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Acrylic TPE Approaching Automotive 7KHUPRSODVWLF (ODVW PDJD]LQH LQWHUQDWLRQDO

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Acrylic TPE Approaching Automotive 7KHUPRSODVWLF (ODVW PDJD]LQH LQWHUQDWLRQDO J. Oertel, S. Kishii, D. Kilian, K. Hamada, Y. Morishita, T. Kurihara, T. Ito V RPHU Acrylic TPE approaching automotive 7KHUPRSODVWLF (ODVW PDJD]LQH LQWHUQDWLRQDO Volume 2, March 2010 P. O. Box 10 41 25 40852 Ratingen/Germany 1| 2010 acrylic tpe PMMA modifications and for combinations Acrylic TPE approaching automotive of LA-Polymer with engineering plastic PBT for targeting automotive applications. J. Oertel, S. Kishii, D. Kilian, K. Hamada, Y. Morishita, T. Kurihara, T. Ito* Figure 1 shows the molecular structure of LA-Polymer, which is fully (meth)acrylic tri- Recently, Kuraray has developed a novel all (meth)acrylic block polymer named block copolymer. It is sequentially prepared LA-Polymer by using its own polymerisation technologies. The structures of LA- by using our living anionic polymerisation Poly mer are triblock copolymers. i. e. poly(methyl methacrylate)-block-poly(n-butyl system. The LA-Polymer is built of two ter- acrylate)-block-poly(methyl methacrylate) [1]. LA-Polymer is processed in Kuraray’s minal hard PMMA blocks (Tg = 100 ~ 120 °C) pilot plant at commercial level in Japan. In this paper, characteristics and some pos- and one inner soft rubbery PnBA block sible application examples of LA-Polymer and its modifications with engineering plas- (Tg = -40 ~ -50 °C). In general LA-Polymer tics for potential automotive use are shown. can be used as a thermoplastic elastomer. The result of SEC (Size Exclusion Chroma- 1. Introduction proofed also for LA-Polymer as well as a high tography) and molecular weight distribution level of transparency (fig. 3). curves of LA-Polymer and conventionally made After Kuraray developed key technology PMMA are depicted in figure 2a. The molecular for mass production of specialised PMMA- In looking at the polar nature of LA-Poly- weight distribution of LA-Polymer is more nar- PnBA-PMMA triblock copolymers, (fig. 1) mer we found good compatibility and adhe- row than the one of a conventional acrylic pol- the use of flexibilised PMMA with no change sion to other polar plastics like PC, ABS, SAN ymer. Moreover, LA-Polymer has a well-defined in transparency was the first exiting char- and even PVC. In fact the polarity seems also structure and a very low content of mono mers acteristic feature. Furthermore, we found causal for good paintablity. With inorganic and oligomers. In figure 2b the grade map monomers and oligomers are absent which fillers we found a good dispersion effect be- is shown with three grades, LA2140e, LA2250 provides basically odourlessness in applica- side good compatibility. Depending on the and LA4285, being produced as pellets in dif- tion. This is also supported by a very narrow molecular weight and structure, LA-Polymer ferent Shore hardnesses (A32-soft, A65-mid- molecular weight distribution (fig. 2a) [2]. show a low to very low melt viscosity. This dle, A95-hard). Hardness generally depends on Because of the intrinsic elastic part PnBA fact is used for adjusting well-set elastified the content of PMMA blocks. rubber, no additional plasticisers are need- ed to get flexibilisation of PMMA in broad hardness and elasticity ranges. The well- All acrylic ABA type triblock copolymer CH HCH known weatherability aspects of PMMA were 3 3 (– CH2 – C –) n – b – (– CH2 – C –) m – b – (– CH2 – C –) n – C = OC = OC = O * Joerg Oertel, Shiro Kishii, Dr. Dirk Kilian OCH3 OC4H9 OCH3 Kuraray Europe GmbH, Frankfurt, Germany PMMA PnBa [email protected] Fig. 1: PMMA Structure of LA-Polymer - by using our living ani- Kenichi Hamada, Yoshihiro Morishita, onic polymerisation Soft block Toyoaki Kurihara, Toshiyuki Ito Hard block system, the acrylic block T − 40 ~ − 50 °C T 100 ~ 120 °C g Kuraray Co. Ltd, Tokyo, Japan copolymers were se- g quentially polymerised. Fig. 2b: Grade map of different LA-Polymer types LA-Polymer 50 Hard LA4285 (Living polymerisation) Hardness A 95, D57 Mw/Mn = 1.28 % 40 Acrylic polymer wt (Radical polymerisation) LA2250 Mw/Mn = 11 30 Hardness A 65 Soft LA2140e Fig. 2a: 20 Hardness A 32 SEC (Size Exclusion Chro- PMMA block cont. matography) and mole- 10 cular weight distribution 102 103 104 105 106 107 curves of LA-Polymer MW and conventionally made 50K 75K 100K 125K Total Mw PMMA 30 TPE Magazine · 1|2010 2. Characteristics The TEM photo also shows that LA-Poly- For structure analysis, TEM micrographs of mer has a well-defined structure. The mi- LA-Polymer are compiled in figure 3. Here 2.1 Morphologies cro-phase separation is very clear and the the black parts represent the PMMA and sample shows cylindrically arranged dark white parts are the PnBA. The LA-Polymer By using Kuraray’s specified staining PMMA micro-domains with an approxi- have different micro-phase separated mor- method, an observation of LA-Polymer with mate diameter size of 10 – 20 nm in a light phologies, which depend on the content ra- TEM has become possible (fig. 3). PnBA matrix. tio of PMMA block and PnBA block: • LA2140e short cylindrical morphology • LA2250 long cylindrical morphology TEM of LA-Polymer • LA4285 lamellar morphology. Black: PMMA domain White: PnBA matrix (hard domain) (rubbery matrix) 2.2 Transparency and durability LA2140e LA2250 LA4285 The dependence of several resins’ trans- mittance on wavelength has been measured (fig. 4). In the range of visible light wave- Fig. 3: length (380 – 780 nm), LA-Polymer has ex- Morphology investiga- cellent transparency (ca. 92 %). It is on the tion of LA-Polymer by same level as polymethyl methacrylate, and 100 nm TEM (Transmission Elec- tron Microscopy) it is suggested to be better than polycar- bonate and polystyrene (ca. 90 %). Fig. 4: Transparency of LA-Polymer compared to polycarbonate (PC) and polystyrene (PS) Figure 5 shows the weather resistance of Sample: 140 µm film LA-Polymer by Sunshine Weather-O-Meter 100 (SWOM) with retention of tensile strength and colour stability. After the specimen (2 mm thickness injection moulded sheets) had been 90 exposed, the values of factors (δa*,δb*,δYI) re- mained low with only little change. Suggest- ing that, the weather resistance of LA-Poly- mer is relatively stable with steady tensile ansmittancy (%) Tr 80 strength and very low yellowing. LA (PMMA = 30 %) PMMA PC TGA curves are shown in figure 6. The PS thermal stability is accounted by a tem- 70 400 500 600 700 800 perature of 5 % loss which is 316 °C in N2 Wave length (nm) atmosphere and 282 °C in air. As indicated above, LA-Polymer has good flow ability and it can be processed below the degrade tem- Fig. 5: Weather resistance test on tensile properties and colour change perature in injection moulding, extrusion moulding, compression moulding, hot-melt Test Method: JASO M346 (Xenon Arc Weather-O-Meter, Samples Before irradiation After irradiation coating, etc. Blending with other polymers 2 BPT 89 ºC, 50 % RH, 100 W/m ) (200 MJ/m2) can be conducted in a mixer or kneader such 200 MJ/m2 means about 10 years exposure = about 10 years for automobile interior parts. as kneader-ruder, extruder, mixing-roll, Ban- 140 LA4285 bury mixer, etc. 120 100 TPU 2.3 Flow properties polyester 80 type 60 TPU Compared to an HSBC with equivalent polyether 40 type molecular weight and hard block content, 20 LA2250 the LA-Polymer shows an extremely high LA4285 TPO Retention of tensile strength (%) 0 melt fluidity (means low melt viscosities) 0255075 100 125 MJ/m2 and softness properties, caused by the PnBA block (tab. 1). TPE Magazine · 1|2010 31 acrylic tpe In a study on the dynamic mechanical by mixing. A mix of LA2250 and LA4285 was 6. Comparison to TPO and TPU properties it was also indicated that LA- done without loss of transparency. Table 2 Polymer is softer than SEBS, and has a good shows properties of the injection-moulding When looking at the key properties of LA- high temperature performance, caused by a grades LA2250 and LA4285 and a 1:1 mix Polymer, it is useful to check the standard higher glass transition temperature (Tg) of of both. materials in these applications, thermoplas- the syndiotactic PMMA block. Molecular Hardness MFR [g/10 min] Because of their high flow and easy to characteristics paint properties, LA-Polymer can be effec- Mw Hard block [Shore A] 190 °C, 230 °C, content 2.16kg 2.16kg tively used in moulding materials, especially Tab. 1: Flow properties of LA-Polymer 77,000 30 wt.% 60 7.0 110 injection moulding. The melt viscosity as a LA-Polymer and HSBC function of shear rate at various tempera- (SEBS) SEBS 80,000 30 wt.% 80 0.04 0.46 tures is given in figure 7. This demonstrates the good processability of LA-Polymer with- out using plasticisers. TG Start Temp.: 30 °C End Temp.: 500 °C Rate: 10 °C/min 100 90 3. Adhesion to polar plastics 80 N2 70 Air Adhesion to plastics is generally request- 60 50 Standard moulding ed for all 2K applications. Conventional TPE eight (%) temperature Fig. 6: W based on HSBC has good adhesion to non- 40 Thermal stability ana- 30 polar plastics (PP, PS, PPE, etc.) but it is dif- lysed by TGA in air and 20 nitrogen. Measurement ficult to bond to polar plastics such as PC, 10 condition: The sample ABS, and PMMA. Recently, a TPV “bondable 0 was heated from 30 °C 0 100 200 300400 500 grade” was developed that shows improved to 500 °C at a rate of Temperature (°C) adhesion to polar plastics. It is used here as 10 °C/min. reference material. Fig. 7: Melt viscosity of LA-Polymer (MnBM) as a function of shear rate at various temperatures To investigate adhesion to polar plastics, an insert moulding system was prepared LA-Polymer SEBS 1.E+05 1.E+05 (fig.
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