JPH0550484A - Method for extruding polyarylene sulfide composition - Google Patents
Method for extruding polyarylene sulfide compositionInfo
- Publication number
- JPH0550484A JPH0550484A JP3011030A JP1103091A JPH0550484A JP H0550484 A JPH0550484 A JP H0550484A JP 3011030 A JP3011030 A JP 3011030A JP 1103091 A JP1103091 A JP 1103091A JP H0550484 A JPH0550484 A JP H0550484A
- Authority
- JP
- Japan
- Prior art keywords
- water content
- composition
- polyarylene sulfide
- extrusion
- extruding
- 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
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/80—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling at the plasticising zone, e.g. by heating cylinders
- B29C48/83—Heating or cooling the cylinders
- B29C48/832—Heating
Landscapes
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
Description
【0001】[0001]
【産業上の利用分野】本発明は、ポリアリーレンスルフ
ィド組成物の押出しに当たり、予め水分含有量を一定に
保ち、溶融時の粘度変化を低く押えて290〜370℃
で溶融押出しを行う方法であって、淡色の押出物特にペ
レット等を得ようとするものである。FIELD OF THE INVENTION The present invention relates to the extrusion of a polyarylene sulfide composition, in which the water content is kept constant in advance and the change in viscosity during melting is kept low at 290 to 370 ° C.
In the method of melt-extruding, a light-colored extrudate, particularly pellets, is to be obtained.
【0002】[0002]
【従来の技術】ポリアリーレンスルフィドは、融点が高
く耐熱性のプラスチックとして近年その用途が広がりつ
つあるが、耐熱性であるが故に溶融時の温度は、必然的
に高くなってしまう。そして、このような高温下では重
合体の分解、架橋を生じ易く得られる物品、特にペレッ
トの溶融粘度が大きく変化したり、色調に変化が見られ
る等安定化した押出しを行うことが簡単ではなかった。
この欠点を改良するために窒素気流下での押出しが試み
られそれなりの効果はあるが、汎用押出し装置への付帯
設備が必要であったり、酸欠による危険防止策が必要で
あったりしてもっと簡便でかつ安定化した押出し方法が
望まれていた。2. Description of the Related Art Polyarylene sulfide has been widely used as a heat-resistant plastic having a high melting point in recent years. However, since it is heat-resistant, the melting temperature is inevitably high. And, under such high temperature, it is not easy to carry out a stable extrusion such as decomposition of the polymer, an article which is likely to cause cross-linking, particularly a large change in melt viscosity of pellets or a change in color tone. It was
Extrusion in a nitrogen stream was tried to improve this drawback, and there were some effects, but additional equipment to a general-purpose extrusion equipment was necessary, and risk prevention measures due to oxygen deficiency were necessary. A simple and stable extrusion method has been desired.
【0003】特開昭63−280740号に示されるご
とく、ベント型の押出機を使用して含水率の高いポリア
リーレンスルフィドを乾燥する方法が提案されている
が、一定の少量の水分を含有せしめて積極的に押出し工
程を安定化させる試みはなされていなかった。As disclosed in JP-A-63-280740, a method of drying a polyarylene sulfide having a high water content by using a vent type extruder has been proposed, but it contains a certain small amount of water. No attempt has been made to positively stabilize the extrusion process.
【0004】[0004]
【発明が解決しようとする課題】本発明が、ポリアリー
レンスルフィド組成物を溶融押出しする際に一定量の水
分を含有させて行い、溶融粘度変化が少なくかつ淡色の
押出し物を安定して得る方法を提供せんとするものであ
る。The present invention is a method for stably obtaining a light-colored extrudate with a small change in melt viscosity, which is carried out when a polyarylene sulfide composition is melt-extruded by containing a certain amount of water. Is intended to be provided.
【0005】[0005]
【課題を解決するための手段】本発明は、溶融時の重合
体の分解、架橋等を低減させるために次のような構成を
備えるものである。すなわち、ポリアリーレンスルフィ
ド組成物の溶融押出しに際し、原料であるポリアリーレ
ンスルフィド組成物の含水率を0.1〜1.5重量%に
調整し、290〜370℃で溶融押出しを行うものであ
る。The present invention is provided with the following constitution in order to reduce the decomposition and crosslinking of the polymer during melting. That is, when melt-extruding the polyarylene sulfide composition, the water content of the polyarylene sulfide composition as a raw material is adjusted to 0.1 to 1.5% by weight, and melt extrusion is performed at 290 to 370 ° C.
【0006】ここで、ポリアリーレンスルフィドは、芳
香族ポリハロゲン化物と硫化アルカリを極性有機溶媒中
で反応させて得られるものであるが、その溶融時の安定
性及び色はその後の重合体の後処理により大きく異なっ
てくる。重合時に比較的低分子量重合体を調整してお
き、空気等の酸化性雰囲気下に分枝あるいは架橋反応を
生ぜしめ、溶融粘度を上昇させるキュアリングを行った
ものは、重合時から高分子量の重合体に比べ溶融時に増
粘し易く、色も更に濃化する傾向にある。The polyarylene sulfide is obtained by reacting an aromatic polyhalide with an alkali sulfide in a polar organic solvent, and the stability and color of the polyarylene sulfide when melted are determined after the subsequent polymer. It depends on the process. When a relatively low molecular weight polymer is prepared at the time of polymerization, a branching or crosslinking reaction is caused in an oxidizing atmosphere such as air, and curing is performed to increase the melt viscosity. Compared with the polymer, the viscosity tends to increase when melted, and the color tends to further thicken.
【0007】本発明は、特にこのキュアリングが行われ
た重合体組成物に対して有効であり、ペレットを造る時
のような押出し時の増粘、濃色化を低減せんとするもの
である。ここで、ポリアリーレンスルフィド組成物と
は、ポリアリーレンスルフィドの重合体のみあるいはこ
れに各種充填剤や添加剤を混入せしめられたものを指
し、充填剤は一般的には無機系のものが広く使用させて
いる。The present invention is particularly effective for this cured polymer composition, and is intended to reduce thickening and darkening during extrusion such as pellet formation. .. Here, the polyarylene sulfide composition refers to a polymer of polyarylene sulfide alone or a mixture thereof with various fillers and additives, and the filler is generally an inorganic one widely used. I am letting you.
【0008】ポリアリーレンスルフィドは、一般式Polyarylene sulfide has the general formula
【化1】 単位で示されるポリアリーレンスルフィドを主成分とす
るものが殆どである。[Chemical 1] Most of them are mainly composed of polyarylene sulfide represented by a unit.
【0009】このポリアリーレンスルフィドは、融点が
高い(約280℃)ことから溶融押出し温度は290〜
370℃の範囲が好ましく、370℃を超すような高温
では重合体の分解、架橋反応がはげしくなり押出し工程
を安定化させることが困難となる。また、水も存在する
ので高温すぎると押出物が発泡してしまうという問題も
ある。水分の測定は、カールフィッシャー法、ガスクロ
マトグラフト法、150℃/1時間の加熱減量法がある
が、中でも加熱減量法が簡便である。Since this polyarylene sulfide has a high melting point (about 280 ° C.), the melt extrusion temperature is 290 to 290.
A range of 370 ° C. is preferable, and at a high temperature exceeding 370 ° C., the decomposition and cross-linking reaction of the polymer becomes violent and it becomes difficult to stabilize the extrusion process. Further, since water is also present, there is a problem that the extrudate foams when the temperature is too high. The water content can be measured by the Karl Fischer method, the gas chromatograph method, or the heating weight loss method at 150 ° C. for 1 hour. Among them, the heating weight loss method is simple.
【0010】本発明における含水率は組成物に対し、
0.1〜1.5重量%が適当であり、少なすぎると効果
は小さく、また多すぎると押出し時の発泡現象が起こり
好ましくない。この含水率に組成物を調整するには、一
定量の水の添加、調湿された雰囲気下での含水などが行
なわれ得るが、一定量の水をヘンシェル型ミキサー等で
均一にブレンドする方法が便利である。The water content in the present invention is based on the composition.
0.1 to 1.5% by weight is suitable, and if it is too small, the effect is small, and if it is too large, a foaming phenomenon at the time of extrusion occurs, which is not preferable. In order to adjust the composition to this water content, a fixed amount of water may be added, or water may be added in a humidity-controlled atmosphere, but a method of uniformly blending a fixed amount of water with a Henschel type mixer or the like. Is convenient.
【0011】このようにして含水率を調整された組成物
が何故押出し中に増粘が少なく、かつ色の変化も少ない
かの理由は明らかではないが、押出し機内での水の蒸発
による不活性化あるいは水そのものがポリアリーレンス
ルフィドの安定化剤であることも考えられる。押出し機
としてはベント型あるいは非ベント型のいずれも効果が
あり、これを限定するものではない。It is not clear why the composition of which the water content is adjusted in this way has a small increase in viscosity during extrusion and a small change in color, but it is inactive due to evaporation of water in the extruder. It is also conceivable that the hydrogenated or water itself is a stabilizer of the polyarylene sulfide. As the extruder, both vent type and non-vent type extruders are effective, and the present invention is not limited thereto.
【0012】[0012]
【作用および発明の効果】本発明は、押出しによるペレ
ットの製造に際し特に有効なものであり、最終製品とな
るべく成形される工程、例えばシート押出しや射出成形
時に本発明の含水率に調整して行なうと発泡や表面粗化
等の欠陥となり易く、中間製品としてのペレット安定化
に有効な方法であるが、ポリアリーレンスルフィドの押
出し、特にペレタイズ時に含水率を一定範囲に調整する
ことにより次のような作用効果を生じるものである。INDUSTRIAL APPLICABILITY The present invention is particularly effective in the production of pellets by extrusion, and is carried out by adjusting the water content of the present invention at the step of forming a final product, such as sheet extrusion or injection molding. It is easy to cause defects such as foaming and surface roughening, and it is an effective method for stabilizing pellets as an intermediate product.However, by extruding polyarylene sulfide, especially by adjusting the water content to a certain range during pelletization, It produces a working effect.
【0013】 (1) ペレットの粘度変化を小さくできる。 (2) ペレットの色調変化を小さくできる。 これにより、さらに射出成形等を行なう際の流動性の安
定化、色相変化を小さくできるようにすることが可能で
ある。(1) A change in viscosity of pellets can be reduced. (2) Change in color tone of pellets can be reduced. As a result, it is possible to further stabilize the fluidity and reduce the change in hue when performing injection molding or the like.
【0014】[0014]
【実施例】以下本発明の実施例をあげ、比較例と対比さ
せながら更に説明する。[Examples] Examples of the present invention will be given below for further explanation in comparison with comparative examples.
【0015】実施例1〜3、比較例1〜3 フィリップス社製PR06(メルトフローレート、以下
MFと略す、124)を用い、日本電気硝子製の13μ
m径チョップドガラス繊維40%を混合した組成物から
ペレットを溶融押出しにより製造するに際し、ヘンシェ
ルミキサーを用い水添加量を変更したもの各種を用意
し、30mm径の2軸べント型押出し機により320℃に
てペレットを製造した。なおベントは500mm Hg の圧
力下に行なった。さらにこれらのペレットを使用し、金
型温度150℃、射出時の温度320℃にてスパイラル
流動長を測定した。なおMFは試料を150℃、2時間
加熱した後、東洋精機製作所製のメルトインデクサーに
より5kgの荷重下に測定した。その結果を表1に示す。Examples 1 to 3 and Comparative Examples 1 to 3 PR06 (melt flow rate, hereinafter abbreviated as MF, 124) manufactured by Philips was used, and 13 μ manufactured by Nippon Electric Glass Co., Ltd.
In producing pellets from a composition in which 40% of m-diameter chopped glass fibers are mixed by melt extrusion, various kinds of water with different amounts of water added are prepared using a Henschel mixer, and a 320 mm twin-screw bent extruder is used. Pellets were manufactured at ° C. The venting was performed under a pressure of 500 mm Hg. Further, using these pellets, the spiral flow length was measured at a mold temperature of 150 ° C. and a temperature at injection of 320 ° C. The MF was measured by heating the sample at 150 ° C. for 2 hours and then using a melt indexer manufactured by Toyo Seiki Seisakusho under a load of 5 kg. The results are shown in Table 1.
【0016】[0016]
【表1】 [Table 1]
【0017】実施例4、比較例4 フィリップス社製PR07(MF620)を用い、実施
例1で使用したガラス繊維30%、炭酸カルシウム30
%を混合し、水0.5%を添加した組成物を320℃お
よび390℃でベントを使用せずに同様の押出し材でペ
レットを製造し、表2の結果を得た。Example 4, Comparative Example 4 Using PR07 (MF620) manufactured by Philips, 30% of glass fiber and 30 of calcium carbonate used in Example 1 were used.
% And water 0.5% was added to the composition at 320 ° C. and 390 ° C. to produce pellets from the same extruded material without using a vent, and the results in Table 2 were obtained.
【0018】[0018]
【表2】 比較例は発泡および分解・架橋がはげしいことを示して
いる。[Table 2] Comparative examples show that foaming and decomposition / crosslinking are severe.
【0019】以上の実施例から、本発明が溶融粘度安定
化や色調安定化に効果を有することが確認できた。From the above examples, it was confirmed that the present invention is effective in stabilizing melt viscosity and color tone.
Claims (1)
率を0.1〜1.5重量%に調整し、290〜370℃
で溶融押出しを行うことを特徴とするポリアリーレンス
ルフィドの押出し方法。1. A water content of the polyarylene sulfide composition is adjusted to 0.1 to 1.5% by weight, and 290 to 370 ° C.
A method for extruding polyarylene sulfide, which comprises melt-extruding at.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP03011030A JP3139024B2 (en) | 1991-01-31 | 1991-01-31 | Method for producing polyarylene sulfide pellets |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP03011030A JP3139024B2 (en) | 1991-01-31 | 1991-01-31 | Method for producing polyarylene sulfide pellets |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH0550484A true JPH0550484A (en) | 1993-03-02 |
JP3139024B2 JP3139024B2 (en) | 2001-02-26 |
Family
ID=11766689
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP03011030A Expired - Fee Related JP3139024B2 (en) | 1991-01-31 | 1991-01-31 | Method for producing polyarylene sulfide pellets |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP3139024B2 (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5151801B2 (en) | 2008-08-22 | 2013-02-27 | オムロンヘルスケア株式会社 | Cuff for blood pressure information measuring device and blood pressure information measuring device provided with the same |
-
1991
- 1991-01-31 JP JP03011030A patent/JP3139024B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JP3139024B2 (en) | 2001-02-26 |
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