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United States Patent Office Patented July 27, 1971

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United States Patent Office Patented July 27, 1971 3,595,819 United States Patent Office Patented July 27, 1971 2 polymers, a homogeneous thermoplastic composition can 3,595,819 HAGHLY TRANSPARENT SELF-EXTENGUISHENG be obtained which is highly transparent, highly resilient COMPOSITIONS OF METHACRYLATE AND and resistant to weather or atmospheric conditions. In WNY CHLORIDE RESNS addition, such a thermoplastic mixture can be character Ibrahim Daki and Tommaso Perotti Nigra, Busto Arsizio, ized as having self-extinguishing properties. and Rinaldo Casiraghi, Milan, Italy, assignors to More particularly, the thermoplastic compositions of Montecatini Edison S.p.A., Milan, Italy the present invention comprise (1) from about 35-55% No Drawing. Continuation-in-part of application Ser. No. by weight of a methacrylate resin containing less than 642,297, May 31, 1967, which is a continuation-in about 0.08% by weight of bivalent sulfur, the resin being part of application Ser. No. 354,79, Mar. 25, 1964, both now abandoned. This application July 24, 1968, O made up of a methyl methacrylate homopolymer and/or Ser. No. 747,107 a copolymer of methyl methacrylate with an alkyl acry ... C. C08f 29/22 late, the alkyl acrylate content of the copolymer being U.S. C. 260-23 6 Claims lower than 5% by weight; (2) from about 45-65% by weight of a vinyl chloride resin made up of a copolymer of vinyl chloride and 2-ethylhexyl acrylate, the 2-ethyl ABSTRACT OF THE DISCLOSURE hexyl acrylate content of the copolymer being from about 3% to 5% by weight; (3) from about 0-10% by weight Highly transparent, self-extinguishing, thermoplastic of a non-flammable, organic phosphoric acid salt plasti compositions having high resistance to chemical reagents cizer; and (4) lubricants and antioxidants. and to atmospheric conditions and good resiliency, com 20 The self-extinguishing, highly transparent thermoplastic prising (1) from about 35-55% by weight of a meth materials of this invention are resistant to various chemical acrylate resin containing less than about 0.08% by weight compositions including the aliphatic hydrocarbons and of bivalent sulfur, the resin being made up of a methyl have particularly outstanding mechanical characteristics. methacrylate homopolymer and/or a copolymer of methyl These thermoplastic materials can be worked, e.g., ex methacrylate with an alkyl acrylate, the alkyl acrylate 25 truded, under conditions normally used in the plastic arts. content of the copolymer being lower than 5% by weight; Moreover, because of their outstanding resistance to attack (2) from about 45-65% by weight of a vinyl chloride by the elements, these materials can be used for many pur resin made up of a copolymer of vinyl chloride with from poses, particularly for the preparation of corrugated or about 3% to 5% by weight of 2-ethylhexyl acrylate; (3) plane sheets, roofings, skylights, walls, panels and similar from about 0-10% by weight of a non-flammable, or 30 articles used in the building industry. Still another im ganic phosphoric acid salt plasticizer; and (4) lubricants portant use for the thermoplastic materials of this inven and antioxidants. tion is in the manufacturing of self-extinguishing trans parent pipes which are highly resistant to chemical re CROSS-REFERENCE TO RELATED agents. Thus, because of their inherent characteristics, APPLICATION 35 articles prepared from these plastics can be employed for This application is a continuation-in-part of copending various uses, and more particularly can be most desirably application Ser. No. 642,297, filed May 31, 1967, now employed in those areas where non-flammable materials abandoned which is in turn a continuation-in-part of ap are required for safety purposes. plication Ser. No. 354,791, filed Mar. 25, 1964, now 40 DESCRIPTION OF THE PREFERRED abandoned. EMBODIMENTS BACKGROUND OF THE INVENTION The term "transparent,” as used herein, includes ma terials which when tested according to ASTM D1003 have (1) Field of the invention been found to have a transparency value higher than 70%. This invention relates to highly transparent, self-ex 45 Likewise, the term "self-extinguishing' is used to designate tinguishing thermoplastic materials which are resistant to materials which are considered non-flammable when tested chemical reagents and to atmospheric conditions and have in accordance with ASTM D635. good resiliency. The methacrylate resins suitable for use in the present invention include methyl methacrylate homopolymers and (2) Description of the prior art 50 copolymers of methyl methacrylate with alkyl acrylates, It is known that polymethyl methacrylate, which is wherein the alkyl group contains from 1 to 10 carbon transparent and substantially resistant to atmospheric con atoms. A preferable alkyl acrylate for incorporation in ditions, is nevertheless unsatisfactory for many applica the methacrylate resin is methyl acrylate. Such resins tions because it is highly flammable. Compositions com should contain no more than about 0.08% by weight of prising methacrylate resins and vinyl chloride resins are bivalent sulfur, e.g., in thio ethers or similar compounds, also known, but these do not solve the problem of obtain in order to avoid yellowing on the finished product and ing manufactured articles which are self-extinguishing, development of a bad smell during the working step. resistant to atmospheric conditions, highly transparent and A typical example of polymerization for preparing a also have outstanding characteristics of resiliency, rigid methyl methacrylate/alkyl acrylate copolymer (95/5) pre ity, hardness and heat resistance. 60 supposes to carry out the reaction in suspension, at a temperature comprised between 80 and 100° C. in the SUMMARY OF THE INVENTION presence of 0.2% of butyl mercaptan. The copolymers of It has been found, quite unexpectedly, that when methyl vinyl chloride which are used for preparing the thermo methacrylate homopolymers or copolymers thereof with plastic compositions of this invention are the copolymers an alkyl acrylate are mixed in certain critical proportions 65 of vinyl chloride with 2-ethylhexyl acrylate. More par with particular vinyl chloride/2-ethylhexyl acrylate co ticularly, it has been found that the 2-ethylhexyl acrylate 3,595,819 3 4. monomer composition of the vinyl chloride copolymer To further improve the polymeric composition, it is must be from about 3% to 5% by weight for the most often desirable to add up to about 10% by weight of the desirable combination of properties of resiliency, resistance total composition of a plasticizer which improves the to heat and workability in extrusion or injection molding. workability of the composition. It is particularly important Thus, it has been found that either the homopolymers that if a plasticizer be employed, it should be non-fam or copolymers of methyl methacrylate can be mixed with mable in order to insure the non-flammability of the final copolymers of vinyl chloride so as to obtain a homo products. Suitable plasticizers include the organic salts geneous thermoplastic composition which is highly trans of phosphoric acid, e.g., trichloroethyl phosphate, tri parent, resilient, resistant to atmospheric conditions and cresyl phosphate, triphenyl phosphate, etc. self-extinguishing. O It has been discovered that in order to obtain a product More specifically, it has been found that, by mixing which is transparent, self-extinguishing and at the same polymethyl methacrylate and/or a methyl methacrylate/ time substantially resistant to weather or atmospheric alkyl acrylate copolymer with a vinyl chloride/2-ethyl conditions, it is necessary to use each of the polymers hexyl acrylate copolymer in certain critical proportions, and/or copolymers in certain critical ratios. Thus, it was it is possible to obtain a thermoplastic material in the discovered, contrary to what might be expected, that by form of sheets or other articles having outstanding char increasing the amount of transparent material, i.e., methyl acteristics which make the thermoplastic material prac methacrylate resin, to an amount Substantially in excess tical for industrial and building uses. The polymers can of 55% by weight, the transparency of the final product be mixed together by various means, using standard equip decreased. Moreover, if the transparent methyl meth ment, including, for example, by mechanically mixing acrylate resin was used in an amount substantially below powders of the different polymers. Still further, it is pos 20 35% by weight, the transparency of the polymeric com sible to prepare a mixture of the polymers by utilizing position also decreased. Consequently, it was found that solutions of polymers which the subsequently dried, leav there was only a narrow range at which the mixture com ing a homogeneous plastic composition. Of the various prising methyl methacrylate resin and vinyl chloride resin methods that may be used in preparing mixtures of the was transparent. polymers, the use of polymeric powders is preferred. The Similar results were discovered in determining the polymeric compositions can be processed by any of the resistance of the compositions to atmosphere or weather known methods used for plastics and are easily extruded conditions. In tests carried out on samples exposed to without loss of any of their outstanding chemical or phys Sunlight, it was found that increasing the amount of vinyl ical characteristics, 30 chloride resin caused a decrease in the resistance to The compositions also include antioxidants in amounts atmospheric conditions. Compositions having vinyl chlo between 0.001 and 1% by weight, such as 4,4'-thio-bis-6- ride resin present in an amount substantially in excess of tert-butyl-metacresol, 2,2'-methylene-bis-(4-methyl-6-tert 65% by weight were found to be unsatisfactory. Like butylphenol), or 2,2'-methylene-bis-(4-ethyl-6-tert-butyl wise, it was discovered that products which contained phenol). Various lubricants which are known to be com increasing amounts of methyl methacrylate resin had a patible with both of the resins, in amounts comprised be 35 decreasing flame resistance.
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