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United States Patent Office Patented Sept 3,467,636 United States Patent Office Patented Sept. 16, 1969 1. 2 SUMMARY OF THE INVENTION 3,467,636 REEDOX CATALYST SYSTEM FOR PREPARING It has unexpectedly been found that vinylidene fluoride WNYLDENE FLUORDE INTERPOLYMERS interpolymers having surprising low Mooney viscosities, Arthur Nersasian, Wilmington, Del, assignor to E. I. which, however, are curable to vulcanizates of high qual du Pont de Nemours and Company, Wilmington, Del, ity, can be prepared by polymerization in an aqueous a corporation of Delaware medium containing (a) water-soluble peroxy catalyst No Drawing. Continuation-in-part of application Ser. No. compounds capable of initiating polymerization of the 618,347, Feb. 24, 1967. This application Nov. 15, 1967, monomers in the system, and (b) a water-soluble iodide, Ser. No. 683,126 Int. CI. C08f 1/06, 15/40, 15/06 bromide, hypochlorite or hypobromite, or aqueous solu U.S. C, 260-80.77 5 Claims 0. tions of iodine, bromine or chlorine. DESCRIPTION OF PREFERRED EMBODIMENTS This invention is applicable to the preparation of inter ABSTRACT OF THE DISCLOSURE polymers of vinylidene fluoride (VF) with other fluorine The preparation of vinylidene fluoride interpolymers 5 containing ethylenically unsaturated monomers copolym (e.g., with hexafluoropropene and tetrafluoroethylene) in erizable therewith. Typical of the latter are hexafluoro aqueous medium with a peroxy compound like ammoni propene (HFP), tetrafluoroethylene (TFE), perfluoro um persulfate and a second component like NaI, NaBr, alkyl perfluorovinyl ethers particularly where the alkyl NaOCl or NaOBr, or I2, Br or Cl2 in water. Exception radical contains from 1 to about 4 carbon atoms such as ally low Mooney viscosity polymers (e.g., ML-10/212 20 perfluoro(methyl vinyl)ether and perfluoro(propyl vinyl) F. of as low as 7) can be prepared which cure to high ether, trifluorochloroethylene, and pentafluoropropylene. quality vulcanizates. Of particular interest are the vinylidene fluoride/hexa fluoropropene copolymers containing from about 70 to about 30 weight percent vinylidene fluoride and about 30 CROSS REFERENCE TO RELATED 25 to about 70 weight percent hexafluoropropene (see Rex APPLICATION ford U.S. Patent 3,051,677). Other important polymers are the terpolymers of vinylidene fluoride/hexafluoropro This application is a continuation-in-part of applicant's pene/tetrafluoroethylene where in the monomer units are copending application Ser. No. 618,347, filed Feb. 24, present in the following mole ratios: about 3 to 35 (pref 1967 and now abandoned. 30 erably 15 to 25) weight percent tetrafluoroethylene units and about 97 to 65 (preferably 85 to 75) weight percent BACKGROUND OF THE INVENTION vinylidene fluoride and hexafluoropropene units, the latter Field of the invention two being present in a weight ratio of from 2.33/1 to 0.677/1. (see Pailthrop and Schroeder U.S. Patent 2,698 This invention relates to vinylidene fluoride interpoly 35 649). mers and, more particularly, their preparation using a par Other vinylidene fluoride polymers and their prepara ticular catalyst system. tion are disclosed in Dittman et al. U.S. Patents 2,738,343 Description of the prior art and 2,752,331, Hanford and Roland U.S. Patent 2,468,- 664, Brubaker U.S. Patent 2,393,967, and Honnet al. U.S. Polymers of vinylidene fluoride, such as vinylidene 40 Patents 2,833,752 and 2,965,619. fluoride/hexafluoropropene copolymers (see Rexford, One component of the catalyst system must be the U.S. Patent 3,051,677) and vinylidene fluoride/hexa water-soluble peroxy catalyst compound capable of initi fluoropropene/tetrafluoroethylene terpolymers (see Pail ating polymerization of the monomers in the system. One thorp and Schroeder, U.S. Patent 2,968,649) are known or mixtures of more than one of such compounds may in the art to be elastomers which exhibit excellent heat 45 be present. All water-soluble persulfates, especially am and chemical resistance. Moreover, their curability pro moniated persulfates, are suitable. Compounds which ex vides for the manufacture of vulcanizates having out hibit low activity in initiating polymerization of the mono standing properties. mers in the system employed are much less preferred, for Many of these vinylidene fluoride interpolymers typi example, sodium perborate, sodium peroxide, and hydro cally exhibit Mooney viscosities (ML-10/212. F.) of 60 50 gen peroxide. or 70 which indicate the polymer to be rather stiff and The second component of the catalyst system is a water somewhat difficult to process. For some time, it has been soluble iodide, bromide, hypochlorite or hypobromite, desired to prepare vinylidene fluoride interpolymers which such as sodium, potassium, or ammonium iodides or bro have excellent vulcanizate properties, but which have a mides, sodium hypochlorite, sodium hypobromite, or an lower Mooney viscosity in the uncured state making then 55 aqueous solution of elemental iodine, bromine or chlo much easier to process. rine. While one or mixtures of more than one of such Typically, vinylidene fluoride interpolymers are pre ingredients can be present as the second component, other pared using an ammonium persulfate-sodium bisulfite conventional reducing agents, such as sodium bisulfite, polymerization catalyst (see Dittman et al. U.S. Patent are to be excluded. 2,689,241). It is known that higher amounts of catalysts 60 When using the catalyst components of the prior art, and higher polymerization temperatures will lead to a such as ammonium persulfate and sodium bisulfite, in reduced Mooney viscosity; however, it has been rather general, the ammonium persulfate is used in substantial difficult to get satisfactory polymers having a Mooney excess. Further, the lower the ratio of ammonium persul viscosity below about 50. It is also known that modifiers fate to sodium bisulfite, the higher the Mooney viscosity such as telomers or transfer agents can be employed to 65 of the polymer obtained. In this invention, an excess of give very low Mooney viscosities in vinylidene fluoride peroxy compounds must be used over the amount of sec polymers; however, such polymers by themselves have ond component (hereinafter referred to simply as sodium often been found to possess rather poor properties in the iodide for the sake of convenience). However, it is un cured state and tend to stick to the processing equipment expected that increasing amounts of sodium iodide cause in the uncured state. For this reason, they are usually 70 the Mooney viscosity of the polymer obtained to decrease. blended with high Mooney polymers to improve the proc As a practical matter, the mole ratio of peroxy com essability of the latter. pound to sodium iodide in this invention must be at least 3,467,686 3 4 about 1.2:1; however, there must be at least one mole of The catalysts and 200 ml. of distilled water are charged sodium iodide per 70 moles of peroxy compound. Pref into a 400 ml. "Type 316' stainless steel shaker bomb. erably, the mole ratio of peroxy compound to sodium The bomb is immersed in a -50 C. cooling bath, pres iodide will range from about 3:1 to 20:1 to obtain the Sured to 10 p.s.i.g. with nitrogen, evacuated, and charged vinylidene fluoride interpolymers of suitably low Mooney with 60 g. of hexafluoropropylene and 40 g. of vinyli viscosity. dene fluoride. The bomb is heated to 100 C, with shak A wide range of catalyst system concentrations will ing and held at 100° C. until the pressure drops. The polymerize the monomers; however, to obtain a Mooney polymer is coagulated, washed, and dried in a 60 C. viscosity below about 50 to about 105 C. polymeriza Wac OWen. tion temperature, one should employ at least one part of EXAMPLES 1. TO 5 the catalyst system per about 150 parts of monomer. IO As previously stated, the polymerization is carried Using the continuous method described, five runs are out in an aqueous system. The weight ratio of water to made using the proportions of reactants shown in Table monomer can range from about 20:1 down to about 1:1. I. Typical results are given therein as indicated. TABLE I Preferably, one should employ from about 2.5 to about 5 4 parts of water for every part of monomer present. Monomer Feed Composition: vinylidene fluoride 59%; hexafluoropro pylene 4.1%. The polymerization temperature should be at least Monon Feed Rate: 4.4b.?hr. Deionized Water Feed Rate: 6,000-6,300 ml/hr. about 60° C. and below about 160 C. It is preferred, (NH4)2SOs: 25 g/hr. particularly for a continuous process, that the tempera Pressure (p.si.g.): 900-950. ture range from about 100° C. to 120° C. 20 Temperature (C.): 111-12. It should be abundantly clear that a wide variety of NaBr or NaI as shown. process parameters will influence the polymerization rate Example and the Mooney viscosity of the polymers obtained. As previously stated, the higher the polymerization tem 1. 2 3 4 5 0.9 1.3 2.6 5.0 ---- perature, the lower the Mooney viscosity. Moreover, in 25 NaBr (glhr)------------------- creasing catalyst system concentration and increasing Mooney viscosity i (M-0212 F 37 32 24 8 12 mole ratios of sodium iodide (up to the maximum mole Winylidene fluoride, (percent) 2.-- 56 57 56 59 .58 ratio permitted) will tend to cause a reduction in Mooney Determined on dried raw polymer per ASTM D-1646–63. viscosity. All these things being considered, one skilled 2 Determined on dried raw polymer by infrared spectroscopic analysis. in the art can vary a great many conditions to achieve 30 If, for comparison, Example 4 is repeated using about the particular polymerization rate and Mooney viscosity 5 g./hr. of sodium bisulfite instead of the NaI, a polymer desired.
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