Patent GB-776101-A (GB)
Title: Processing of rubber
IPC: C08K5/00
Filed: 1955-06-09
Abstract: A butadiene-styrene copolymer is peptized by incorporating therein 0.0005 to 0.5 per cent by weight of an iron phthalocyanine or a chloro or nitro derivative thereof, or a combination of the latter, or a compound which generates an iron phthalocyanine under the peptizing conditions, e.g. a leuco derivative of iron phthalocyanine. In addition there may be incorporated in the elastomer 0.005 to 5 per cent of a known rubber peptizing agent selected from substituted hydrazines and their derivatives, aryl mercaptans and their divalent metal salts, arylene mercapto thiazoles or other mercapto compounds, aromatic disulphides, and aromatic nitroso compounds.  Examples describe the peptizing of a butadiene-styrene copolymer using mixtures of iron phthalocyanine and mercaptobenzothiazole, and of iron phthalocyanine and zinc pentachlorophenyl mercaptide, respectively.  The preparation of iron phthalocyanine and of leuco derivatives thereof is described (see Group IV (c)) Specifications 322,169, [Class 2 (iii)], 389,842, 464,126, 464,673, [three in Group IV], [467,243, 480,178, 490,292, 677,408] [all in Group V], 745,359, [Group IV (c)], and U.S.A.  Specifications 2,018,643, 2,124,419, 2,190,587, 2,402,167, 2,470,948, 2,504,903, 2,629,755 and 2,658,091 are referred to.ALSO:An iron phthalocyanine for use as a peptizer for natural rubber or a butadienestyrene copolymer (see Group V) is prepared by heating phthalic anhydride, urea, and anhydrous ferric chloride in trichlrobenzene in the presence of ammonium molybdate as catalyst, the iron phthalocyanine being isolated by treatment with sodium carbonate solution, distilling off the trichlorbenzene, filtering, washing, and drying.  As peptizer may also be used a leuco derivative of iron phthalocyanine which may be either a precursor or a propigment.  The precursor is prepared by heating for 16 hours at 90 DEG C. a mixture of 58 parts anhydrous ferrous chloride suspended in 372 parts ethylene glycol monoethyl ester and saturated with ammonia, 200 parts phthalonitrile and 12 parts methyl glucamine.  The reaction mass is then filtered and washed, and the brown precipitate resulting extracted with hot methanol.  The propigment may be prepared by treating with 4 parts of chlorine for 1 hour, a suspension of 12.5 parts iron phthalocyanine in 200 parts of methanol.  The unreacted phthalocyanine is filtered off, and the resulting solution drowned in dilute hydrochloric acid.  The precipitated product is washed and dried to form a light yellow powder.  Specifications 322,169 [Class 2(iii)], 389,842, 464,126, 464,673 [all in Group IV] [467,243, 480,178, 490,292, 677,408 [all in Group V]] 745,359 and U.S.A.  Specifications 2,018,643, 2,124,419, 2,190,587, 2,402,167, 2,470,948, 2,504,903, 2,629,755 and 2,658,091 are referred to.ALSO:Natural rubber or a butadiene-styrene copolymer is peptized by incorporating therein 0,0005 to 0,5 per cent by weight of an iron phthalocyanine or a chloro or nitro derivative thereof, or a combination of the latter, or a compound which generates an iron phthalocyanine under the peptizing conditions, e.g. a leuco derivative of iron phthalocyanine.  In addition there may be incorporated in the elastomer 0,005 to 5 per cent of a known rubber peptizing agent selected from substituted hydrazines and their derivatives, aryl mercaptans and their divalent metal salts, arylene mercapto thiazoles or other mercapto compounds, aromatic disulphides, and aromatic nitroso compounds.  Examples 1 to 5 describe the peptizing of natural rubber using (1) an iron phthalocyanine, (2) an iron trinitrophthalocyanine, (3) an iron mono-4-chloro-phthalocyanine, (4) an iron phthalocyanine "precursor" leuco derivative prepared from phthalonitrile and anhydrous ferrous chloride, (5) a "propigment" leuco derivative of iron phthalocyanine. Examples 6 to 19 describe the peptizing of natural rubber utilizing mixtures of an iron phthalocyanine and (6) zinc pentachlorothiophenol, (7) pentachlorothiophenol, (8) thiobetanaphthol (9) xylyl mercaptan, (10) zinc xylyl mercaptide, (11) tetrachlorobenzenedithiol, (12) mercaptobenzothiazole, (13) o-mercapto methyl benzoate, (14) phenyl hydrazine, (15) dibenzoyl disulphide, (16) o, o1-dibenzamido diphenyl disulphide, (17) dibenzothiazyl disulphide, (18) nitrosobetanaphthol, (19) zinc o-benzamido thiophenol.  Examples 20 and 21 describe the peptizing of a butadienestyrene copolymer using (20) an iron phthalocyanine and mercaptobenzothiazole, (21) zinc pentachlorophenyl mercaptide and an iron phthalocyanine.  The preparation of the iron phthalocyanine and of the leuco derivatives employed in the examples is described (see Group IV(c)).  Specifications 322,169 [Class 2(iii)], 389,842, 464,126, 464,673 [all in Group IV], 467,243, 480,178, 490,292, 677,408, 745,359 [Group IV(c)] and U.S.A.  Specifications 2,018,643, 2,124,419, 2,190,587, 2,402,167, 2,470,948, 2,504,903, 2,629,755 and 2,658,901 are referred to.