JP2004168876A - Masterbatch - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a masterbatch enabling the inorganic filler as a component to be homogeneously dispersed as a whole when blended with a main material and capable of obtaining a compound material with stable physical properties including tensile elongation and Izod impact strength. <P>SOLUTION: The masterbatch, being 125-160°C in melting point, comprises a resin component comprising crystalline propylene random copolymer resin 110-155°C in melting point( e.g. propylene-ethylene copolymer resin, MFR:1-50 g/10min ) and optionally an ethylene-propylene block copolymer resin, a rubber component( e.g. ethylene-1-octene copolymer ) and the inorganic filler( e.g. talc, aspect ratio:2-20 ). <P>COPYRIGHT: (C)2004,JPO

Description

【００３７】
［３］テストピースの作製
［２］で得られた実施例１〜６及び比較例１、２の各マスターバッチペレットと、主材［三井住友ポリオレフィン株式会社製、商品名「ＢＪ４Ｈ−１００（３）」（エチレン・プロピレンブロック共重合樹脂）］とを、１：２の質量比にてドライブレンドし、略均一にブレンドしたペレットを得た。この混合ペレットを日精樹脂工業株式会社製の１００ｔｏｎ射出成形機のホッパーに投入し、成形物を得て、下記の引張試験用、曲げ試験用及びアイゾット衝撃試験用のテストピースを作製した。
【００３８】
［４］評価
［３］で得られた各テストピースを用いて下記の試験及び測定を行い、各性能を評価した。各々の測定結果を表２に示す。
▲１▼引張試験
ＪＩＳ Ｋ ７１１３に準拠し、二号ダンベル形状のテストピースを使用して、引張速度１０ｍｍ／分にて、引張強度及び引張伸びを測定した。
▲２▼曲げ試験
ＪＩＳ Ｋ ７１７１に準拠し、曲げ弾性率を測定した。
▲３▼アイゾット衝撃試験
ＪＩＳ Ｋ ７１１０に準拠し、ノッチ無しで試験温度−２０℃にてアイゾット衝撃値を測定した。
尚、各試験は、１０回ずつ実施し、最大及び最小のデータを各２個ずつ削除し、残りの６個のデータにおける、最大値、最小値、平均値及び最大値と最小値との差（バラツキ）を記録した。
【００３９】
【表２】

【００４０】
［５］実施例の効果
表２によれば、結晶性プロピレンランダム共重合樹脂を含有せず、融点が１６３℃と高い比較例１のマスターバッチでは、引張伸びにおいて、平均値が３００％と低く、且つ最大値と最小値との差が２８０％と大きく、この性能に劣っていた。また、アイゾット衝撃値では、最大値と最小値との差が１１ｋＪ／ｍ^２と大きく、この性能は安定していなかった。
融点が１６１℃と高い比較例２のマスターバッチでは、引張伸びにおいて、平均値が３５０％と低く、且つ最大値と最小値との差が１７０％と大きく、この性能に劣っていた。また、アイゾット衝撃値では、最大値と最小値との差が９ｋＪ／ｍ^２と大きく、この性能は安定していなかった。
尚、比較例１、２において、引張強度及び曲げ弾性率は共に問題なかった。
【００４１】
これらに対して、マスターバッチの融点が１４０〜１５９℃である実施例１〜６では、引張伸びにおいて、平均値が４３０〜４８０％と高く、且つ最大値と最小値との差が２０〜７０％と小さく、この性能は良好であった。また、アイゾット衝撃値では、平均値が４０〜６０ｋＪ／ｍ^２と高く、且つ最大値と最小値との差が３〜６ｋＪ／ｍ^２と小さく、この性能も良好であった。更に、引張強度では、平均値が２２．６〜２３．３ＭＰａと高く、且つ最大値と最小値との差が０．５〜１．３ＭＰａと小さく、この性能も良好であった。また、曲げ弾性率においても、１６８０〜２０５９ＭＰａと高く、優れた性能を有していた。
以上のことより、実施例１〜６の各マスターバッチは、主材と混合した際に、主材と均一に混合可能であり、性能バランスに優れるコンパウンド材料が得られることが分かった。
【００４２】
【発明の効果】
本発明のマスターバッチは、主材と混合した際に、主材と均一に混合可能であるため、物性が安定しており、性能バランスに優れたコンパウンド材料を得ることができる。そのため、自動車部品等に使用されるコンパウンド材料に好適である。
また、マスターバッチのＭＦＲを特定の値とした場合には、主材と混合した際の分散性をより向上させることができる。
更に、他の樹脂成分として、エチレン・プロピレンブロック共重合樹脂を含有させた場合には、主材と混合した際の分散性をより向上させることができる。
また、樹脂成分における結晶性プロピレンランダム共重合樹脂の割合を特定の範囲とした場合には、主材と混合した際の分散性をより向上させることができる。
更に、無機充填剤の含有量を特定の範囲とした場合には、有効な量の無機充填剤が均一に分散しているマスターバッチとなる。
また、特定の無機充填剤を用いた場合には、より優れた補強効果を有するコンパウンド材料となる。
【図面の簡単な説明】
【図１】実施例２におけるマスターバッチのＤＳＣ曲線を説明する模式図である。
【図２】比較例１におけるマスターバッチのＤＳＣ曲線を説明する模式図である。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a masterbatch. More specifically, the present invention relates to a masterbatch capable of uniformly dispersing an inorganic filler as a whole when mixed with a main material and obtaining a compound material having stable physical properties such as tensile elongation and Izod impact value.
The masterbatch of the present invention is widely used in the production of various industrial articles such as automobile parts such as bumpers, instrument panels, ceilings, doors and sun visors, and parts of home electric appliances such as televisions, VTRs and washing machines.
[0002]
[Prior art]
Conventionally, a ternary composite material of polypropylene / rubber / inorganic filler (such as talc), a so-called compound material, has been used as a general olefin-based material, particularly a polypropylene resin material, used for automobile parts and the like. Many. This polypropylene compound material is widely used because it is excellent in moldability, mechanical strength, and the like, and is economically advantageous.
Such a compound material is obtained by compounding a minimum amount of additives to a powdery polypropylene neat polymer, pelletizing via a kneading extruder, further compounding rubber, talc, etc., and re-mixing the kneading extruder. Can be produced by pelletizing via
[0003]
The composition corresponding to the above compound material is prepared by mixing rubber and talc at a high concentration in advance with polypropylene as a carrier resin, and pelletizing the mixture through a kneading extruder (master batch). (Base resin) is blended with polypropylene at a specific ratio, dry blended uniformly and then put into a hopper. When plasticized in an injection molding machine, both components are melted and subjected to shearing force with a screw. Can be prepared by a so-called master batch method in which the mixture is uniformly dispersed and kneaded so as to finally have a desired composition.
When a compound material is used by this master batch method, a specific function can be added only by changing the composition of the master batch while keeping the main material common, and the performance of the compound material finally prepared is improved. Can be changed. Further, the preparation by the master batch method has been attracting attention because the kneading processing cost is reduced.
[0004]
Examples of an application relating to a masterbatch for preparing such a compound material include, for example, a compound in which a talc component having a specific particle size and a metal soap component are mixed in a specific amount to an elastomer component having a specific fluidity ( For example, see Patent Document 1.) Further, a specific polypropylene resin, a specific inorganic filler and a specific polyethylene and / or a lubricating component, optionally a dispersion accelerating component, an ethylene / α-olefin copolymer rubber, and a compound in which a coloring component is blended in a specific ratio may be used. (For example, see Patent Document 2).
[0005]
[Patent Document 1]
JP 2000-273190 A [Patent Document 2]
JP 2002-3667 A
[Problems to be solved by the invention]
The preparation of the compound material by the masterbatch method is performed by mixing a masterbatch having a large difference in melting properties and dispersion properties with a main material in an injection molding machine having a weaker shearing force than a twin-screw extruder usually used for kneading and extrusion. In many cases, the mixture is kneaded with a single screw or the like, and it is necessary to uniformly mix with such a low shear force. If the mixing is insufficient, the physical properties are not stable, and the performance may vary.
However, inorganic fillers such as talc are components that are not melted by heat and do not participate in melting. Therefore, in order to uniformly mix the masterbatch and the main material, a masterbatch having a dispersibility enough to homogenize the inorganic filler included only in one side as a whole, and further includes a component that easily melts. There is a need for a masterbatch having a composition.
[0007]
The present invention has been made to solve the above problems, and when mixed with a main material, can uniformly disperse the inorganic filler as a whole, tensile elongation, a compound material having stable physical properties such as Izod impact value. The aim is to provide a masterbatch that can be obtained.
[0008]
[Means for Solving the Problems]
The present inventors have studied the improvement of the dispersibility of the inorganic filler when the masterbatch and the main material are mixed, and as a result, have a crystalline propylene random copolymer resin as a carrier resin and have a specific range of melting point. By using a masterbatch, it has been found that when a masterbatch containing a high concentration of inorganic filler and the main material are mixed, the inorganic filler can be uniformly dispersed as a whole, and the present invention has been completed. Was.
[0009]
The masterbatch of the present invention contains a resin component containing a crystalline propylene random copolymer resin having a melting point of 110 to 155 ° C, a rubber component, and an inorganic filler, and has a melting point of 125 to 160 ° C. And
Further, a master batch having a melt flow rate (MFR) of 0.1 to 30 g / 10 min can be obtained.
Further, the resin component can be a masterbatch further containing an ethylene / propylene block copolymer resin.
Further, when the above resin component is 100 parts by mass, a master batch in which the amount of the crystalline propylene random copolymer resin is 20 parts by mass or more can be obtained.
Furthermore, when the total of the resin component, the rubber component, and the inorganic filler is 100 parts by mass, a masterbatch in which the inorganic filler is 40 to 75 parts by mass can be obtained.
In addition, a master batch in which the inorganic filler has an aspect ratio of 2 to 20 can be obtained.
Further, the inorganic filler may be a masterbatch that is at least one of talc and wollastonite.
In the present invention, the “melting point” means the maximum value among the melting peak temperatures measured by a differential scanning calorimeter (DSC). The “MFR” is a value measured at 230 ° C. under a load of 2.16 kg according to JIS K7210.
[0010]
BEST MODE FOR CARRYING OUT THE INVENTION
Hereinafter, the present invention will be described in detail.
The “crystalline propylene random copolymer resin” has a melting point of 110 to 155 ° C. This melting point is preferably from 115 to 150 ° C, more preferably from 120 to 145 ° C, even more preferably from 125 to 140 ° C. If the melting point is lower than 110 ° C., it is not preferable because the mechanical strength and the like of a molded product obtained by using this master batch are reduced. On the other hand, when the melting point exceeds 155 ° C., it is difficult to reduce the melting point of the master batch to 160 ° C. or less, and the dispersibility of the inorganic filler decreases, which is not preferable.
[0011]
Examples of the crystalline propylene random copolymer resin include a random copolymer resin of propylene and an α-olefin other than propylene.
Examples of the α-olefin include ethylene, 1-butene, 1-pentene, 4-methyl-1-pentene and 1-octene. Of these, ethylene is preferred. These α-olefins may be used alone or in combination of two or more.
[0012]
Further, the crystallinity of the crystalline propylene random copolymer resin is preferably 40% or more (usually 75% or less), and more preferably 50 to 70%. When the crystallinity is less than 40%, the resin becomes rubbery, and a resin having a desired melting point may not be obtained. The degree of crystallinity is a value calculated based on the amount of heat required for dissolving the crystals measured by DSC.
Furthermore, the content ratio of the propylene unit in the crystalline propylene random copolymer resin is not particularly limited, but is preferably 50% by mass or more, more preferably 80% by mass or more, and further preferably 90% by mass or more. If this content ratio is less than 50% by mass, the composition becomes rubbery, and a resin having a desired melting point may not be obtained.
[0013]
Further, the MFR of the crystalline propylene random copolymer resin is preferably 1 to 50 g / 10 min, more preferably 1.2 to 30 g / 10 min, and still more preferably 1.5 to 10 g / 10 min. When the MFR is 1 to 50 g / 10 min, the miscibility and dispersibility can be improved when mixed with the main material.
[0014]
Examples of commercially available crystalline propylene random copolymer resin include, for example, "Chisso Polypro XF1800" (trade name, manufactured by Chisso Petrochemical Co., Ltd., [melting point: 140 ° C, MFR: 1.8 g / 10 min], Nippon Polychem Co., Ltd.) Company name, Wintec XK1159 (melting point; 125 ° C., MFR: 7 g / 10 min), product name “Polypropylene Sun Allomer PC540R” (melting point: 132 ° C., MFR; 5 g / 10 min), manufactured by Sun Allomer Co., Ltd. Can be In addition, even a resin called a block copolymer which is a commercially available product, a resin which forms a sea-island structure microscopically and whose matrix is composed of a random copolymer can be used in the present invention. .
[0015]
In the “resin component”, the ratio of the crystalline propylene random copolymer resin is preferably 20 parts by mass or more, more preferably 50 to 90 parts by mass, and still more preferably, when the resin component is 100 parts by mass. Is 50 to 80 parts by mass. Incidentally, all the resin components may be a crystalline propylene random copolymer resin. When this content is 20 parts by mass or more, when mixed with the main material, it is possible to uniformly disperse the inorganic filler as a whole, and to obtain a compound material having stable physical properties and excellent performance balance. Obtainable.
[0016]
As the resin component, other resins may be contained in addition to the crystalline propylene random copolymer resin. The other resin is not particularly limited, and examples thereof include an olefin-based resin.
Examples of the olefin-based resin include a propylene homopolymer resin, a propylene copolymer resin other than the crystalline propylene random copolymer resin, and the like. These may be used alone or as a mixture of two or more.
Examples of the propylene copolymer resin include a copolymer resin of propylene with an α-olefin other than propylene, a vinyl ester, or the like. This copolymer resin may be any of a block copolymer resin, a random copolymer resin, and a graft copolymer resin. Among them, a block copolymer resin is preferable.
Examples of the α-olefin include ethylene, 1-butene, 1-pentene, 4-methyl-1-pentene and 1-octene. Among them, ethylene is preferable. Examples of the vinyl ester include vinyl acetate.
[0017]
The content ratio of the propylene unit in the propylene copolymer resin is not particularly limited, but is preferably 50% by mass or more, more preferably 80% by mass or more, and further preferably 90% by mass or more.
Among them, the propylene copolymer resin is preferably an ethylene / propylene block copolymer resin, and particularly preferably a propylene unit resin having a propylene unit content of 80% by mass or more, more preferably 90% by mass or more.
Incidentally, the ethylene / propylene block copolymer resin means a resin obtained by polymerizing propylene and ethylene in the presence of polypropylene.
In particular, in the present invention, as the resin component, it is possible to contain this ethylene-propylene block copolymer resin, in this case, when mixed with the ethylene-propylene block copolymer resin often used as the main material Dispersibility can be further improved.
Further, the ratio of the ethylene / propylene block copolymer resin is preferably 80 parts by mass or less, more preferably 10 to 50 parts by mass, and still more preferably 20 to 50 parts by mass when the resin component is 100 parts by mass. Department.
[0018]
Further, in order to improve the dispersibility of the inorganic filler, an acid-modified resin can be contained as a resin component. The acid-modified resin is not particularly limited as long as the resin has an acid group bonded thereto. Note that, in addition to the acid group, an NH ₂ group, an OH group, a CO group, or a CONH ₂ group may be bonded.
The resin is not particularly limited, but usually, a resin having low polarity is used. Examples of such a resin include an olefin resin.
Examples of the olefin-based resin include polyolefins obtained by polymerizing α-olefins alone or using two or more kinds.
Examples of the α-olefin include ethylene, propylene, 1-butene, 1-hexene, 4-methyl-1-pentene and 1-octene.
[0019]
The acid group, CO ₂ H group, CO ₂ ^- group, acid anhydride group, and the like.
For the introduction of the acid group into the resin, an unsaturated compound having an acid group such as an unsaturated carboxylic acid having such an acid group and an unsaturated carboxylic acid anhydride can be used. These may be used alone or as a mixture of two or more.
Examples of the unsaturated carboxylic acid include acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, citraconic acid, and nadic acid. Examples of the unsaturated carboxylic anhydride include maleic anhydride, itaconic anhydride, citraconic anhydride, allylsuccinic anhydride, nadic anhydride and the like.
Specific introduction methods include, for example, (1) a method of copolymerizing an unsaturated compound at the time of resin production, and (2) mixing of a resin, an unsaturated compound, and a small amount of an organic peroxide, followed by melt-kneading. And (3) a method in which a resin is dissolved in a solvent, an unsaturated compound and a small amount of an organic peroxide are added thereto, and a graft reaction is performed in a solution state.
[0020]
Examples of such an acid-modified resin include ethylene-acrylic acid copolymer resin, maleic acid-modified polyethylene, maleic acid-modified polypropylene, EVA-graft acrylic acid copolymer resin, and ethylene-ethyl acrylate-maleic acid copolymer resin. No. Further, an ionomer resin such as an ethylene / (meth) acrylic acid ionomer may be used.
These acid-modified resins may be used alone or as a mixture of two or more.
When the acid-modified resin is blended, the ratio of the acid-modified resin is preferably 0.6 to 15 parts by mass, more preferably 1.5 to 13 parts by mass when the resin component is 100 parts by mass. It is 5 parts by mass, more preferably 3 to 12 parts by mass.
[0021]
The content of these resin components is preferably 15 to 50 parts by mass, more preferably 15 to 40 parts by mass, when the total of the resin component, the rubber component and the inorganic filler is 100 parts by mass. Preferably it is 20 to 40 parts by mass. When the content is 15 to 50 parts by mass, a masterbatch capable of uniformly dispersing the inorganic filler as a whole when mixed with the main material can be obtained.
[0022]
Further, the resin component in the present invention can be composed of a crystalline propylene random copolymer resin and an ethylene / propylene block copolymer resin. In this case, when mixed with the main material, it can be more uniformly mixed with the main material, so that a compound material having more stable physical properties and excellent performance balance can be obtained. Further, in this case, the ratio of the resin component (crystalline propylene random copolymer resin: ethylene / propylene block copolymer resin) is preferably 40:60 to 90:10, more preferably 50:50 by mass ratio. ９０90: 10, more preferably 50:50 to 80:20.
[0023]
The “rubber component” is not particularly limited, and includes various rubbers. For example, olefin-based rubber, styrene-based thermoplastic elastomer and the like can be mentioned. Of these, olefin rubbers are preferred.
Examples of the olefin rubber include an ethylene / α-olefin copolymer rubber and an ethylene / α-olefin / non-conjugated diene copolymer rubber. Among them, ethylene / α-olefin copolymer rubber is preferable.
Examples of the α-olefin include propylene, 1-butene, 1-pentene, 4-methyl-1-pentene, 1-octene and the like.
Examples of the styrene-based thermoplastic elastomer include styrene / butadiene / styrene triblock copolymer (SBS), styrene / isoprene / styrene triblock copolymer (SIS), hydrogenated SBS (SEBS), and SIS Hydrogenated product (SEPS).
As the styrene-based thermoplastic elastomer, SEBS and SEPS are particularly preferable because the weather resistance can be improved.
These olefin rubbers and styrene thermoplastic elastomers may be used alone or in combination of two or more. Further, an olefin rubber and a styrene thermoplastic elastomer can be used in combination.
In addition, a functional group such as a CO ₂ H group, an NH ₂ group, or an OH group may be introduced into these rubber components in order to increase compatibility with the inorganic filler.
[0024]
The content of the rubber component is preferably 0.5 to 20 parts by mass, more preferably 1 to 15 parts by mass, when the total of the resin component, the rubber component and the inorganic filler is 100 parts by mass. Preferably it is 3 to 15 parts by mass. When the content is 0.5 to 20 parts by mass, a masterbatch capable of uniformly dispersing the inorganic filler as a whole when mixed with the main material can be obtained.
[0025]
The "inorganic filler" is not particularly limited, for example, talc, wollastonite, kaolin, clay, pyrophyllite, mica, montmorillonite, bentonite, sepiolite, zonotolite, natural silica, synthetic silica, various glass fillers, zeolite , Diatomaceous earth, halloysite, and the like. These may be surface-treated with various coupling agents, metal salts, or the like in order to further enhance dispersibility. These may be used alone or as a mixture of two or more. Of these, talc and wollastonite are preferred.
The inorganic filler preferably has an aspect ratio of 2 to 20, more preferably 4 to 20, and still more preferably 5 to 20. When the aspect ratio is from 2 to 20, a compound material having a sufficient reinforcing effect and having excellent dimensional stability of a molded product is obtained.
In particular, as the inorganic filler, at least one of talc and wollastonite having an aspect ratio of 2 to 20 is preferable. Further, talc having an aspect ratio of 2 to 20 is preferable because a more excellent reinforcing effect can be obtained.
[0026]
The average particle size of the inorganic filler is not particularly limited. For example, when talc is used, the average particle size is preferably 1 to 15 μm, more preferably 1.5 to 10 μm, and further preferably 2 to 8 μm. When wollastonite is used, the thickness is preferably 5 to 50 μm, more preferably 5 to 45 μm, and still more preferably 5 to 40 μm.
[0027]
The content of the inorganic filler is preferably 40 to 75 parts by mass, more preferably 40 to 70 parts by mass, and more preferably 40 to 70 parts by mass, when the total of the resin component, the rubber component and the inorganic filler is 100 parts by mass. Is 50 to 70 parts by mass. When the content is 40 to 75 parts by mass, a master batch in which an effective amount of the inorganic filler is uniformly dispersed is obtained.
[0028]
Further, a fatty acid metal salt can be blended in the master batch of the present invention. When the fatty acid metal salt is blended, the dispersibility of the inorganic filler contained in the master batch can be further improved. Further, when mixed with the main material, the inorganic filler can be more uniformly dispersed as a whole.
The fatty acid metal salt is not particularly limited, and examples thereof include a metal stearate, a metal laurate, a metal behenate, a metal montanate, and a metal hydroxystearate. Examples of the metal element include lithium, sodium, magnesium, calcium, barium, zinc, and aluminum. Among them, magnesium stearate, calcium stearate, lithium stearate, zinc stearate and the like are preferable.
[0029]
The content of the fatty acid metal salt is preferably 0.2 to 1 part by mass, more preferably 0.3 to 1 part by mass, when the total of the resin component, the rubber component and the inorganic filler is 100 parts by mass. And more preferably 0.3 to 0.8 parts by mass. When this content is 0.2 to 1 part by mass, the masterbatch is excellent in dispersibility of the inorganic filler and can uniformly disperse the inorganic filler as a whole when mixed with the main material. It can be. Further, a compound material having more excellent moldability can be obtained. When the content is less than 0.2 parts by mass, the effect of improving dispersibility is small. On the other hand, when the amount exceeds 1 part by mass, mold contamination due to bleed may be deteriorated.
[0030]
Further, the masterbatch of the present invention may contain any other additives and the like as long as the effects of the present invention are not impaired. Other additives include, for example, antioxidants, nucleating agents, light stabilizers, ultraviolet absorbers, coloring agents, antistatic agents, flame retardants, lubricants, and dispersion accelerators.
In particular, when the antioxidant is compounded, the compounding amount is preferably 0.01 to 1 part by mass, when the total of the resin component, the rubber component and the inorganic filler is 100 parts by mass, and more preferably. It is 0.05 to 0.5 parts by mass.
Moreover, when mix | blending a nucleating agent, the compounding quantity is preferably 0.05-5 mass parts, More preferably, it is 0.1-3 mass parts.
Further, when the light stabilizer is compounded, the compounding amount is preferably 0.01 to 1 part by mass, and more preferably 0.05 to 0.5 part by mass.
Moreover, when compounding an ultraviolet absorber, the compounding quantity is preferably 0.01 to 0.5 part by mass, more preferably 0.01 to 0.3 part by mass.
[0031]
Further, the MFR of the masterbatch of the present invention is preferably 0.1 to 30 g / 10 min, more preferably 0.2 to 15 g / 10 min, and still more preferably 0.3 to 10 g / 10 min. When the MFR is 0.1 to 30 g / 10 min, the dispersibility when mixed with the main material can be further improved.
[0032]
The method for producing the masterbatch of the present invention is not particularly limited, but (1) each component such as a resin component, a rubber component, and an inorganic filler is dry-blended at a predetermined ratio, and a single-screw extruder, a twin-screw extruder, It can be manufactured by a method of kneading and granulating using a general kneading machine such as a Banbury mixer, a roll mixer and a kneader. Also, (2) a so-called stirring kneading granulation method or the like, in which a mixture is obtained while stirring with a high-speed rotary stirring mixer such as a super mixer or a Henschel mixer, and then kneaded and granulated with an extruder, can be used. .
In addition, at the time of kneading and granulation, the compound of each of the above components may be kneaded at the same time, or each component may be divided in order to improve performance, for example, first, a rubber component and a part of an inorganic filler. Alternatively, it is also possible to knead all the components, and then knead and granulate the remaining components.
[0033]
Further, the masterbatch of the present invention is used as a compound material by mixing with the main material.
As the main material, the same material as the olefin-based resin can be used, and usually, the same or similar one is used in which the olefin-based resin and the type of the monomer, the ratio of the monomer units, and the like are the same. . In particular, an ethylene / propylene block copolymer resin is often used.
The method for preparing the compound material using the main material and the masterbatch is not particularly limited, but generally, each is dry-blended at an arbitrary ratio and then subjected to an injection molding method (including a gas injection molding method) or an injection molding method. When molding by a compression molding method or the like, it can be prepared in an extruder of each molding machine. In this case, the mixing ratio (mass ratio) of the main material and the master batch is preferably 90:10 to 40:60, and more preferably 90:10 to 50:50.
[0034]
【Example】
Hereinafter, the present invention will be described in more detail with reference to examples.
[1] Raw material used (A) Crystalline propylene random copolymer resin (1) “Chisso Polypro XF1800” manufactured by Chisso Petrochemical Co., Ltd., melting point: 140 ° C., MFR: 1.8 g / 10 min
(2) Sun Allomer Co., Ltd., trade name "Polypropylene PC540R", melting point: 132 ° C, MFR: 5 g / min
(B) Other resin components (ethylene / propylene block copolymer resin)
(1) Idemitsu Petrochemical Co., Ltd., product name "J966HP"
(2) Product name “PMA80X” manufactured by Sun Allomer Co., Ltd.
(C) Rubber component ethylene / 1-octene copolymer; manufactured by Dow Elastomer Co., Ltd., trade name "Engage 8200"
(D) Inorganic filler talc; trade name "LMS-200", manufactured by Fuji Talc Co., Ltd., aspect ratio: 15
(E) Fatty acid metal salt magnesium stearate; Sakai Chemical Industry Co., Ltd. (F) Antioxidant Ciba Specialty Chemicals Co., Ltd., trade name "Irganox 1010"
(G) Nucleating agent Asahi Denka Co., Ltd., trade name "NA-21"
(H) Light stabilizer Hindered amine light stabilizer, manufactured by Ciba Specialty Chemicals Co., Ltd., trade name "Kimasorb 119FL"
(I) UV absorber Ciba Specialty Chemicals Co., Ltd., trade name "Tinuvin 328"
[0035]
[2] Preparation of master batch Examples 1 to 6 and Comparative Examples 1 and 2
Each component was premixed at a predetermined ratio shown in Table 1 with a Henschel mixer, and the obtained premix was passed through a TEX44 (L / D = 49) co-rotating twin-screw kneading extruder manufactured by Nippon Steel Works, Ltd. The resulting mixture was uniformly kneaded and pelletized to prepare a master batch pellet.
At this time, the melting point and MFR of each master batch were measured by the methods described above. The results are also shown in Table 1.
Further, FIG. 1 (Example 2) and FIG. 2 (Comparative Example 1) are explanatory diagrams based on DSC curves of each master batch in Example 2 and Comparative Example 1.
[0036]
[Table 1]

[0037]
[3] Preparation of test piece Each master batch pellet of Examples 1 to 6 and Comparative Examples 1 and 2 obtained in [2] and a main material [trade name “BJ4H-100 (3) manufactured by Sumitomo Mitsui Polyolefin Co., Ltd.” ) "(Ethylene-propylene block copolymer resin)] at a mass ratio of 1: 2 to obtain pellets substantially uniformly blended. The mixed pellets were put into a hopper of a 100-ton injection molding machine manufactured by Nissei Plastic Industrial Co., Ltd. to obtain a molded product, and the following test pieces for a tensile test, a bending test, and an Izod impact test were prepared.
[0038]
[4] Evaluation The following tests and measurements were performed using each test piece obtained in [3], and each performance was evaluated. Table 2 shows the measurement results.
(1) Tensile test In accordance with JIS K 7113, tensile strength and tensile elongation were measured at a tensile speed of 10 mm / min using a No. 2 dumbbell-shaped test piece.
{Circle around (2)} Bending test The bending elastic modulus was measured according to JIS K7171.
{Circle around (3)} Izod impact test According to JIS K 7110, the Izod impact value was measured at a test temperature of −20 ° C. without a notch.
Each test was performed 10 times, and the maximum and minimum data were deleted two by two. The maximum value, minimum value, average value, and the difference between the maximum value and the minimum value in the remaining six data were determined. (Variation) was recorded.
[0039]
[Table 2]

[0040]
[5] Effect of Example According to Table 2, in the masterbatch of Comparative Example 1 containing no crystalline propylene random copolymer resin and having a high melting point of 163 ° C., the average value in tensile elongation was as low as 300%. In addition, the difference between the maximum value and the minimum value was as large as 280%, and this performance was inferior. Further, in the Izod impact value, the difference between the maximum value and the minimum value was as large as 11 kJ / m ^2, and this performance was not stable.
In the masterbatch of Comparative Example 2 having a high melting point of 161 ° C., the average value in tensile elongation was as low as 350%, and the difference between the maximum value and the minimum value was as large as 170%. Further, in the Izod impact value, the difference between the maximum value and the minimum value was as large as 9 kJ / m ^2, and this performance was not stable.
In Comparative Examples 1 and 2, both tensile strength and flexural modulus were satisfactory.
[0041]
On the other hand, in Examples 1 to 6 in which the melting point of the masterbatch is 140 to 159 ° C, the average value in tensile elongation is as high as 430 to 480%, and the difference between the maximum value and the minimum value is 20 to 70%. %, And this performance was good. In addition, the average value of the Izod impact value was as high as 40 to 60 kJ / m ² , and the difference between the maximum value and the minimum value was as small as ³ to 6 kJ / m ² . Further, in the tensile strength, the average value was as high as 22.6 to 23.3 MPa, and the difference between the maximum value and the minimum value was as small as 0.5 to 1.3 MPa, and this performance was also good. Also, the flexural modulus was as high as 1680 to 2059 MPa and had excellent performance.
From the above, it was found that each of the master batches of Examples 1 to 6 can be uniformly mixed with the main material when mixed with the main material, and a compound material having an excellent performance balance can be obtained.
[0042]
【The invention's effect】
Since the masterbatch of the present invention can be uniformly mixed with the main material when mixed with the main material, a compound material having stable physical properties and excellent performance balance can be obtained. Therefore, it is suitable for compound materials used for automobile parts and the like.
Further, when the MFR of the master batch is set to a specific value, the dispersibility when mixed with the main material can be further improved.
Furthermore, when an ethylene / propylene block copolymer resin is contained as another resin component, the dispersibility when mixed with the main material can be further improved.
When the proportion of the crystalline propylene random copolymer resin in the resin component is in a specific range, the dispersibility when mixed with the main material can be further improved.
Furthermore, when the content of the inorganic filler is in a specific range, a master batch in which an effective amount of the inorganic filler is uniformly dispersed is obtained.
Further, when a specific inorganic filler is used, the compound material has a more excellent reinforcing effect.
[Brief description of the drawings]
FIG. 1 is a schematic diagram illustrating a DSC curve of a master batch in Example 2.
FIG. 2 is a schematic diagram illustrating a DSC curve of a master batch in Comparative Example 1.

Claims (7)

A master batch comprising a resin component containing a crystalline propylene random copolymer resin having a melting point of 110 to 155 ° C, a rubber component, and an inorganic filler, and having a melting point of 125 to 160 ° C. The masterbatch according to claim 1, wherein the melt flow rate is 0.1 to 30 g / 10 min. The masterbatch according to claim 1, wherein the resin component further contains an ethylene / propylene block copolymer resin. The masterbatch according to any one of claims 1 to 3, wherein the crystalline propylene random copolymer resin is at least 20 parts by mass when the resin component is 100 parts by mass. 5. The inorganic filler according to claim 1, wherein the total amount of the resin component, the rubber component, and the inorganic filler is 100 parts by mass, and the inorganic filler is 40 to 75 parts by mass. 6. Master Badge. The masterbatch according to any one of claims 1 to 5, wherein the inorganic filler has an aspect ratio of 2 to 20. The masterbatch according to claim 6, wherein the inorganic filler is at least one of talc and wollastonite.

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