JP3901169B2 - Process for producing antistatic injection-molding ethylene-based resin composition - Google Patents
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- JP3901169B2 JP3901169B2 JP2004138239A JP2004138239A JP3901169B2 JP 3901169 B2 JP3901169 B2 JP 3901169B2 JP 2004138239 A JP2004138239 A JP 2004138239A JP 2004138239 A JP2004138239 A JP 2004138239A JP 3901169 B2 JP3901169 B2 JP 3901169B2
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本発明は、帯電防止性射出成形用エチレン系樹脂組成物の製造方法に関するものである。更に詳しくは、本発明は、少量の帯電防止剤の使用により十分に高い帯電防止性を得ることができ、よってコスト的に有利であり、かつ表面外観に優れた成形品を提供し得る帯電防止性射出成形用エチレン系樹脂組成物の製造方法に関するものである。 The present invention relates to a method for producing an antistatic injection-molding ethylene-based resin composition. More specifically, the present invention can obtain a sufficiently high antistatic property by using a small amount of an antistatic agent, and is therefore advantageous in terms of cost and can provide a molded product having an excellent surface appearance. The present invention relates to a method for producing an ethylene resin composition for flexible injection molding.
工業部品、容器の蓋、キャップ、人工芝、スキーブーツなどの射出成形品には、汚れを防止するため、帯電防止性を有することが要求される。かかる帯電防止性を付与するためには、樹脂に帯電防止剤を添加して用いられるのが一般である。ここで、高い帯電防止性を得るために多量の帯電防止剤を使用した場合、ブリードの発生などにより成形品の表面外観が悪化するという問題があった。 Injection molded products such as industrial parts, container lids, caps, artificial turf and ski boots are required to have antistatic properties in order to prevent contamination. In order to impart such antistatic properties, it is common to add an antistatic agent to the resin. Here, when a large amount of antistatic agent is used in order to obtain high antistatic properties, there is a problem that the surface appearance of the molded product is deteriorated due to generation of bleeding.
かかる現状に鑑み、本発明が解決しようとする課題は、少量の帯電防止剤の使用により十分に高い帯電防止性を得ることができ、よってコスト的に有利であり、かつ表面外観に優れた成形品を提供し得る帯電防止性射出成形用エチレン系樹脂組成物の製造方法を提供する点に存するものである。 In view of the current situation, the problem to be solved by the present invention is that a sufficiently high antistatic property can be obtained by the use of a small amount of an antistatic agent, and thus it is advantageous in terms of cost and has excellent surface appearance. The present invention resides in providing a method for producing an antistatic injection-type ethylene resin composition capable of providing a product.
すなわち、本発明は、エチレン−α−オレフィン共重合体に対し、グリセリン脂肪酸エステル、直鎖脂肪族アルコール及びアルキルジエタノールアミドを配合してなる帯電防止性射出成形用エチレン系樹脂組成物の製造方法であって、エチレン−α−オレフィン共重合体のメルトフローレートが１〜１００ｇ／１０分であり、エチレン−α−オレフィン共重合体の密度が０．９１６〜０．９３０ｇ／ｃｍ3であり、エチレン−α−オレフィン共重合体１００重量部あたりのグリセリン脂肪酸エステル、直鎖脂肪族アルコール及びアルキルジエタノールアミドの合計配合量が０．０３〜０．１５重量部であり、エチレン−α−オレフィン共重合体、グリセリン脂肪酸エステル、直鎖脂肪族アルコール及びアルキルジエタノールアミドを混練する帯電防止性射出成形用エチレン系樹脂組成物の製造方法に係るものである。 That is, the present invention is a method for producing an antistatic injection-molding ethylene-based resin composition obtained by blending an ethylene-α-olefin copolymer with a glycerin fatty acid ester, a linear aliphatic alcohol, and an alkyldiethanolamide. The melt flow rate of the ethylene-α-olefin copolymer is 1 to 100 g / 10 minutes, the density of the ethylene-α-olefin copolymer is 0.916 to 0.930 g / cm 3 , The total blending amount of glycerin fatty acid ester, linear aliphatic alcohol and alkyldiethanolamide per 100 parts by weight of the α-olefin copolymer is 0.03 to 0.15 parts by weight, and the ethylene-α-olefin copolymer , glycerin fatty acid ester, kneading the straight chain fatty alcohols and alkyl diethanolamide charged Those relating to the manufacturing method of the sealing properties for injection molding ethylene resin composition.
本発明により、少量の帯電防止剤の使用により十分に高い帯電防止性を得ることができ、よってコスト的に有利であり、かつ表面外観に優れた成形品を提供し得る帯電防止性射出成形用エチレン系樹脂組成物の製造方法を提供することができる。 According to the present invention, a sufficiently high antistatic property can be obtained by using a small amount of an antistatic agent, and therefore it is advantageous in terms of cost and can provide a molded product having an excellent surface appearance. A method for producing an ethylene-based resin composition can be provided.
以下、詳細に説明する。 Details will be described below.
本発明のエチレン−α−オレフィン共重合体のα−オレフィンとしては、プロピレン、ブテン−１、４−メチルペンテン−１、ヘキセン−１、オクテン−１、デセン−１などが用いられるが、炭素数３〜１０のものが好ましい。これらα−オレフィンは、その一種を単独で用いてもよく、二種以上を併用してもよい。 As the α-olefin of the ethylene-α-olefin copolymer of the present invention, propylene, butene-1, 4-methylpentene-1, hexene-1, octene-1, decene-1, etc. are used. The thing of 3-10 is preferable. These α-olefins may be used alone or in combination of two or more.
本発明のエチレン−α−オレフィン共重合体のメルトフローレートは１〜１００ｇ／１０分、好ましくは３〜５０ｇ／１０分である。メルトフローレートが過小であると射出成形性に劣り、メルトフローレートが過大であると強度に劣る。なお、本発明におけるメルトフローレートは、ＪＩＳ−Ｋ７２１０に基づき温度１９０℃、荷重２．１６ｋｇにおける値である。 The melt flow rate of the ethylene-α-olefin copolymer of the present invention is 1 to 100 g / 10 minutes, preferably 3 to 50 g / 10 minutes. If the melt flow rate is too low, the injection moldability is poor, and if the melt flow rate is too high, the strength is poor. In addition, the melt flow rate in this invention is a value in temperature 190 degreeC and load 2.16kg based on JIS-K7210.
本発明のエチレン−α−オレフィン共重合体の密度は０．９１６〜０．９３０ｇ／ｃｍ3、好ましくは０．９１８〜０．９２８ｇ／ｃｍ3である。密度が過小又は過大であると多量の帯電防止剤を使用する必要があり、コスト面で不都合であり、かつ多量の帯電防止剤を使用によりブリードの発生を伴い、表面外観を悪化させる。 The density of the ethylene-α-olefin copolymer of the present invention is 0.916 to 0.930 g / cm 3 , preferably 0.918 to 0.928 g / cm 3 . If the density is too low or too high, it is necessary to use a large amount of an antistatic agent, which is inconvenient in terms of cost, and the use of a large amount of antistatic agent causes bleed and deteriorates the surface appearance.
本発明のエチレン−α−オレフィン共重合体の製造方法としては、エチレンとα−オレフィンを遷移金属触媒を使用して重合する方法をあげることができる。重合反応は、通常３０〜３００℃の重合温度下、常圧〜３０００ｋｇ／ｃｍ2の重合圧力下、溶媒の存在下又は不存在下、気−固、液−固又は均一液相下で実施される。 Examples of the method for producing the ethylene-α-olefin copolymer of the present invention include a method of polymerizing ethylene and α-olefin using a transition metal catalyst. The polymerization reaction is usually carried out at a polymerization temperature of 30 to 300 ° C., a polymerization pressure of normal pressure to 3000 kg / cm 2 , in the presence or absence of a solvent, and in a gas-solid, liquid-solid or homogeneous liquid phase. The
本発明の帯電防止性射出成形用エチレン系樹脂組成物は、上記のエチレン−α−オレフィン共重合体に対し、グリセリン脂肪酸エステル、直鎖脂肪族アルコール及びアルキルジエタノールアミドを配合してなるものである。ここで、グリセリン脂肪酸エステル、直鎖脂肪族アルコール及びアルキルジエタノールアミドは帯電防止剤として機能する。 The antistatic injection-molding ethylene-based resin composition of the present invention is obtained by blending glycerin fatty acid ester, linear aliphatic alcohol and alkyldiethanolamide with the above-mentioned ethylene-α-olefin copolymer. . Here, glycerin fatty acid ester, linear aliphatic alcohol and alkyldiethanolamide function as an antistatic agent.
グリセリン脂肪酸エステルとしては、たとえばグリセリンモノステアリン酸エステル、グリセリンモノヘプタデシル酸エステル、グリセリンモノパルミチン酸エステル、グリセリンモノミリスチル酸エステル、グリセリンモノラウリル酸エステル、グリセリンモノカプリン酸エステル、グリセリンモノペラルゴン酸エステルなどがあげられる。 Examples of glycerin fatty acid esters include glycerin monostearate, glycerin monoheptadecyl ester, glycerin monopalmitate, glycerin monomyristylate, glycerin monolaurate, glycerin monocaprate, glycerin monopelargonate, etc. Can be given.
アルキルジエタノールアミドとしては、たとえばステアリルジエタノールアミド、ラウリンジエタノールアミド、オレイルジエタノールアミドなどがあげられる。 Examples of the alkyl diethanolamide include stearyl diethanolamide, laurin diethanolamide, oleyl diethanolamide, and the like.
本発明の帯電防止性射出成形用エチレン系樹脂組成物は、エチレン−α−オレフィン共重合体１００重量部あたりのグリセリン脂肪酸エステル、直鎖脂肪族アルコール及びアルキルジエタノールアミドの合計配合量が０．０３〜０．１５重量部、好ましくは０．０３〜０．１０重量部のものである。該配合量が過少であると帯電防止性に劣り、一方該配合量が過多であると表面外観に劣る。 The ethylene-based resin composition for antistatic injection molding of the present invention has a total amount of 0.03 of glycerin fatty acid ester, linear aliphatic alcohol and alkyldiethanolamide per 100 parts by weight of ethylene-α-olefin copolymer. To 0.15 parts by weight, preferably 0.03 to 0.10 parts by weight. When the amount is too small, the antistatic property is inferior, whereas when the amount is too large, the surface appearance is inferior.
グリセリン脂肪酸エステル、直鎖脂肪族アルコール及びアルキルジエタノールアミドの使用割合としては、その合計量を１００重量％として、グリセリン脂肪酸エステル４０〜８０重量％、直鎖脂肪族アルコール１０〜４０重量％及びアルキルジエタノールアミド１０〜３０重量％とすることが、本発明の目的を十分に発現する観点から好ましい。 The proportions of glycerin fatty acid ester, linear fatty alcohol and alkyldiethanolamide used are 100% by weight, glycerin fatty acid ester 40 to 80% by weight, linear aliphatic alcohol 10 to 40% by weight and alkyldiethanolamine. 10 to 30% by weight is preferable from the viewpoint of sufficiently expressing the object of the present invention.
本発明の帯電防止性射出成形用エチレン系樹脂組成物を得る方法としては、エチレン−α−オレフィン共重合体、グリセリン脂肪酸エステル、直鎖脂肪族アルコール及びアルキルジエタノールアミドを、タンブラーブレンダー法、ヘンシェルミキサー法、バンバリーミキサー法、押出造粒法などにより混練する方法をあげることができる。なお、混練時に、中和剤、分散剤、酸化防止剤、滑剤、耐候性改良剤、帯電防止剤、顔料、フィラーなどの他の付加的成分を本発明の効果を阻害しない範囲で配合してもよい。 The antistatic injection molding ethylene-based resin composition of the present invention includes an ethylene-α-olefin copolymer, a glycerin fatty acid ester, a linear aliphatic alcohol, and an alkyldiethanolamide, a tumbler blender method, a Henschel mixer. Examples thereof include kneading by a method, Banbury mixer method, extrusion granulation method and the like. During kneading, other additional components such as a neutralizer, a dispersant, an antioxidant, a lubricant, a weather resistance improver, an antistatic agent, a pigment, and a filler are blended within a range that does not impair the effects of the present invention. Also good.
以下、本発明を実施例によって説明する。
実施例１〜２及び比較例１〜５
表１に示す配合をバンバリーミキサーにて１５０℃の温度で１０分間混練し、６５ｍｍｍ径のスクリューを有する押出機にて１８０℃で造粒し評価を行なった。結果を表１に示した。評価項目及び評価方法は次のとおりである。
Hereinafter, the present invention will be described by way of examples.
Examples 1-2 and Comparative Examples 1-5
The formulations shown in Table 1 were kneaded at a temperature of 150 ° C. for 10 minutes with a Banbury mixer, and granulated at 180 ° C. with an extruder having a 65 mm diameter screw, and evaluated. The results are shown in Table 1. Evaluation items and evaluation methods are as follows.
（１）メルトフローレート（ＭＦＲ）
ＪＩＳ−Ｋ７２１０に基づき、測定温度１９０℃、荷重２．１６ｋｇで測定した。
(1) Melt flow rate (MFR)
Based on JIS-K7210, measurement was performed at a measurement temperature of 190 ° C. and a load of 2.16 kg.
（２）密度
１５０℃で厚さ１ｍｍにプレス成形したシートを使用し、ＪＩＳ−Ｋ６７６０により測定した。
(2) Density A sheet press-molded to a thickness of 1 mm at 150 ° C. was used and measured according to JIS K6760.
（３）帯電防止性
射出成形機（東芝機械社製、商品名 ＩＳ−１００ＥＮ）を使用し、射出圧力が８００ｋｇ／ｃｍ2、シリンダー温度が２００℃、金型温度が４０℃、成形サイクルが４０秒の条件によって１５ｃｍ角、１．５ｃｍ厚さの成形品を成形した。成形品を４０℃のオーブン中で１０日間経時させた後取り出し、２３±２℃、相対湿度５０±５％の状態で２時間調整した後、宍戸電気（株）製オネストメーターアナライザーを使用し、印加電圧１０ｋｖ、回転数１０００ｒｐｍの条件で試料に電圧を印加し帯電させ、印加停止後帯電圧が半分となる時間（半減期）を測定した。半減期が短い程、帯電防止性に優れる。
(3) Antistatic property Using an injection molding machine (trade name IS-100EN manufactured by Toshiba Machine Co., Ltd.), injection pressure is 800 kg / cm 2 , cylinder temperature is 200 ° C., mold temperature is 40 ° C., molding cycle is 40 A molded article having a size of 15 cm square and a thickness of 1.5 cm was formed according to the conditions of the second. After the molded article was aged for 10 days in an oven at 40 ° C., it was taken out and adjusted for 2 hours at 23 ± 2 ° C. and a relative humidity of 50 ± 5%. A voltage was applied to the sample to charge it under the conditions of an applied voltage of 10 kv and a rotational speed of 1000 rpm, and the time (half-life) when the applied voltage was halved after the application was stopped was measured. The shorter the half-life, the better the antistatic property.
（４）表面外観
帯電防止性評価用に成形した成形品を４０℃のオーブン中で１０日間経時させた後取り出し、表面外観を目視観察し、○（ブリードがなく良好）及び×（ブリードがあり不良）により評価した。
(4) Surface appearance Molded product molded for evaluation of antistatic properties was taken out after 10 days in an oven at 40 ° C. and then taken out. The surface appearance was visually observed, and ○ (good with no bleed) and x (with bleed) Bad).
結果から次のことがわかる。本発明の条件を充足するすべての実施例は、帯電防止性及び表面外観において満足すべき結果を示している。一方、帯電防止剤の添加量が過多な比較例１は表面外観に劣る。また、密度が過小なエチレン−α−オレフィン共重合体を用いた比較例２〜５は、いずれも帯電防止性に劣る。 The results show the following. All examples satisfying the conditions of the present invention show satisfactory results in antistatic properties and surface appearance. On the other hand, Comparative Example 1 in which the addition amount of the antistatic agent is excessive is inferior in surface appearance. Moreover, all of Comparative Examples 2 to 5 using an ethylene-α-olefin copolymer having an excessively low density are inferior in antistatic properties.
＊１ エチレン−α−オレフィン共重合体
Ａ１：エチレン−ブテン−１共重合体（ブテン−１含量＝７重量％）
Ａ２：エチレン−ブテン−１共重合体（ブテン−１含量＝９重量％）
Ａ３：エチレン−ブテン−１共重合体（ブテン−１含量＝３重量％）
* 1 Ethylene-α-olefin copolymer A1: Ethylene-butene-1 copolymer (butene-1 content = 7% by weight)
A2: Ethylene-butene-1 copolymer (butene-1 content = 9% by weight)
A3: Ethylene-butene-1 copolymer (butene-1 content = 3% by weight)
＊２ 帯電防止剤
Ｂ１：グリセリンモノステアリン酸エステル（６０重量％）＋ステアリルアルコール（２０重量％）＋ステアリルジエタノールアミド（２０重量％）
* 2 Antistatic agent B1: Glycerol monostearate (60% by weight) + stearyl alcohol (20% by weight) + stearyl diethanolamide (20% by weight)
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| JP2004138239A JP3901169B2 (en) | 2004-05-07 | 2004-05-07 | Process for producing antistatic injection-molding ethylene-based resin composition |
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| JP11986795A Division JP3572720B2 (en) | 1995-05-18 | 1995-05-18 | Antistatic ethylene resin composition for injection molding |
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| JP3901169B2 true JP3901169B2 (en) | 2007-04-04 |
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