WO2016052029A1 - ウエザストリップ用摺動材の製造方法 - Google Patents
ウエザストリップ用摺動材の製造方法 Download PDFInfo
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/16—Ethene-propene or ethene-propene-diene copolymers
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- C08L2312/00—Crosslinking
Definitions
- the present invention relates to a method for producing a weatherstrip sliding material.
- the weather strip is generally formed of an olefin polymer (rubber, thermoplastic resin, or thermoplastic elastomer), and in particular, a glass run, an inner weather strip, an outer wafer, which is attached to a window frame and is in sliding contact with glass.
- olefin polymer rubber, thermoplastic resin, or thermoplastic elastomer
- the following means are known in order to improve the slidability of the glass.
- Patent Document 1 discloses a sliding material obtained by extruding a raw material in which a silicone compound is blended in an olefin polymer in an amount of 5 to 20% by weight, and the surface of a portion that is in sliding contact with glass using the sliding material. A weatherstrip with molded parts is described.
- the silicone compound imparts slidability, but as a contradiction, there is a problem that a cross-sectional cutting step is required because the adhesiveness with the mold part is lowered when the blending amount is large.
- Patent Document 2 (2) Mixing of resin fine particles
- an olefinic thermoplastic elastomer is used as the material of the weather strip body, and a polyethylene powder or particles are mixed into the base material of the olefinic resin as the material of the thin protective film.
- a method for producing a weather strip using resin and simultaneously extruding with two extruders is described. Since polyethylene powder or particles having high viscosity and low fluidity are used, extrusion molding is performed while maintaining a certain degree of powder or particle shape, and a rough surface portion with fine irregularities is formed on the surface.
- the base material of the thin protective film is a resin, so that the flexibility is inferior.
- an olefin-based thermoplastic elastomer composed of a polymer obtained by dynamically dispersing and kneading an ethylene-based copolymer rubber with an olefin-based resin is blended with an acrylic-modified organopolysiloxane, and further a polyethylene-based fine particle powder.
- a composition comprising at least one fine particle powder selected from polystyrene fine particle powder and acrylic fine particle powder (average particle size is 30 to 80 ⁇ m), and a portion which is in sliding contact with glass of the weather strip using the composition Is described.
- sufficient slidability was not obtained even by this method.
- an object of the present invention is to provide a weather strip sliding material having a small coefficient of friction, sliding resistance, wear amount, etc. and good slidability.
- Thermoplastic elastomer is a polymer composed of thermoplastic resin and rubber.
- TPE produced by a reactive process called Dynamic Vulcanization is dynamically cross-linked thermoplastic elastomer (TPV).
- Thermoplastic Vulcanizates Dynamic cross-linking is a process of melt-kneading a thermoplastic resin and rubber and simultaneously cross-linking the rubber under shear, and is referred to as a process of statically cross-linking ordinary rubber.
- TPV has a sea-island structure in which a crosslinked rubber is dispersed as a domain (island phase) in a thermoplastic resin that is a matrix (sea phase).
- weatherstrips are polypropylene (PP), one of olefinic thermoplastic resins, and ethylene-propylene-diene copolymer rubber (EPDM), one of olefinic rubbers. Is an olefinic TPV.
- PP polypropylene
- EPDM ethylene-propylene-diene copolymer rubber
- the present inventors have found that it is possible to improve the dispersibility and size uniformity of PE particles by kneading PP, EPDM before cross-linking, and polyethylene (PE) particles.
- the present invention has been reached.
- the present invention is for a weather strip made of an olefinic TPV in which PE particles are dispersed by introducing PPDM, EPDM before crosslinking, and PE particles into a twin screw extruder and dynamically crosslinking EPDM while melt kneading. This is a method of manufacturing a sliding material.
- the PE particles When PP, EPDM and PE particles before cross-linking are introduced into a twin screw extruder, the PE particles are easily dispersed in PP as a matrix. Also, in the process where PP, EPDM and PE particles before cross-linking are melt-kneaded through a twin screw extruder, the PE particles are refined by shearing by biaxial rotation and the particle size becomes uniform. , Easier to disperse.
- the PE particles have a surface of the weatherstrip sliding material used for the glass sliding contact portion of the weatherstrip with a uniform pitch and a convex height to reduce the contact area with the glass. The amount of wear is reduced and the slidability is improved.
- the PE particles may be put into a hopper in the first half of the axial length of the twin screw extruder where dynamic crosslinking of EPDM has not progressed so much, for example, PP and EPDM before crosslinking are simultaneously fed into the same hopper. It can be added to a hopper adjacent to the PP and the EPDM hopper before crosslinking.
- the blending amount of the PE particles is 10 to 90 parts by mass with respect to 100 parts by mass in total of PP and EPDM.
- the blending amount of the PE particles is less than 10 parts by mass, the friction coefficient and the sliding resistance are increased.
- the blending amount is more than 90 parts by mass, the wear of the glass in sliding contact is increased.
- the average particle size of the PE particles is 30 to 200 ⁇ m before being charged, and is preferably 10 to 50 ⁇ m in the weatherstrip sliding material produced by refinement by melt-kneading. This is because the particle size of the PE particles is made uniform by being refined within this range.
- the average particle size of the PE particles in the present invention is 100 g using 9 types of sieves (openings: 710 ⁇ m, 500 ⁇ m, 425 ⁇ m, 300 ⁇ m, 212 ⁇ m, 150 ⁇ m, 106 ⁇ m, 75 ⁇ m, 53 ⁇ m) defined in JIS Z8801. This is a value obtained by measuring the particle diameter of 50% in the integral curve obtained by integrating the weight of the particles remaining on each sieve obtained when the particles are classified from the side having a large opening.
- PE particles examples include medium density PE (MDPE), high density PE (HDPE), high molecular weight PE (HMWPE), and ultra high molecular weight PE (UHMWPE), but compared with general MDPE and the like. UHMWPE having abrasion resistance several times or more is preferable.
- MDPE medium density PE
- HDPE high density PE
- HMWPE high molecular weight PE
- UHMWPE ultra high molecular weight PE
- the weatherstrip sliding material may further contain 30 parts by mass or less of a silicone compound with respect to 100 parts by mass in total of PP and EPDM in order to improve the slidability of the glass.
- the blending amount of the silicone compound is 30 parts by mass or less when the weatherstrip sliding material is used for the glass sliding contact portion of the weather strip so that the adhesive property between the glass sliding contact portion and the weather strip main body is increased. It is because it does not worsen.
- the silicone compound may be charged into the twin screw extruder and kneaded with PP and EPDM and PE particles before crosslinking, (2) The olefinic TPV in which the PE particles obtained by the twin screw extruder are dispersed and the silicone compound may be newly added to the twin screw extruder and melt kneaded.
- silicone compound examples include silicone oil, silicone gum, silicone copolymer and the like.
- cross-linking agent cross-linking agent, cross-linking accelerator, etc.
- other blends include compatibilizers, carbon black, antioxidants, processing aids, colorants and the like.
- the manufactured weather strip sliding material preferably has a static friction coefficient of 0.4 or less, a dynamic friction coefficient of 0.2 or less, and a sliding resistance of 10.0 N or less after 50000 cycles. More preferably, it is 5.0 N or less at 50000 times.
- Examples of the weather strip that is an application of the sliding material of the present invention include a glass run, an inner weather strip, an outer weather strip, and the like that are attached to a window frame portion and are in sliding contact with glass. It is suitable for forming a glass sliding contact portion.
- the manufacturing method of the sliding material for weather strips which concerns on an Example is shown, (a) is schematic when throwing PP, EPDM and PE particle
- (A1) is a side view of the wear test
- (a2) is a cross-sectional view of the test piece after the wear test
- (b1) is a side view of the sliding resistance measurement
- (b2) is a plan view of the sliding resistance measurement.
- the weatherstrip sliding material of the example was molded using the sliding contact portion with the glass, (a) is a cross-sectional view of the glass run, (b) is a cross-sectional view of the inner weather strip and the outer weather strip is there.
- (a) is the schematic when the olefin type TPV and PE particle
- (b ) Is a schematic diagram showing the structure of the weatherstrip sliding material obtained in (a).
- the blending amount of PE particles is 10 to 90 parts by mass with respect to 100 parts by mass in total of PP and EPDM.
- the average particle size of the PE particles is 30 to 200 ⁇ m before being charged, and is preferably 10 to 50 ⁇ m in the weatherstrip sliding material produced by refinement by melt-kneading.
- the material of the PE particles is preferably ultra high molecular weight PE.
- the weatherstrip sliding material may further contain 30 parts by mass or less of a silicone compound with respect to 100 parts by mass of PP and EPDM in total.
- the silicone compound can be charged into the twin screw extruder and kneaded with PP, EPDM and PE particles before crosslinking.
- the olefinic TPV in which the PE particles obtained by the twin-screw extruder are dispersed and the silicone compound can be newly introduced into the twin-screw extruder and melt-kneaded.
- the olefinic TPVs weather strips for weather strips
- Examples 1 to 7 and Comparative Example 1 having the composition shown in the following Table 1 were prepared.
- the blending numerical value is 100 parts by mass of the total of PP and EPDM, and indicates the parts by mass of other materials.
- ⁇ PP Block PP, trade name of Nippon Polypro Co., Ltd. “Novatech PP EC7”
- EPDM JSR Corporation trade name “EP98” -PE particles: UHMWPE particles, trade name “Hi-Zex Million 240S” (average molecular weight: about 2 million, average particle size: about 120 ⁇ m)
- Compatibilizer Trade name “Tuffmer 7080” of Mitsui Chemicals
- Carbon black Carbon black masterbatch (MB), trade name “MFP-CB45L” of Mifuku Industry Co., Ltd.
- Crosslinking agent Phenol resin, trade name of Taoka Chemical Co., Ltd.
- Antioxidant Hindered phenolic antioxidant, trade name “IRGANOX1010” of BASF Silicone compound: Pellet-like silicone, trade name “BY27-001” of Toray Dow Corning Co., Ltd.
- the olefinic TPVs of Examples 1 to 7 and Comparative Example 1 were prepared by the following two steps.
- (1) Step for producing olefinic TPV in which PE particles are dispersed As shown in FIG. 1A, PP and EPDM before crosslinking are compatibilized in a first hopper 11 at the base end of a twin screw extruder 10. , Carbon black, a crosslinking agent and an antioxidant are added together, and PE particles are introduced into the second hopper 12 adjacent thereto (in the first half of the axial length of the twin-screw extruder) and passed through the twin-screw extruder 10.
- the olefinic TPV1 in which the PE particles were dispersed was extruded by dynamically crosslinking the EPDM while melt-kneading the PP, the EPDM before crosslinking, and the PE particles by shearing by biaxial rotation. And this olefin type TPV1 was pelletized. In addition, you may throw these materials into the 1st hopper 11 collectively.
- FIG. 1 (c) schematically shows an enlarged structure of the olefinic TPV2 produced in Examples 1-7.
- the olefinic TPV2 of Examples 1 to 7 had a sea-island structure in which EPDM4 was dispersed as a domain (island phase) in PP3 as a matrix (sea phase), and PE particles 5 were further dispersed. Compared with the conventional example of FIG. 4B described above, both the EPDM 4 and the PE particles 5 were more dispersible.
- the average particle size of the PE particles 5 was about 120 ⁇ m before being charged, but was refined by melt-kneading and was about 50 ⁇ m in the produced olefin TPV2, and was uniformed.
- Static friction coefficient dynamic friction coefficient Based on JIS K7125, it calculated from the load when moving at 100 mm / min. The static friction coefficient was evaluated as “good” when 0.4 or less, and “impossible” when more than 0.4. The coefficient of dynamic friction was evaluated as “good” when 0.2 or less and “impossible” when more than 0.2.
- a test piece 2 a having a width of 5 mm, a length of 160 mm, and a thickness of 2 mm formed with an olefin-based TPV 2 is produced, and the test piece 2 a is placed on the holder 15. Attached and set to testing machine.
- a plate-shaped glass wear piece 16 having a sliding direction length of 30 mm is placed on the test piece 2a, a load of 10N is applied, and the surface of the test piece 2a is reciprocated in the length direction at a sliding speed of 150 mm / second. It was.
- the load in the horizontal direction at the number of reciprocating sliding times of 50000 was measured and used as a sliding resistance value.
- the sliding resistance was evaluated as “good” when 10 N or less, and “impossible” when over 10 N.
- Abrasion amount by glass As shown in FIG. 2 (b 1), a test piece 2 b having a width of 20 mm, a length of 160 mm, and a thickness of 2 mm formed by an olefin-based TPV 2 is prepared, and the test piece 2 b is attached on the holder 17. It was set in a testing machine. A glass wear piece 18 having a bottom surface width of 50 mm ⁇ sliding direction length of 20 mm (with R10 mm) is placed on the test piece 2b, a load of 30N is applied, and the surface of the test piece 2b is slid 60 times in the length direction. It was slid back and forth at / min. As shown in FIG.
- the amount of wear (mm) of the test piece 2b after reciprocating 10,000 times was measured.
- the wear amount was evaluated as “good” when 0.10 mm or less, “good” when 0.10 mm to 0.11 mm or less, and “impossible” when more than 0.11 mm.
- Each of the olefinic TPVs 2 of Examples 1 to 7 includes, for example, a glass run 31 as shown in FIG. 3 (a), an inner weather strip 32 and an outer weather strip 33 as shown in FIG. 3 (b). It can be used as a weather strip sliding material at the sliding contact portion with 40.
- this invention is not limited to the said Example, In the range which does not deviate from the meaning of invention, it can change suitably and can be actualized.
- the silicone compound was kneaded in the second step, but the silicone compound may be charged into the twin screw extruder 10 in the first step and kneaded together with the PP, the EPDM and PE particles before crosslinking.
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Abstract
Description
特許文献1には、オレフィン系ポリマーにシリコーン化合物を5~20重量%配合した原料の押し出しにより得られる摺動材料と、それを使用してガラスと摺接する部位の表面部分を成形したウエザストリップが記載されている。
しかし、シリコーン化合物は、摺動性は付与するが、その背反事項として、配合量が多いと型部との接着性を低下させるため、断面の切り出し工程が必要になるという問題がある。
特許文献2には、ウエザストリップ本体の材料としてオレフィン系熱可塑性エラストマーを使用し、薄保護膜の材料としてオレフィン系樹脂のベース材料にポリエチレン粉末又は粒子を混合した合成樹脂を使用して、二台の押し出し成形機で同時押し出し成形するウエザストリップの製造方法が記載されている。ポリエチレン粉末又は粒子は、高粘度・低流動性のものを用いるので、ある程度の粉末又は粒子の形状を維持したままで押し出し成形され、表面に細かい凹凸の粗面部を形成するとしている。
しかし、本発明者らの検討によると、薄保護膜のベース材料が樹脂であるため、柔軟性に劣るという問題があった。
しかし、本発明者らの検討によると、この手法によっても十分な摺動性は得られなかった。
なお、本発明におけるPE粒子の平均粒径は、JIS Z8801で規定された9種類の篩(目開き:710μm、500μm、425μm、300μm、212μm、150μm、106μm、75μm、53μm)を用いて、100gの粒子を分級した際に得られる各篩に残った粒子の重量を目開きの大きい側から積分した積分曲線において、50%の重量になる粒子径を測定することにより得られた値である。
(1)シリコーン化合物を前記二軸押出機に投入してPPと架橋前のEPDMとPE粒子とともに混練してもよいし、
(2)前記二軸押出機で得られたPE粒子が分散したオレフィン系TPVとシリコーン化合物とを新たに二軸押出機に投入して溶融混練してもよい。
・PP:ブロックPP、日本ポリプロ株式会社の商品名「ノバテックPP EC7」
・EPDM:JSR株式会社の商品名「EP98」
・PE粒子:UHMWPE粒子、三井化学株式会社の商品名「ハイゼックスミリオン240S」(平均分子量約200万、平均粒径約120μm)
・相溶化剤:三井化学株式会社の商品名「タフマー7080」
・カーボンブラック:カーボンブラックマスターバッチ(MB)、三福工業株式会社の商品名「MFP-CB45L」
・架橋剤:フェノール樹脂、田岡化学工業株式会社の商品名「タッキロール250I」
・酸化防止剤:ヒンダードフェノール系酸化防止剤、BASF社の商品名「IRGANOX1010」
・シリコーン化合物:ペレット状シリコーン、東レ・ダウコーニング株式会社の商品名「BY27-001」
(1)PE粒子が分散したオレフィン系TPVの作製ステップ
図1(a)に示すように、二軸押出機10の基端の第1ホッパ11に、PPと架橋前のEPDMとを相溶化剤、カーボンブラック、架橋剤及び酸化防止剤とともに投入し、その隣の第2ホッパ12(二軸押出機の軸長の前半部にある)にPE粒子を投入して、二軸押出機10を通る過程で二軸の回転によるせん断によりPPと架橋前のEPDMとPE粒子とを溶融混練しながらEPDMを動的架橋することにより、PE粒子が分散したオレフィン系TPV1を押し出した。そして、このオレフィン系TPV1をペレット化した。
なお、第1ホッパ11に、これらの材料をまとめて投入してもよい。
図1(b)に示すように、前記二軸押出機10で得られたオレフィン系TPV1のペレットを、新たに二軸押出機20の基端の第1ホッパ21に投入し、その隣の第2ホッパ22にシリコーン化合物を投入して、これらを混練し、シリコーン化合物を含むオレフィン系TPV2を押し出した。
なお、第1ホッパ21に、これらの材料をまとめて投入してもよい。
JIS K6251に準拠し、常温で引張試験を行い、引張強度と伸び(切断時伸び)を測定した。引張強度は6.0MPa以上を「良」、6.0MPa未満を「不可」と評価した。伸びは70%以上を「良」、70%未満を「不可」と評価した。
JIS K7125に準拠し、100mm/分で移動させたときの荷重から算出した。静摩擦係数は0.4以下を「良」、0.4超を「不可」と評価した。動摩擦係数は0.2以下を「良」、0.2超を「不可」と評価した。
図2(a1)(a2)に示すように、オレフィン系TPV2で成形した幅5mm、長さ160mm、厚さ2mmの試験片2aを作製し、試験片2aを保持具15の上に取り付け、試験機にセットした。板状で摺動方向長さ30mmのガラス製摩耗子16を試験片2aに載せ、10Nの荷重を加え、試験片2aの表面をその長さ方向に摺動速度150mm/秒で往復摺動させた。往復摺動回数50000回目の水平方向の荷重を測定して摺動抵抗の値とした。摺動抵抗は10N以下を「良」、10N超を「不可」と評価した。
図2(b1)に示すように、オレフィン系TPV2で成形した幅20mm、長さ160mm、厚さ2mmの試験片2bを作製し、試験片2bを保持具17の上に取り付け、試験機にセットした。底面が幅50mm×摺動方向長さ20mm(R10mm付)のガラス製摩耗子18を試験片2bに載せ、30Nの荷重を加え、試験片2bの表面をその長さ方向に摺動速度60回/分で往復摺動させた。図2(b2)に示すように、往復10000回摺動後の試験片2bの磨耗量(mm)を測定した。摩耗量は0.10mm以下を「良」、0.10mm超~0.11mm以下を「可」、0.11mm超を「不可」と評価した。
(1)実施例ではシリコーン化合物を2ステップ目で混練したが、シリコーン化合物を1ステップ目の二軸押出機10に投入して前記PPと架橋前のEPDMとPE粒子とともに混練してもよい。
2 オレフィン系TPV(シリコーン化合物を含む)
2a 試験片
2b 試験片
3 PP
4 EPDM
5 PE粒子
10 二軸押出機
11 第1ホッパ
12 第2ホッパ
15 保持具
16 ガラス製摩耗子
17 保持具
18 ガラス製摩耗子
20 二軸押出機
21 第1ホッパ
22 第2ホッパ
31 ガラスラン
32 インナウエザストリップ
33 アウタウエザストリップ
Claims (7)
- PPと架橋前のEPDMとPE粒子とを二軸押出機に投入して溶融混練しながらEPDMを動的架橋することにより、PE粒子が分散したオレフィン系TPVよりなるウエザストリップ用摺動材を製造する方法。
- PPとEPDMとの合計100質量部に対して、PE粒子の配合量が10~90質量部である請求項1記載のウエザストリップ用摺動材を製造する方法。
- PE粒子の平均粒径は、投入前に30~200μmであり、溶融混練で微細化し、製造されたウエザストリップ用摺動材中において10~50μmである請求項1又は2記載のウエザストリップ用摺動材を製造する方法。
- PE粒子の材料が、超高分子量PEである請求項1~3のいずれか一項に記載のウエザストリップ用摺動材を製造する方法。
- ウエザストリップ用摺動材は、PPとEPDMとの合計100質量部に対して、さらに30質量部以下のシリコーン化合物を配合したものである請求項1~4のいずれか一項に記載のウエザストリップ用摺動材を製造する方法。
- シリコーン化合物は前記二軸押出機に投入してPPと架橋前のEPDMとPE粒子とともに混練する請求項5記載のウエザストリップ用摺動材を製造する方法。
- 前記二軸押出機で得られたPE粒子が分散したオレフィン系TPVとシリコーン化合物とを新たに二軸押出機に投入して溶融混練する請求項5記載のウエザストリップ用摺動材を製造する方法。
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WO2020005442A1 (en) * | 2018-06-29 | 2020-01-02 | Dow Global Technologies Llc | Thermoplastic vulcanizates modified polypropylene for subsea insulation |
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