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公开(公告)号:DE1493773A1
公开(公告)日:1970-02-05
申请号:DE1493773
申请日:1965-01-12
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR
Abstract: Silanol containing impurities, which adversely affect polymerization, are removed from cyclic organopolysiloxanes, by contacting the siloxane with a heat-activated hydride of Ca, Ba or Mg and thereafter separating the treated silicoxane from the hydride. The organopolysiloxane may be hydrocarbon-substituted. Examples are: hexamethylcyclolicsiloxane, 2,4,6-triphenyl - 2,4,6 - trimethylcyclosiloxane, 2-methyl, 2-ethyl, 4,4,6,6 - tetraphenylcyclolicsiloxane and 2,2-dimethyl-4,4,6,6-tetraphenylcyclolicsiloxane. The hydride may be heat-activated under vacuum below 50 m Hg at 300-600 DEG C. until substantially free from surface moisture. Examples relate to the purification of the cyclic organo-polysiloxanes listed above and illustrate the higher molecular weight obtained on polymerization of the purified product.ALSO:Heat activated hydrides of Ca, Mg and Ba are prepared by heating under vacuum of below 50 m Hg at from 300-600 DEG C. until substantially free from surface moisture. Examples of suggested structures are CaH2.CaH and CaH2.Ca2.
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公开(公告)号:DE1770314A1
公开(公告)日:1970-04-02
申请号:DE1770314
申请日:1968-05-02
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR , FRIEDRICH KLEBE JOHANN
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公开(公告)号:DE1720900A1
公开(公告)日:1971-09-02
申请号:DE1720900
申请日:1968-03-15
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR
Abstract: 1,213,403. Polysiloxane-coated ZnO and ZnS. GENERAL ELECTRIC CO. 20 Feb., 1968 [17 March, 1967], No. 8203/68. Heading C1A. [Also in Division C3] Heat activated ZnO or ZnS is coated with an organopolysiloxane by exposure to light of 3200-7000 A in the presence of a cyclotrisiloxane selected from: (I) hexamethylcyclotrisiloxane; (II) cis-2,4,6-trimethyl-2,4,6-triphenylcyclotrisiloxane; (III) cyclotrisiloxanes of formula and (IV) mixtures of the above.
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公开(公告)号:DE1720899A1
公开(公告)日:1971-07-29
申请号:DE1720899
申请日:1968-03-15
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR
Abstract: 1,213,404. Polysiloxane-coated ZnO and ZnS. GENERAL ELECTRIC CO. 20 Feb., 1968 [17 March, 1967], No. 8204/68. Heading C1A. [Also in Division C3] Zinc oxide or zinc sulphide coated with an organopolysiloxane is prepared by heating a cyclotrisiloxane selected from hexamethylcyclotrisiloxane, 2,4,6 - trimethyl - 2,4,6 - triphenylcyclotrisiloxane, cyclosiloxanes of formula mixtures thereof and mixtures of the above with hexaphenylcyclotrisiloxane in the presence of the heat-activated zinc chalcogen at 50-250 C. From 0-1 to 1600 parts of the zinc chalcogen may be used per 100 parts of cyclotrisiloxane. The ZnO or ZnS is heat activated by heating at 200-550 C. at pressures from 760 mm. to 10 -6 mm. Hg.
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公开(公告)号:DE1913941A1
公开(公告)日:1969-10-09
申请号:DE1913941
申请日:1969-03-19
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR
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公开(公告)号:DE1768991A1
公开(公告)日:1971-12-02
申请号:DE1768991
申请日:1968-07-20
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR
Abstract: 1,234,614. Organometallic compounds; stilbene dicarboxylic acid. GENERAL ELECTRIC CO. 27 June, 1968 [21 Aug., 1967], No. 30742/68. Headings C2C and C2J. Solvated metal-hydrocarbon complexes of polynuclear aromatic hydrocarbons or conjugated olefinic hydrocarbons with Be, Mg, Ca, Sr or Ba may be prepared by reacting, under anhydrous conditions and under an atmosphere free from oxygen, moisture and oxides of carbon, at a temperature of 5-120‹ C., the metal with the hydrocarbon, in the solvating solvent which is hexamethyl phosphoramide, octamethylpyrophosphoramide, tetrahydrofuran, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, N,N,N 1 ,N 1 -tetramethyl ethylene diamine, or a mixture of two or more of these. The solvated complex may be isolated from solution by precipitation, drying and recrystallization. In Example 7, a deep purple-coloured solution of strontium-trans-stilbene-hexamethylphosphoramide treated with solid dry CO 2 , and subsequently acidified, gave stilbene-1,2-dicarboxylic acid (m.pt. 224‹ C.).
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公开(公告)号:DE1720826A1
公开(公告)日:1971-07-22
申请号:DE1720826
申请日:1967-04-10
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR
IPC: C08G77/44 , C08G77/442 , C08G31/09
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公开(公告)号:DE1931589A1
公开(公告)日:1970-01-08
申请号:DE1931589
申请日:1969-06-21
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR
Abstract: 1,267,568. Polymerization of cyclic siloxanes in the presence of metal complexes. GENERAL ELECTRIC CO. 10 June, 1969 [24 June, 1968], No. 29430/69. Heading C3T. Essentially linear polydiorganosiloxanes are prepared by heating a cyclic organosiloxane [R 1 R 11 SiO]x, wherein R 1 and R 11 are each H or a monovalent hydrocarbon, halohydrocarbon or cyanoalkyl radical and x is 3-7 with a complex of a compound M ++ R- - or M ++ (R - ) 2 , wherein M is Be, Mg, Ca, Sr or Ba and R is a polynuclear hydrocarbon or conjugated hydrocarbon, with an aprotic dipolar solvent. The complex is prepared by reaction of the metal with the hydrocarbon in the presence of the solvent; it may be used after isolation with the molten cyclic siloxane or dispersed in the complexing solvent or a different aprotic solvent. In Examples complexes are prepared of hexamethyl-phosphoramide with Ba diphenylethylene, Ba and Ca cyclooctatetraenes, Ba trans-stilbene, Sr tetraphenylethylene and Mg m-terphenyl and of tetrahydrofuran with Ba diphenylethylene. A few drops of the product solutions are added to melts of: trans- or cistrimethyl triphenyl cyclotrisiloxane, alone or mixed with tetramethyl tetrakis-cyanoethyl cyclotetrasiloxane or hexaphenyl cyclotrisiloxane; hexamethyl cyclotrisiloxane, alone or mixed with tetramethyl tetrakis-cyanoethyl cyclotetrasiloxane; or tricyclopentamethylene cyclotrisiloxane.
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公开(公告)号:DE1801230A1
公开(公告)日:1969-04-30
申请号:DE1801230
申请日:1968-10-04
Applicant: GEN ELECTRIC
Inventor: EARL BOSTICK EDGAR , STUART HAY ALLAN , JOHN CHALK ALAN
IPC: C08F283/06 , C08F283/08
Abstract: 1,241,683. Grafted poly(1,4-phenylene ethers). GENERAL ELECTRIC CO. 2 Oct., 1968 [5 Oct., 1967], No. 46868/68. Headings C3G, C3R and C3T. A graft copolymer comprises a poly (1,4- phenylene ether) backbone having grafted on to it a polymer of an anionically polymerizable monomer. Specified monomers are 1-alkenes having 2 to 8 carbon atoms, monomers of formula where R is hydrogen, C 1 to C 8 -alkyl or chlorine, X is chlorine, -CN or -COOR 1 , where R 1 is hydrogen, C 1 to C 8 -alkyl or phenyl, cyclic organosil oxanes, alkyl or aryl isocyanates having up to 18 carbon atoms in the alkyl or aryl group and 1,2-epoxyalkanes having 2 to 8 carbon atoms. The poly- (1,4-phenylene ether) is metalated by reaction with an alkyl or aryl alkali metal compound before being grafted. Examples are given in which poly(2,6-dimethyl1-1,4-phenylene ether) is metalated with butyl lithium prior to being grafted with styrene, acrylonitrile, isoprene or methyl methacrylate. In other examples, the lithiated polyether is reacted with (a) tetramethylethylene diamine before being grafted with styrene, (b) 1,1-diphenyl ethylene before being grafted with methyl methacrylate or (c) titanium tetrachloride before being grafted with ethylene. The polyether is metalated in Example II with the potassium dianion of α-methylstyrene dimer and grafted with styrene. In Examples 7, 12 and 13, the lithiated polyether is grafted with hexamethylcyclotrisiloxane, the graft reaction is terminated by addition of dimethyl sulphate or trimethylchlorosilane and the graft polymer of Example 13 is mixed with pyridine, lauric acid or trichloracetic acid and heated. The lithiated polyether is reacted in Example 8 with tetramethylethylene diamine and grafted with phenyl isocyanate, using methyl iodide as terminator. In Example 18, the polyether is metalated with a Na, K or Li alkyl and grafted with ethylene oxide. Poly- (2 - methyl - 6 - phenyl - 1,4 - phenylene ether) is metalated in Example 14 with butyl lithium prior to being grafted with styrene, or reacted with 1,1-diphenylethylene and grafted with methyl methacrylate. In Examples 15 and 16, poly(2,6-diphenyl-1,4-phenylene ether) is similarly metalated and grafted with styrene or methyl methacrylate.
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