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Process for Preparing Thermoplastic Composites

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Process for Preparing Thermoplastic Composites Europaisches Patentamt 0 369 206 j» European Patent Office © Publication number: A2 Office europeen des brevets EUROPEAN PATENT APPLICATION © Application number: 89119633.9 int. CIA C08L 69/00, C08L 83/10, B32B 27 28 © Date of filing: 23.10.89 © Priority. 18.11.88 US 273246 © Applicant: GENERAL ELECTRIC COMPANY 1 River Road @ Date of publication of application: Schenectady New York 12305(US) 23.05.90 Bulletin 90/21 © Inventor: Curry, Herbert Leard © Designated Contracting States: 800 Magnolia Drive DE FR GB IT NL Mount Vernon Indiana 47620(US) © Representative: Catherine, Alain General Electric France Service de Propriete Industrielle 18 Rue Horace Vernet F-92136 Issy-Les-Moulineaux Cedex(FR) © Process for preparing thermoplastic composites. © Thermoplastic composites of polycarbonate and siloxane-polycarbonate block copolymer layers are pro- duced by a coextrusion process. The composites are useful for the production of high-strength and impact resistant laminate glazing panels. CO o CM O> CO CO LU Xerox Copy Centre EP 0 369 206 A2 PROCESS FOR PREPARING THERMOPLASTIC COMPOSITES BACKGROUND OF THE INVENTION The present invention relates to processes for preparing thermoplastic composites. More particularly, 5 the present invention relates to processes for preparing composites of a polycarbonate with an elastomeric siloxane-polycarbonate block copolymer. Safety glazing or penetration resistant glazing for structural items such as windows, windshields and the like including multiple glass and/or high-strength polymeric structural layers are well-known. Glass and polycarbonate resin laminates are disclosed in U.S. patent no. 3,666,614, the glass and polycarbonate being w sealed or joined together by an ethylene-vinyl acetate copolymer. In U.S. patent no. 3,520,768, there are disclosed laminates of relatively thick glass sheets with a thin polycarbonate foil disposed between the glass sheets as the cohering material. Also known (from U.S. patent no. 3,979,548) are laminates wherein self-healing, chemically resistant polyurethane films or layers are adhered to glass. U.S. patent no. 4,027,072 discloses laminates comprising polycarbonates and siloxane polycarbonate block copolymers and 75 glass in various combinations and in which an ultraviolet, mar resistant, hard coat is utilized on at least one external surface or both external surfaces of such laminates. U.S. patent 4,204,026 discloses glass- polycarbonate laminates wherein the glass and polycarbonate are bonded together by a bonding system comprised of an aminoalkyl tris[poly(aryloxysiloxane)] primer and a siloxane-polycarbonate block copolymer bonding agent. U.S. patent 4,312,903 discloses multi-ply laminates which contain polycarbonate layers 20 bonded into the laminates with a siloxane-polycarbonate block copolymer. These last-mentioned laminates are particularly useful in structural items such as bullet resistant glass, windshields, windows and as transparencies for gas masks and the like. It is normal practice in constructing certain of such laminates to utilize glass or relatively hard solid resinous materials as impact- or shock-receiving layers and to utilize polycarbonate as the layer presented to the person or object being protected. 25 The above-described laminates have been prepared by so-called "laying up" of the laminate. Such them laying up involves physically placing the individual sheets in contact with one another and bonding together by means of heat and pressure. This procedure suffers from certain disadvantages. The laying up procedure is often done by hand or is only semi-automated and thus is labor intensive. In addition, it is difficult to exclude airborne paniculate matter from the sheets during the laying up procedure. When 30 trapped between the sheets, such particulate matter decreases the optical clarity and aesthetic appearance of the laminate and, in extreme cases, can lead to subsequent delamination. A need exists for an efficient method for preparing such laminates which reduces the overall labor requirement and which minimizes the chances of trapping contaminating particulate matter within the laminate. 35 Summary of the Invention 40 In accordance with the present invention, a process for preparing a composite of a polycarbonate with a siloxane-polycarbonate block copolymer comprises coextruding the polycarbonate and siloxane-polycar- bonate block copolymer The use of the coextrusion process avoids the need to lay up the polycarbonate and siloxane-polycarbonate block copolymer layers and thus greatly reduces the occurrence of undesirable trapped foreign matter within the finished product. The coextruded product is useful for the production of 45 high-impact strength safety and penetration resistant glazing panels. Detailed Description Of The Invention 50 Procedures for coextruding composites of thermoplastic sheets and films are generally known. Such procedures are described, for example, in the Modern Plastics Encyclopedia, Vol. 64, No. 10A, pp. 228-238, McGraw Hill, October, 1987. Coextruded sheets and films are made for example using a multi-manifold die such as a coextrusion feedblock for flat cast film and sheet. Procedures and equipment for coextrusion of multi-layered sheets and films are described in detail by M.H, Naitove, Plastics Technology, February 1977, EP 0 369 206 A2 pp. 61-71. In the present invention, polycarbonate and siloxane-polycarbonate block copolymer thermoplastics are coextruded to form multi-layered composites which take advantage of the various properties of the different layers. The composites are prepared as sheets including at least one thermoplastic layer consisting of 5 polycarbonate and at least one adjacent thermoplastic layer consisting of siloxane-polycarbonate block copolymer. These polycarbonate and siloxane-polycarbonate block copolymer composites are useful for further processing into e.g. high strength glazing laminate panels. Depending on the ultimate use of the composites, a siloxane-polycarbonate block copolymer layer may be disposed on one or both sides of the polycarbonate layer. The siloxane-polycarbonate block copolymer may serve as an adhesive layer for w bonding the composite to other sheet materials, such as glass or polycarbonate. As used herein, the term 'polycarbonate" includes polymers prepared by reacting a dihydric phenol with a carbonate precursor as well as copolyestercarbonates, which are prepared by reacting an aromatic dicarboxylic acid or reactive derivative thereof, a dihydric phenol and a carbonate precursor. Because the melt flow characteristics of siloxane-polycarbonate block copolymers differ substantially 75 from those of polycarbonates, composites of these materials have not heretofore been prepared by coextrusion. It has now been found that optically clear composites, having strong inter-layer bonds can be prepared by coextrusion. Moreover, such composites can be prepared without using an adhesive between the layers of the composites. Generally, any polycarbonate resin can be used in the composites of the present invention including but 20 not limited to those described in U.S. patents 3,161,615; 3,220,973; 3,312,659; 3,312,660; 3,313,777; 3,666,614; and 3,989,672, all of which are incorporated herein by reference. Generally, carbonate polymers used in the instant composites are high molecular weight, thermoplastic, aromatic polymers and include homopolycarbonates, copolycarbonates and copolyestercarbonates and mixtures thereof which have aver- and age molecular weights of about 8,000 to more than 200,000, preferably of about 20,000 to 80,000 an 25 I.V. of 0.40 to 1.0 dl/g as measured in methylene chloride at 25° C. In one embodiment, the polycarbonates are derived from dihydric phenols and carbonate precursors and generally contain recurring structural units of the formula: O fO-Y-O-6-^- 30 where Y is a divalent aromatic radical of the dihydric phenol employed in the polycarbonate producing reaction. Suitable dihydric phenols for producing polycarbonates include the dihydric phenols such as, for example, 2,2-bis(4-hydroxyphenyl)propane, bis(4-hydroxyphenyl)methane, 2,2-bis(4-hydroxy-3-methyl- phenyl)propane, 4,4-bis(4-hydroxyphenyl)heptane, 2,2-(3,5,3',5';tetrachioro-4,4'-dihydroxyphenyl)propane, 35 2,2-(3,5,3',5'-tetrabromo-4,4'-dihydroxyphenyl)propane, and 3,3'-dichloro-4,4'-dihydroxydiphenyl)methane. Other dihydric phenols which are also suitable for use in the preparation of the above polycarbonates are disclosed in U.S. Patent Nos. 2,999,835, 3,038,365, 3,334,154, and 4,131,575, incorporated herein by reference. It is of course possible to employ two or more different dihydric phenols or a copolymer of a dihydric 40 phenol with a glycol or with a hydroxy or acid terminated polyester, or with a dibasic acid in the event a carbonate copolymer or interpolymer rather than a homopolymer is desired for use in the preparation of the composites of the invention. Blends of any of the above materials can also be employed to provide the aromatic polycarbonate. In addition, branched polycarbonates such as are described in U.S. Patent No. 4,001,184, can also be utilized in the practice of this invention, as can blends of a linear polycarbonate and 45 a branched polycarbonate. The carbonate precursor employed can be either a carbonyl halide, a carbonate ester or a haloformate. The carbonyl halides which can be employed are carbonyl bromide, carbonyl chloride and mixtures thereof. Typical of the carbonate esters which can be employed are diphenyl carbonate, a di(halophenyl)carbonate
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