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  • 1
    Electronic Resource
    Electronic Resource
    Control of debromination in solution polymerisation of copper(I) 4-bromobenzenethiolate (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Polymer International 33 (1994), S. 19-23 
    Details
    ISSN: 0959-8103
    Keywords: poly(1,4-phenylene sulphide) ; copper(I) 4-bromobenzenethiolate ; debromination ; polymerisation ; molar mass ; high-temperature viscometry ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Debromination of poly(1,4-phenylene sulphide), PPS, chains during formation by solution polymerisation of copper(I) 4-bromobenzenethiolate, CBT, in quinoline and quinoline/pyridine mixtures at temperatures in the range 180-225°C has been investigated. The results are consistent with previously-reported model compound studies and show that debromination is insignificant if the polymerisation temperatures is ≤ 200°C. Pyridine was shown not to be essential for the formation of high molar mass PPS. The optimum conditions for preparing high molar mass PPS in high yield with no significant debromination were polymerisation of CBT at a concentration of 1.0 mol dm-3 in dry quinoline under a flowing dry nitrogen atmosphere at a controlled temperature of 200°C for about 24 h.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/pi.1994.210330103
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  • 2
    Electronic Resource
    Electronic Resource
    Synthesis and characterisation of poly(arylene sulfides), 9Part 8: cf. P. A. Lovell, R. H. Still, Polym. Degrad. Stab. (1987), in press.. Optimisation of the solvent composition for solution polymerisation of copper(I) 4-bromobenzenethiolate at atmospheric pressure and structural investigations of low molar mass poly(1,4-phenylene sulfide) (1987)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 188 (1987), S. 1561-1573 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Solution polymerisation of copper(I) 4-bromobenzenethiolate (CBT) was effected at atmospheric pressure using a range of quinoline/pyridine solvent mixtures. Yields of poly(1,4-phenylene sulfide) (PPS) were evaluated and PPS fractionated into toluene soluble (TS) and 1-chloronaphthalene soluble (CNS) material. The fractions were characterised by end-group analysis, viscometry and differential scanning calorimetry. The yield of CNS PPS is optimum for solvent mixtures comprising 70-80 vol.-% quinoline, whereas the molar mass of this fraction is at a maximum for 95 vol.-% quinoline. Results are discussed in terms of the effects of reaction temperature, complexing of CBT by quinoline and pyridine, and copper(I) bromide-catalysed debromination. A low molar mass TS PPS fraction prepared in pyridine was subjected to detailed structural analysis by IR, 1H NMR and Raman spectroscopy. Evidence is presented to show that this material contains disulfide linkages and that thiol end-groupings are absent. These results are discussed relative to possible structures for poly(arylene sulfides). The relevance of this observation to high molar mass samples of PPS and their chain extension and degradative behaviour is also discussed.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1987.021880703
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  • 3
    Electronic Resource
    Electronic Resource
    Synthesis and characterisation of poly(arylene sulfide)s, 5Part 4: cf. A. B. Port, R. H. Still, Polymer Deg. Stabil. 2, 1 (1980).. Model compound studies of debromination reactions which occur during the synthesis of poly(arylene sulfide)s from copper(I) 4-bromobenzenethiolates [copper(I) 4-bromothiophenoxides] (1987)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 188 (1987), S. 111-118 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Debromination side-reactions which occur during the synthesis of poly(arylene sulfide)s from copper(I) 4-bromothiophenoxidesSystematic name: Copper(I) 4-bromobenzenethiolates. were investigated using bromobenzene as a model for the end unit in a poly(1,4-phenylene sulfide) chain. Model reactions were conducted in quinoline, pyridine, and 10:1 (v/v) quinoline/pyridine solution in the presence and absence of copper(I) bromide, the condensation product of polymerisation. Reaction liquors were subjected to GLC and MS analysis and evidence is presented which indicates that a copper(I) initiated debromination reaction occurs yielding monophenylquinolines. A mechanism is proposed for the reaction and critically discussed. The consequences of the reaction at the macromolecular level are also described.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1987.021880110
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  • 4
    Electronic Resource
    Electronic Resource
    Synthesis and characterisation of poly(arylene sulfides), 6Part 5: cf.16. Synthesis of block copoly(arylene sulfides) (1987)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 188 (1987), S. 1537-1549 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Novel ABA block copolymers of poly(1,4-phenylene sulfide) (PPS(A)) and poly-(2-methyl-1,4-phenylene sulfide) (PMPS(B)) were synthesised from bis(4-bromophenyl) sulfone (BBS) by sequential reaction with copper(I) 4-bromo-2-methylbenzenethiolate (CBMT) and copper(I) 4-bromobenzenethiolate (CBT). PPS, PMPS and PPS/PMPS random copolymers were also prepared to aid block copolymer characterisation. Polymer fractions were studied by hot-stage microscopy to evaluate melting ranges, and molar masses were computed from bromine end-group concentrations and from gel permeation chromatography studies. Compositional analyses were made by IR and 1H NMR spectroscopy leading to confirmation of the block copolymer structure and to evaluation of the degrees of polymerisation of the individual blocks.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1987.021880701
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  • 5
    Electronic Resource
    Electronic Resource
    Synthesis and characterisation of poly(arylene sulfides), 7Part 6: cf.1. Transitional behavior of random and block copoly(arylene sulfides) (1987)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 188 (1987), S. 1551-1560 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Differential scanning calorimetry was used to evaluate first and second order transition temperatures and % crystallinity of poly(1,4-phenylene sulfide) (PPS), poly(2-methyl-1,4-phenylene sulfide) (PMPS), their blends and random and block copolymers comprising thio-1,4-phenylene and thio-2-methyl-1,4-phenylene units. Results are discussed in terms of the miscibility of PPS and PMPS in the melt phase and disruption of the crystallisation of PPS units by PMPS units. Microphase separation in the block copolymers was shown to be dominated by crystallisation of the PPS blocks. The application of Krause's microphase separation theory to prediction of the transitional behaviour of the block copolymers is critically discussed.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1987.021880702
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