JP2008093919A - Method for producing mini-pellet made of polypropylene resin composition - Google Patents
Method for producing mini-pellet made of polypropylene resin composition Download PDFInfo
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- JP2008093919A JP2008093919A JP2006277219A JP2006277219A JP2008093919A JP 2008093919 A JP2008093919 A JP 2008093919A JP 2006277219 A JP2006277219 A JP 2006277219A JP 2006277219 A JP2006277219 A JP 2006277219A JP 2008093919 A JP2008093919 A JP 2008093919A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/80—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling at the plasticising zone, e.g. by heating cylinders
- B29C48/802—Heating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means 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
- B29C48/397—Means 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 a single screw
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means 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
- B29C48/40—Means 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
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- Processes Of Treating Macromolecular Substances (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
本発明は、単軸押出機において安定的に高吐出量で溶融混練することができ、粒重量が均一に揃ったポリプロピレン系樹脂組成物からなるミニペレットの製造方法に関する。 The present invention relates to a method for producing mini-pellets made of a polypropylene resin composition that can be stably melt-kneaded at a high discharge rate in a single screw extruder and have a uniform grain weight.
ビーズ法型内発泡成形法において、ポリプロピレン系樹脂に水添石油樹脂を添加した樹脂組成物からなる予備発泡粒子が、型内発泡成形時の成形蒸気圧を低減させる効果があることが知られている(特許文献1)。しかし、予備発泡粒子を作製するための樹脂粒子、いわゆるミニペレットを製造する際、ポリプロピレン系樹脂と水添石油樹脂を単軸押出機で溶融混練して工業生産に耐える高吐出量で押出し、均一なペレット形状に成形することは困難であるため、一般的には、マスターバッチや二軸押出機が用いられる。例えば、特許文献2はフィルムの製法に関する文献であるが、ポリプロピレン系樹脂と水添石油樹脂を押出機の温度を210℃にして単軸押出機でペレットを作製することが開示されている。当該文献ではシートを作製するためのペレットを製法するものであるため、ペレットの粒重量の均一性については特に要求されず、言及もされていない。しかしながら、当該文献の実施例の記載から推察するに、ポリプロピレン系樹脂に水添石油樹脂15〜30重量%を配合しているため、ストランドが柔らかくなりすぎて得られるペレットの形状が不均一になり、しかも、吐出量を上げるとペレット同士が融着するため、低吐出量でしかペレット化できないことが予想される。 In the in-mold foam molding method for beads, it is known that pre-expanded particles made of a resin composition obtained by adding a hydrogenated petroleum resin to a polypropylene resin have the effect of reducing the molding vapor pressure during in-mold foam molding. (Patent Document 1). However, when producing resin particles for making pre-expanded particles, so-called mini-pellets, polypropylene resin and hydrogenated petroleum resin are melt-kneaded with a single screw extruder and extruded at a high discharge rate that can withstand industrial production. In general, a master batch or a twin-screw extruder is used because it is difficult to form the pellet into a simple pellet shape. For example, Patent Document 2 is a document relating to a film production method, but discloses that a polypropylene resin and a hydrogenated petroleum resin are used to produce pellets with a single screw extruder at an extruder temperature of 210 ° C. In this document, since a pellet for producing a sheet is manufactured, the uniformity of the pellet weight is not particularly required or mentioned. However, as inferred from the description of the examples of the document, since the hydrogenated petroleum resin 15 to 30% by weight is blended with the polypropylene-based resin, the shape of the pellet obtained when the strand becomes too soft becomes non-uniform. Moreover, since the pellets are fused when the discharge amount is increased, it is expected that the pellets can be formed only with a low discharge amount.
一方、予備発泡粒子は粒重量が均一であることが要求され、そのためには樹脂粒子の粒重量が均一であることが要求される。しかしながら、このような状態では、予備発泡粒子に適した粒重量が均一に揃ったミニペレットの製造はできない。
本発明の目的は、単軸押出機でポリプロピレン系樹脂と水添石油樹脂を安定的に高吐出で溶融混練することができ、予備発泡粒子に適した粒重量が均一に揃ったミニペレットの製造方法を提供することにある。 The object of the present invention is to produce mini-pellets that can stably melt and knead polypropylene resin and hydrogenated petroleum resin with high discharge in a single-screw extruder, and have uniform particle weights suitable for pre-expanded particles. It is to provide a method.
本発明者らは、かかる課題を達成すべく鋭意検討を行った。その結果、ポリプロピレン系樹脂組成物中、水添石油樹脂の添加量を1〜10重量%とし、かつ単軸押出機のフィード部のシリンダー温度を200℃以上にすることにより、ポリプロピレン系樹脂組成物からなるミニペレットが均一な粒重量で得られることを見出し、本発明を完成するに至った。 The inventors of the present invention have intensively studied to achieve this problem. As a result, in the polypropylene resin composition, the amount of hydrogenated petroleum resin added is 1 to 10% by weight, and the cylinder temperature of the feed part of the single screw extruder is set to 200 ° C. or higher, whereby the polypropylene resin composition The present inventors have found that mini-pellets made of can be obtained with a uniform grain weight and have completed the present invention.
即ち本発明の第1は、単軸押出機で溶融混練して、水添石油樹脂1〜10重量%を含んでなるポリプロピレン系樹脂組成物からなるミニペレットを製造する方法であって、押出機フィード部のシリンダー温度を200℃以上とすることを特徴とするポリプロピレン系樹脂組成物からなるミニペレットの製造方法に関する。 That is, the first of the present invention is a method of producing mini-pellets made of a polypropylene resin composition containing 1 to 10% by weight of hydrogenated petroleum resin by melt-kneading with a single screw extruder, The present invention relates to a method for producing mini-pellets made of a polypropylene resin composition, characterized in that the cylinder temperature of the feed section is 200 ° C. or higher.
好ましい実施態様としては、
(1)前記水添石油樹脂の軟化点が110℃以上である、
(2)前記水添石油樹脂が脂環式系水添石油樹脂であることを特徴とする、
前記記載のミニペレットの製造方法に関する。
As a preferred embodiment,
(1) The softening point of the hydrogenated petroleum resin is 110 ° C. or higher.
(2) The hydrogenated petroleum resin is an alicyclic hydrogenated petroleum resin,
The present invention relates to a method for producing the mini-pellets described above.
本発明のミニペレットの製造方法によれば、単軸押出機でポリプロピレン系樹脂と水添石油樹脂を安定的に高吐出量で溶融混練することができ、粒重量が均一に揃ったミニペレットを提供することが出来る。 According to the method for producing mini-pellets of the present invention, a polypropylene resin and a hydrogenated petroleum resin can be stably melt-kneaded at a high discharge rate with a single-screw extruder, and mini-pellets having a uniform grain weight can be obtained. Can be provided.
本発明は、単軸押出機で溶融混練して、水添石油樹脂1〜10重量%を含んでなるポリプロピレン系樹脂組成物からなるミニペレットを製造する方法であって、押出機フィード部のシリンダー温度を200℃以上とすることを特徴とするポリプロピレン系樹脂組成物からなるミニペレットの製造方法である。 The present invention relates to a method for producing mini-pellets made of a polypropylene resin composition containing 1 to 10% by weight of a hydrogenated petroleum resin by melt-kneading with a single screw extruder, the cylinder of the extruder feed section It is a manufacturing method of the mini pellet which consists of a polypropylene resin composition characterized by making temperature 200 degreeC or more.
本発明のポリプロピレン系樹脂としては、単量体として、プロピレンを好ましくは、90重量%以上、より好ましくは95重量%以上含むものであればよく、例えば、プロピレン単独重合体、エチレン−プロピレンランダム共重合体、プロピレン−ブテンランダム共重合体、エチレン−プロピレンブロック共重合体、エチレン−プロピレン−ブテン三元共重合体など、さらにはこれらの変性物が挙げられる。なお、合成法に特に制限はなく、これらのポリプロピレン系樹脂は通常公知の方法、すなわちMgCl2型担持型触媒を用いるBASF法、AMDCD法、UCC法、ハイポール法等の気相重合法の他、高活性なメタロセン触媒を用いた方法や、従来型のTiCl3触媒を利用した方法等で製造できる。 The polypropylene resin of the present invention may contain propylene as a monomer, preferably 90% by weight or more, more preferably 95% by weight or more. For example, propylene homopolymer, ethylene-propylene random copolymer. Examples thereof include polymers, propylene-butene random copolymers, ethylene-propylene block copolymers, ethylene-propylene-butene terpolymers, and these modified products. There is no particular limitation on the synthesis method, and these polypropylene resins are generally known methods, that is, gas phase polymerization methods such as BASF method, AMDCD method, UCC method, and Hypol method using a MgCl 2 type supported catalyst, It can be produced by a method using a highly active metallocene catalyst or a method using a conventional TiCl 3 catalyst.
また、ポリプロピレン系樹脂組成物中にポリプロピレン系樹脂以外の他の合成樹脂を添加しても良い。ポリプロピレン系樹脂以外の他の合成樹脂としては、高密度ポリエチレン、中密度ポリエチレン、低密度ポリエチレン、直鎖状低密度ポリエチレン、直鎖状超低密度ポリエチレン、エチレン−酢酸ビニル共重合体、エチレン−アクリル酸共重合体、エチレン−メタアクリル酸共重合体等のエチレン系樹脂、ポリスチレン、スチレン−無水マレイン酸共重合体等のスチレン系樹脂等が例示される。 Moreover, you may add synthetic resins other than a polypropylene resin in a polypropylene resin composition. Synthetic resins other than polypropylene resins include high density polyethylene, medium density polyethylene, low density polyethylene, linear low density polyethylene, linear ultra-low density polyethylene, ethylene-vinyl acetate copolymer, ethylene-acrylic. Examples thereof include ethylene resins such as acid copolymers and ethylene-methacrylic acid copolymers, and styrene resins such as polystyrene and styrene-maleic anhydride copolymers.
本発明におけるポリプロピレン系樹脂の融点に特に制限はないが、130℃以上170℃以下が好ましく、135℃以上160℃以下がより好ましく、140℃以上150℃以下がさらに好ましい。 Although there is no restriction | limiting in particular in melting | fusing point of the polypropylene resin in this invention, 130 to 170 degreeC is preferable, 135 to 160 degreeC is more preferable, 140 to 150 degreeC is further more preferable.
本発明におけるポリプロピレン系樹脂のメルトインデックスは特に制限はなく、好ましくは0.2g/10min以上50g/10min以下、より好ましくは1g/10min以上30g/10min以下、さらに好ましくは3g/10min以上12g/10min以下である。メルトインデックスが0.2g/10min未満である場合、溶融粘度が高すぎて高発泡の予備発泡粒子が得られにくい傾向にあり、50g/10minより大きい場合、発泡時の樹脂の伸びに対する溶融粘度が低く、破泡しやすい傾向にある。メルトインデックスは、例えば、有機過酸化物の使用などにより調整する事ができる。 There is no restriction | limiting in particular in the melt index of the polypropylene resin in this invention, Preferably it is 0.2g / 10min or more and 50g / 10min or less, More preferably, it is 1g / 10min or more and 30g / 10min or less, More preferably, it is 3g / 10min or more and 12g / 10min. It is as follows. When the melt index is less than 0.2 g / 10 min, the melt viscosity tends to be too high and it is difficult to obtain highly expanded pre-expanded particles. When the melt index is greater than 50 g / 10 min, the melt viscosity with respect to the elongation of the resin at the time of expansion is low. It is low and tends to break. The melt index can be adjusted, for example, by using an organic peroxide.
本発明に用いる水添石油樹脂とは、石油類の熱分解により生成する分解油留分を混合物のままカチオン的に重合して得られる熱可塑性樹脂をいい、シクロペンタジエン等の石油系不飽和炭化水素、高級オレフィン系炭化水素、または芳香族炭化水素等を主原料(50重量%以上)とする石油樹脂を水素添加したものをいう。また、水添石油樹脂の中でも、水添率80%以上、特に90%以上のものが好ましい。さらに本発明の水添石油樹脂の軟化点は110℃以上であることが好ましい。ここでの軟化点とはJIS−K2207(環球式)に準拠した測定値である。軟化点が110℃未満では押出機フィード部のシリンダー温度との差が大きすぎるため水添石油樹脂がはやく溶け、ポリプロピレン樹脂への溶解が不均一になる場合がある。水添石油樹脂の添加量としては、ポリプロピレン系樹脂組成物中、1〜10重量%であり、1〜5重量%が好ましい。 The hydrogenated petroleum resin used in the present invention refers to a thermoplastic resin obtained by cationically polymerizing a cracked oil fraction generated by thermal decomposition of petroleum, and is a petroleum unsaturated carbonization such as cyclopentadiene. This refers to hydrogenated petroleum resin containing hydrogen, higher olefinic hydrocarbons, or aromatic hydrocarbons as the main raw material (50% by weight or more). Of the hydrogenated petroleum resins, those having a hydrogenation rate of 80% or more, particularly 90% or more are preferred. Furthermore, the softening point of the hydrogenated petroleum resin of the present invention is preferably 110 ° C. or higher. The softening point here is a measured value based on JIS-K2207 (ring and ball type). If the softening point is less than 110 ° C., the difference from the cylinder temperature of the extruder feed section is too large, so that the hydrogenated petroleum resin dissolves quickly and the dissolution in the polypropylene resin may become uneven. The addition amount of the hydrogenated petroleum resin is 1 to 10% by weight, preferably 1 to 5% by weight, in the polypropylene resin composition.
水添石油樹脂は、脂肪族系水添石油樹脂、脂環式系水添石油樹脂、芳香族系水添石油樹脂に大別できる。 Hydrogenated petroleum resins can be broadly classified into aliphatic hydrogenated petroleum resins, alicyclic hydrogenated petroleum resins, and aromatic hydrogenated petroleum resins.
脂肪族系水添石油樹脂とは、C4またはC5留分のオレフィン、ジオレフィン、例えば主要成分としてイソブチレン、ブタジエン、イソプレン、ピペリンなどを重合原料とする樹脂である。代表的な市販品としては、クリアロンP−125(ヤスハラケミカル社製)、クイントンA100(日本ゼオン(株)製)、クイントンK100(日本ゼオン(株)製)、ハイレッツC110X(三井化学(株)製)、ハイレッツR100X(三井化学(株)製)、タッキロール(住友化学(株)製)等が挙げられる。 The aliphatic hydrogenated petroleum resin is a resin using a olefin or diolefin of a C 4 or C 5 fraction, for example, isobutylene, butadiene, isoprene, piperine or the like as a main component as a polymerization raw material. Typical commercial products include Clearon P-125 (manufactured by Yashara Chemical Co., Ltd.), Quinton A100 (manufactured by Nippon Zeon Co., Ltd.), Quinton K100 (manufactured by Nippon Zeon Co., Ltd.), Hiretsu C110X (manufactured by Mitsui Chemicals, Inc.) Highlets R100X (manufactured by Mitsui Chemicals, Inc.), tackolol (manufactured by Sumitomo Chemical Co., Ltd.) and the like.
また、脂環式系水添石油樹脂とは、脂環式留分、例えばシクロペンタジエン、ジシクロペンタジエンなどを重合するかまたは芳香族石油樹脂を水素化して得られるものである。代表的な市販品としては、アルコンP−115(荒川化学(株)製)、アルコンP−125(荒川化学(株)製)、アルコンP−140(荒川化学(株)製)、クイントン1325(日本ゼオン(株)製)、クイントン1345(日本ゼオン(株)製)、クイントン1500(日本ゼオン(株)製)、クイントン1700(日本ゼオン(株)製)、マルカレッツM−845A(丸善石油化学(株)製)、マルカレッツM−890A(丸善石油化学(株)製)、Escorez5320(Exxon Mobile Chemical社製)、Escorez5340(Exxon Mobile Chemical社製)、Escorez5415(Exxon Mobile Chemical社製)、Oppera PR100A(Exxon Mobile Chemical社製)、Oppera PR102J(Exxon Mobile Chemical社製)、Oppera PR103J(Exxon Mobile Chemical社製)、Oppera PR104J(Exxon Mobile Chemical社製)、Oppera PR130J(Exxon Mobile Chemical社製)、Regalite R1125(Eastman社製)、Plastolyn R1140(Eastman社製)等が挙げられる。 The alicyclic hydrogenated petroleum resin is obtained by polymerizing an alicyclic fraction such as cyclopentadiene or dicyclopentadiene or hydrogenating an aromatic petroleum resin. Typical commercial products include Alcon P-115 (Arakawa Chemical Co., Ltd.), Alcon P-125 (Arakawa Chemical Co., Ltd.), Alcon P-140 (Arakawa Chemical Co., Ltd.), Quinton 1325 ( ZEON Co., Ltd.), Quinton 1345 (Nihon Zeon Co., Ltd.), Quinton 1500 (Nihon Zeon Co., Ltd.), Quinton 1700 (Nihon Zeon Co., Ltd.), Marukaretsu M-845A (Maruzen Petrochemical Co., Ltd.) Co., Ltd.), Marcaretz M-890A (manufactured by Maruzen Petrochemical Co., Ltd.), Escorez 5320 (manufactured by Exxon Mobile Chemical), Escorez 5340 (manufactured by Exxon Mobile Chemical Company), Escorez 5415 (manufactured by Exxon Mobile Corp.) Mobile Chemical), Opera PR102J (Exxon Mobile Chemical), Opera PR103J (Exxon Mobile Chemical 11), Opera PR104J (Exxon Mobile), PR 100J (Exxon Mobile Chemical). And Plastolyn R1140 (manufactured by Eastman).
芳香族系水添石油樹脂とは、C9またはC10留分、例えば主成分としてビニルトルエン、インデン、メチルインデンなどを原料とする樹脂である。代表的な市販品としては、アルコンM−115(荒川化学(株)製)、アルコンM−135(荒川化学(株)製)、ネオポリマー120(新日本石油(株)製)、ネオポリマー130(新日本石油(株)製)、ネオポリマー140(新日本石油(株)製)、ペトロジン120(三井化学(株)製)等が挙げられる。 The aromatic hydrogenated petroleum resin is a resin made from a C 9 or C 10 fraction, for example, vinyl toluene, indene, methyl indene or the like as a main component. Typical commercial products include Archon M-115 (Arakawa Chemical Co., Ltd.), Archon M-135 (Arakawa Chemical Co., Ltd.), Neopolymer 120 (Shin Nippon Oil Co., Ltd.), Neopolymer 130. (Manufactured by Nippon Oil Corporation), Neopolymer 140 (manufactured by Nippon Oil Corporation), Petrogin 120 (manufactured by Mitsui Chemicals) and the like.
また、本発明では上記水添石油樹脂の代わりにテルペン系水添樹脂を用いることもできる。ここでいうテルペン系水添樹脂とは、(C5H8)の組成で表される炭化水素化合物、例えば、ピネン、ジペンテン、リモネン、オシメン、ミルセン、カレン、テルピノレン、テルピネン、トタレン、ミレン、カンホレン、サンタレン、ジンギベレン、ビサボレン、トリシクレンなどを原料とする樹脂である。 In the present invention, a terpene-based hydrogenated resin can be used instead of the hydrogenated petroleum resin. The terpene-based hydrogenated resin here is a hydrocarbon compound represented by a composition of (C 5 H 8 ), for example, pinene, dipentene, limonene, osimene, myrcene, karen, terpinolene, terpinene, totalene, mylene, camphorene. , Santalene, Genghibelen, Bisabolene, Tricyclene, etc.
これらの中でもポリプロピレン系樹脂への相溶性が高い脂肪族系水添石油樹脂及び脂環式系水添石油樹脂が好ましく、さらには、低成形圧の効果が高い脂環式系水添石油樹脂が好ましい。 Among these, aliphatic hydrogenated petroleum resins and alicyclic hydrogenated petroleum resins having high compatibility with polypropylene resins are preferable, and alicyclic hydrogenated petroleum resins having a high effect of low molding pressure are also preferable. preferable.
本発明では、さらに必要に応じて、タルク等のセル造核剤をはじめ酸化防止剤、金属不活性剤、燐系加工安定剤、紫外線吸収剤、紫外線安定剤、蛍光増白剤、金属石鹸などの安定剤または架橋剤、連鎖移動剤、滑剤、可塑剤、充填剤、強化剤、顔料、染料、難燃剤、帯電防止剤等をポリプロピレン系樹脂組成物中に含有させてもよい。 In the present invention, if necessary, cell nucleating agents such as talc, antioxidants, metal deactivators, phosphorus processing stabilizers, UV absorbers, UV stabilizers, fluorescent brighteners, metal soaps, etc. These stabilizers or crosslinking agents, chain transfer agents, lubricants, plasticizers, fillers, reinforcing agents, pigments, dyes, flame retardants, antistatic agents and the like may be contained in the polypropylene resin composition.
本発明における単軸押出機とは、シリンダーに1本のスクリューを装着した押出機をいい、一般的に使用されているものである。主要構造は、ホッパー、駆動装置、減速機、スクリュー、シリンダー、加熱・冷却装置(ヒーター・ブロワー)、温度制御装置などから成り、シリンダーの先端にアダプターを介して所望のダイスを取り付ける。 The single screw extruder in the present invention refers to an extruder having a single screw mounted on a cylinder, and is generally used. The main structure consists of a hopper, drive unit, speed reducer, screw, cylinder, heating / cooling device (heater / blower), temperature control device, etc., and a desired die is attached to the tip of the cylinder via an adapter.
本発明において、押出機フィード部のシリンダー(C1)とは、シリンダーにおいて、樹脂を投入するホッパー下の部分を指し、C1から樹脂が押出される方向に従って設定温度を変更できる部分を順次C2、C3、・・・Cnとする。また、ダイス(D)の位置はアダプター(A)の横でも下でも良い。本発明では、押出機フィード部のシリンダー(C1)の設定温度は200℃以上であることが必要で、好ましくは210℃以上260℃以下である。設定温度が260℃を超えると水添石油樹脂の分解が始まりダイスからの発煙が多くなる傾向がある。さらに、単軸押出機のスクリューの種類は、特に限定はなく、フルフライト型やダルメージ型等が挙げられ、いずれも本発明のミニペレットの製造に使用可能であるが、ダルメージ型が押出しの混練性が優れているので好ましい。ポリプロピレン系樹脂組成物の溶融混練物を紐状にして押出すダイスの口径は1.0〜3.0mmが好ましく、高吐出量で粒重量の揃ったミニペレットを得るためには、1.0〜1.8mmがより好ましい。続いて残りのシリンダー(C2〜Cn)、アダプター(A)、ダイス(D)の設定温度条件を説明する。各部位の温度は、
C1−30℃≦C2〜Cn≦C1+50℃、
C1−30℃≦A≦C1+50℃、
C1−30℃≦D≦C1+50℃、
であることが好ましく、シリンダー・アダプター・ダイスのいずれも260℃以下がより好ましい。
In the present invention, the cylinder (C 1 ) of the feed section of the extruder refers to a portion under the hopper into which the resin is charged in the cylinder, and the portions where the set temperature can be changed according to the direction in which the resin is extruded from C 1 are sequentially C 2 , C 3 ,..., C n . The position of the die (D) may be next to or below the adapter (A). In the present invention, the set temperature of the cylinder (C 1 ) of the extruder feed section needs to be 200 ° C. or higher, preferably 210 ° C. or higher and 260 ° C. or lower. When the set temperature exceeds 260 ° C., decomposition of the hydrogenated petroleum resin starts and smoke from the dice tends to increase. Furthermore, the type of screw of the single screw extruder is not particularly limited, and examples thereof include a full flight type and a dalmage type, both of which can be used for the production of the mini pellet of the present invention. It is preferable because of its excellent properties. The diameter of a die for extruding a melt-kneaded product of a polypropylene resin composition in the form of a string is preferably 1.0 to 3.0 mm, and in order to obtain a mini pellet having a high discharge rate and a uniform grain weight, 1.0 -1.8 mm is more preferable. Next, set temperature conditions for the remaining cylinders (C 2 to C n ), adapter (A), and die (D) will be described. The temperature of each part is
C 1 −30 ° C. ≦ C 2 to C n ≦ C 1 + 50 ° C.,
C 1 −30 ° C. ≦ A ≦ C 1 + 50 ° C.,
C 1 −30 ° C. ≦ D ≦ C 1 + 50 ° C.
It is preferable that both the cylinder, the adapter, and the die are more preferably 260 ° C. or lower.
本発明におけるミニペレットとは、長さ1.5〜4.0mm、かつ厚みが0.4〜1.0mmの円柱形状であることが好ましく、その粒重量が0.3〜3.0mgであることが好ましい。このミニペレットを予備発泡粒子にして成形体を作る際、粒重量は0.5〜1.2mgがより好ましい。ここでいう予備発泡粒子とは、例えばミニペレットを発泡剤と共に耐圧容器内で水中に分散させ、ミニペレットが軟化する温度以上に加熱してミニペレット内に発泡剤を含浸させたのち容器内より低圧の雰囲気に放出して得られる発泡粒子のことをいい、公知の方法で作製することできる。このようにして得られた予備発泡粒子を金型に詰めて水蒸気で加熱発泡させることにより低加熱圧で成形体を作製することができる。 The mini-pellet in the present invention is preferably a cylindrical shape having a length of 1.5 to 4.0 mm and a thickness of 0.4 to 1.0 mm, and its particle weight is 0.3 to 3.0 mg. It is preferable. When making this minipellet into pre-expanded particles to form a molded body, the particle weight is more preferably 0.5 to 1.2 mg. Pre-expanded particles as used herein means, for example, that mini-pellets are dispersed in water in a pressure-resistant container together with a foaming agent, heated above the temperature at which the mini-pellets soften, and impregnated with the foaming agent in the mini-pellets. This refers to expanded particles obtained by discharging into a low-pressure atmosphere, and can be produced by a known method. The pre-expanded particles thus obtained are packed in a mold and heated and foamed with water vapor to produce a molded body with a low heating pressure.
本発明の製造方法で作製されたミニペレットは、粒重量バラツキが好ましくは0.15以内と小さいため、予備発泡粒子に好適に用いることができる。本発明においてミニペレットの粒重量バラツキは、得られたミニペレットを無作為に30粒採取し、その30粒の重量の平均値をAavとする。i番目の粒重量測定値をAiとして下記式にて計算された値である。
粒重量バラツキ(σ)=[{Σ(Ai−Aav)2}/29]1/2
Mini-pellets produced by the production method of the present invention preferably have small particle weight variations of 0.15 or less, and can be suitably used for pre-expanded particles. In the present invention, the particle size variation of mini-pellets is obtained by randomly collecting 30 particles of the obtained mini-pellets and setting the average value of the 30 particles as Aav. The i-th grain weight measurement value is Ai and is a value calculated by the following formula.
Grain weight variation (σ) = [{Σ (Ai−Aav) 2 } / 29] 1/2
〈メルトフローインデックス測定〉
メルトフローインデックスの測定はJIS−K7210に準拠して、オリフィス2.0959±0.005mmφ、オリフィス長さ8.000±0.025mm、加重2160g、230±0.2℃の条件下で測定した。
<Melt flow index measurement>
The melt flow index was measured under the conditions of orifice 2.0959 ± 0.005 mmφ, orifice length 8.000 ± 0.025 mm, load 2160 g, 230 ± 0.2 ° C. in accordance with JIS-K7210.
〈粒重量バラツキ(σ)〉
ペレタイザーでカットされたミニペレットを無作為に30粒採取し、その30粒の重量の平均値をAavとする。i番目の粒重量測定値をAiとして粒重量バラツキ(σ)は以下の式にて表される。
粒重量バラツキ(σ)=[{Σ(Ai−Aav)2}/29]1/2
〈吐出安定性〉
吐出安定性を以下の基準に準じて評価し、合否判定を行った。
◎: 吐出量の変化がなく、樹脂圧力変動幅が10kgf/cm2以内で粒重量バラツキ(σ)が0.15以内
○: 吐出量の変化はないが、樹脂圧力変動幅が10kgf/cm2より大きく15kgf/cm2以内で粒重量バラツキ(σ)が0.15以内
×: 粒重量バラツキ(σ)が0.15を超える
(実施例1)
エチレン−プロピレンランダム共重合体(樹脂密度0.90g/cm3、メルトフローインデックス4.8g/10分、結晶融点146℃)97重量%に水添石油樹脂である荒川化学(株)製アルコンP−140(軟化点140℃)を3重量%配合した樹脂混合物をドライブレンドし、該ブレンド物を口径1.2mmのダイスを備えた50mm単軸押出機を用いてシリンダー、アダプター、ダイスの温度をそれぞれC1=210℃、C2=210℃、C3=210℃、C4=220℃、A=230℃、D=230℃、スクリューの回転数80rpmの条件で押出し、引き取り後、カットしてミニペレットを得た。2時間吐出量が変化することなく、樹脂圧力変動幅も10kgf/cm2以内、かつ、粒重量バラツキ(σ)が0.15以内だったので吐出安定性が良好であったといえる。結果を表1に示す。
<Grain weight variation (σ)>
Thirty mini-pellets cut with a pelletizer are randomly sampled, and the average value of the weights of the 30 pellets is defined as Aav. The grain weight variation (σ) is expressed by the following formula, where the i-th grain weight measurement value is Ai.
Grain weight variation (σ) = [{Σ (Ai−Aav) 2 } / 29] 1/2
<Discharge stability>
The ejection stability was evaluated according to the following criteria, and a pass / fail judgment was made.
A: No change in discharge amount, resin pressure fluctuation range within 10 kgf / cm 2 and grain weight variation (σ) within 0.15 ○: No change in discharge amount, but resin pressure fluctuation range is 10 kgf / cm 2 Greater than 15 kgf / cm 2 and grain weight variation (σ) is within 0.15 ×: grain weight variation (σ) exceeds 0.15 (Example 1)
Alcon P manufactured by Arakawa Chemical Co., Ltd., which is a hydrogenated petroleum resin with 97% by weight of ethylene-propylene random copolymer (resin density 0.90 g / cm 3 , melt flow index 4.8 g / 10 min, crystal melting point 146 ° C.) -Blend of a resin mixture containing 3% by weight of -140 (softening point 140 ° C.), and the temperature of the cylinder, adapter and die is adjusted using a 50 mm single screw extruder equipped with a die having a diameter of 1.2 mm. C 1 = 210 ° C., C 2 = 210 ° C., C 3 = 210 ° C., C 4 = 220 ° C., A = 230 ° C., D = 230 ° C. To obtain a mini-pellet. It can be said that the ejection stability was good because the resin pressure fluctuation range was within 10 kgf / cm 2 and the grain weight variation (σ) was within 0.15 without changing the ejection amount for 2 hours. The results are shown in Table 1.
実施例1においてスクリューの回転数を50mm押出機の最大回転数である100rpmに代えた以外は実施例1と同様の方法により押出した。2時間吐出量が変化することなく、樹脂圧力変動幅も10kgf/cm2以内で粒重量バラツキ(σ)が0.15以内だったので吐出安定性が良好であったといえる。結果を表1に示す。
Extrusion was carried out in the same manner as in Example 1, except that the screw rotation speed was changed to 100 rpm which is the maximum rotation speed of the 50 mm extruder in Example 1. It can be said that the discharge stability was good because the resin pressure fluctuation range was within 10 kgf / cm 2 and the particle weight variation (σ) was within 0.15 without changing the discharge amount for 2 hours. The results are shown in Table 1.
(実施例3)
実施例1においてシリンダー温度をC1=250℃、C2=230℃、C3=220℃に代えた以外は実施例1と同様の方法により押出した。2時間吐出量が変化することなく、樹脂圧力変動幅も10kgf/cm2以内で粒重量バラツキ(σ)が0.15以内だったので良好な吐出安定性であったといえる。結果を表1に示す。
(Example 3)
Extrusion was carried out in the same manner as in Example 1 except that the cylinder temperature was changed to C 1 = 250 ° C., C 2 = 230 ° C., and C 3 = 220 ° C. in Example 1. The discharge amount did not change for 2 hours, the resin pressure fluctuation range was within 10 kgf / cm 2 , and the grain weight variation (σ) was within 0.15, so it can be said that the discharge stability was good. The results are shown in Table 1.
(実施例4)
実施例1において、エチレン−プロピレンランダム共重合体90重量%、水添石油樹脂アルコンP−140の添加量を10重量%とした以外は実施例1と同様の方法により押出した。2時間吐出量が変化することなく、樹脂圧力変動幅も10kgf/cm2以上15kgf/cm2以内で粒重量バラツキ(σ)が0.15以内だったので良好な吐出安定性であった。結果を表1に示す。
Example 4
Extrusion was carried out in the same manner as in Example 1, except that 90% by weight of the ethylene-propylene random copolymer and 10% by weight of the hydrogenated petroleum resin Alcon P-140 were added. Without 2 hours discharge amount is changed, the resin pressure fluctuation width 10 kgf / cm 2 or more 15 kgf / cm 2 within the grain weight variation (sigma) was good ejection stability because it was 0.15. The results are shown in Table 1.
(実施例5)
実施例1において脂環式系水添石油樹脂アルコンP−140の代わりに、脂肪族系水添石油樹脂であるヤスハラケミカル社製のクリアロンP−125(軟化点125℃)を用いた以外は実施例1と同様の方法により押出した。2時間吐出量が変化することなく、樹脂圧力変動幅も10kgf/cm2以内で粒重量バラツキ(σ)が0.15以内だったので優れた吐出安定性であった。結果を表1に示す。
(Example 5)
In Example 1, instead of the alicyclic hydrogenated petroleum resin Alcon P-140, Example 1 was used except that Clearon P-125 (softening point 125 ° C.) manufactured by Yashara Chemical Co., which is an aliphatic hydrogenated petroleum resin, was used. Extrusion was carried out in the same manner as in 1. Without changing the discharge amount for 2 hours, the resin pressure fluctuation range was within 10 kgf / cm 2 , and the grain weight variation (σ) was within 0.15, so the discharge stability was excellent. The results are shown in Table 1.
(実施例6)
実施例1においてアルコンP−140の代わりにアルコンP−115(軟化点115℃)を用いた以外は、実施例1と同様の方法により押出した。2時間吐出量が変化することなく、樹脂圧力変動幅も10kgf/cm2以内で粒重量のバラツキ(σ)が0.15以内だったので優れた吐出安定性であった。結果を表1に示す。
(Example 6)
Extrusion was performed in the same manner as in Example 1, except that Alcon P-115 (softening point 115 ° C.) was used instead of Alcon P-140 in Example 1. The discharge amount did not change for 2 hours, the resin pressure fluctuation range was within 10 kgf / cm 2 , and the variation (σ) in grain weight was within 0.15, so the discharge stability was excellent. The results are shown in Table 1.
(比較例1)
シリンダー温度をC1=170℃、C2=180℃、C3=200℃に代えた以外は、実施例1と同様の方法により押出した。20分でスクリューが滑り始め吐出量が大幅に低下し、単軸押出機から樹脂を押出せなくなった。結果を表1に示す。
(Comparative Example 1)
Extrusion was carried out in the same manner as in Example 1 except that the cylinder temperature was changed to C 1 = 170 ° C., C 2 = 180 ° C., and C 3 = 200 ° C. In 20 minutes, the screw began to slide, and the discharge amount decreased significantly, making it impossible to extrude the resin from the single screw extruder. The results are shown in Table 1.
(比較例2)
シリンダー温度をC1=190℃、C2=200℃、C3=200℃に代えた以外は、実施例1と同様の方法により押出した。樹脂圧力変動幅は10kgf/cm2以内であったが、吐出量が徐々に低下し粒重量バラツキがひどくなった。結果を表1に示す。
(Comparative Example 2)
Extrusion was carried out in the same manner as in Example 1 except that the cylinder temperature was changed to C 1 = 190 ° C., C 2 = 200 ° C., and C 3 = 200 ° C. The fluctuation range of the resin pressure was within 10 kgf / cm 2 , but the discharge amount gradually decreased and the grain weight variation became severe. The results are shown in Table 1.
(比較例3)
エチレン−プロピレンランダム共重合体85重量%、水添石油樹脂アルコンP−140の添加量を15%とした以外は、実施例1と同様の方法により押出した。スクリューが徐々に滑り始め吐出量が低下し吐出安定性に劣る結果であった。結果を表1に示す。
(Comparative Example 3)
Extrusion was performed in the same manner as in Example 1, except that 85% by weight of the ethylene-propylene random copolymer and 15% of the hydrogenated petroleum resin Alcon P-140 were added. As a result, the screw began to slide gradually and the discharge amount decreased, resulting in poor discharge stability. The results are shown in Table 1.
実施例1〜6および比較例1〜3に示すとおり、本発明によれば単軸押出機でポリプロピレン系樹脂と水添石油樹脂を安定的に高吐出で溶融混練することができ、予備発泡粒子に適した粒重量が均一に揃ったミニペレットを提供できることがわかる。 As shown in Examples 1 to 6 and Comparative Examples 1 to 3, according to the present invention, a polypropylene resin and a hydrogenated petroleum resin can be stably melt-kneaded with high discharge in a single screw extruder, and pre-expanded particles It can be seen that mini-pellets with uniform grain weights suitable for can be provided.
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JP2021014552A (en) * | 2019-07-16 | 2021-02-12 | 株式会社プライムポリマー | Resin composition pellet, and method for manufacturing the same |
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JP2021014552A (en) * | 2019-07-16 | 2021-02-12 | 株式会社プライムポリマー | Resin composition pellet, and method for manufacturing the same |
JP7332368B2 (en) | 2019-07-16 | 2023-08-23 | 株式会社プライムポリマー | Resin composition pellet and method for producing the same |
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