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United States Patent 0 3,299?-l7 United States Patent 0 " IC€ Patented Jan. 17, 1967 1 2 amount of a norbornadiene. As determined by infrared 3,299,017 analysis, the product obtained from this polymerization COlPOLYMlERS OF 1,3-BUTADIENE AND A NORBORNADHENE reaction is a copolymer of 1,3-butadiene and a norborna Robert P. Zelinski and Floyd E. Naylor, lliartlesville, diene in which at least 85 percent, e.g., from 85 to 98 Okla, assignors to Phillips Petroleum Company, a cor percent and higher, of the butadiene units have a cis 1,4 poration of Delaware con?guration. This novel copolymer has a greatly re No Drawing. Filed Apr. 29, 1963, Ser. No. 276,166 duced tendency to cold flow while still retaining the desir 12 ‘Claims. (Cl. 26tl—82.l) able physical properties of conventional cis-polybutadi ene. Furthermore, the copolymer of this invention pos This invention relates to novel polymers of 1,3-butadi sesses improved processing characteristics. For example, ene. In one aspect, it relates to a method for producing in the compounding of the copolymers, shorter mixing a polymer of 1,3-butadiene having a reduced tendency to times are required. This results from the fact that there cold ?ow. In another aspect, it relates to a method for is a more rapid heat buildup during mixing as compared improving the processability of polymers of 1,3-butadi to conventional cis-polybutadiene, which facilitates the ene. 15 incorporation of compounding ingredients. Further A great deal of research work has been conducted dur more, the novel copolymers have better extrusion and ing the last few years with the object of producing im milling characteristics and exhibit a considerably longer proved rubbery polymers. One of the products that has scorch time than cis-polybutadienes prepared according to attracted widespread attention because of its superior previous methods. When copolymers prepared in ac properties is a polybutadiene containing a high percent cordance with the process of this invention are blended age, e.g., at least 85 percent, of cis 1,4-addition. The with other rubbers, e.g., a copolymer of butadiene ‘and physical properties of this polymer are of such a nature styrene, the resulting compositions have better processing that it is particularly suitable for the fabrication of auto characteristics than those prepared ‘with conventional cis mobile and truck tires and other articles for which con polybutadiene. Other unsaturated cyclic compounds, ventional synthetic polymers have heretofore been com 25 such as 1,5-cyclooctadiene, cyclododecatriene, dicyclopen paratively unsatisfactory. However, in the processing of tadiene, norbornylene (bicycloheptene), and cyclooctate the polymer, particularly in packaging, shipping and stor~ traene, have been added to polymerization ‘systems em age, a certain amount of dif?culty has been encountered ployed in producing cisapolybutadiene, but these mate because of the tendency of the polymer to cold ?ow when rials were found to have little, if any, effect on the prop in the unvulcanized state. For example, if cracks or 30 erties of the polymer products. It was completely unex punctures develop in the packages used in storing the pected, therefore, when it was found that the addition of polymer, polymer will flow from the packages with a re a norbornadiene to the polymerization systems resulted sulting loss or contamination and sticking together of the in the formation of a copolymer having such outstanding stacked packages. It has also been found that cis-poly properties. butadiene is often dif?cult to process. It is essential that 35 The norbornadienes, often referred to \as bicyclo(2,2, a polymer be processable, for otherwise its use is seriously 1)-hepta-2,5-dienes, employed in the practice of the pres limited. ent process can be represented by the formula It is an object of this invention, therefore, to provide a polybutadiene composition containing a high percent age of cis 1,4-addition, which has a reduced tendency to 40 cold ?ow when in the unvulcaniz-ed state and which pos sesses improved processing characteristics. Another object of the invention is to provide a method for eliminating or substantially reducing the tendency of cis-polybutadiene to cold flow when in the unvulcanized 45 state. Still another object of the invention is to provide a proc ess for improving the processability of cis~polybutadiene. A further object of the invention is to provide a novel copolymer of 1,3-butadiene and a norbornadiene. 50 Other and further objects and advantages of the inven tion will be apparent to those skilled in the art upon con sideration of the accompanying disclosure. wherein R is hydrogen or an alkyl group containing from The present invention is concerned with the production 1 to 4, inclusive, carbon atoms and wherein at least two of polymers of 1,3-butadiene having a reduced tendency 55 of the R groups are hydrogen. It is often preferred to to cold ?ow ‘and possessing improved processing charac use norbornadiene itself, i.e., the compound according to teristics. Thus, the invention relates to an improvement the foregoing formula in which each R is hydrogen. Of in a process for polymerizing 1,3-butadiene with a cata the a-lkyl derivatives, it is generally preferred to use those lyst system which forms on mixing components compris that are substituted in the 7-position. Examples of these ing an organometal component and an iodine-containing 60 latter compounds include 7-methylnorbornadiene, 7~ethyl component. Broadly speaking, the improvement com norbornadiene, 7-n-propylnorbornadiene, 7-isopropylnor prises adding to the polymerization mixture a minor bornadiene, 7-n-butylnorbornadiene and 7-t-ert-butylnor 3,299,017 3 4 bornadiene. Other examples of norbornadienes that can titanium tetraiodide and titanium tetrachloride; triphenyl be employed are l-methylnorbornadiene, 2-methylnor_ aluminum, titanium tetrachloride and iodine; tri - alpha - bornadiene, Z-ethylnorbornadiene, l-isopropylnorbornadi naphthylaluminum, titanium tetrachloride and iodine; ene, 2-n-butylnorbornadiene, and the like. tribenzylaluminum, titanium tetrabromide and iodine; di As mentioned above, only a minor amount of the nor ethylmagnesium, titanium tetrachloride and hydrogen bornadiene is added to the polymerization system. The iodide; diphenylmagnesium, titanium tetrabromide and actual amount used will depend, at least to some degree, hydrogen iodide; triethylalurninum, titanium tetrachloride upon the particular type of product desired. The amount and hydrogen iodide; diethylmalgnesium, titanium tetra is usually in the range of 0.01 to 10 parts by weight, pref chloride, and lithium iodide; tri-n-butylaluminum, titanium erably in the range of 0.05 to 2 parts by weight, per 100 tetrabromide and lithium iodide; diisobutylaluminum hy parts by weight of monomer. The norbornadiene can be 10 dride, titanium tetrachloride and lithium iodide; diphenyl added to the polymerization zone by itself or it can be magnesium, titanium tetrachloride and iodine trichloride; charged as a solution in a hydrocarbon, preferably similar triethylaluminum, titanium tetrachloride and iodine mono to ‘the hydrocarbon used as the polymerization diluent. ‘chloride; diphenylaluminum hydride, titanium tetra The novel copolymer of this invention can be prepared 15 bromide and iodine tribromide; triisobutylaluminum, ti \by polymerizing 1,3-butadiene and a norbornadiene with tanium tetrachloride and isobutyl iodide; triethylalurni any one of a large number of stereo-speci?c catalyst num, titanium tetrachloride an iodoform; diethylmag systems. It is usually preferred to employ a catalyst nesium, titanium tetrabromide and methyl iodide; di which is selected from the group consisting of (1) a phenylzinc and titanium tetraiodide; di - 2 - tolylmercury catalyst which forms on mixing components comprising and titanium tetraiodide; tricyclohexylaluminum, titanium an organometal compound having the formula RmM, tetrachloride and titanium tetraiodide; ethylcyclopentyl wherein R is an alkyl, cycloalkyl, aryl, alkaryl, aralkyl, zinc and titanium tetraiodide; tri (3-isobutylcyclohexyl) alu alkylcycloalkyl, cycloalkylalkyl, arylcycloalkyl or cyclo minum and titanium tetraiodide; tetraethyllead, titanium alkylaryl radical, M is aluminum, mercury, zinc, beryl tetrachloride and titanium tetraiodide; trimethylphenyl lium, cadmium, magnesium, sodium or potassium, and 25 lead, titanium tetrachloride and titanium tetraiodide; di m is equal to the valence of the metal M, and titanium phenylmagnesium and titanium tetraiodide; di - n - propyl tetraiodide, (2) a catalyst which forms on mixing com magnesium, titanium tetrachloride and titanium tetra ponents comprising an organometal compound having iodide; dimethylmagnesium, titanium tetrachloride and the formula RnM', wherein R is an organo radical as iodine; diphenylmagnesium, titanium tetrabromide and de?ned above, M’ is aluminum, magnesium, lead, sodium 30 iodine; methylethylmagnesi-um, and titanium tetraiodide; or potassium, and n is equal to the valence of the metal dibutylberyllium and titanium tetraiodide; diethylcadmium M’, titanium tetrachloride and titanium tetraiodide, (3) a and titanium tetraiodide; diisopropylcadmium an titanium catalyst which forms on ‘mixing components comprising an tetraioide; triisobutylaluminum, titanium tetrachloride, organometal compound having the formula RaM” or and antimony triiodide; triisobutylaluminum, titanium RzAlH, wherein ‘R is an organo radical as de?ned above, 35 tetrachloride and aluminum triiodide; triisobutylalumi
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