JP2002292626A - Method for manufacture of thermoplastic resin pellet - Google Patents

Method for manufacture of thermoplastic resin pellet

Info

Publication number
JP2002292626A
JP2002292626A JP2001095161A JP2001095161A JP2002292626A JP 2002292626 A JP2002292626 A JP 2002292626A JP 2001095161 A JP2001095161 A JP 2001095161A JP 2001095161 A JP2001095161 A JP 2001095161A JP 2002292626 A JP2002292626 A JP 2002292626A
Authority
JP
Japan
Prior art keywords
thermoplastic resin
screw
resin
extruder
region
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
Application number
JP2001095161A
Other languages
Japanese (ja)
Other versions
JP4329273B2 (en
Inventor
Katsumi Akaike
克美 赤池
Hiroshi Nagano
啓 永野
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.)
Toray Industries Inc
Original Assignee
Toray Industries Inc
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 Toray Industries Inc filed Critical Toray Industries Inc
Priority to JP2001095161A priority Critical patent/JP4329273B2/en
Publication of JP2002292626A publication Critical patent/JP2002292626A/en
Application granted granted Critical
Publication of JP4329273B2 publication Critical patent/JP4329273B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/285Feeding the extrusion material to the extruder
    • B29C48/297Feeding the extrusion material to the extruder at several locations, e.g. using several hoppers or using a separate additive feeding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a method for manufacture of a thermoplastic resin pellet which is excellent in quality wherein foreign matter such as a gelling material, carbide and the like is little by improving a conveying capacity and a self screening capacity of a double axes extruder while a method for manufacture of a polyamideimide resin pellet is especially provided. SOLUTION: When a thermoplastic resin pellet is manufactured by using a bent type double axes extruder, a melt-conveying area is shortened by carrying out a cylinder and screw arrangement without substantially providing a vacuum degassing area, and an attendant air amount to a transfer area is decreased by providing an extruding material-compressing area in a solid conveying area to control generation of a carbide. Further, by feeding the thermoplastic resin pellet having the almost same composition as that of thermoplastic resin pellet to be discharged by being melted and kneaded, a powder conveying capacity and a self screening capacity in the transfer area are improved to control the generation of the carbide.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、2軸押出し機を用
いて熱可塑性樹脂または熱可塑性樹脂と添加剤を溶融・
混練し、熱可塑性樹脂ペレットを製造する方法に関す
る。詳しくは、2軸押出し機の搬送能力とセルフクリー
ニング能力を改善し、ゲル化物・炭化物の発生を抑制す
る技術であって、ゲル化物・炭化物等の異物の少ない品
質の優れた熱可塑性樹脂ペレットの製造方法に関する。
特に、ポリアミドイミド樹脂ペレットの製造方法に関す
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method of melting a thermoplastic resin or a thermoplastic resin and additives using a twin screw extruder.
The present invention relates to a method for producing a thermoplastic resin pellet by kneading. More specifically, it is a technology to improve the conveying capacity and self-cleaning capacity of a twin-screw extruder and to suppress the generation of gelled materials and carbides. It relates to a manufacturing method.
In particular, it relates to a method for producing polyamide-imide resin pellets.

【0002】[0002]

【従来の技術】2軸押出し機を用いて溶融・混練し熱可
塑性樹脂ペレットを製造する場合、押出し材料に随伴さ
れた空気(以下、随伴空気)やスクリュー回転による剪
断発熱、押出し機シリンダーとスクリューの形状に起因
する滞留部とによって、押出し材料の一部が、酸化また
は熱分解してゲル化物・炭化物等(以下、炭化物)が生
成し製品としてのペレットに混入することがある。
2. Description of the Related Art When thermoplastic resin pellets are produced by melting and kneading using a twin-screw extruder, air accompanying the extruded material (hereinafter referred to as "associated air"), shear heat generated by screw rotation, extruder cylinder and screw In some cases, the extruded material may be oxidized or thermally decomposed to produce a gelled substance or carbide (hereinafter referred to as carbide) due to the stagnation portion caused by the shape of the material, and the extruded material may be mixed into pellets as a product.

【0003】この対策としては、2軸押出し機の吐出側
シリンダー先端内部に、生成した炭化物の濾過・除去を
目的としてフィルターが設けられ、定期的に交換するの
が一般的である。
As a countermeasure, a filter is generally provided inside the tip of the cylinder on the discharge side of the twin-screw extruder for the purpose of filtering and removing generated carbide, and the filter is regularly replaced.

【0004】随伴空気による酸化防止対策としては、窒
素ガスを押出し機の供給口等から供給し酸素濃度を低減
することによって、炭化物の生成を抑制する技術が特公
平6−206216号公報に開示されている。
As a countermeasure against oxidation by accompanying air, Japanese Patent Publication No. 6-206216 discloses a technique for suppressing the formation of carbides by supplying nitrogen gas from a supply port of an extruder and reducing the oxygen concentration. ing.

【0005】滞留部の少ないスクリュー形状としては、
セルフクリーニングタイプと称される深溝2条ネジの完
全噛み合いタイプのスクリューがある。このスクリュー
形状に関しては、例えば特開平8−258110号公報
には、スクリューフライト先端部の厚さを第1軸スクリ
ューと第2軸スクリューで各々変えることで、セルフク
リーニング性を向上させる技術が開示されている。
[0005] As a screw shape having a small staying part,
There is a screw of a completely meshing type of a double-groove double-thread screw called a self-cleaning type. Regarding this screw shape, for example, Japanese Patent Application Laid-Open No. 8-258110 discloses a technique of improving the self-cleaning property by changing the thickness of the tip end of a screw flight between a first screw and a second screw. ing.

【0006】また、粉体状材料の搬送能力を改善する技
術としては、たとえば、特開平6−166082号公報
や特開2000−25094号公報に、押出し機の空気
抜き装置や含有空気を脱気しながら材料を供給する手段
が開示されている。
[0006] As a technique for improving the ability to convey a powdery material, for example, Japanese Patent Application Laid-Open Nos. 6-166082 and 2000-25094 disclose an air bleeding device of an extruder and deaeration of contained air. Means for feeding the material are disclosed.

【0007】また特開平5−286011号公報には、
ホッパーシリンダー中にスクリューを設けて粉体を圧縮
して供給する方法、また、特開平11−291323号
公報には、押出し機投入前に材料粉体を振動篩いにより
分級する方法等が開示されている。
[0007] Also, Japanese Patent Application Laid-Open No. 5-286011 discloses that
A method in which a powder is compressed and supplied by providing a screw in a hopper cylinder, and a method in which a material powder is classified by a vibrating sieve before feeding into an extruder is disclosed in JP-A-11-291323. I have.

【0008】また、特開平10−180840号公報に
は、粉体状材料の搬送能力改善を目的としたスクリュー
形状が、実開平6−68815号公報には、フルフライ
トスクリューのフライト幅を広くして漏洩流を減少させ
るスクリュー構造が開示されている。
Japanese Patent Application Laid-Open No. Hei 10-180840 discloses a screw shape for improving the ability to transport powdery materials, and Japanese Utility Model Application Laid-Open No. Hei 6-68815 discloses a method for increasing the flight width of a full flight screw. A screw structure for reducing leakage flow is disclosed.

【0009】また、脱揮を効果的に行うため、2軸押出
し機には、シリンダーにベント孔を設けるのが一般的で
ある。
In order to effectively perform devolatilization, a twin-screw extruder is generally provided with a vent hole in a cylinder.

【0010】[0010]

【発明が解決しようとする課題】炭化物を除去するため
に、フィルターを設ける方法は、フィルターの交換が煩
雑であるだけでなく、たとえばポリアミドイミド樹脂等
の溶融粘度の高い樹脂ではフィルターを設置できず、ス
クリューとシリンダーの洗浄を頻繁に行う必要があっ
た。
The method of providing a filter for removing carbides not only requires complicated replacement of the filter but also makes it impossible to install the filter with a resin having a high melt viscosity such as a polyamideimide resin. In addition, it was necessary to frequently clean the screw and the cylinder.

【0011】また、窒素ガスを供給する方法は、随伴空
気を置換するだけの窒素ガスを供給すると、材料がスク
リュー流路を逆流・供給口へ吹上げる現象を引き起こし
やすく、搬送能力を低下かつ不安定にし、溶融樹脂の吐
出も不安定にする現象を引き起こすことがあった。とく
に材料が粉体である場合、搬送能力の低下、吐出の不安
定化につながりやすかった。
Further, in the method of supplying nitrogen gas, if nitrogen gas is supplied only to replace the accompanying air, the material tends to cause a phenomenon that the material flows up the screw flow path to the backflow / supply port, so that the carrying capacity is reduced and improper. In some cases, a phenomenon in which the ejection of the molten resin becomes stable and the ejection of the molten resin becomes unstable is caused. In particular, when the material is a powder, it tends to lead to a decrease in the carrying capacity and an unstable discharge.

【0012】また、セルフクリーニングタイプと称され
るスクリューであっても、2軸スクリュー同士の回転に
よる摩擦・摩耗を避けるために、スクリュー間には隙間
があるため、溶融樹脂搬送領域では、スクリューおよび
シリンダー表面への溶融樹脂の付着滞留を防止するには
不十分なものであった。
[0012] Even in the case of a screw called a self-cleaning type, there is a gap between the screws to avoid friction and abrasion due to the rotation of the twin screw. However, it was insufficient to prevent adhesion of the molten resin to the cylinder surface.

【0013】また、特開平6−166082号公報、特
開2000−25094号公報、特開平5−28601
1号公報、特開平11−291323号公報、特開平1
0−180840号公報、実開平6−68815号公報
等の搬送能力を改善する方法は、プロセスが煩雑になっ
たり汎用性に欠けるなどの欠点を有しているだけでな
く、炭化物防止に対しては、効果が小さかった。
Further, Japanese Patent Application Laid-Open Nos. 6-166082, 2000-25094, 5-28601
No. 1, JP-A-11-291323, JP-A-11-291323
The methods for improving the transfer capacity described in Japanese Patent Application Laid-Open Nos. 0-180840 and 6-68815 not only have drawbacks such as a complicated process or lack of versatility, but also have a disadvantage in preventing carbide. Was less effective.

【0014】また、ベント孔を設けると、シリンダー自
体が長くなり溶融樹脂の付着滞留量の総量が増えたり、
ベント孔の接続面・取付け面が溶融樹脂の滞留部とな
り、炭化物を増やすことがあった。
Further, when the vent hole is provided, the cylinder itself becomes longer, and the total amount of the deposited molten resin increases.
The connection surface / mounting surface of the vent hole became a stagnation portion of the molten resin, and sometimes increased the amount of carbide.

【0015】また、ベント孔は脱揮を主目的とするもの
であるから、単にベント孔を設置しないだけでは、材料
の脱揮が不十分となり、吐出が不安定になる問題があっ
た。
Further, since the vent hole is mainly intended for devolatilization, there is a problem that the devolatilization of the material becomes insufficient and the discharge becomes unstable if only the vent hole is not provided.

【0016】以上の問題に鑑みて、本発明の目的は、熱
可塑性樹脂材料を2軸押出し機を用いて溶融・混練し、
ペレット状熱可塑性樹脂を製造する方法において、炭化
物の生成を効果的に抑制する熱可塑性樹脂ペレットの製
造方法を提供することにある。
In view of the above problems, an object of the present invention is to melt and knead a thermoplastic resin material using a twin screw extruder,
It is an object of the present invention to provide a method for producing a thermoplastic resin pellet, which is a method for producing a thermoplastic resin pellet, which effectively suppresses the generation of carbides.

【0017】[0017]

【課題を解決するための手段】すなわち本発明は、次か
らなる。 (1)2軸押出し機を用いて、熱可塑性樹脂、または熱
可塑性樹脂と添加剤を溶融・混練して口金から吐出する
熱可塑性樹脂ペレットの製造方法であって、2軸押出し
機が下記、A〜Cの領域を有することを特徴とする熱可
塑性樹脂ペレットの製造方法。 A.2軸押出し機内において、熱可塑性樹脂の圧縮・昇
圧領域となるスクリューエレメントを設けた圧縮領域お
よび該圧縮領域に続けて降圧となるスクリューエレメン
トを設けた降圧領域を含み、搬送する熱可塑性樹脂のガ
ラス転移温度(Tg)未満あるいは融点(Tm)未満か
つ熱可塑性樹脂が実質的に溶融しない温度で予熱された
搬送領域。 B.熱可塑性樹脂が溶融する遷移領域。 C.実質的に真空脱揮領域が無く、溶融樹脂のシリンダ
ー内自由体積充満率が実質的に100%近くに達してい
る領域を溶融樹脂吐出口金側に接して形成された溶融樹
脂搬送領域。 (2)2軸押出機を用いて熱可塑性樹脂、または熱可塑
性樹脂と添加剤を、溶融・混練し熱可塑性樹脂ペレット
を製造するにあたり、溶融・混練されて吐出される熱可
塑性樹脂ペレットと略同じ組成を有する熱可塑性樹脂ペ
レットを供給口から、押出し機の溶融樹脂吐出量の1/
1000〜1/2に相当する割合で、供給することを特
徴とする熱可塑性樹脂ペレットの製造方法。 (3)溶融・混練されて吐出される熱可塑性樹脂ペレッ
トと略同じ組成を有する熱可塑性樹脂ペレットを供給口
から、押出し機の溶融樹脂吐出量の1/1000〜1/
2に相当する割合で、供給することを特徴とする(1)
記載の熱可塑性樹脂ペレットの製造方法。 (4)熱可塑性樹脂が粉体状であり、(イ)該粉体の平
均粒子径が0.1〜700μm、あるいは(ロ)嵩密度
が0.1〜0.8g/mlの性状をもつ粉体である
(1)〜(3)のいずれか記載の熱可塑性樹脂ペレット
の製造方法。(5)熱可塑性樹脂が、下記一般式(I )
That is, the present invention comprises the following. (1) A method for producing a thermoplastic resin or a thermoplastic resin pellet which is melted and kneaded with a thermoplastic resin and an additive and discharged from a die using a twin-screw extruder. A method for producing a thermoplastic resin pellet, comprising regions A to C. A. In the twin-screw extruder, a thermoplastic resin glass including a compression region provided with a screw element serving as a compression / pressurization region of a thermoplastic resin and a pressure reduction region provided with a screw element for reducing pressure following the compression region A transport region preheated at a temperature lower than the transition temperature (Tg) or lower than the melting point (Tm) and at which the thermoplastic resin does not substantially melt. B. Transition region where the thermoplastic resin melts. C. A molten resin conveying region formed substantially in contact with the molten resin discharge mouth side in a region where there is substantially no vacuum devolatilization region and the free volume filling rate of the molten resin in the cylinder substantially approaches 100%. (2) In producing a thermoplastic resin pellet by melting and kneading a thermoplastic resin or a thermoplastic resin and an additive using a twin-screw extruder, the thermoplastic resin pellet is melted, kneaded and discharged. The thermoplastic resin pellets having the same composition are supplied from the supply port to 1/100 of the molten resin discharge amount of the extruder.
A method for producing thermoplastic resin pellets, comprising supplying at a ratio corresponding to 1000 to 1/2. (3) The thermoplastic resin pellets having substantially the same composition as the thermoplastic resin pellets that are melted and kneaded and discharged are supplied from the supply port to 1/1000 to 1/100 of the molten resin discharge amount of the extruder.
It is characterized in that it is supplied at a rate corresponding to 2. (1)
A method for producing the thermoplastic resin pellet according to the above. (4) The thermoplastic resin is in the form of a powder, and (a) the powder has an average particle diameter of 0.1 to 700 μm, or (b) a bulk density of 0.1 to 0.8 g / ml. The method for producing a thermoplastic resin pellet according to any one of (1) to (3), which is a powder. (5) The thermoplastic resin has the following general formula (I)

【0018】[0018]

【化2】 Embedded image

【0019】(式中、Rは2価の芳香族残基および/ま
たは脂肪族残基)で表される繰り返し単位を主要構造単
位として有するポリアミドイミド樹脂粉体であることを
特徴とする、(1)〜(4)のいずれか記載の熱可塑性
樹脂ペレットの製造方法。
(Wherein, R is a divalent aromatic residue and / or an aliphatic residue) is a polyamideimide resin powder having a repeating unit represented by the following formula as a main structural unit. The method for producing a thermoplastic resin pellet according to any one of 1) to (4).

【0020】[0020]

【発明の実施の形態】以下、本発明を詳細に説明する。
図1に本発明で用いる2軸押出し機の例を示す。図1に
おいて1は押出機のシリンダー、2はスクリュー、3は
吐出口金、4と5は第1、第2供給口、6は脱揮口であ
って9の遷移領域での昇圧・溶融化に伴い逆流した随伴
空気の排出口となる。7は熱可塑性樹脂の圧縮・昇圧領
域となる圧縮領域、8は降圧領域である。
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.
FIG. 1 shows an example of a twin-screw extruder used in the present invention. In FIG. 1, 1 is a cylinder of an extruder, 2 is a screw, 3 is a discharge mouthpiece, 4 and 5 are first and second supply ports, 6 is a devolatilization port, and the pressure is raised and melted in a transition region 9. The outlet of the associated air that has flowed back along with it. Reference numeral 7 denotes a compression region which is a compression / pressure increase region of the thermoplastic resin, and reference numeral 8 denotes a pressure reduction region.

【0021】図1中に固体搬送(領域)を記載したが、
本発明の熱可塑性樹脂が実質的に溶融しない温度で予熱
された搬送領域とは、少なくとも7と8の領域を含む固
体搬送領域のことであり、本例では第1供給口を有する
ブロックから8までの領域を指す。9は昇圧・溶融を行
う遷移領域、10は溶融・混練領域、11は自由体積の
溶融樹脂充満率が実質的に100%近くとなる溶融樹脂
搬送領域である。
FIG. 1 shows the solid transportation (area).
The transfer region preheated at a temperature at which the thermoplastic resin of the present invention does not substantially melt is a solid transfer region including at least the regions 7 and 8, and in this example, the block from the block having the first supply port to the transfer region 8 Point to the area up to. Reference numeral 9 denotes a transition region in which the pressure is raised and melted, 10 denotes a melting / kneading region, and 11 denotes a molten resin transport region in which a free volume of the molten resin is substantially close to 100%.

【0022】図1中の固体搬送領域においては熱可塑性
樹脂が溶融しない温度で予熱を行う。ここで、熱可塑性
樹脂が実質的に溶融しない温度で予熱する方法としては
特に限定されず、たとえば、シリンダー温度を熱可塑性
樹脂の融点(Tm)かガラス転移温度(Tg)未満に設
定することであって、スクリュー回転による剪断発熱量
と加熱量を合わせても搬送する熱可塑性樹脂が溶融しな
いシリンダー温度を設定することで行う。
In the solid conveying area in FIG. 1, preheating is performed at a temperature at which the thermoplastic resin does not melt. Here, the method of preheating at a temperature at which the thermoplastic resin does not substantially melt is not particularly limited. For example, by setting the cylinder temperature to be lower than the melting point (Tm) of the thermoplastic resin or lower than the glass transition temperature (Tg). The temperature is set by setting a cylinder temperature at which the thermoplastic resin to be conveyed does not melt even when the amount of heat generated by shearing and the amount of heat generated by screw rotation are combined.

【0023】また、溶融樹脂搬送領域9〜11には、ベ
ント孔等が無く、実質的に真空脱揮領域は存在しない。
Further, the molten resin conveying regions 9 to 11 have no vent holes and the like, and have substantially no vacuum devolatilizing region.

【0024】次に、図2に従来の2軸押出し機の例(実
施例、比較例として使用)を示す。図2において1〜5
は図1と同じ。
Next, FIG. 2 shows an example of a conventional twin-screw extruder (used as an example and a comparative example). In FIG.
Is the same as FIG.

【0025】12は樹脂が溶融した領域における脱気口
であり、揮発分や残留モノマー・オリゴマー等を真空脱
揮し除去・排出したり、オープン脱気口または供給口と
しても使用される。
Reference numeral 12 denotes a degassing port in a region where the resin is melted, which is also used as an open degassing port or a supply port, for removing and discharging volatile components and residual monomers and oligomers by vacuum devolatilization.

【0026】13は昇圧・溶融される遷移領域、14は
シリンダー内の自由体積中の溶融樹脂充満率が実質的に
100%に近い領域、15は一旦昇圧溶融された樹脂の
降圧となる領域、16は昇圧領域、17は再び自由体積
の溶融樹脂充満率が実質的に100%近くとなる領域で
ある。
13 is a transition region where the pressure is raised and melted, 14 is a region where the filling ratio of the molten resin in the free volume in the cylinder is substantially close to 100%, 15 is a region where the pressure of the resin once raised and melted is reduced, Reference numeral 16 denotes a pressure rising region, and reference numeral 17 denotes a region where the filling ratio of the molten resin in the free volume becomes substantially close to 100% again.

【0027】ここで、溶融樹脂搬送領域は13〜17で
あり、ベント孔(真空脱揮口)12は溶融樹脂搬送領域
に設けられている。
Here, the molten resin transport area is 13 to 17, and a vent hole (vacuum devolatilization port) 12 is provided in the molten resin transport area.

【0028】図1、2における熱可塑性樹脂の圧縮領域
および遷移領域となるスクリューエレメントとしてはた
とえば、3条ネジタイプの場合はテーパ(深溝→浅溝)
スクリューや浅溝スクリュー、2条ネジタイプの場合は
逆ネジスクリューあるいはリード長を徐々に短くするス
クリューアレンジ、又はニーディングスクリュー等が好
ましく用いられる。原料が粉体の場合、圧縮領域に用い
る逆ネジスクリューはスクリュー径即ちフライト高さが
低いものが好ましく用いられる。
In FIG. 1 and FIG. 2, the screw element serving as the compression region and the transition region of the thermoplastic resin is, for example, a taper (deep groove → shallow groove) in the case of a triple thread type.
In the case of a screw, a shallow groove screw, and a double-start screw type, a reverse screw, a screw arrangement in which the lead length is gradually shortened, or a kneading screw is preferably used. When the raw material is a powder, the reverse screw used in the compression region preferably has a small screw diameter, that is, a flight height.

【0029】降圧領域となるスクリューエレメントとし
てはたとえば、3条ネジタイプの場合は逆テーパ(浅溝
→深溝)スクリューや深溝スクリュー、2条ネジタイプ
の場合はリード長を徐々に長くするスクリューアレンジ
等が好ましく用いられる。
As the screw element serving as the pressure-reducing region, for example, a reverse taper (shallow groove → deep groove) screw in the case of a three-start screw type, a deep groove screw, a screw arrangement in which the lead length is gradually increased in the case of a double-start screw type, etc. Is preferably used.

【0030】また、溶融・混練領域となるスクリューエ
レメントとしてはたとえば、3条ネジタイプの場合は浅
溝スクリュー、2条ネジタイプの場合は逆ネジスクリュ
ーやリード長の短いスクリュー、又はニーディングスク
リュー等が好ましく用いられる。
The screw element serving as the melting / kneading region is, for example, a shallow groove screw in the case of a three-thread screw type, a reverse screw, a screw having a short lead length, or a kneading screw in the case of a two-thread screw type. Is preferably used.

【0031】また、溶融樹脂搬送領域のスクリューエレ
メントとしてはたとえば、3条ネジタイプの場合は浅溝
スクリューやリード長の短いスクリュー、2条ネジタイ
プの場合はリード長の短いスクリュー等が好ましく用い
られる。
As the screw element in the molten resin conveying area, for example, a shallow groove screw in the case of a triple screw type, a screw having a short lead length, and a screw having a short lead length in the case of a double screw type are preferably used. .

【0032】本発明において熱可塑性樹脂とは、溶融押
出機によってペレット化することのできる熱可塑性樹脂
であって、たとえば、ポリアミドイミド、ポリフェニレ
ンサルファイド、ポリカーボネート、ポリオレフィン系
樹脂(ポリエチレン、ポリプロピレン等)、ポリスチレ
ン、ポリ塩化ビニリデン系樹脂、ポリアミド(ナイロン
6、ナイロン66等)、ポリエステル(ポリエチレンテ
レフタレート、ポリブチレンテレフタレート、液晶ポリ
マ等)、ポリアセタール、アクリロニトリル/スチレン
/ブタジエン系共重合体などである。
In the present invention, the thermoplastic resin is a thermoplastic resin that can be pelletized by a melt extruder, for example, polyamide imide, polyphenylene sulfide, polycarbonate, polyolefin resin (polyethylene, polypropylene, etc.), polystyrene Polyvinylidene chloride resin, polyamide (nylon 6, nylon 66, etc.), polyester (polyethylene terephthalate, polybutylene terephthalate, liquid crystal polymer, etc.), polyacetal, acrylonitrile / styrene / butadiene copolymer and the like.

【0033】特に、ポリアミドイミド樹脂が好ましく用
いられる。
In particular, a polyamideimide resin is preferably used.

【0034】熱可塑性樹脂の形状は、特に制限が無く、
粉体状、ペレット状、フレーク状など任意の形状のもの
を使用できるが、粉体状の原料が好ましく用いられる。
The shape of the thermoplastic resin is not particularly limited.
Any shape such as a powder, a pellet, and a flake can be used, but a powdery raw material is preferably used.

【0035】また添加剤とは、たとえばガラスビーズ、
ガラスフレーク、タルク、マイカ、二酸化チタンなどの
無機充填剤、滑剤、核剤、可塑剤、難燃剤、加工安定
剤、酸化防止剤、紫外線吸収剤、離型剤、着色剤、帯電
防止剤、表面処理剤、架橋剤、カップリング剤、および
摺動性改善のためのポリテトラフルオロエチレン、衝撃
性向上のためのゴム状樹脂などの第2成分の熱可塑性樹
脂など、熱可塑性樹脂と混練されうるすべての添加剤を
言う。
The additives include, for example, glass beads,
Inorganic fillers such as glass flakes, talc, mica, and titanium dioxide, lubricants, nucleating agents, plasticizers, flame retardants, processing stabilizers, antioxidants, ultraviolet absorbers, release agents, coloring agents, antistatic agents, surfaces It can be kneaded with a thermoplastic resin such as a treating agent, a crosslinking agent, a coupling agent, and a second component thermoplastic resin such as polytetrafluoroethylene for improving slidability, and a rubber-like resin for improving impact resistance. Say all additives.

【0036】次に、溶融・混練されて吐出される熱可塑
性樹脂ペレットと略同じ組成を有する熱可塑性樹脂ペレ
ットを供給口から、押出し機の溶融樹脂吐出量の1/1
000〜1/2に相当する割合で、供給することを特徴
とする熱可塑性樹脂ペレットの製造方法について述べ
る。
Next, thermoplastic resin pellets having substantially the same composition as the thermoplastic resin pellets to be discharged after being melted and kneaded are supplied from the supply port to a 1/1 of the molten resin discharge amount of the extruder.
A method for producing thermoplastic resin pellets, characterized in that the pellets are supplied at a rate corresponding to 000 to 2, will be described.

【0037】溶融・混練されて吐出される熱可塑性樹脂
と略同じ組成を有する熱可塑性樹脂ペレットとは、当該
押出し機を運転してダイス口金から吐出された樹脂と略
同じ組成を有するペレットであればよく、たとえば吐出
された樹脂そのもの、それに添加剤等を加えたものが使
用できる。もちろん、別途作製されたものであってもよ
い。
The thermoplastic resin pellets having substantially the same composition as the thermoplastic resin discharged after being melted and kneaded are pellets having substantially the same composition as the resin discharged from the die die by operating the extruder. What is necessary is just to use, for example, the discharged resin itself, and a resin to which an additive or the like is added. Of course, it may be separately manufactured.

【0038】溶融・混練されて吐出される熱可塑性樹脂
と略同じ組成を有する熱可塑性樹脂ペレットを供給する
ことにより、セルフクリーニング性が向上し、炭化物を
減少させることができる。当該ペレットの供給方法は特
に限定されないが、押出し機内に形成される遷移領域
(図1では9)よりも上流(駆動モータ側)に存在する
供給口から供給されるのが好ましい。供給口数は特に限
定されず、1ヶ所以上の供給口から供給されるのであれ
ば良い。
By supplying thermoplastic resin pellets having substantially the same composition as the thermoplastic resin discharged after being melted and kneaded, self-cleaning properties can be improved and carbides can be reduced. The method of supplying the pellets is not particularly limited, but it is preferable that the pellets are supplied from a supply port located upstream (on the side of the drive motor) of a transition region (9 in FIG. 1) formed in the extruder. The number of supply ports is not particularly limited as long as it is supplied from one or more supply ports.

【0039】溶融・混練されて吐出される熱可塑性樹脂
と略同じ組成を有する熱可塑性樹脂ペレットの供給量
は、押出し機の溶融樹脂吐出量の1/1000〜1/2
に相当する割合であり、好ましくは1/500〜1/
3、より好ましくは1/100〜1/4である。1/1
000未満では炭化物抑制効果が小さく、1/2を越え
ると生産性が低下するため好ましくない。
The supply amount of the thermoplastic resin pellet having substantially the same composition as the thermoplastic resin discharged after being melted and kneaded is 1/1000 to 1/2 of the molten resin discharge amount of the extruder.
And preferably 1/500 to 1/500.
3, more preferably 1/100 to 1/4. 1/1
If it is less than 000, the effect of suppressing carbide is small, and if it exceeds 1 /, the productivity is lowered, which is not preferable.

【0040】本発明に用いる熱可塑性樹脂としては、粉
体状であることが好ましく、平均粒子径が0.1〜70
0μm、あるいは嵩密度が0.1〜0.8g/mlの粉
体であることが好ましい。粉体状の原料を使用すること
で、本発明の炭化物抑制効果がより顕著に発揮される。
The thermoplastic resin used in the present invention is preferably in a powder form, and has an average particle diameter of 0.1 to 70.
It is preferable that the powder has a particle diameter of 0 μm or a bulk density of 0.1 to 0.8 g / ml. By using a powdery raw material, the carbide suppressing effect of the present invention is more remarkably exhibited.

【0041】ここで、平均粒子径と嵩密度は、以下の方
法で求めた値とする。平均粒子径は、粉体の粒度分布測
定をJIS Z8801に準拠して求めた。つまり、使
用した網篩いの篩い分け重量と篩いの公称目開きから算
出して求める。具体的には、例えばTyler篩いの呼
び(メッシュ)で#24/#32/#48/#60/#
200/#270の篩いを用いて乾式の機械式振動ふる
い分けを10分間行い、各篩い上の重量分率を求める。
その篩いわけ重量分率と各篩いの公称目開き(mm)
0.701/0.495/0.295/0.246/
0.074/0.053から平均粒子径を算出した。
Here, the average particle diameter and the bulk density are values determined by the following methods. The average particle size was determined by measuring the particle size distribution of the powder in accordance with JIS Z8801. That is, it is calculated from the sieving weight of the used sieve and the nominal size of the sieve. Specifically, for example, in a call (mesh) of a Tyler sieve, # 24 / # 32 / # 48 / # 60 / #
Dry mechanical vibration sieving is performed for 10 minutes using a 200 / # 270 sieve, and the weight fraction on each sieve is determined.
The weight fraction of the sieve and the nominal opening of each sieve (mm)
0.701 / 0.495 / 0.295 / 0.246 /
The average particle diameter was calculated from 0.074 / 0.053.

【0042】また、嵩密度は、JIS K6891に準
拠し求めた値とする。
The bulk density is a value determined according to JIS K6891.

【0043】本発明の熱可塑性樹脂としては、ポリアミ
ドイミド樹脂粉体を用いるのが、より好ましい。ここ
で、ポリアミドイミド樹脂としては、下記一般式(I )
(式中、Rは2価の芳香族残基および/または脂肪族残
基、ここで2価の芳香族残基および/または脂肪族残基
の具体例としては下記一般式(II)などを挙げることが
できる)で表される繰り返し単位を主な構造単位として
有するものが用いられる。
As the thermoplastic resin of the present invention, it is more preferable to use a polyamideimide resin powder. Here, as the polyamideimide resin, the following general formula (I)
(In the formula, R is a divalent aromatic residue and / or an aliphatic residue. Here, specific examples of the divalent aromatic residue and / or the aliphatic residue include the following general formula (II) and the like. And a repeating unit represented by the following formula (1) can be used as a main structural unit.

【0044】[0044]

【化3】 Embedded image

【0045】[0045]

【化4】 Embedded image

【0046】ポリアミドイミド樹脂粉体を用いること
で、本発明の炭化物抑制効果をより顕著に発揮させるこ
とができる。
By using the polyamideimide resin powder, the carbide suppressing effect of the present invention can be more remarkably exhibited.

【0047】[0047]

【実施例】以下、実施例・比較例を挙げて本発明を具体
的に説明する。
The present invention will be specifically described below with reference to examples and comparative examples.

【0048】まず、得られたペレットの評価方法を記載
する。本発明の炭化物抑制効果を評価する方法として
は、得られた熱可塑性樹脂ペレット中の炭化物混入量の
測定を行った。ペレット中の炭化物混入量の測定方法
は、旧大蔵省印刷局製造のきょう雑物測定図表を基準に
して、0.08〜0.5mm 2に相当する大きさのもの
を炭化物(小)とし、50gのペレットにつき、ペレッ
ト表面に炭化物(小)が1個以上存在したペレットの個
数を計数した。
First, the evaluation method of the obtained pellet is described.
I do. As a method for evaluating the carbide suppressing effect of the present invention
Is the amount of carbide mixed in the obtained thermoplastic resin pellets.
A measurement was made. Method for measuring the amount of carbide mixed in pellets
Is based on a foreign matter measurement chart manufactured by the former Ministry of Finance Printing Bureau.
0.08-0.5mm TwoOf a size equivalent to
Is a carbide (small) and pelletized per 50g pellet
Pellets with one or more carbides (small) on the surface
The number was counted.

【0049】この50gのペレットは、以下に示す実施
例、比較例における押出し機での運転開始後、吐出量が
約25kg/hとなる運転条件に設定し、連続2時間の
運転後にサンプリングしたものを用いた。
The pellets of 50 g were sampled after the start of the operation in the extruder in the following Examples and Comparative Examples, under the operating conditions where the discharge rate was about 25 kg / h, and after the continuous two hours of operation. Was used.

【0050】また混練効果の指標として、比エネルギー
(吐出量あたりの押出し機モータ動力:Kwh/kg)を算出
すると共に、得られたペレットの引っ張り強度をAST
M638に準拠して測定した。
As an index of the kneading effect, the specific energy (motor power of the extruder per discharge amount: Kwh / kg) is calculated, and the tensile strength of the obtained pellet is determined by AST.
It was measured according to M638.

【0051】更にペレット残存揮発分の量を、ペレット
の加熱減量を測定して比較した。次に示す実施例・比較
例でのポリアミドイミド樹脂については、熱風乾燥機
(HIGHTEMP OVEN HPS-222/TABAI MFG.CO.,LTD)を用いて
の当該ペレットの340℃2時間処理における加熱重量
減少値を残存揮発分として測定・評価した。
Further, the amount of the volatile matter remaining in the pellet was compared by measuring the loss on heating of the pellet. Regarding the polyamide-imide resin in the following Examples and Comparative Examples, the weight of the pellets decreased by heating at 340 ° C. for 2 hours using a hot air dryer (HIGHTEMP OVEN HPS-222 / TABAI MFG.CO., LTD). The value was measured and evaluated as residual volatile matter.

【0052】実施例1:本発明(1)の実施例(その
1) 使用した材料は、ポリアミドイミド樹脂粉体であって、
平均粒径0.39mm、嵩密度0.34g/mlのもの
を使用した。
Example 1: Example (1) of the present invention (1) The material used was a polyamide-imide resin powder,
Those having an average particle size of 0.39 mm and a bulk density of 0.34 g / ml were used.

【0053】このポリアミドイミド樹脂は、前記一般式
(I )(式中、Rは2価の芳香族残基および/または脂
肪族残基)で表される繰り返し単位を主な構造単位とし
て有し、2価の芳香族残基としてのRの構造が下記Aで
ある構造単位と、Bである構造単位の両方を有し、Aが
70モル%、Bが30モル%の割合であるポリアミドイ
ミド樹脂を使用した。
The polyamide-imide resin has, as a main structural unit, a repeating unit represented by the general formula (I) (wherein, R is a divalent aromatic residue and / or an aliphatic residue). A polyamideimide having both a structural unit in which R as a divalent aromatic residue is the following structural unit A and a structural unit in which B is A, wherein A is 70 mol% and B is 30 mol% Resin was used.

【0054】[0054]

【化5】 Embedded image

【0055】添加剤は、粉体状無機フィラーとして、二
酸化チタンTR700(富士チタン工業製)を、3重量
%添加した。
As an additive, 3% by weight of titanium dioxide TR700 (manufactured by Fuji Titanium Industry Co., Ltd.) was added as a powdery inorganic filler.

【0056】使用した2軸押出し機の構成としては、図
1の9個のブロックシリンダーから成り、第1番目と第
2番目のブロックシリンダーに供給口を有し、第6番目
のブロックシリンダーに脱気口(ただし、いわゆる強制
ベントでは無くナチュラルベントで自然排気とする)を
有する2条ネジタイプのスクリュー(直径56mm・長さ
1625mm)の同方向回転2軸押出機を使用した。
The structure of the twin-screw extruder used is composed of nine block cylinders shown in FIG. 1, with supply ports in the first and second block cylinders, and with the sixth block cylinder. A co-rotating twin-screw extruder having a double-screw type screw (diameter: 56 mm, length: 1625 mm) having an air port (however, natural exhaust instead of so-called forced vent and natural exhaust) was used.

【0057】第1番目シリンダー供給口(第1供給口)
からは、ポリアミドイミド樹脂粉体を25kg/h、第
2番目シリンダー供給口(第2供給口)からは酸化チタ
ンを0.75kg/hで定量供給した。
First cylinder supply port (first supply port)
, 25 kg / h of polyamide-imide resin powder, and 0.75 kg / h of titanium oxide from the second cylinder supply port (second supply port).

【0058】スクリューの配列は、スクリューの駆動側
端 (シリンダーの駆動側端と同じ)から720mmまでは
フルフライト・スクリュウの配列で、720mmから90
0mmまで(圧縮領域)は粉体の圧縮となる様に押出方向
に沿って漸次スクリュー・ピッチが小さくなるようなフ
ルフライト・スクリューとスクリュー外径の小さい(5
3mm)逆ネジスクリューを配列し、900mmから12
60mmまで(降圧領域)はフルフライト・スクリューの
配列で、1260mmから1350mmまで(遷移領域)は
漸次スクリュー・ピッチが小さくなるスクリューとニー
ディングスクリューを用いた溶融・混練させるためのス
クリュー・エレメントの配列で、1350mmから144
5mmまでは溶融後の混練り領域、1445mmから162
5mmまで(溶融樹脂搬送領域)はフルフライト・スクリ
ューで漸次スクリュー・ピッチが小さくなるようにして
押出圧力を発生させるようなスクリュー配列とした。
The arrangement of the screws is a full flight screw arrangement from the driving end of the screw (same as the driving end of the cylinder) to 720 mm, and from 720 mm to 90 mm.
Up to 0 mm (compression region), a full flight screw and a small screw outer diameter (5) in which the screw pitch gradually decreases along the extrusion direction so as to compress the powder.
3mm) Arrange the reverse screw, from 900mm to 12mm
Up to 60 mm (pressure reduction area) is a full flight screw arrangement, and from 1260 mm to 1350 mm (transition area), a screw element with a gradually decreasing screw pitch and a screw element arrangement for melting and kneading using a kneading screw. And from 1350mm to 144
Kneading area after melting up to 5 mm, from 1445 mm to 162
Up to 5 mm (the molten resin transport region), a screw arrangement was used in which the extrusion pressure was generated by gradually decreasing the screw pitch with a full flight screw.

【0059】樹脂の溶融・混練を行う領域に相当するシ
リンダー設定温度は330℃、固体搬送領域に相当する
シリンダー設定温度は200℃の外部加熱条件とし、、
モータ動力のトルク を目安にして前記吐出量(25k
g/h)を安定吐出できる範囲でスクリュー回転数の調
整を行った(およそ200rpmとした)。
Cylinder set temperature corresponding to the region where the resin is melted and kneaded is set to 330 ° C., and cylinder set temperature corresponding to the solid transfer region is set to 200 ° C. under external heating conditions.
The discharge amount (25 k
g / h) was adjusted within the range where stable discharge was possible (at approximately 200 rpm).

【0060】吐出した樹脂のカッティング方式はホット
カット方式とし、直径2.5mm、長さ2.5mmの円筒状
のペレットを得た(ペレット形状ばらつきは、長さ2.
5mmに対し±0.02mmであった。)。
The cutting method of the discharged resin was a hot cut method, and cylindrical pellets having a diameter of 2.5 mm and a length of 2.5 mm were obtained.
It was ± 0.02 mm for 5 mm. ).

【0061】比較例1:使用した2軸押出し機の構成と
しては、図2の9個のブロックシリンダーから成り、第
1番目と第2番目のブロックシリンダーに供給口を有
し、第6番目のブロックシリンダーに樹脂が溶融した領
域における脱気口12を有する2条ネジタイプのスクリ
ュー(直径56mm・長さ1625mm)の同方向回転2軸
押出機を使用した。
Comparative Example 1: The twin screw extruder used was composed of nine block cylinders as shown in FIG. 2, the first and second block cylinders had supply ports, and the sixth A co-rotating twin-screw extruder of a double thread type screw (diameter 56 mm, length 1625 mm) having a deaeration port 12 in a region where the resin was melted in the block cylinder was used.

【0062】スクリューの配列は、脱気口12で真空強
制脱揮を行うため、スクリューの駆動側端 (バレルの駆
動側端と同じ) から540mmまでは押出方向に沿って漸
次スクリュー・ピッチが小さくなるようなフルフライト
・スクリューの配列とし、540mm以降は遷移領域を経
て全て溶融状態になるようなスクリューアレンジとし
た。
In the arrangement of the screws, since the vacuum forcible devolatilization is performed at the deaeration port 12, the screw pitch gradually decreases along the extrusion direction from the driving end of the screw (same as the driving end of the barrel) to 540 mm. The screw arrangement was such that the full flight screws were arranged in such a manner that all of them became molten after 540 mm through the transition region.

【0063】脱気口12からは、溶融樹脂から発生した
揮発分を真空に引き、取り除いた。減圧度は、−720
mmHgとした。なお、使用した原料およびその他の条件
は、実施例1と同様とした。
From the vent 12, the volatile components generated from the molten resin were evacuated and removed. Decompression degree is -720
mmHg. The used raw materials and other conditions were the same as in Example 1.

【0064】実施例2:本発明(1)の実施例(その
2) 3条ネジタイプのスクリュー(直径44mm、長さ144
5mm)の同方向回転2軸押出機を使用したほかは、実施
例1と同様、図1の構成を採用(ただし、各々の領域の
長さはほぼ比例圧縮した)し熱可塑性樹脂ペレットを製
造した。
Example 2: Example of the present invention (1) (part 2) A three-thread screw (diameter: 44 mm, length: 144)
Except for using a 5 mm) co-rotating twin-screw extruder, the same configuration as in Example 1 was adopted (however, the length of each area was almost proportionally compressed) to produce thermoplastic resin pellets. did.

【0065】比較例2:3条ネジタイプのスクリュウ
(直径44mm、長さ1445mm)の同方向回転2軸押出
機を使用したほかは、比較例1と同様、図2の構成を採
用(ただし、各々の領域の長さはほぼ比例圧縮した)し
熱可塑性樹脂ペレットを製造した。
Comparative Example 2: The same configuration as in Comparative Example 1 was adopted except that a co-rotating twin-screw extruder having a three-thread screw (diameter: 44 mm, length: 1445 mm) was used (however, The length of each area was approximately proportionally compressed) to produce thermoplastic resin pellets.

【0066】実施例3:本発明(2)の実施例 比較例1と同じスクリュー・シリンダーアレンジ(配
列)の同方向回転2軸押出機を使用した。押し出し材料
の供給も比較例1と同じとした。
Example 3: Example of the present invention (2) A co-rotating twin-screw extruder having the same screw / cylinder arrangement (arrangement) as in Comparative Example 1 was used. The supply of the extruded material was the same as in Comparative Example 1.

【0067】この時、脱気口12を用い、溶融・混練さ
れて吐出される熱可塑性樹脂と同じ組成を有するペレッ
トを、スクリュー式フィーダーを用いて1kg/時間で
供給した。
At this time, pellets having the same composition as the thermoplastic resin to be melted, kneaded and discharged using the deaeration port 12 were supplied at a rate of 1 kg / hour using a screw type feeder.

【0068】実施例4:本発明(3)の実施例(その
1) 実施例2と同じスクリュー・シリンダーアレンジ(配
列)の同方向回転2軸押出機を使用した。押し出し材料
の供給も実施例2と同じとした。
Example 4: Example (3) of the present invention (3) A co-rotating twin-screw extruder having the same screw / cylinder arrangement (arrangement) as in Example 2 was used. The supply of the extruded material was the same as in Example 2.

【0069】この時、第6番目シリンダーのベント孔よ
り、溶融・混練されて吐出される熱可塑性樹脂と同じ組
成を有するペレットを、スクリュー式フィーダーを用い
て1kg/hでの供給した。
At this time, pellets having the same composition as the thermoplastic resin melted and kneaded and discharged from the sixth cylinder were supplied at a rate of 1 kg / h using a screw feeder.

【0070】実施例5:本発明(3)の実施例(その
2) 実施例4の運転条件で、第6番目シリンダーのベント孔
より、溶融・混練されて吐出される熱可塑性樹脂と同じ
組成を有するペレットをスクリュー式フィーダーを用い
て5kg/hで供給した。
Example 5: Example (3) of the present invention (3) Under the operating conditions of Example 4, the same composition as the thermoplastic resin which is melted, kneaded and discharged through the vent hole of the sixth cylinder. Was supplied at 5 kg / h using a screw feeder.

【0071】実施例6:本発明(3)の実施例(その
3) 実施例2と同じスクリュー・シリンダーアレンジ(配
列)の同方向回転2軸押出機を使用した。
Example 6: Example (3) of the present invention (3) A co-rotating twin-screw extruder having the same screw / cylinder arrangement (arrangement) as in Example 2 was used.

【0072】この時、第1番目の供給口より、溶融・混
練されて吐出される熱可塑性樹脂と同じ組成を有するペ
レットをスクリュー式フィーダーを用いて1kg/時間
で供給した。第2番目の供給口よりあらかじめ酸化チタ
ン含量3重量%となる様に配合した粉体状ポリアミドイ
ミド樹脂を25kg/時間で供給した。
At this time, pellets having the same composition as the thermoplastic resin to be melted and kneaded and discharged from the first supply port were supplied at a rate of 1 kg / hour using a screw type feeder. From the second supply port, a powdery polyamide-imide resin previously blended so as to have a titanium oxide content of 3% by weight was supplied at a rate of 25 kg / hour.

【0073】実施例1〜6および比較例1〜2で製造し
たペレットの炭化物測定結果等は、まとめて表1に示し
た。
Table 1 summarizes the results of carbide measurement of the pellets produced in Examples 1 to 6 and Comparative Examples 1 and 2.

【0074】[0074]

【表1】 [Table 1]

【0075】表1から、本発明の実施例1〜6において
は、炭化物量が少ないペレットが得られた。特に、実施
例4〜6では、炭化物の抑制に画期的効果が見られた。
From Table 1, in Examples 1 to 6 of the present invention, pellets having a small amount of carbide were obtained. In particular, in Examples 4 to 6, an epoch-making effect was observed in suppressing carbides.

【0076】また、実施例1〜6で得られるペレットの
揮発分は、真空ベントを行う比較例1〜2の方法と差が
なかった。引張り強度、破断伸びは同等であった。
The volatile components of the pellets obtained in Examples 1 to 6 were not different from those of Comparative Examples 1 and 2 in which vacuum venting was performed. The tensile strength and elongation at break were equivalent.

【0077】一方、真空ベントを行う方法(比較例1〜
2)では、炭化物量が多かった。
On the other hand, a method of performing a vacuum vent (Comparative Examples 1 to 5)
In 2), the amount of carbide was large.

【0078】[0078]

【発明の効果】本発明によれば、熱可塑性樹脂または熱
可塑性樹脂と添加剤を押出機内で混練して熱可塑性樹脂
ペレットを製造するにあたり、実質的に真空脱揮領域を
設けない2軸押出し機のスクリュー配列を行なうことに
よって、固体搬送領域を長くとることができ、得られる
熱可塑性樹脂ペレット中に含まれる炭化物を減少させる
ことができる。
According to the present invention, in producing thermoplastic resin pellets by kneading a thermoplastic resin or a thermoplastic resin and an additive in an extruder, twin-screw extrusion substantially not having a vacuum devolatilization region is provided. By performing the screw arrangement of the machine, the solid conveying area can be lengthened, and the carbide contained in the obtained thermoplastic resin pellets can be reduced.

【0079】また、溶融・混練されて吐出される熱可塑
性樹脂ペレットと略同じ組成を有する熱可塑性樹脂ペレ
ットを、押出し機の供給口から供給することによって、
得られる熱可塑性樹脂ペレット中に含まれる炭化物を大
幅に減少させることができる。
Further, thermoplastic resin pellets having substantially the same composition as the thermoplastic resin pellets which are melted, kneaded and discharged are supplied from the supply port of the extruder, whereby:
The carbide contained in the obtained thermoplastic resin pellets can be significantly reduced.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明の2軸押出し機のシリンダー・スクリュ
ーアレンジ(配列)例
FIG. 1 shows an example of a cylinder / screw arrangement of a twin-screw extruder according to the present invention.

【図2】従来の2軸押出し機のシリンダー・スクリュー
アレンジ(配列)例:実施例および比較例に使用
FIG. 2 shows a cylinder / screw arrangement (arrangement) example of a conventional twin-screw extruder: used in Examples and Comparative Examples

【符号の説明】[Explanation of symbols]

1:シリンダー 2:スクリュー 3:吐出口金 4:第1供給口 5:第2供給口 6:脱気口 7:圧縮領域 8:降圧領域 9:遷移領域 10:溶融・混練領域 11:溶融樹脂搬送領域 12:樹脂が溶融した領域における脱気口 13〜17:溶融体の搬送領域 1: Cylinder 2: Screw 3: Discharge mouthpiece 4: First supply port 5: Second supply port 6: Deaeration port 7: Compression area 8: Pressure reduction area 9: Transition area 10: Melting / kneading area 11: Molten resin Transport area 12: Deaeration port in area where resin melts 13-17: Transport area of melt

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 FI テーマコート゛(参考) B29K 503:06 B29K 503:06 C08L 79:08 C08L 79:08 Fターム(参考) 4F070 AA04 AA07 AA08 AA12 AA13 AA15 AA18 AA22 AA24 AA35 AA42 AA47 AA50 AA58 AC15 AC27 AC28 AC31 FB06 FC06 4F201 AA40 AB11 AC04 AP05 BA01 BA02 BC01 BC13 BC17 BC19 BC37 BK02 BK13 BK26 BK36 BK40 BK49 BL09 BL43 BN31──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) B29K 503: 06 B29K 503: 06 C08L 79:08 C08L 79:08 F term (Reference) 4F070 AA04 AA07 AA08 AA12 AA13 AA15 AA18 AA22 AA24 AA35 AA42 AA47 AA50 AA58 AC15 AC27 AC28 AC31 FB06 FC06 4F201 AA40 AB11 AC04 AP05 BA01 BA02 BC01 BC13 BC17 BC19 BC37 BK02 BK13 BK26 BK36 BK40 BK49 BL09 BL43 BN31

Claims (5)

【特許請求の範囲】[Claims] 【請求項1】2軸押出し機を用いて、熱可塑性樹脂、ま
たは熱可塑性樹脂と添加剤を溶融・混練して口金から吐
出する熱可塑性樹脂ペレットの製造方法であって、2軸
押出し機が下記、A〜Cの領域を有することを特徴とす
る熱可塑性樹脂ペレットの製造方法。 A.2軸押出し機内において、熱可塑性樹脂の圧縮・昇
圧領域となるスクリューエレメントを設けた圧縮領域お
よび該圧縮領域に続けて降圧となるスクリューエレメン
トを設けた降圧領域を含み、搬送する熱可塑性樹脂のガ
ラス転移温度(Tg)未満あるいは融点(Tm)未満か
つ熱可塑性樹脂が実質的に溶融しない温度で予熱された
搬送領域。 B.熱可塑性樹脂が溶融する遷移領域。 C.実質的に真空脱揮領域が無く、溶融樹脂のシリンダ
ー内自由体積充満率が実質的に100%近くに達してい
る領域を溶融樹脂吐出口金側に接して形成された溶融樹
脂搬送領域。
1. A method for producing a thermoplastic resin pellet by melting and kneading a thermoplastic resin or a thermoplastic resin and an additive by using a twin-screw extruder and discharging the molten resin from a die. A method for producing a thermoplastic resin pellet, comprising the following regions A to C. A. In a twin-screw extruder, a thermoplastic resin glass including a compression area provided with a screw element serving as a compression / pressure increase area of a thermoplastic resin and a pressure reduction area provided with a screw element for reducing pressure following the compression area. A transport region preheated at a temperature lower than the transition temperature (Tg) or lower than the melting point (Tm) and at which the thermoplastic resin does not substantially melt. B. Transition region where the thermoplastic resin melts. C. A molten resin conveying region formed substantially in contact with the molten resin discharge mouthpiece in a region where there is substantially no vacuum devolatilization region and the free volume filling rate of the molten resin in the cylinder substantially approaches 100%.
【請求項2】2軸押出機を用いて熱可塑性樹脂、または
熱可塑性樹脂と添加剤を、溶融・混練し熱可塑性樹脂ペ
レットを製造するにあたり、溶融・混練されて吐出され
る熱可塑性樹脂ペレットと略同じ組成を有する熱可塑性
樹脂ペレットを供給口から、押出し機の溶融樹脂吐出量
の1/1000〜1/2に相当する割合で、供給するこ
とを特徴とする熱可塑性樹脂ペレットの製造方法。
2. A thermoplastic resin pellet which is melted and kneaded and discharged when a thermoplastic resin or a thermoplastic resin and an additive are melted and kneaded using a twin screw extruder. A thermoplastic resin pellet having substantially the same composition as the above is supplied from a supply port at a rate corresponding to 1/1000 to 1/2 of a molten resin discharge amount of an extruder. .
【請求項3】溶融・混練されて吐出される熱可塑性樹脂
ペレットと略同じ組成を有する熱可塑性樹脂ペレットを
供給口から、押出し機の溶融樹脂吐出量の1/1000
〜1/2に相当する割合で、供給することを特徴とする
請求項1記載の熱可塑性樹脂ペレットの製造方法。
3. A thermoplastic resin pellet having substantially the same composition as thermoplastic resin pellets which are melted and kneaded and discharged is supplied from a supply port to a supply port of 1/1000 of a molten resin discharge amount of an extruder.
The method for producing thermoplastic resin pellets according to claim 1, wherein the thermoplastic resin pellets are supplied at a rate corresponding to 1 /.
【請求項4】熱可塑性樹脂が粉体状であり、(イ)該粉
体の平均粒子径が0.1〜700μm、あるいは(ロ)
嵩密度が0.1〜0.8g/mlの性状をもつ粉体であ
る請求項1〜3のいずれか記載の熱可塑性樹脂ペレット
の製造方法。
4. The thermoplastic resin is in the form of a powder, and (A) the powder has an average particle diameter of 0.1 to 700 μm;
The method for producing thermoplastic resin pellets according to any one of claims 1 to 3, wherein the powder has a bulk density of 0.1 to 0.8 g / ml.
【請求項5】熱可塑性樹脂が、下記一般式(I ) 【化1】 (式中、Rは2価の芳香族残基および/または脂肪族残
基)で表される繰り返し単位を主要構造単位として有す
るポリアミドイミド樹脂粉体であることを特徴とする、
請求項1〜4のいずれか記載の熱可塑性樹脂ペレットの
製造方法。
5. The thermoplastic resin is represented by the following general formula (I): (Wherein, R is a divalent aromatic residue and / or an aliphatic residue) a polyamideimide resin powder having a repeating unit represented by the following formula as a main structural unit:
A method for producing a thermoplastic resin pellet according to claim 1.
JP2001095161A 2001-03-29 2001-03-29 Method for producing thermoplastic resin pellets Expired - Lifetime JP4329273B2 (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008155570A (en) * 2006-12-26 2008-07-10 Mitsubishi Engineering Plastics Corp Manufacturing process of thermoplastic resin composition
JP2011051349A (en) * 2007-05-01 2011-03-17 Agri Future Joetsu Co Ltd Manufacturing apparatus for polymeric composite material and manufacturing method for the same
JP2020131630A (en) * 2019-02-22 2020-08-31 東レ株式会社 Manufacturing method of polyamide-imide resin pellet
JP2020175649A (en) * 2019-04-19 2020-10-29 旭化成株式会社 Manufacturing method of polyphenylene ether-based resin composition
CN112743702A (en) * 2019-10-30 2021-05-04 住友化学株式会社 Resin pellet and method for producing resin pellet
CN113474138A (en) * 2019-03-29 2021-10-01 陶氏环球技术有限责任公司 Hollow pellets and soaking method

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JPS5358965U (en) * 1976-10-21 1978-05-19
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JPH07214547A (en) * 1994-02-04 1995-08-15 Mitsui Toatsu Chem Inc Preparation of thermoplastic resin pellet
JPH1024483A (en) * 1996-07-12 1998-01-27 Asahi Chem Ind Co Ltd Powder extruder and extruding method using the extruder
JPH10180840A (en) * 1996-12-24 1998-07-07 Asahi Chem Ind Co Ltd Highly productive extruder and extrusion method using that
JP2000015628A (en) * 1998-07-06 2000-01-18 Toshiba Mach Co Ltd Screw of twin-screw extruder for kneading inorganic filler

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5358965U (en) * 1976-10-21 1978-05-19
JPH06190891A (en) * 1992-08-31 1994-07-12 Hiroshi Morohashi Plasticization apparatus and plasticization method using the same
JPH07214547A (en) * 1994-02-04 1995-08-15 Mitsui Toatsu Chem Inc Preparation of thermoplastic resin pellet
JPH1024483A (en) * 1996-07-12 1998-01-27 Asahi Chem Ind Co Ltd Powder extruder and extruding method using the extruder
JPH10180840A (en) * 1996-12-24 1998-07-07 Asahi Chem Ind Co Ltd Highly productive extruder and extrusion method using that
JP2000015628A (en) * 1998-07-06 2000-01-18 Toshiba Mach Co Ltd Screw of twin-screw extruder for kneading inorganic filler

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008155570A (en) * 2006-12-26 2008-07-10 Mitsubishi Engineering Plastics Corp Manufacturing process of thermoplastic resin composition
JP2011051349A (en) * 2007-05-01 2011-03-17 Agri Future Joetsu Co Ltd Manufacturing apparatus for polymeric composite material and manufacturing method for the same
JP2020131630A (en) * 2019-02-22 2020-08-31 東レ株式会社 Manufacturing method of polyamide-imide resin pellet
JP7236049B2 (en) 2019-02-22 2023-03-09 東レ株式会社 METHOD FOR MANUFACTURING POLYAMIDEIMIDE RESIN PELLET
CN113474138A (en) * 2019-03-29 2021-10-01 陶氏环球技术有限责任公司 Hollow pellets and soaking method
JP2020175649A (en) * 2019-04-19 2020-10-29 旭化成株式会社 Manufacturing method of polyphenylene ether-based resin composition
JP7409900B2 (en) 2019-04-19 2024-01-09 旭化成株式会社 Method for producing polyphenylene ether resin composition
CN112743702A (en) * 2019-10-30 2021-05-04 住友化学株式会社 Resin pellet and method for producing resin pellet

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