JP4193009B2 - Method for producing polycarbonate resin molding material and transparent molded product thereof - Google Patents
Method for producing polycarbonate resin molding material and transparent molded product thereof Download PDFInfo
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- polycarbonate resin
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Description
【0001】
【発明の属する技術分野】
本発明はポリカーボネート樹脂成形材料の製造方法と、得られた成形材料を成形して得られる透明成形品に関するものであり、押出機の樹脂フィルターについて、特定の前処理を行った後に、樹脂フィルターに溶融樹脂を通すことによるゲル化物の発生を抑制した樹脂の製造方法及びゲル化物が無いかほとんど外観に影響しない透明成形品に関する。
【0002】
【従来の技術】
ポリカーボネート樹脂溶液からの成形材料の製造法としては、溶液から樹脂を分離、乾燥し、押出機でペレット化する方法が使用されている。
【0003】
しかし、ポリカーボネート樹脂の押出は高温条件下で行うため、原料の一部が熱分解し、ゲル化物、炭化物等が生成することは避けられないものと思われていた。
【0004】
ポリカーボネート樹脂は、透明性に優れる特性から光学用途や医療用途、建材用シートに使用されており、光学ディスクではミクロンオーダーの異物は信号の書き込みや読み取りにエラーを引き起こして情報の信頼性を大きく低下させ、また医療用品や建材用シートでは目認できる異物は製品の強度低下や透明外観において商品価値を低下させる。そのため、異物除去を目的として、溶融樹脂の濾過のために樹脂フィルターを取り付けている。
【0005】
【発明が解決しようとする課題】
しかし、押出を開始してから運転状態が安定してゲル化物、炭化物等による異物の発生が所定量以下になるまでには20時間以上の時間を必要とし、生産効率を著しく悪化させていた。このうち、樹脂フィルターでは捕捉除去されず押し出されたポリカーボネート樹脂に残留するゲル化物は、その後の成形品において金属異物や樹脂やけ炭化物等のように明確な核のある異物とは異なり、目視又は顕微鏡の観察で核は無いが、成形品にした場合、光線が散乱される現象(シルバー)を起こすため、光学ディスクの信号エラー及び医療用品や建材用シートの外観不良になる不良要因となっていた。
【0006】
特開平2−135222号には押出操作によるゲル化の発生や増加を抑えるため、ベントの減圧度を調節してあまり高くしないようにすることで対処する方法が記載されているが、ベントはポリカーボネート樹脂中に含まれている低分子量体や溶媒等の不純物を除去するためのものであり、その減圧度をあまり高くしないことは不純物の除去が不十分となり、結果として成形品を射出成形するときに成形品の外観不良や金型汚染を引き起こして、成形品の製造に著しい生産性の低下を引き起こすため、完全な解決策にはなっていない。
【0007】
そこで、本発明者等はゲル化物の発生を低減すべく、押出機、樹脂フィルター等を検討した結果、樹脂フィルターに滞留した空気が溶融樹脂と接触して樹脂の熱分解を生じ、このことがゲル化物発生の原因になること、及び特定の方法で押出機シリンダーと樹脂フィルターの処理を行えば、ゲル化物の発生が実質的に抑制されることを見出し、本発明に到達した。
【0008】
【課題を解決するための手段】
即ち本発明は、ポリカーボネート樹脂の素材粉末を溶融押出ししてポリカーボネート成形材料を製造する方法において、押出機に装着する樹脂フィルターのハウジングと金属エレメントを水で十分置換洗浄したところで、溶融樹脂を通すことによる、ゲル化物の発生を実質的に抑制したポリカーボネート樹脂成形材料の製造方法である。
【0009】
【発明の実施の形態】
本発明においてポリカーボネート樹脂は、ビスフェノールをモノマーとし、ホスゲン法、エステル交換法、ピリジン法、その他によりビスフェノールを炭酸エステル結合して製造される芳香族ポリカーポネート樹脂である。
【0010】
ビスフェノールの代表的な例を挙げると、2,2-ビス(4-ヒドロキシフェニル)プロパン、1,1-ビス(4-ヒドロキシフェニル)エタン、2,2-ビス(4-ヒドロキシ−3-メチルフェニル)プロパン、1,1-ビス(4-ヒドロキシフェニル)シクロヘキサン等がある。好ましいビスフェノールはビス(4-ヒドロキシフェニル)アルカン系化合物、特に2,2-ビス(4-ヒドロキシフェニル)プロパン(以下、ビスフェノールAと記す。)である。ビスフェノールは単独で、又は2種以上混合して使用することができる。また、このポリカーボネート樹脂と他の樹脂とのグラフト共重合体などの透明樹脂にも適用可能である。
【0011】
本発明においてポリカーボネート樹脂粉末は、例えばホスゲン法の場合、重合溶液からポリカーボネート樹脂溶液を分離し、洗浄精製した後、更に精密濾過、遠心分離等により、異物やイオン性の不純物を除去して精製されたポリカーボネート樹脂の溶媒溶液を得る。
【0012】
次いで行われる樹脂の分離方法としては、▲1▼樹脂溶液をそのままあるいはこれに貧溶媒を沈殿が生じない程度に加えてなる樹脂溶液を濃縮ゲル化する方法(”ゲル濃縮法”:溶媒留去ゲル化、フラッシュ濃縮ゲル化等)又は該樹脂溶液を温水中に滴下し溶媒を留去しゲル化する”温水滴下法”、▲2▼貧溶媒中にポリカーボネート樹脂溶液を滴下するか或いは該樹脂溶液中に貧溶媒を滴下する方法である”沈澱法”等が採用される。
【0013】
ポリカーボネート樹脂粉末とは、”温水滴下法”により得られた湿潤粉末、或いは沈澱法により得た粉末に水を加え、適宜湿式粉砕をしながら加熱して溶媒を留去する方法等により製造される湿潤粉末である。湿潤粉末をベント部よりの揮発成分の除去の容易な押出機に導入し、押出と共に溶媒を留去する方法は、乾燥工程における熱履歴がないので熱劣化の防止からも好ましい。
【0014】
本発明において押出機としては、ベント付き単軸押出機、ベント付き2軸押出機、あるいはコ・ニーダ、プラネタリ−スクリュー押出機などの特殊押出機等各種のものを用いることができる。
【0015】
本発明で用いる押出機バレル内面は、クロムタングステン鋼(SKS)、クロムバナジウム鋼(SKD)、ニッケルクロム鋼(SNC)、ニッケルクロムモリブデン鋼(SNCM)、クロムモリブデン鋼(SCM)又はアルミニウムクロムモリブデン鋼(SACM)等の高強度鋼材の窒化処理したものを挙げることができるが、特に、ステライト、ハステロイ又はコルモノイを溶射したものが好適に使用される。また、スクリューとしては、クロムタングステン鋼(SKS)、クロムバナジウム鋼(SKD)、ニッケルクロム鋼(SNC)、ニッケルクロムモリブデン鋼(SNCM)、クロムモリブデン鋼(SCM)に硬質クロムメッキあるいはNiカニゼンメッキしたもの、マルテンサイト系ステンレス鋼を熱処理したのも、又はクロムタングステン鋼、クロムパラジウム鋼、ニッケルクロム鋼、ニッケルクロムモリブデン鋼、クロムモリブデン鋼を基材として山材にステライトを肉盛りしたものが用いられる。特に、クロムバナジウム鋼(SKD)、ニッケルクロム鋼(SNC)、クロムモリブデン鋼(SCM)またはニッケルクロムモリブデン鋼(SNCM)に硬質クロムメッキあるいはNiカニゼンメッキしたものが好ましい。
【0016】
本発明の樹脂フィルターエレメントは、通常オーステナイト系ステンレス鋼が使用される。例えば、SUS304,SUS304L、SUS316、SUS316L、SUS309S、SUS310S、SUS317およびSUS317L等を挙げることができる。樹脂フィルターの公称濾過口径は通常1〜100μm、好ましくは1〜60μm、さらに好ましくは2〜40μmである。フィルターはディスクフィルター、リーフディスクフィルター、円筒フィルター、チューブ型フィルター等の各種のものかあげられるが、特にリーフディスクフィルター、ディスクフィルターが好ましい。フィルターメディアは金属の繊維を不織布とし、該不織布を焼結して多孔体とした金属繊維焼結体が望ましい。
【0017】
樹脂フィルターはフィルターエレメントをハウジング内に固定し、押出機に装着する前に水で十分置換洗浄し、残留する空気を置換することで、その後溶融ポリカーボネート樹脂がフィルター部分にやってきても空気と接触することがなく、熱分解によるゲル化が抑制される。ここで、使用される洗浄水は上水をイオン交換したものが使用され、電気伝導率は5μS/cm以下であることが好ましく、更に1μS/cm以下であることが特に好ましい。
【0018】
ゲル化物の判定は、ポリカーボネート樹脂ペレット1Kgを50〜200μmのフィルム成形を行い、CCD光学カメラによる50μm以上の異物検出を行い、その中で目視ないしは顕微鏡観察によりゲル化物に識別されるものを確認する方法によった。ゲル化物の個数は、フィルムの厚みにより若干の差はあるが、30個/Kg以下、好ましくは10個/Kg以下、さらに好ましくは5個/Kg以下である。
【0019】
【実施例】
以下、実施例等により本発明を説明するが、本発明はこれらの例によってなんら限定されるものではない。
【0020】
実施例等におけるゲル化物の測定は、ポリカーボネート樹脂ペレット1Kgを150〜200μmのフィルム成形を行い、CCD光学カメラによる50μm以上の異物検出を行い、その中で目視によりゲル化物に識別されるものを確認する方法によった。
【0021】
実施例1
50mmφベント付き押出機(バレル内面:コルモノイ溶射処理、スクリュー:クロムモリブデン鋼に硬質クロムメッキ処理)を用い、樹脂フィルターとして公称濾過口径40μmのSUS316L製フィルターエレメントをハウジングにセットし、フィルターエレメントとハウジング内を、電気伝導率が1μS/cmの水で十分置換洗浄した後押出機に取り付けた。 その後、ポリカーボネート樹脂粉末を高温(330℃)で押出し始め、ベントの真空度20Torr以下にし、3時間後得られたペレットをフィルム成形し、異物検査によりゲル化物の個数測定を行った。また、上記ペレットを射出成形機により直径120mm、厚さ1.2mmのディスクを200枚成形し、ゲル化物に起因するシルバーの発生枚数を測定した。結果を表1に示す。
【0022】
比較例1
比較のためフィルタ―エレメントとハウジング内を水で十分置換洗浄を行わない以外は、実施例1と同様にして得られたペレットの異物検査およびペレットを射出成形して得られたディスクのゲル化物に起因するシルバー検査を実施例1と同様に行った。結果を表1に示す。
【0023】
【表1】
【0024】
【発明の効果】
本発明によれば、ポリカーボネート樹脂粉末を溶融押出ししてポリカーボネート樹脂成形材料を製造する方法において、非常に簡単な操作で、樹脂フィルターによって除去出来なかったゲル化物を実質的に含まないポリカーボネート樹脂成形材料を製造することができ、光ディスク、医療用品あるいは建材用シートの成形材料として好適に使用される。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a polycarbonate resin molding material and a transparent molded product obtained by molding the obtained molding material. After a specific pretreatment is performed on a resin filter of an extruder, the resin filter The present invention relates to a resin production method that suppresses the generation of a gelled product by passing a molten resin, and a transparent molded product that has no gelled product or hardly affects the appearance.
[0002]
[Prior art]
As a method for producing a molding material from a polycarbonate resin solution, a method in which the resin is separated from the solution, dried, and pelletized with an extruder is used.
[0003]
However, since the extrusion of the polycarbonate resin is performed under high temperature conditions, it has been considered inevitable that a part of the raw material is thermally decomposed to produce a gelled product, a carbide or the like.
[0004]
Polycarbonate resin is used in optical, medical and building material sheets due to its excellent transparency. On optical discs, foreign matter in the micron order causes errors in signal writing and reading, greatly reducing the reliability of information. In addition, foreign substances that can be recognized in medical supplies and building material sheets reduce the product value in terms of reduced strength and transparent appearance. Therefore, a resin filter is attached for filtering the molten resin for the purpose of removing foreign substances.
[0005]
[Problems to be solved by the invention]
However, it took 20 hours or more from the start of extrusion until the operating state was stabilized and the generation of foreign matter due to gelled products, carbides and the like was less than a predetermined amount, which significantly deteriorated the production efficiency. Among these, the gelled product remaining in the extruded polycarbonate resin without being captured and removed by the resin filter is different from the foreign material having a clear nucleus such as a metal foreign material, resin, or carbide in the subsequent molded product. Although there was no nucleus in the observation of this, when it was made into a molded product, it caused the phenomenon of light scattering (silver), which caused a signal error of the optical disc and a defect cause of poor appearance of medical supplies and building material sheets .
[0006]
Japanese Patent Application Laid-Open No. 2-135222 describes a method of coping with the occurrence of an increase in gelation due to an extrusion operation by adjusting the degree of pressure reduction of the vent so as not to be too high. It is for removing impurities such as low molecular weight substances and solvents contained in the resin. If the degree of vacuum is not so high, the removal of impurities becomes insufficient, and as a result when molding molded products. However, this is not a complete solution because it causes poor appearance of molded products and contamination of molds, resulting in a significant decrease in productivity in the production of molded products.
[0007]
Therefore, as a result of studying an extruder, a resin filter, etc. in order to reduce the generation of gelled substances, the present inventors have contacted the molten resin with air staying in the resin filter, which causes thermal decomposition of the resin. It has been found that the generation of gelled products is caused, and that the generation of gelled products can be substantially suppressed by processing the extruder cylinder and the resin filter by a specific method.
[0008]
[Means for Solving the Problems]
That is, according to the present invention, in a method for producing a polycarbonate molding material by melt-extruding a polycarbonate resin material powder, a resin filter housing and a metal element mounted on an extruder are sufficiently replaced and washed with water, and then the molten resin is passed. Is a method for producing a polycarbonate resin molding material in which generation of a gelled product is substantially suppressed.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
In the present invention, the polycarbonate resin is an aromatic polycarbonate resin produced by using bisphenol as a monomer and bisphenol carbonate bonding by phosgene method, transesterification method, pyridine method, or the like.
[0010]
Representative examples of bisphenol include 2,2-bis (4-hydroxyphenyl) propane, 1,1-bis (4-hydroxyphenyl) ethane, and 2,2-bis (4-hydroxy-3-methylphenyl) ) Propane, 1,1-bis (4-hydroxyphenyl) cyclohexane and the like. A preferred bisphenol is a bis (4-hydroxyphenyl) alkane compound, particularly 2,2-bis (4-hydroxyphenyl) propane (hereinafter referred to as bisphenol A). Bisphenol can be used individually or in mixture of 2 or more types. Moreover, it is applicable also to transparent resins, such as a graft copolymer of this polycarbonate resin and other resin.
[0011]
In the present invention, for example, in the case of the phosgene method, the polycarbonate resin powder is purified by separating the polycarbonate resin solution from the polymerization solution, washing and purifying it, and further removing foreign substances and ionic impurities by microfiltration, centrifugation, etc. A solvent solution of the obtained polycarbonate resin is obtained.
[0012]
Next, as a method for separating the resin, (1) a method of concentrating the resin solution as it is or adding a poor solvent to the resin solution to such an extent that no precipitation occurs (“gel concentration method”: solvent distillation) Gelation, flash concentration gelation, etc.) or “warm water dropping method” in which the resin solution is dropped into warm water and the solvent is distilled off to gel, or (2) the polycarbonate resin solution is dropped into a poor solvent or the resin A “precipitation method” which is a method of dropping a poor solvent into the solution is employed.
[0013]
Polycarbonate resin powder is produced by a method in which water is added to a wet powder obtained by a “hot water dropping method” or a powder obtained by a precipitation method, and the solvent is distilled off by heating with appropriate wet grinding. It is a wet powder. A method in which the wet powder is introduced into an extruder that easily removes volatile components from the vent portion, and the solvent is distilled off together with the extrusion is preferable from the viewpoint of preventing thermal deterioration because there is no thermal history in the drying process.
[0014]
In the present invention, various types of extruders such as a single-screw extruder with a vent, a twin-screw extruder with a vent, or a special extruder such as a co-kneader or a planetary screw extruder can be used.
[0015]
The inner surface of the extruder barrel used in the present invention is chrome tungsten steel (SKS), chrome vanadium steel (SKD), nickel chrome steel (SNC), nickel chrome molybdenum steel (SNCM), chrome molybdenum steel (SCM), or aluminum chrome molybdenum steel. Examples of the high-strength steel material such as (SACM) that have been subjected to nitriding treatment include those obtained by spraying stellite, hastelloy, or colmonoy. In addition, as a screw, chromium tungsten steel (SKS), chromium vanadium steel (SKD), nickel chromium steel (SNC), nickel chromium molybdenum steel (SNCM), chromium molybdenum steel (SCM) were plated with hard chromium or Ni Kanigen. , Martensitic stainless steel heat treated, or chrome tungsten steel, chromium palladium steel, nickel chrome steel, nickel chrome molybdenum steel, chrome molybdenum steel base material with stellite overlaid . Particularly, chromium vanadium steel (SKD), nickel chrome steel (SNC), chrome molybdenum steel (SCM) or nickel chrome molybdenum steel (SNCM) plated with hard chrome or Ni Kanigen is preferable.
[0016]
Austenitic stainless steel is usually used for the resin filter element of the present invention. Examples thereof include SUS304, SUS304L, SUS316, SUS316L, SUS309S, SUS310S, SUS317, and SUS317L. The nominal filtration aperture of the resin filter is usually 1 to 100 μm, preferably 1 to 60 μm, and more preferably 2 to 40 μm. The filter includes various types such as a disc filter, a leaf disc filter, a cylindrical filter, and a tube filter, and a leaf disc filter and a disc filter are particularly preferable. The filter media is preferably a metal fiber sintered body in which a metal fiber is a nonwoven fabric and the nonwoven fabric is sintered to form a porous body.
[0017]
The resin filter fixes the filter element in the housing, thoroughly replaces and cleans with water before installing it in the extruder, and replaces the remaining air, so that the molten polycarbonate resin will come into contact with the air even if it reaches the filter part afterwards. And gelation due to thermal decomposition is suppressed. Here, the washing water used is one obtained by ion-exchanging clean water, and the electric conductivity is preferably 5 μS / cm or less, more preferably 1 μS / cm or less.
[0018]
The gelled product is determined by forming a film of polycarbonate resin pellets 1 kg in a thickness of 50 to 200 μm, detecting a foreign matter of 50 μm or more with a CCD optical camera, and confirming what is identified as a gelated product by visual observation or microscopic observation. According to the method. The number of gelled products varies slightly depending on the thickness of the film, but is 30 pieces / kg or less, preferably 10 pieces / kg or less, more preferably 5 pieces / kg or less.
[0019]
【Example】
EXAMPLES Hereinafter, although an Example etc. demonstrate this invention, this invention is not limited at all by these examples.
[0020]
Measurement of gelled product in Examples etc. is carried out by forming a film of 150-200 μm of polycarbonate resin pellets 1 Kg, detecting foreign matter of 50 μm or more with a CCD optical camera, and confirming what is identified as a gelated product by visual inspection. According to the method to do.
[0021]
Example 1
Using a 50mmφ vented extruder (barrel inner surface: Colmonoy thermal spray treatment, screw: hard chromium plating treatment on chrome molybdenum steel), a SUS316L filter element with a nominal filtration diameter of 40μm is set in the housing as a resin filter. Was sufficiently substituted and washed with water having an electric conductivity of 1 μS / cm, and then attached to the extruder. Thereafter, the polycarbonate resin powder was extruded at a high temperature (330 ° C.), the degree of vacuum of the vent was reduced to 20 Torr or less, and the pellets obtained after 3 hours were formed into a film, and the number of gelled products was measured by foreign matter inspection. Further, 200 pieces of discs having a diameter of 120 mm and a thickness of 1.2 mm were formed from the pellets by an injection molding machine, and the number of silver generated due to the gelled product was measured. The results are shown in Table 1.
[0022]
Comparative Example 1
For comparison, except that the filter element and the inside of the housing are not sufficiently replaced and washed with water, the foreign matter inspection of the pellet obtained in the same manner as in Example 1 and the gelled product of the disk obtained by injection molding the pellet The resulting silver inspection was performed in the same manner as in Example 1. The results are shown in Table 1.
[0023]
[Table 1]
[0024]
【The invention's effect】
According to the present invention, in a method for producing a polycarbonate resin molding material by melt-extruding a polycarbonate resin powder, a polycarbonate resin molding material that does not substantially contain a gelled product that could not be removed by a resin filter by a very simple operation. And can be suitably used as a molding material for optical disks, medical supplies or building material sheets.
Claims (3)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP10114598A JP4193009B2 (en) | 1998-04-13 | 1998-04-13 | Method for producing polycarbonate resin molding material and transparent molded product thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP10114598A JP4193009B2 (en) | 1998-04-13 | 1998-04-13 | Method for producing polycarbonate resin molding material and transparent molded product thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH11291237A JPH11291237A (en) | 1999-10-26 |
JP4193009B2 true JP4193009B2 (en) | 2008-12-10 |
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JP10114598A Expired - Fee Related JP4193009B2 (en) | 1998-04-13 | 1998-04-13 | Method for producing polycarbonate resin molding material and transparent molded product thereof |
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JP6006653B2 (en) * | 2013-02-04 | 2016-10-12 | 出光興産株式会社 | Polycarbonate resin extrusion granulator and polycarbonate resin extrusion granulation method |
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JPH11291237A (en) | 1999-10-26 |
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