は飛
沫状となって回転翼から飛散した重合体スラリーは分散
槽の壁面に衝突し更に薄膜状となる。
In Fig. 1, a polymer slurry is introduced from a slurry intake port 1 into a dispersion tank 4 maintained in a reduced pressure system, and the centrifugal force causes the slurry to be transferred between the rotary blade surface and between the rotary blades via a rotary blade rotated by a motor 3. The slurry is dispersed in the form of a thin film and/or droplets. The rotor is rotated to the extent that the slurry becomes a sufficiently thin film or provides sufficient centrifugal force to disperse the slurry into droplets. Usually 500~2000R
Preferably, the rotation is performed at a speed of pm. The polymer slurry scattered from the rotor in the form of a thin film or droplets collides with the wall surface of the dispersion tank and becomes further into a thin film.

この間に重合体中に付着残存するVCMは気相に移行し
VCM減圧吸引口を経てVCM回収槽に回収される。V
CMを除去した重合体スラリーを、前記したスラリー取
入口に再度循環させ前記回転翼を通過させることにより
、より効果的にVCMを除去することができる。また、
重合体スラリ−を水蒸気と接触させながら又は重合体の
品質低下を起さない程度に加熱することにより、VCM
除去の効率を高めることができる。
During this time, the VCM remaining attached to the polymer moves to the gas phase and is recovered into the VCM recovery tank via the VCM vacuum suction port. V
VCM can be removed more effectively by circulating the polymer slurry from which CM has been removed again through the slurry intake port and passing through the rotary blade. Also,
VCM is produced by heating the polymer slurry while contacting it with water vapor or to an extent that does not cause deterioration of the quality of the polymer.
Removal efficiency can be increased.

これらは併用することもでき、例えば重合体スラリーを
循環させる際に行うことが好ましい。本発明で処理しう
る重合体は通常の重合方法で得る塩化ビニル単独重合体
又は共重合体のスラリーである。本発明は塩化ビニル又
は塩化ビニル系の重合体中に残存する単量体を効率良く
除去することができる。
These can also be used in combination, and it is preferable to use them, for example, when circulating the polymer slurry. The polymer that can be treated in the present invention is a vinyl chloride homopolymer or copolymer slurry obtained by conventional polymerization methods. The present invention can efficiently remove monomers remaining in vinyl chloride or vinyl chloride-based polymers.

本発明の方法で処理した重合体を用いて加工した加工品
は良好な性質を有する。
Processed products using polymers treated with the method of the invention have good properties.

次に実施例で本発明を詳細に説明する。Next, the present invention will be explained in detail with reference to Examples.

実施例 1 回分式重合缶で、塩化ビニルを平均重合度1000にな
るまで重合した後重合物を60℃に保ち、重合缶内圧を
lk9/地まで減圧して未反応塩化ビニル単量体を回収
した。
Example 1 In a batch polymerization reactor, vinyl chloride was polymerized until the average degree of polymerization reached 1000, and then the polymerized product was maintained at 60°C and the internal pressure of the polymerization reactor was reduced to lk9/kg to recover unreacted vinyl chloride monomer. did.

重合物は蝿洋装暦付ブローダウンタンクに移し、ブロー
ダウンタンク底部から、密閉節を通して、ブローダウン
タンクの上部に設置した、一0.3〜0.8k9/c紬
こ減圧吸引している分散槽にスラリーポンプを介して送
り、分散槽内で高速回転している分散槽に接触させた。
The polymerized material was transferred to a blowdown tank equipped with an air conditioner, and a 10.3 to 0.8 k9/c tsumugi vacuum suction was carried out from the bottom of the blowdown tank through a sealed joint. The slurry was sent to the tank via a slurry pump and brought into contact with a dispersion tank rotating at high speed within the dispersion tank.

このさし、重合体から除去された塩化ビニル単量体は減
圧吸引口より回収した。また塩化ビニル単量体を除去し
た重合体スラリーはブローダウンタンクにもどした。
The vinyl chloride monomer removed from the polymer was recovered from the vacuum suction port. The polymer slurry from which the vinyl chloride monomer was removed was returned to the blowdown tank.

またさらに、重合体スラリーは前記した循環系を循環さ
せた。2時間循環させた後重合体中の単量体濃度は65
0功風から100瓜伽こ減少した。
Furthermore, the polymer slurry was circulated through the circulation system described above. After 2 hours of circulation, the monomer concentration in the polymer was 65
100 urigako decreased from 0 gofu.

処理後の重合体は通常の方法で乾燥し次の配合および条
件で加工した。
The treated polymer was dried in a conventional manner and processed under the following formulation and conditions.

結果を第1表に示す。The results are shown in Table 1.

配合条件 重合体 150夕 錫系安定剤(N−200肥) 3夕 〃 (E−101) 3タ 加工条件 ロール温度 1560取出し厚さ
lm/仇 加 圧 175o01正け実施
例 2分散槽入口で、重合体スラリーを80ooに加熱
した以外は実施例1に準じて処理したところ重合体中の
VCMは30Q側‘こ減少した。
Compounding conditions Polymer 150% Tin stabilizer (N-200 fertilizer) 3% (E-101) 3% Processing conditions Roll temperature 1560 Take-out thickness
1m/d Pressure 175o01 Correct Example 2 The procedure of Example 1 was followed except that the polymer slurry was heated to 800°C at the inlet of the dispersion tank, and the VCM in the polymer was reduced by 30Q.

また、実施例1に準じて重合体を加工した。結果を第1
表に示す。実施例 3分散槽入口で重合体スラリーを8
0qoに加熱しさらに水蒸気を吹込んだ以外は実施例1
に準じて処理したところ重合体中のVCMは150柳に
減少した。
Further, the polymer was processed according to Example 1. Results first
Shown in the table. Example 3 At the inlet of the dispersion tank, the polymer slurry was
Example 1 except that it was heated to 0qo and further steam was blown into it.
When the polymer was treated according to the same procedure, the VCM in the polymer was reduced to 150 Yanagi.

また実施例1に準じて重合体を加工した。Further, the polymer was processed according to Example 1.

結果を第1表に示す。実施例 4 約5重量%酢酸ビニルを含む塩化ビニルー酢酸ビニル共
重合体スラリーを実施例1に準じて処理したところ重合
体中の単量体濃度は6150脚から75の肌こ減少した
The results are shown in Table 1. Example 4 When a vinyl chloride-vinyl acetate copolymer slurry containing about 5% by weight of vinyl acetate was treated according to Example 1, the monomer concentration in the polymer was reduced by 75 points from 6150 points.

実施例 5 約10重量%のエチレン一酢酸ピニル共重合体(酢酸ビ
ニル含量26%)と塩化ビニルとのグラフト共重合体ス
ラリ−を実施例1に準じて処理したところ重合体中の塩
化ピニル単量体濃度は560助風から60の伽こ減少し
た。
Example 5 When a graft copolymer slurry of about 10% by weight of ethylene monoacetate pinyl copolymer (vinyl acetate content 26%) and vinyl chloride was treated according to Example 1, the pinyl chloride monopolymer in the polymer was removed. The mass concentration decreased from 560 to 60.

比較例 1 重合体スラリーは分散槽を通さず、ブローダウンタンク
のみで60午○、一0.3〜0.8kg/ので2時間減
圧吸引した以外は実施例1に準じて処理したところ重合
体中のVCM濃度は500■奴となった。
Comparative Example 1 The polymer slurry was treated in the same manner as in Example 1 except that it was not passed through a dispersion tank and was sucked under reduced pressure for 2 hours using only a blowdown tank at 60 pm at 0.3 to 0.8 kg/kg. The VCM concentration inside was 500cm.

比較例 2フローダウンタンクでの重合体スラリー温度
を7ぴ0とした以外は比較例1に準じて処理したところ
、重合体中のVCM濃度は350瓜血となった。
Comparative Example 2 The procedure of Comparative Example 1 was followed except that the temperature of the polymer slurry in the flow down tank was set at 7.0 psi, and the VCM concentration in the polymer was 350 psi.

また実験例1に準じて重合体を加工した。結果を第1表
に示す。比較例 3 比較例2において温度を80qCとした以外は比較*例
2に準じて処理したところ重合体中のVCM濃度は30
0の血となった。
Further, the polymer was processed according to Experimental Example 1. The results are shown in Table 1. Comparative Example 3 When treated according to Comparative Example 2 except that the temperature was 80 qC in Comparative Example 2, the VCM concentration in the polymer was 30 qC.
It became 0 blood.

また実験例1に準じて重合体を加工した。結果を第1表
に示す。第1表 ※ 熱安定性試験は1孫のロールシ−トを180℃,9
0分間処理して行ったo※※ フィンシュァィ個数はシ
−ト25の中に存在する個数である。
Further, the polymer was processed according to Experimental Example 1. The results are shown in Table 1. Table 1 * Thermal stability test was performed using a roll sheet of 1st grade at 180℃, 9
The number of o** fins that are processed for 0 minutes is the number that exists in the sheet 25.

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

第1図は、重合体スラリーを薄膜状および/又は飛沫状
に飛散させる装置の一例で、その縦断面図を示す。 図中1は重合体スラリ−取入口、2は回転翼、3は回転
翼を回転させるモーター、4は分散槽、5は重合体スラ
リー出口、6はVCM減圧吸引口である。 第1図
FIG. 1 shows a longitudinal cross-sectional view of an example of an apparatus for scattering polymer slurry in the form of a thin film and/or droplets. In the figure, 1 is a polymer slurry inlet, 2 is a rotor, 3 is a motor for rotating the rotor, 4 is a dispersion tank, 5 is a polymer slurry outlet, and 6 is a VCM vacuum suction port. Figure 1

Claims (1)

【特許請求の範囲】[Claims] 1 塩化ビニル重合体又は塩化ビニル系共重合体スラリ
ーを常圧又は減圧下の分散槽内の回転翼に接触させて薄
膜状および/又は飛沫状に分散させることを特徴とする
重合体中に残存する塩化ビニル単量体の除去方法。
1 Residual in a polymer characterized by dispersing a vinyl chloride polymer or a vinyl chloride copolymer slurry into a thin film and/or droplet by contacting it with a rotary blade in a dispersion tank under normal pressure or reduced pressure. A method for removing vinyl chloride monomer.
JP13845874A 1974-12-04 1974-12-04 Method for removing vinyl chloride monomer remaining in polymer Expired JPS6020404B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13845874A JPS6020404B2 (en) 1974-12-04 1974-12-04 Method for removing vinyl chloride monomer remaining in polymer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13845874A JPS6020404B2 (en) 1974-12-04 1974-12-04 Method for removing vinyl chloride monomer remaining in polymer

Publications (2)

Publication Number Publication Date
JPS5165188A JPS5165188A (en) 1976-06-05
JPS6020404B2 true JPS6020404B2 (en) 1985-05-22

Family

ID=15222478

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13845874A Expired JPS6020404B2 (en) 1974-12-04 1974-12-04 Method for removing vinyl chloride monomer remaining in polymer

Country Status (1)

Country Link
JP (1) JPS6020404B2 (en)

Also Published As

Publication number Publication date
JPS5165188A (en) 1976-06-05

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