JP2003071834A - Crystallization treatment method for polyester resin - Google Patents
Crystallization treatment method for polyester resinInfo
- Publication number
- JP2003071834A JP2003071834A JP2001268405A JP2001268405A JP2003071834A JP 2003071834 A JP2003071834 A JP 2003071834A JP 2001268405 A JP2001268405 A JP 2001268405A JP 2001268405 A JP2001268405 A JP 2001268405A JP 2003071834 A JP2003071834 A JP 2003071834A
- Authority
- JP
- Japan
- Prior art keywords
- crystallization
- polyester resin
- temperature
- resin
- pellets
- 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.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明はポリエステル樹脂を
溶融押出し成型にする際に、優れた成形品を提供するた
めに必要な、ポリエステル樹脂の結晶化方法に関するも
のである。さらに詳しくは、ポリエステル樹脂ペレット
を乾燥する際に、ペレット同士の融着を防ぐために行う
結晶化処理を効率よく連続的に行うポリエステル樹脂の
結晶化処理方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for crystallizing a polyester resin, which is necessary for providing an excellent molded product when the polyester resin is melt-extruded. More specifically, the present invention relates to a crystallization treatment method for a polyester resin, in which, when the polyester resin pellets are dried, a crystallization treatment for preventing fusion between the pellets is efficiently and continuously performed.
【０００２】[0002]
【従来の技術】ポリエステル樹脂等は、溶融押出し成形
により、各種容器、フイルム、機械部品などに加工され
て使用されている。本発明は、これらの熱可塑性ポリエ
スエテル樹脂は、成形品の品質を良好に保つためには、
押出す前にポリエスエテル樹脂ペレットに含まれる水分
を除去する必要があり、一般に熱風あるいは減圧下で樹
脂ペレットを加熱乾燥して使用する。しかしながら、未
結晶状態の樹脂ペレットを短時間で乾燥するために、高
温で乾燥するとペレット同士の融着が発生し、押出機へ
の供給が困難になる。2. Description of the Related Art Polyester resins and the like are used by being processed into various containers, films, machine parts and the like by melt extrusion molding. The present invention, these thermoplastic polyester resins, in order to keep the quality of the molded article good,
It is necessary to remove the water contained in the polyester resin pellets before extrusion, and generally, the resin pellets are dried by heating under hot air or reduced pressure before use. However, since the uncrystallized resin pellets are dried in a short time, when they are dried at a high temperature, fusion of the pellets occurs, which makes it difficult to supply the pellets to the extruder.
【０００３】これらの問題を解決する方法として、例え
ば特開２０００‐２７１９３１号公報には、バッチ式の
結晶化装置が提案されている。しかしバッチ式の場合、
ペレットの融着を防ぐには、ペレットを容器内に投入す
る際に昇温開始する温度を、ペレットのガラス転移温度
より低くする必要があり、かつ段階的に結晶化温度まで
昇温していく必要があることから、結晶化完了するまで
に時間を要し、結晶化処理能力が劣るという問題があ
る。As a method for solving these problems, for example, Japanese Patent Application Laid-Open No. 2000-271931 proposes a batch type crystallization apparatus. But in the case of batch type,
In order to prevent fusion of the pellets, the temperature at which the temperature starts to be raised when the pellets are put into the container must be lower than the glass transition temperature of the pellets, and the temperature is gradually raised to the crystallization temperature. Since it is necessary, it takes a long time to complete the crystallization, and there is a problem that the crystallization processing ability is poor.
【０００４】また特開平９‐２４１３６０号公報には、
水分の供給下で、ペレット仕込み時の乾燥機内温度がＤ
ＳＣで測定される結晶化前のＴｇ未満であり、連続また
は間欠的に結晶化処理する方法が提案されている。しか
し、この方法によって結晶化されたペレットは、水分を
多く含んでおり、その後の乾燥工程で樹脂の粘度低下が
発生しやすいという欠点を有する。Further, Japanese Patent Laid-Open No. 9-241360 discloses that
When supplying pellets, the temperature inside the dryer is D when water is supplied.
It is less than Tg before crystallization measured by SC, and a method of performing crystallization treatment continuously or intermittently has been proposed. However, the pellet crystallized by this method has a drawback that it contains a large amount of water and the viscosity of the resin is likely to decrease in the subsequent drying step.
【０００５】[0005]
【発明が解決しようとする課題】本発明の目的は、上記
従来の問題点を解消せんとするものであり、ポリエステ
ル樹脂ペレットを乾燥する際に、ペレット同士の融着を
防ぐために行う結晶化処理を効率よく連続的に行うこと
が可能なポリエステル樹脂の結晶化処理方法を提供する
ことにある。SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems of the prior art. When drying polyester resin pellets, a crystallization treatment for preventing fusion between the pellets is performed. It is an object of the present invention to provide a method for crystallization treatment of a polyester resin, which can efficiently and continuously perform crystallization.
【０００６】[0006]
【課題を解決するための手段】前記した本発明の目的
は、 ポリエステル樹脂を装置内に熱風を供給すること
により加熱しながら連続的に結晶化処理を行うに際し、
装置内の樹脂結晶化領域の温度を検知し、連続的に結晶
化する単位時間当たりの排出量（処理量）を前記検知温
度に基づいて変化させることにより、装置内の樹脂結晶
化領域の温度を樹脂結晶化温度（Ｔｃ）±２０℃の範囲
に保つことを特徴とするポリエステル樹脂の結晶化処理
方法によって達成できる。The above-mentioned object of the present invention is to continuously crystallize a polyester resin while heating it by supplying hot air into the apparatus.
The temperature of the resin crystallization area in the device is detected by detecting the temperature of the resin crystallization area in the device and changing the discharge amount (processing amount) for continuous crystallization per unit time based on the detected temperature. At a resin crystallization temperature (Tc) of ± 20 ° C.
【０００７】[0007]
【発明の実施の形態】上記目的を達成すべく鋭意検討を
重ねた結果、ポリエステル樹脂を装置内に熱風を供給す
ることで加熱しながら、連続的に結晶化処理を行うに際
し、装置内の温度を検知し、それに応じて連続的に結晶
化する単位時間当たりの排出量（処理量）を変化させる
ことにより、装置内の温度を制御することを特徴とする
結晶化処理方法を見出した。DETAILED DESCRIPTION OF THE INVENTION As a result of intensive studies to achieve the above-mentioned object, the temperature in the apparatus was increased during continuous crystallization while heating the polyester resin by supplying hot air into the apparatus. Has been detected, and the temperature in the apparatus has been controlled by changing the discharge amount (treatment amount) per unit time for continuous crystallization in accordance with the detected temperature.
【０００８】以下、本発明で好適に用いることのできる
縦型結晶化装置について、図１に示す一実施態様に基づ
いて詳細に説明する。A vertical crystallization apparatus that can be preferably used in the present invention will be described below in detail with reference to an embodiment shown in FIG.
【０００９】本装置は縦型円筒と下部が逆円錐状の組合
せからなる結晶化槽１に、原料ポリエステル樹脂ペレッ
ト投入口２、および熱風供給口６、排気孔３、結晶化完
了ペレット計量排出装置７が設けられている。装置内部
の攪拌部は水平方向の翼５を複数本有する攪拌軸４で構
成されている。This apparatus comprises a raw material polyester resin pellet charging port 2, a hot air supply port 6, an exhaust hole 3 and a crystallization-completed pellet measuring and discharging device in a crystallization tank 1 which is a combination of a vertical cylinder and a lower cone. 7 is provided. The stirring unit inside the apparatus is composed of a stirring shaft 4 having a plurality of horizontal blades 5.
【００１０】結晶化に際しては、まずポリエステル樹脂
のガラス転移温度以下の熱風を熱風供給口６より連続的
に供給し、さらに攪拌軸４を回転させた状態で、ペレッ
ト投入口２より未結晶のポリエステル樹脂を定量投入す
る。投入終了後熱風の温度を段階的に上げていき、装置
内の上部の温度（Ｔ１）が所定の温度に到達後、計量排
出装置７から連続的に計量排出を始める。結晶化装置に
取りつけられた粒面レベル計８によりペレットの粒面レ
ベルを検知し、粒面レベルが一定になるように未結晶状
態のポリエステル樹脂ペレットを供給する。In the crystallization, first, hot air having a temperature not higher than the glass transition temperature of the polyester resin is continuously supplied from the hot air supply port 6, and the stirring shaft 4 is further rotated, and the amorphous polyester is supplied from the pellet input port 2. Add a fixed amount of resin. After the charging is completed, the temperature of the hot air is gradually increased, and after the temperature (T1) in the upper part of the apparatus reaches a predetermined temperature, the metering and discharging device 7 continuously starts metering and discharging. The grain surface level meter 8 attached to the crystallizer detects the grain surface level of the pellet, and the polyester resin pellets in an uncrystallized state are supplied so that the grain surface level becomes constant.
【００１１】この時、未結晶状態のペレットは結晶化が
進行する際に結晶化熱が発生するために、この結晶化に
よる発熱量が多いと、結晶化装置内のペレット温度が上
昇することにより、熱風温度が供給時の温度よりも高く
なり、ペレット同士、あるいはペレット攪拌翼、壁面と
融着が発生する。槽内の温度を制御し連続的に結晶化処
理を安定して行うに際し、槽内の結晶化領域のペレット
温度（Ｔ２）を検知し、該検知温度の結果に基づいて連
続的に結晶化する単位時間当たりの処理量、すなわち計
量排出装置７により結晶化ペレットの排出量を変化させ
ることにより、結晶化装置内の結晶化による単位時間当
たりの発熱量を増減し、装置内のペレット温度を結晶化
温度（Ｔｃ）〜Ｔｃ＋２０℃、あるいは（Ｔｃ）〜Ｔｃ
−２０℃の範囲に制御するものである。すなわち、装置
内のペレット温度が結晶化温度（Ｔｃ）＋２０℃を超え
るときには、計量排出装置７による結晶化ペレットの排
出量を多くし、（Ｔｃ）−２０℃より低いときには、計
量排出装置７による結晶化ペレットの排出量を少なくな
るように制御するものである。At this time, the uncrystallized pellets generate heat of crystallization as crystallization progresses. Therefore, if the amount of heat generated by this crystallization is large, the temperature of the pellets in the crystallization apparatus rises. The hot air temperature becomes higher than the temperature at the time of supply, and fusion occurs between the pellets or the pellet stirring blades and the wall surface. When controlling the temperature in the tank and continuously and stably performing the crystallization process, the pellet temperature (T2) in the crystallization region in the tank is detected, and the crystallization is continuously performed based on the result of the detected temperature. By changing the processing amount per unit time, that is, the discharge amount of the crystallized pellets by the metering and discharging device 7, the calorific value per unit time due to crystallization in the crystallization device is increased or decreased to crystallize the pellet temperature in the device. Temperature (Tc) to Tc + 20 ° C, or (Tc) to Tc
The temperature is controlled within the range of -20 ° C. That is, when the pellet temperature in the device exceeds the crystallization temperature (Tc) + 20 ° C., the discharge amount of the crystallized pellets by the metering and discharging device 7 is increased, and when it is lower than (Tc) −20 ° C., the metering and discharging device 7 is used. The amount of crystallized pellets discharged is controlled to be small.
【００１２】また結晶化前のポリエステル樹脂が装置上
部より供給され、装置下部から結晶化されたポリエステ
ル樹脂が連続的に排出されることが好ましい。上部より
供給された未結晶ポリエステル樹脂は、下部より供給さ
れた熱風で、徐々に加熱されながら装置の下部に順次結
晶化度を高めながら下りて行き、目的の結晶化度に到達
後排出口より排出される。この時不連続に排出すると、
結晶化装置内のポリエステル樹脂ペレットの流れに乱れ
が生じて、結晶化にバラツキを生じることになるので好
ましくない。Further, it is preferable that the polyester resin before crystallization is supplied from the upper part of the apparatus, and the crystallized polyester resin is continuously discharged from the lower part of the apparatus. The amorphous polyester resin supplied from the upper part is gradually heated by the hot air supplied from the lower part and gradually descends to the lower part of the device while gradually increasing the crystallinity, and after reaching the target crystallinity, from the discharge port. Is discharged. At this time, if the discharge is discontinuous,
The flow of the polyester resin pellets in the crystallization device is disturbed, which causes variations in crystallization, which is not preferable.
【００１３】さらに、結晶化装置内のポリエステル樹脂
ペレットの流れを均一にするには、結晶化装置内のペレ
ットの垂直方向の粒面高さ（Ｌ）と水平方向断面の直径
（Ｄ）の比（Ｌ／Ｄ）が３以上６以下であることが好ま
しい。Ｌ／Ｄが３未満では、結晶化装置内のポリエステ
ル樹脂ペレットの流れに乱れが生じて、結晶化にバラツ
キを生じることになる。またＬ／Ｄが６を超えてもこれ
以上結晶化の均一性は得られず、装置が必要以上に大型
化し無駄である。Furthermore, in order to make the flow of the polyester resin pellets in the crystallizer uniform, the ratio of the grain surface height (L) in the vertical direction of the pellets in the crystallizer to the diameter (D) of the horizontal cross section. It is preferable that (L / D) is 3 or more and 6 or less. When L / D is less than 3, turbulence occurs in the flow of the polyester resin pellets in the crystallization device, which causes variations in crystallization. Further, even if L / D exceeds 6, the uniformity of crystallization cannot be obtained any more, and the apparatus is unnecessarily increased in size.
【００１４】本発明の結晶化処理方法は結晶化発熱量が
１Ｊ／ｇ以上、特に５Ｊ／ｇ以上あるポリエステル樹脂
に対して有効である。このようなポリエステル樹脂は結
晶化時の発熱のために、熱風が逆に熱せられて、導入温
度よりも高くなり過ぎるとペレット同士の融着の原因と
なる。装置内での結晶化発熱量を先に述べた方法により
制御することにより、安定した結晶化処理が可能とな
る。The crystallization treatment method of the present invention is effective for polyester resins having a crystallization heat value of 1 J / g or more, especially 5 J / g or more. Such a polyester resin is heated by the hot air on the contrary due to the heat generated during crystallization, and when the temperature becomes higher than the introduction temperature, it causes fusion between the pellets. By controlling the amount of heat generated by crystallization in the apparatus by the method described above, a stable crystallization process becomes possible.
【００１５】結晶化ペレットの排出量の制御としては、
例えば、装置内のペレット温度を熱電対により検出し、
この検出値を電気信号として取り出し、計量排出装置と
して、例えば、ロータリーフィーダー（回転式の計量装
置）を使用し、インバーター（周波数変換装置）を用い
て、ロータリーフィーダーの回転数を上記熱電対からの
電気信号で制御することにより可能である。The control of the discharge amount of the crystallized pellets is as follows.
For example, the temperature of the pellet in the device is detected by a thermocouple,
This detection value is taken out as an electric signal, and, for example, a rotary feeder (rotary weighing device) is used as a metering / discharging device, and an inverter (frequency converter) is used to determine the rotation speed of the rotary feeder from the thermocouple. It is possible by controlling with an electric signal.
【００１６】本発明におけるポリエステル樹脂として
は、ジカルボン酸とグリコールとの重縮合反応から製造
され、ジカルボン酸として例えばテレフタル酸、イソフ
タル酸、ナフタレンジカルボン酸、ジフェニルジカルボ
ン酸、ジフェニルスルホンジカルボン酸、ジフェノキシ
エタンジカルボン酸、５−ナトリウムスルホイソフタル
酸、フタル酸等の芳香族ジカルボン酸、シュウ酸、コハ
ク酸、アジピン酸、セバシン酸、ダイマー酸、マレイン
酸、フタル酸等の脂肪族ジカルボン酸、シクロヘキシン
ジカルボン酸等の脂環族ジカルボン酸、ｐ−オキシ安息
酸等のオキシカルボン酸等を挙げることができる。グリ
コール成分としては、エチレングリコール、プロパンジ
オール、ブタンジオール、ペンタンジオール、ヘキサン
ジオール、ネオペンチルグリコールなどの脂肪族グリコ
ール、シクロヘキサンジメタノール等の脂環族グリコー
ル、ビスフェノールＡ、ビスフェノールＳ等の芳香族グ
リコール等が挙げられる。なお、これらのジカルボン酸
成分、グリコール成分は２種類以上を０〜２５モル％共
重合してもよい。また、重縮合方法としては、エステル
交換法、エステル反応法（直接重合法）のどちらを用い
ても良い。The polyester resin in the present invention is produced by polycondensation reaction of dicarboxylic acid and glycol, and examples of the dicarboxylic acid include terephthalic acid, isophthalic acid, naphthalenedicarboxylic acid, diphenyldicarboxylic acid, diphenylsulfonedicarboxylic acid and diphenoxyethane. Aromatic dicarboxylic acids such as dicarboxylic acid, 5-sodium sulfoisophthalic acid, phthalic acid, oxalic acid, succinic acid, adipic acid, sebacic acid, dimer acid, maleic acid, aliphatic dicarboxylic acids such as phthalic acid, cyclohexyne dicarboxylic acid Alicyclic dicarboxylic acids such as, and oxycarboxylic acids such as p-oxybenzoic acid. Examples of the glycol component include aliphatic glycols such as ethylene glycol, propanediol, butanediol, pentanediol, hexanediol and neopentyl glycol, alicyclic glycols such as cyclohexanedimethanol, and aromatic glycols such as bisphenol A and bisphenol S. Is mentioned. Two or more kinds of these dicarboxylic acid components and glycol components may be copolymerized in an amount of 0 to 25 mol%. As the polycondensation method, either the transesterification method or the ester reaction method (direct polymerization method) may be used.
【００１７】[0017]
【実施例】以下実施例に基づいて本発明をさらに具体的
に説明するが、本発明に使用したポリエステル樹脂の特
性の測定方法は次の通りである。
（１）ポリエステル樹脂の結晶化発熱量
示差走査熱量計（パーキンエルマー社製ＤＳＣ‐７型）
により、１０℃／分の昇温速度で測定した。
（２）ポリエステル樹脂の結晶化度
臭化ナトリウム水溶液による密度勾配管を作成し、２５
℃における密度を測定した。結晶化度Ｃは、完全非晶密
度ｄａ＝１．３３５ｇ／ｃｍ3 、完全結晶密度ｄｃ＝
１．４５５ｇ／ｃｍ3 として、測定した密度ｄより次式
により求めた。EXAMPLES The present invention will be described in more detail based on the following examples. The methods for measuring the properties of the polyester resin used in the present invention are as follows. (1) Crystallization calorific value of polyester resin Differential scanning calorimeter (DSC-7 type manufactured by Perkin Elmer)
Was measured at a heating rate of 10 ° C./min. (2) Crystallinity of Polyester Resin A density gradient tube made of an aqueous solution of sodium bromide was prepared.
The density at ° C was measured. Crystallinity C is completely amorphous density da = 1.335 g / cm 3 , perfect crystal density dc =
The value was 1.455 g / cm 3 and was determined from the measured density d by the following formula.
【００１８】結晶化度Ｃ＝［（ｄ−ｄａ）／（ｄｃ−ｄ
ａ）］×１００ ％
（３）ペレットの融着
結晶化装置から排出する際に格子（目開き６ｍｍ）を設
置し、４トン処理後それに捕捉された２連以上のペレッ
ト重量で融着度を判断する。実施例、比較例であげた各
フイルムの評価結果を表１にまとめた。Crystallinity C = [(d-da) / (dc-d)
a)] × 100% (3) Fusion of pellets A lattice (opening of 6 mm) is installed at the time of discharging from the crystallization apparatus, and after 4 tons of treatment, the fusion degree is determined by the weight of two or more pellets trapped in it. to decide. Table 1 shows the evaluation results of the films mentioned in Examples and Comparative Examples.
【００１９】(実施例１)融点２２３℃、結晶化発熱量１
５Ｊ／ｇのイソフタル酸を１０モル％共重合したポリエ
チレンテレフタレートを結晶化するに際し、内径Ｄが１
１００ｍｍの結晶化槽に、ガラス転移温度（７５℃）以
下の温度７０℃の熱風を風量２８ｍ2 ／分で連続的に供
給し、さらに攪拌軸４を回転させた状態で、ペレット投
入口より未結晶の該ポリエステル樹脂を粒面高さＬが４
４００ｍｍになるように投入した（Ｌ／Ｄ＝４．４）。
投入終了後熱風の温度を段階的に所定の温度（該樹脂の
結晶化温度）１２０℃に上げていき、上部温度（Ｔ１）
が１１０℃に到達後、計量排出装置７から連続的に計量
排出を始めた。この時の排出量（結晶化処理量）が平均
６００ｋｇ／ｈｒであり、結晶化領域温度（Ｔ２）を検
知し、下記式を用いて排出量の自動制御を行った。結晶
化装置に取りつけられた粒面レベル計８によりペレット
の粒面レベルを検知し、粒面高さＬが一定になるように
該未結晶ポリエステル樹脂ペレットを供給した。
結晶化処理量（ｋｇ）＝平均結晶化処理量（６００ｋ
ｇ）×（１−（Ｔ２−Ｔｃ）÷Ｔｃ）
（実施例２）粒面計の位置を変更し、ポリエステル樹脂
を粒面高さＬが３２００ｍｍ（Ｌ／Ｄ＝３．２）、熱風
風量を２０ｍ2 ／分、平均結晶化処理量を４００ｋｇ／
ｈｒにする以外は、実施例１と同様な方法で結晶化処理
を実施した。Example 1 Melting point 223 ° C., crystallization heat value 1
When crystallizing polyethylene terephthalate obtained by copolymerizing 10 mol% of 5 J / g of isophthalic acid, the inner diameter D was 1
A 100 mm crystallization tank was continuously supplied with hot air at a temperature of 70 ° C. that was lower than or equal to the glass transition temperature (75 ° C.) at an air volume of 28 m 2 / min. The crystalline polyester resin has a grain surface height L of 4
It was thrown in so that it might become 400 mm (L / D = 4.4).
After completion of the charging, the temperature of the hot air is gradually increased to a predetermined temperature (crystallization temperature of the resin) 120 ° C., and the upper temperature (T1)
After reaching 110 ° C., the metering and discharging device 7 started to measure and discharge continuously. The discharge amount (crystallization treatment amount) at this time was 600 kg / hr on average, the crystallization region temperature (T2) was detected, and the discharge amount was automatically controlled using the following formula. The grain surface level meter 8 attached to the crystallizer detected the grain surface level of the pellets, and the uncrystallized polyester resin pellets were supplied so that the grain surface height L became constant. Crystallization throughput (kg) = average crystallization throughput (600k
g) × (1− (T2-Tc) ÷ Tc) (Example 2) The position of the grain surface meter was changed, and the polyester resin had a grain surface height L of 3200 mm (L / D = 3.2) and a hot air flow rate. 20 m 2 / min, average crystallization treatment amount 400 kg /
Crystallization treatment was performed in the same manner as in Example 1 except that the time was changed to hr.
【００２０】（実施例３）粒面計の位置を変更し、ポリ
エステル樹脂を粒面高さＬが５６００ｍｍ（Ｌ／Ｄ＝
６．６）、熱風風量を３８ｍ2 ／分、平均結晶化処理量
を７５０ｋｇ／ｈｒにする以外は、実施例１と同様な方
法で結晶化を実施した。(Embodiment 3) By changing the position of the grain surface meter, the grain surface height L of the polyester resin was 5600 mm (L / D =
6.6) Crystallization was performed in the same manner as in Example 1 except that the hot air flow rate was 38 m 2 / min and the average crystallization treatment rate was 750 kg / hr.
【００２１】（実施例４）ポリエステル樹脂として、融
点２１５℃結晶化発熱量７Ｊ／ｇのシクロヘキサンジメ
タノール（ＣＨＤＭ）を１５モル％共重合したポリエチ
レンテレフタレート樹脂を使用し、熱風温度（結晶化温
度）を１１０℃にする以外は、実施例１と同様な方法で
結晶化を実施した。Example 4 As the polyester resin, a polyethylene terephthalate resin in which 15 mol% of cyclohexanedimethanol (CHDM) having a melting point of 215 ° C. and a heating value of crystallization of 7 J / g was copolymerized is used, and a hot air temperature (crystallization temperature) is used. Was crystallized in the same manner as in Example 1 except that the temperature was set to 110 ° C.
【００２２】（比較例１）結晶化処理量が平均６００ｋ
ｇ／ｈｒであり、自動制御を行わない以外は、実施例１
と同様な方法で結晶化を行った。中部温度が１１０〜１
４５℃と不安定になり、融着ペレットが０．５ｋｇ捕捉
された。(Comparative Example 1) The amount of crystallization treatment is 600 k on average.
g / hr, Example 1 except that automatic control is not performed
Crystallization was performed in the same manner as in. Middle temperature is 110-1
The temperature became unstable at 45 ° C., and 0.5 kg of the fused pellet was captured.
【００２３】[0023]
【表１】 [Table 1]
【００２４】[0024]
【発明の効果】ポリエステル樹脂ペレットを乾燥する際
に、ペレット同士の融着を防ぐために行う結晶化処理を
効率よく連続的に行うことが可能となる。When the polyester resin pellets are dried, it is possible to efficiently and continuously perform the crystallization treatment for preventing the fusion of the pellets.
【図１】本発明で好適に用いることのできる縦型結晶化
装置の一実施態様を示す概略図である。FIG. 1 is a schematic view showing an embodiment of a vertical crystallization apparatus that can be preferably used in the present invention.
【符号の説明】 １：結晶化槽 ２：ポリエステル樹脂ペレット投入口 ３：排気孔 ４：攪拌軸 ５：翼 ６：熱風供給口 ７：ペレット計量排出装置 ８：粒面レベル計 Ｔ１：装置内の上部の温度 Ｔ２：結晶化領域のペレット温度 Ｌ：ペレットの垂直方向の粒面高さ Ｄ：水平方向断面の直径[Explanation of symbols] 1: Crystallization tank 2: Polyester resin pellet input port 3: Exhaust hole 4: Stirrer shaft 5: wings 6: Hot air supply port 7: Pellet measuring and discharging device 8: Grain surface level meter T1: Temperature of the upper part in the device T2: pellet temperature in the crystallization region L: Vertical grain surface height of pellet D: Diameter of horizontal section
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4F201 AA24 AR06 AR13 BA04 BC19 BD05 BN03 BN24 BQ47 BQ57 4J029 AA01 AB07 AD08 KD01 KH03 KH06 KJ05 LB05 LB07 LB09 ─────────────────────────────────────────────────── ─── Continued front page F-term (reference) 4F201 AA24 AR06 AR13 BA04 BC19 BD05 BN03 BN24 BQ47 BQ57 4J029 AA01 AB07 AD08 KD01 KH03 KH06 KJ05 LB05 LB07 LB09
Claims (4)
ることにより加熱しながら連続的に結晶化処理を行うに
際し、装置内の樹脂結晶化領域の温度を検知し、連続的
に結晶化する単位時間当たりの排出量を前記検知温度に
基づいて変化させることにより、装置内の樹脂結晶化領
域の温度を樹脂結晶化温度（Ｔｃ）±２０℃の範囲に保
つことを特徴とするポリエステル樹脂の結晶化処理方
法。Claim: What is claimed is: 1. A unit for continuously crystallizing a polyester resin by detecting the temperature of a resin crystallization region in the apparatus when the polyester resin is continuously crystallized while being heated by supplying hot air into the apparatus. A polyester resin crystal characterized in that the temperature of the resin crystallization region in the apparatus is kept within a resin crystallization temperature (Tc) ± 20 ° C. by changing the discharge amount per time based on the detection temperature. Processing method.
り供給され、装置下部から結晶化されたポリエステル樹
脂が連続的に排出されることを特徴とする請求項１に記
載のポリエステル樹脂の結晶化処理方法。2. The crystallization of the polyester resin according to claim 1, wherein the polyester resin before crystallization is supplied from the upper part of the apparatus, and the crystallized polyester resin is continuously discharged from the lower part of the apparatus. Processing method.
（Ｌ）と水平方向断面の直径（Ｄ）の比（Ｌ／Ｄ）が３
以上６以下であることを特徴とする請求項１または２に
記載のポリエステル樹脂の結晶化処理方法。3. The ratio (L / D) of the grain surface height (L) of the vertical method of pellets in the apparatus to the diameter (D) of the horizontal section is 3.
The method for crystallizing a polyester resin according to claim 1 or 2, wherein the number is 6 or more.
ｇ以上であることを特徴とする請求項１〜３のいずれか
に記載のポリエステル樹脂の結晶化処理方法。4. The heat of crystallization of polyester resin is 1 J /
It is g or more, The crystallization treatment method of the polyester resin in any one of Claims 1-3 characterized by the above-mentioned.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001268405A JP2003071834A (en) | 2001-09-05 | 2001-09-05 | Crystallization treatment method for polyester resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001268405A JP2003071834A (en) | 2001-09-05 | 2001-09-05 | Crystallization treatment method for polyester resin |
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| Publication Number | Publication Date |
|---|---|
| JP2003071834A true JP2003071834A (en) | 2003-03-12 |
Family
ID=19094391
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010147176A1 (en) * | 2009-06-17 | 2010-12-23 | 東レ株式会社 | Method for producing crystallized polyester |
| US8029881B2 (en) | 2005-11-04 | 2011-10-04 | Serious Energy, Inc. | Radio frequency wave reducing material and methods for manufacturing same |
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| JP2012172011A (en) * | 2011-02-18 | 2012-09-10 | Toray Ind Inc | Method of producing polyester resin pellet |
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2001
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8181417B2 (en) | 2003-09-08 | 2012-05-22 | Serious Energy, Inc. | Acoustical sound proofing material and methods for manufacturing same |
| US8495851B2 (en) | 2004-09-10 | 2013-07-30 | Serious Energy, Inc. | Acoustical sound proofing material and methods for manufacturing same |
| US8029881B2 (en) | 2005-11-04 | 2011-10-04 | Serious Energy, Inc. | Radio frequency wave reducing material and methods for manufacturing same |
| US8424251B2 (en) | 2007-04-12 | 2013-04-23 | Serious Energy, Inc. | Sound Proofing material with improved damping and structural integrity |
| US8397864B2 (en) | 2007-04-24 | 2013-03-19 | Serious Energy, Inc. | Acoustical sound proofing material with improved fire resistance and methods for manufacturing same |
| JP5682309B2 (en) * | 2009-06-17 | 2015-03-11 | 東レ株式会社 | Method for producing crystallized polyester |
| WO2010147176A1 (en) * | 2009-06-17 | 2010-12-23 | 東レ株式会社 | Method for producing crystallized polyester |
| US8901275B2 (en) | 2009-06-17 | 2014-12-02 | Toray Industries, Inc. | Method for producing crystallized polyester |
| JP2012172011A (en) * | 2011-02-18 | 2012-09-10 | Toray Ind Inc | Method of producing polyester resin pellet |
| CN112240680A (en) * | 2019-07-17 | 2021-01-19 | 株式会社松井制作所 | Drying device for powder material and drying method for powder material |
| JP2021017989A (en) * | 2019-07-17 | 2021-02-15 | 株式会社松井製作所 | Device of drying granular material, and method of drying granular material |
| CN112240680B (en) * | 2019-07-17 | 2022-06-07 | 株式会社松井制作所 | Drying device for powder material and drying method for powder material |
| US11435140B2 (en) | 2019-07-17 | 2022-09-06 | Matsui Mfg. Co., Ltd. | Drying apparatus for granular materials and drying method for granular materials |
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