JPS59126411A - After-treatment of styrene polymerization product - Google Patents
After-treatment of styrene polymerization productInfo
- Publication number
- JPS59126411A JPS59126411A JP112583A JP112583A JPS59126411A JP S59126411 A JPS59126411 A JP S59126411A JP 112583 A JP112583 A JP 112583A JP 112583 A JP112583 A JP 112583A JP S59126411 A JPS59126411 A JP S59126411A
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- Japan
- Prior art keywords
- stirring
- degassing section
- polymerization reaction
- content
- styrene
- 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.)
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- Graft Or Block Polymers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Description
【発明の詳細な説明】
本発明はスチレン系重合反応物の後処理方法に関し、詳
しくは２段階による脱気処理を行なうスチレン系重合反
応物の後処理方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for post-treatment of a styrenic polymerization reaction product, and more particularly to a method for post-treatment of a styrene-based polymerization reaction product that performs a two-step degassing treatment.
スチレン系重合体は、その重合体中に未反応物や溶剤等
が残存していると、抜形時に焼けが発生したり、成形品
の外観不良（シルバー、フラッシュ）を起こし、成形品
の物性を著しく低下させるという欠点がある。そこで、
これら未反応物や溶剤等を該重合体から分離する方法が
種々検討されており、たとえば特公昭５６−３’９６５
５号、特開昭５３−４０８９号などに開示されている。If unreacted substances or solvents remain in the styrene-based polymer, it may cause burns during molding or poor appearance of the molded product (silver, flash), and the physical properties of the molded product may deteriorate. The disadvantage is that it significantly reduces the Therefore,
Various methods have been studied to separate these unreacted substances, solvents, etc. from the polymer.
No. 5, Japanese Patent Application Laid-Open No. 53-4089, etc.
しかしながら、未反応モノマーの含有量や溶剤の量が多
い場合、これらの方法では脱気に相当の負荷がかかり、
しかもこれら未反応物や溶剤等を所定量脱気するまでに
スチレン系重合体を長時間高温かつ高剪断下に保持する
必要がある。そのため、生産効率が悪く、かつ滞留によ
り該重合体は熱劣化し、物性が低下するという欠点があ
った。However, when the content of unreacted monomers or the amount of solvent is large, these methods impose a considerable burden on degassing.
Moreover, it is necessary to hold the styrenic polymer at high temperature and under high shear for a long period of time until a predetermined amount of these unreacted substances, solvent, etc. are degassed. Therefore, the production efficiency is poor, and the polymer is thermally degraded due to stagnation, resulting in a decrease in physical properties.
本発明は、上記のような欠点を解消したスチレン系重合
反応物の後処理方法の提供を目的としており、未反応物
や溶剤等の含有量が少なく、かつ熱劣化を防止して物性
、特に耐衝撃性に優れたスチレン系重合体を与える後処
理方法である。The present invention aims to provide a post-treatment method for styrenic polymerization reactants which eliminates the above-mentioned drawbacks, and which reduces the content of unreacted substances and solvents, prevents thermal deterioration, and improves physical properties, especially This is a post-treatment method that provides a styrenic polymer with excellent impact resistance.
本発明は、重合反応終了後のスチレン系重合反応物から
未反応物や溶剤等を除去する後処理方法において、加熱
機構を有し、さらに複数本の回転軸のそれぞれに少なく
とも２個の攪拌翼を固着し気部にスチレン系重合反応物
を順次導入すると共に、該第１脱気部と第２鋭気部のい
ずれ・か一方もしくは両者に酸化防止剤゛を供給するむ
とによって前記スチレン系重合反応物と接触させ、かつ
第１脱気部においては温度１５０〜３００℃、圧力０．
１〜６００トルの条件で攪拌を行ない未反応物や溶剤等
をスチレン系重合体中の含有率が０．５〜５０重量ヂに
なるまで脱気し、次の第２脱気部においては温度２００
〜３００°Ｃ１圧力５０トル以下の条件で攪拌を行ない
未反応物や溶剤等のスチレン系重合体中の含有率が１重
量％以下となるように未反応物や溶剤等を除去すること
を特徴とするスチレン系重合反応物の後処理方法である
。The present invention provides a post-treatment method for removing unreacted substances, solvents, etc. from a styrene-based polymerization reaction product after completion of a polymerization reaction, which includes a heating mechanism and further includes at least two stirring blades on each of a plurality of rotating shafts. The styrene-based polymerization reaction is carried out by fixing the styrene-based polymerization reaction product into the gas section and supplying an antioxidant to either or both of the first degassing section and the second degassing section. In the first degassing section, the temperature is 150 to 300°C and the pressure is 0.
Stirring is performed under conditions of 1 to 600 torr to degas unreacted substances and solvents until the content in the styrene polymer becomes 0.5 to 50 wt. In the next second degassing section, the temperature is 200
It is characterized by stirring at ~300°C and a pressure of 50 torr or less to remove unreacted substances and solvents so that the content of such substances in the styrenic polymer is 1% by weight or less. This is a method for post-treatment of styrenic polymerization reaction products.
本発明の方法が適用されるスチレン系重合反応物には制
限がなく、スチレン、ビニルトルエン。The styrenic polymerization reactant to which the method of the present invention is applied is not limited, and includes styrene and vinyltoluene.
α−メチルスチレンなどのスチレン系モノマーの単独重
合物や共重合物のほかスチレン系モノマーとアクリロニ
トリル、アクリル酸メチル、メタアクリル酸メチルなど
のモノマーとの共重合物やスチレン系モノマーと共重合
可能なゴム状物との共重合体などがあり、塊状重合、溶
液重合などによって得られる重合反応物について後処理
、を行なう。In addition to homopolymers and copolymers of styrene monomers such as α-methylstyrene, copolymers of styrene monomers with monomers such as acrylonitrile, methyl acrylate, and methyl methacrylate, and copolymers with styrene monomers are possible. There are copolymers with rubber-like materials, etc., and post-treatment is performed on polymerization reaction products obtained by bulk polymerization, solution polymerization, etc.
本発明は後処理を２段階に分けて行なうことに特色があ
り、第１図は本発明の方法のフローについて概略を説明
したものである。The present invention is characterized in that the post-processing is carried out in two stages, and FIG. 1 schematically explains the flow of the method of the present invention.
本発明における第１脱気部Ｂは第１図に示しだ如上外形
が筒状体の装置からなり、該筒状体１は二重壁構造とな
っており、壁間にスチーム捷たは熱媒体油を通して加熱
し、スチレン系重合体を加熱すると共に、脱気工程での
揮発物の露点温度以上に加熱する加熱機構２を有してい
る。また、該筒状体には平行に設けられた複数本の回転
軸３゜３′があり、この回転軸のそれぞれに少なくとも
２個の攪拌翼４を固着してあり、攪拌翼は通常、図示し
た如く一方の回転軸と他方の回転軸に適当な間隔をあけ
て設ける。回転軸の回転方向は交互に逆回転とすること
が好ましい。まだ、必要に応じて回転軸内に加熱手段を
設けることもできる。攪拌翼は、前記したように少なく
とも２個であり、一般的には２〜８個が適当である。偶
数個の場合は、回転軸を中心に対称形に設ける。なお、
攪拌翼は図示した如く回転軸に対向して相互、に１８０
度の位相角にて取付ける゛ほか、１２０度あるいは９０
度の位相角にて複数個取付けることもできる。The first degassing section B of the present invention is composed of a device having a cylindrical outer shape as shown in FIG. It has a heating mechanism 2 that heats the styrenic polymer by passing medium oil through it and heats it to a temperature higher than the dew point temperature of the volatiles in the degassing step. Further, the cylindrical body has a plurality of rotating shafts 3゜3' provided in parallel, and at least two stirring blades 4 are fixed to each of the rotating shafts, and the stirring blades are usually not shown in the figure. As described above, one rotating shaft and the other rotating shaft are provided with an appropriate distance between them. It is preferable that the rotating directions of the rotating shafts are alternately rotated in opposite directions. However, heating means may be provided within the rotating shaft if necessary. As mentioned above, there are at least two stirring blades, and generally two to eight stirring blades are appropriate. In the case of an even number, they are arranged symmetrically around the rotation axis. In addition,
As shown in the figure, the stirring blades are arranged 180 degrees opposite each other to the rotating shaft.
In addition to mounting at a phase angle of 120 degrees or 90 degrees,
Multiple units can be installed at a phase angle of degrees.
攪拌翼の形状は特に制限はガく、第２図ａ〜Ｃはその態
様を示したものである。この攪拌翼を膨出状にすると脱
気効果が向上し、また膨出した部分の中央近辺に透孔１
６を設けると脱気効果がさらに向上するばかりでなく、
動力を減少させることができる。攪拌翼４の先端には該
攪拌翼と直交するように剥離板１５を設けてあり、これ
により攪拌効果が犬となり、筒状体内部にデッドスペー
スが生じることを防止でき、かつスチレン系重合体の表
面更新効果を大きくすることができる。この剥離板は筒
状体の内壁に近接して設けることが好ましく、さらに剥
離板に透孔ぞ設けてもよい。There are no particular restrictions on the shape of the stirring blade, and FIGS. 2a to 2C show its embodiments. Making the stirring blades bulge improves the deaeration effect, and there is also a through hole near the center of the bulge.
6 not only further improves the degassing effect, but also
Power can be reduced. A peeling plate 15 is provided at the tip of the stirring blade 4 so as to be perpendicular to the stirring blade, which improves the stirring effect and prevents dead space from forming inside the cylindrical body. The surface renewal effect can be increased. This peeling plate is preferably provided close to the inner wall of the cylindrical body, and the peeling plate may also be provided with through holes.
上記第１脱気部Ｂにおいては、反応槽Ａからの粘稠なス
チレン系重合反応物を上部から供給し、液位を適宜調節
し１５０〜３００°Ｃ１好ましくは１５０〜２６０°Ｇ
の温度、０．１〜６００トル、好ましくは１００〜５０
０トル、さらに好ましくは１５０〜３５ｏトルの圧力の
条件で攪拌を行なうことによりスチレン系重合体中の未
反応物や溶剤等の含有率が０．５〜５０重量％、好まし
くは０．５〜３０重量％となるまで脱気する。こ＼で温
度が１５０℃未満ではスチレン反応物の粘度が上がシ高
負荷、高剪断になり好ましくない。一方、３００℃を超
えると解重合が起こり好ましくない。特に共重合物の場
合に架橋度が上がり耐衝撃性が低下し好ましくない。ま
た、圧力が０．１トル未満では、特に共重合物の場合、
ゴム分のサラミ構造の破壊を招き好ましくなく、６００
）ル全超、えると、脱気効率が落ち生産性が劣ることと
なる。第１脱気部における脱気処理を未反応物や溶剤等
の含有率が０．５重量％未満とすると、特に架橋反応が
進行し難くなシ耐衝撃性が低下する。一方、５０重量％
を超える脱気処理では架橋反応が過度に進行し、重合体
の物性低下をきたす。In the first degassing section B, the viscous styrene-based polymerization reaction product from the reaction tank A is supplied from the upper part, and the liquid level is appropriately adjusted to 150 to 300°C, preferably 150 to 260°G.
temperature, 0.1 to 600 torr, preferably 100 to 50
By stirring at a pressure of 0 torr, more preferably 150 to 35 torr, the content of unreacted substances, solvents, etc. in the styrenic polymer can be reduced to 0.5 to 50% by weight, preferably 0.5 to 35% by weight. Degas until it becomes 30% by weight. If the temperature is below 150°C, the viscosity of the styrene reactant increases, resulting in high load and high shear, which is not preferable. On the other hand, if the temperature exceeds 300°C, depolymerization occurs, which is not preferable. Particularly in the case of copolymers, the degree of crosslinking increases and impact resistance decreases, which is not preferable. Also, when the pressure is less than 0.1 torr, especially in the case of copolymers,
This is undesirable as it leads to the destruction of the salami structure of the rubber component.
) If the amount exceeds the total amount, the degassing efficiency will decrease and productivity will be poor. If the content of unreacted substances, solvent, etc. is less than 0.5% by weight in the degassing treatment in the first degassing section, the crosslinking reaction will be particularly difficult to proceed and the impact resistance will deteriorate. On the other hand, 50% by weight
If the degassing treatment exceeds 100%, the crosslinking reaction will proceed excessively, resulting in a decrease in the physical properties of the polymer.
次に、第２脱気部Ｃは第１図に示した如く縦型筒状の装
置からなり、剪断作用による加熱手段９と薄膜蒸発用攪
拌手段１ｏを備えたものであシ、具体的には特公昭４７
−１３０４１号、・特公昭５７−２２３２５号、特′開
昭５６−４５７０４号などに開示された遠心薄膜蒸発機
が好ましい。Next, the second degassing section C consists of a vertical cylindrical device as shown in FIG. is a special public official in Showa 47.
Centrifugal thin film evaporators disclosed in Japanese Patent Publication No. 13041, Japanese Patent Publication No. 57-22325, Japanese Patent Publication No. 45704/1988 are preferred.
上記第２脱気部Ｃにおいては、第１脱気部からのスチレ
ン系重合反応物を２００〜３００℃、好ましくは２１０
〜２８５℃の温度、５０トル以下、好ましくは１０トル
以下の圧力の条件で攪拌を行ない未反応物や溶剤等の含
有率が１重量係以下となるように脱気する。こ＼で温度
が２００℃未満ではスチレン系重合反応物の粘度が上昇
し脱気効率が低下する。一方、３００℃を超えると熱劣
化が生起するので好ましくない。また、圧力が５０トル
以上では未反応物や溶剤等の飽和濃度が増大し、そのだ
め脱気効果が低下し未反応物や溶剤等が残留することと
なる。この第一２脱気部において未反応物や溶剤等の含
有率が１重量％を超えるような脱気処理を行なうと、ス
チレン系重合体は残存する未反応物や溶剤等に起因して
ヤケ、外観不良（シルバー、フラッシュ）等を生じ、ま
た機械的物性も低下し好ましくない。In the second degassing section C, the styrene polymerization reaction product from the first degassing section is heated to a temperature of 200 to 300°C, preferably 210°C.
Stirring is carried out at a temperature of -285 DEG C. and a pressure of 50 Torr or less, preferably 10 Torr or less, and degassing is carried out so that the content of unreacted substances, solvent, etc. is 1 part by weight or less. If the temperature is below 200°C, the viscosity of the styrene polymerization reaction product will increase and the degassing efficiency will decrease. On the other hand, if the temperature exceeds 300°C, thermal deterioration will occur, which is not preferable. Furthermore, if the pressure is 50 torr or more, the saturation concentration of unreacted substances, solvent, etc. will increase, and as a result, the degassing effect will decrease, and unreacted substances, solvent, etc. will remain. If deaeration treatment is performed in this first and second degassing section in such a way that the content of unreacted substances, solvent, etc. This is undesirable because it causes poor appearance (silver, flash) and deteriorates mechanical properties.
本発明において上記第１脱気部と第２脱気部のいずれか
一方もしくは両者に加えてスチレン系重合反応物と接触
させる酸化防止剤は融点３５℃以上のものが好ましく、
特にフェノール系のものが好ましい。フェノール系酸化
防止剤を具体的に例示すると、４−ヒドロキシメチル−
２，６−シブチルフェノール、ｎ−オクタデシル−β−
（４’−ヒドロキシ−３’、５’−ジ−ｔ−ブチルフェ
ニル）プロピオネート、２−ｔ−ブチル−４−メＩ・キ
ンフェノール、２．６−ジーｔ−ブチル−４−メチルフ
ェノール、 ２ 、２’−メチレノビス（４−メグ−
ル−６−を−）゛チルフコニノール）、２，２′−メチ
レンビス（４−エチル−６−ｔ −ブチルフェノール）
、ビス（３−シクロへキシル−２−ヒドロキシ−５−メ
チルフェニル）メタン、ビス（３、３’−ビス（４′−
ヒドロキシ−３’−ｔ−ブチルフェニル）ブチリックア
シッド）グリコールエステル、４；４′−ブチリデンビ
ス（６−１−ブチル−ｍ−クレゾール）、４，４′−チ
オビス（３−メチル−６−１−ブチルフェノール）、１
．１．３−）リス（２−メチル−４−ヒドロキシ−５−
’、、ｔ・−ブチルフェニル）ブタン、１、−３．５’
−トリメチル−２゜４．６−）リス（３，５−ジ−ｔ−
ブチル−４−チレンー３− （３’ 、 ５’−ジ−ｔ
−ブチル−４−ヒドロキシフェニル）フロビオネートコ
メタン、２゜４．５−）リヒドロキシブチロフエノン、
ｐ−ｔ−プチルフェニルサリシレートなどがある。酸化
防止剤の添加量は樹脂溶融体１００重量部に対して０．
００５〜２．０重量部の範囲とすればよい。酸化防止剤
の第１脱気部と第２脱気部への供給比については特に制
限はないが、前者：後者＝１００〜２０：０〜８０の範
囲、好ましくは７０〜８０：２０〜３０の範囲で選択す
ることにより生産効率を高めることができる。In the present invention, the antioxidant that is brought into contact with the styrene polymerization reaction product in addition to one or both of the first degassing section and the second degassing section preferably has a melting point of 35° C. or higher,
Particularly preferred are phenolic ones. Specific examples of phenolic antioxidants include 4-hydroxymethyl-
2,6-sibutylphenol, n-octadecyl-β-
(4'-Hydroxy-3',5'-di-t-butylphenyl)propionate, 2-t-butyl-4-meI-quinphenol, 2.6-di-t-butyl-4-methylphenol, 2 , 2'-methylenobis (4-meg-
2,2'-methylenebis(4-ethyl-6-t-butylphenol)
, bis(3-cyclohexyl-2-hydroxy-5-methylphenyl)methane, bis(3,3'-bis(4'-
Hydroxy-3'-t-butylphenyl)butyric acid) glycol ester, 4;4'-butylidenebis(6-1-butyl-m-cresol), 4,4'-thiobis(3-methyl-6-1- butylphenol), 1
．． 1.3-) Lis(2-methyl-4-hydroxy-5-
',,t-butylphenyl)butane, 1,-3.5'
-trimethyl-2゜4.6-)lis(3,5-di-t-
Butyl-4-tyrene-3-(3', 5'-di-t
-butyl-4-hydroxyphenyl) flobionate comethane, 2゜4.5-)lyhydroxybutyrophenone,
Examples include pt-butylphenyl salicylate. The amount of antioxidant added is 0.00 parts by weight per 100 parts by weight of the resin melt.
The amount may be in the range of 0.005 to 2.0 parts by weight. There is no particular restriction on the supply ratio of the antioxidant to the first degassing section and the second degassing section, but the former: the latter = 100 to 20: 0 to 80, preferably 70 to 80: 20 to 30. Production efficiency can be increased by selecting within this range.
本発明ではスチレン系重合反応物からの脱気工程を２段
階としたことにより該重合反応物中の未反応物や溶剤等
の含有量に応じてスチレン系重合体を劣化させることな
く、シかも最適の運転条件を選択して効率よく生産する
ことができる。未反名物や溶剤等を多量に含むものにあ
っては第１脱気部において粗脱気し、第２脱気部におい
て精密脱気を行なうことによって未反応物や溶剤等を効
率よく、かつ精留することができる。また、酸化防止剤
を第１脱気部に導入すると攪拌手段によって該酸化防止
剤を重合反応物中に均一に分散させることが可能であシ
、スチレン系重合体の熱劣化を効果的に防止することが
できる。In the present invention, the degassing process from the styrene polymerization reaction product is carried out in two stages, so that the styrene polymer can be removed without deterioration depending on the content of unreacted substances, solvents, etc. in the polymerization reaction product. Efficient production can be achieved by selecting the optimal operating conditions. For unreacted products or materials containing a large amount of solvent, etc., unreacted materials and solvents can be removed efficiently and efficiently by performing rough deaeration in the first deaeration section and precise deaeration in the second deaeration section. Can be rectified. In addition, when the antioxidant is introduced into the first degassing section, the antioxidant can be uniformly dispersed in the polymerization reaction product by the stirring means, and the thermal deterioration of the styrenic polymer can be effectively prevented. can do.
なお、スチレン系重合体の製品中の揮発物（未反応物や
溶剤等）の許容濃度は０．１％以下であり、またアイゾ
ツト衝撃強度は８．０以上、Ｙｌ は２．５以下であ
ることが必要である。The permissible concentration of volatile substances (unreacted substances, solvents, etc.) in styrenic polymer products is 0.1% or less, and the Izot impact strength is 8.0 or more and Yl is 2.5 or less. It is necessary.
次に、本発明を実施例により説明する。Next, the present invention will be explained by examples.
実施例１〜１１
第１図に示した装置を用いて実施した。なお、第１脱気
部Ｂとして４０！容の筒状脱気装置で各回転軸（軸間距
離１１ｃｍ）には各々１０枚のひょうたん形の攪拌翼（
長径１５ｃｍ）を１０ｃｍ間隔で設け、かつ該攪拌翼の
先端には直立するように３０×２ｃｍの剥離板を設けた
ものを使用した。また、二蓋壁構造とした筒状脱気装置
の壁間、に・熱媒を循環させた。第２脱気部Ｃ゛として
１５．、ｅ３容の縦型筒状脱気装置で、供給口付近に直
径１５ｃｍ１長さ２０ｃｒｎの剪断加熱用ローターを取
付け、その下方に２枚の攪拌翼（５ｃＩｎＸ ４ ＱＣ
ｎ ）を有する薄膜蒸発用の攪拌手段を備えたものを使
用した。また、この装置にも第１脱気部と同様にジャケ
ットを装備し、熱媒を循環させた。Examples 1 to 11 Examples were carried out using the apparatus shown in FIG. In addition, the first degassing section B is 40! It is a cylindrical deaerator with 10 gourd-shaped stirring blades (
The stirring blades (long diameter 15 cm) were provided at 10 cm intervals, and a 30 x 2 cm peeling plate was provided at the tip of the stirring blade so as to stand upright. In addition, a heat medium was circulated between the walls of the cylindrical deaerator, which had a double-wall structure. 15. As the second degassing section C'. , e3 capacity vertical cylindrical deaerator, a shear heating rotor with a diameter of 15 cm and a length of 20 crn is installed near the supply port, and two stirring blades (5 cInX 4 QC
n) equipped with stirring means for thin film evaporation was used. Further, this device was also equipped with a jacket like the first degassing section, and the heat medium was circulated.
ポリブタジェン（ムーニー粘度３５（１００°Ｃ））を
スチレン単量体中に溶解し、下記の原料組成にて重合し
、樹脂溶融体とした。Polybutadiene (Mooney viscosity 35 (100°C)) was dissolved in styrene monomer and polymerized with the following raw material composition to obtain a resin melt.
スチレン単量体 ９・１部
ポリブタジェン ６部
エチルベンゼン ３部
得られた樹脂溶融体には未反応のスチレン単量体１５重
量係、エチルベンゼン３重量％が含まれていた。この樹
脂溶融体を前記第１脱気部および第２脱気部に表示した
条件にて通して後処理を行なった。Styrene monomer 9.1 parts Polybutadiene 6 parts Ethylbenzene 3 parts The resulting resin melt contained 15% by weight of unreacted styrene monomer and 3% by weight of ethylbenzene. This resin melt was passed through the first degassing section and the second degassing section under the indicated conditions for post-treatment.
得られたスチレン系重合体の性状を脱気条件と共に第１
表に示す。The properties of the obtained styrenic polymer were evaluated in the first step along with the degassing conditions.
Shown in the table.
比較例１〜８
脱気条２件を変更したこと以外は実施例に準じて行なっ
た。結果を第１表に示す。Comparative Examples 1 to 8 Comparative Examples 1 to 8 were carried out according to the examples except that two degassing conditions were changed. The results are shown in Table 1.
＊Ｉ ＪＩＳＫ−７１１０
＊２ 酸化防止剤は樹脂溶融体１００重量部に所定量を
１０倍量のベンゼンで溶解して添加した。*I JISK-7110 *2 A predetermined amount of the antioxidant was dissolved in 10 times the amount of benzene and added to 100 parts by weight of the resin melt.
Ａ： ４−ヒドロキシメチル２，６−シブチルフェノー
ル
Ｂ： ｎ−オクタデシル−β−（４′−ヒドロキシ−３
’、 ５’−）−ｔ −フｆルフェニルグロピオネートA: 4-hydroxymethyl 2,6-sibutylphenol B: n-octadecyl-β-(4'-hydroxy-3
', 5'-)-t-fluorophenylgropionate
第１図は本発明の方法のフローの概略を示す説明図、第
２図ａ −ｃは本発明−の方法に用いる攪拌翼の態様の
正面図である。
Ａ・・・・・・反応槽、Ｂ・・・・・・・・・第１脱気
部、Ｃ・・・・・・・・第２脱気部、１−・・・・・・
・・・筒状体、２・・・・・・・・加熱機構、３，３′
・・・・・回転軸、４ ・・・・・・・攪拌翼、５・・
・・−・供給口、６・−・・・・排出口、７ ・・・・
・脱気口、８・・−・・・ ポンフ０．９ ・・・・
・・剪断加熱用ローター、１０ ・ ・薄膜蒸発用攪拌
手段、１１・・・・・・・・軸封装置、１２・・・・
七−ター、１３・・・・供給口、１４ ・ 排出ｌコ
、１５・・・・・・・・剥離板、１６・・・・・−・透
孔。FIG. 1 is an explanatory diagram showing an outline of the flow of the method of the present invention, and FIGS. 2 a to 2 c are front views of embodiments of stirring blades used in the method of the present invention. A...Reaction tank, B...First degassing section, C...Second degassing section, 1-...
...Cylindrical body, 2...Heating mechanism, 3, 3'
... Rotating shaft, 4 ... Stirring blade, 5 ...
...--Supply port, 6...-Discharge port, 7...
・Deaeration port, 8... Pump 0.9...
... Rotor for shear heating, 10 ... Stirring means for thin film evaporation, 11 ... ... Shaft sealing device, 12 ...
7-ter, 13...supply port, 14/discharge port, 15...peeling plate, 16...through hole.
Claims (1)
応物や溶剤等を除去する後処理方法において、加熱機構
を有し、さらに複数本の回転軸のそれぞれに少なくとも
２個の攪拌翼を固着した攪拌機構を備えた第１脱気部お
よび剪断作用による加熱手段と薄膜蒸発用攪拌手段を備
えた第２脱気部にスチレン系重合反応物を順次導入する
と共に、該第１脱気部と第２脱気部のいずれか一方もし
くは両者に酸化防止剤を供給することによって前記スチ
レン系重合反応物と接触させ、かつ第１脱気部において
は温度１５０〜３００℃、圧力０．１〜６００トルの条
件で攪拌を行ない未反応物や溶剤等をスチレン系重合体
中の含有率が０．５〜５０重量％になるまで脱気し、次
の第２脱気部においては温度２００〜３００℃、圧力５
０トル以下の条件で攪拌を行ない未反応物や溶剤等のス
チレ、；／−系重合体中の含有率が１重量％以下となる
ように未反応物や溶剤等を除去することを特徴とするス
チレン系重合反応物の後処理方法。 ２ 酸化防止剤がフェノール系化合物である特許請求の
範囲第１項記載の方法。 ３ 第１脱気部の攪拌翼の先端に、該攪拌翼と直交する
剥離板を設けた特許請求の範囲第１項記載の方法。[Claims] 1. A post-treatment method for removing unreacted substances, solvents, etc. from a styrene polymerization reaction product after the completion of a polymerization reaction, which comprises a heating mechanism, and further includes at least two rotary shafts on each of a plurality of rotating shafts. The styrene-based polymerization reaction product is sequentially introduced into a first degassing section equipped with a stirring mechanism in which several stirring blades are fixed, and a second degassing section equipped with a heating means by shearing action and a stirring means for thin film evaporation. An antioxidant is supplied to either or both of the first degassing section and the second degassing section to bring them into contact with the styrenic polymerization reaction product, and the temperature in the first degassing section is 150 to 300°C; Stirring is performed under pressure conditions of 0.1 to 600 torr to degas unreacted substances, solvent, etc. until the content in the styrenic polymer becomes 0.5 to 50% by weight. At a temperature of 200-300℃ and a pressure of 5
Stirring is carried out under conditions of 0 Torr or less to remove unreacted substances, solvents, etc. such that the content of such substances in the ;/- system polymer is 1% by weight or less. A post-treatment method for styrenic polymerization reactants. 2. The method according to claim 1, wherein the antioxidant is a phenolic compound. 3. The method according to claim 1, wherein a peeling plate is provided at the tip of the stirring blade in the first degassing section, and is perpendicular to the stirring blade.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP112583A JPS59126411A (en) | 1983-01-10 | 1983-01-10 | After-treatment of styrene polymerization product |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP112583A JPS59126411A (en) | 1983-01-10 | 1983-01-10 | After-treatment of styrene polymerization product |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59126411A true JPS59126411A (en) | 1984-07-21 |
| JPH0373570B2 JPH0373570B2 (en) | 1991-11-22 |
Family
ID=11492722
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP112583A Granted JPS59126411A (en) | 1983-01-10 | 1983-01-10 | After-treatment of styrene polymerization product |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59126411A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59227938A (en) * | 1983-06-10 | 1984-12-21 | Mitsui Toatsu Chem Inc | Polymer composition |
| US5565537A (en) * | 1992-06-17 | 1996-10-15 | Nippon Shokubai Co., Ltd. | Maleimide-based copolymer and process for producing it |
| US6100366A (en) * | 1998-09-18 | 2000-08-08 | Nippon Shokubai Co., Ltd. | Cyclic imino ether group containing polymer and production process therefor |
| CN113877498A (en) * | 2021-09-30 | 2022-01-04 | 长春工业大学 | Device and method for preparing SAN resin with stable composition and low volatile component |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5543121A (en) * | 1978-09-22 | 1980-03-26 | Hitachi Ltd | Removal of monomer from polystyrene resin |
| JPS57135814A (en) * | 1981-02-17 | 1982-08-21 | Nippon Steel Chem Co Ltd | Production of styrene/methyl methacrylate copolymer |
-
1983
- 1983-01-10 JP JP112583A patent/JPS59126411A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5543121A (en) * | 1978-09-22 | 1980-03-26 | Hitachi Ltd | Removal of monomer from polystyrene resin |
| JPS57135814A (en) * | 1981-02-17 | 1982-08-21 | Nippon Steel Chem Co Ltd | Production of styrene/methyl methacrylate copolymer |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59227938A (en) * | 1983-06-10 | 1984-12-21 | Mitsui Toatsu Chem Inc | Polymer composition |
| US5565537A (en) * | 1992-06-17 | 1996-10-15 | Nippon Shokubai Co., Ltd. | Maleimide-based copolymer and process for producing it |
| US6100366A (en) * | 1998-09-18 | 2000-08-08 | Nippon Shokubai Co., Ltd. | Cyclic imino ether group containing polymer and production process therefor |
| CN113877498A (en) * | 2021-09-30 | 2022-01-04 | 长春工业大学 | Device and method for preparing SAN resin with stable composition and low volatile component |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0373570B2 (en) | 1991-11-22 |
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