Polymer Sulfonation without Cross Linking. The Sulfur Trioxide-Phosphate System

Turbak, Albin F.

doi:10.1021/i360004a012

Cited by 50 publications

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“…Sulfonation of polystyrene (PS) has been studied by a number of researchers, [1][2][3] however, little detail is available in the literature about the sulfonation reactions and the thermal properties of the product. Sulfonation is defined as a substitution reaction used to attach the ~SO 3 H group on the molecule of an organic compound via chemical bond to carbon or, less frequently, to a nitrogen atom of the organic compound.…”

Section: Introductionmentioning

confidence: 99%

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Synthesis in pilot plant scale and physical properties of sulfonated polystyrene

Martins¹,

Ruggeri²,

Paoli³

2003

J. Braz. Chem. Soc.

146

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A sulfonação homogênea do poliestireno foi desenvolvida em escala pré-piloto produzindo polímeros com diferentes graus de sulfonação (18 a 22 mol % de unidades estirênicas sulfonadas). O rendimento da reação depende principalmente da razão entre a concentração de sulfato de acetila e de poliestireno. As propriedades morfológicas e térmicas dos poliestirenos sulfonados, obtidas pela sulfonação homogênea, foram estudadas por microscopia eletrônica de varredura, calorimetria diferencial de varredura e termogravimetria. A temperatura de transição vítrea do poliestireno sulfonado aumenta em relação ao poliestireno puro e a ∆Cp foi calculada a fim de confirmar as fortes interações com os grupos ~SO 3 H.The homogenous sulfonation of polystyrene was developed in a pilot plant scale producing polymers with different sulfonation degrees (18 to 22 mole % of sulfonated styrene units). The reaction yield depends chiefly on the concentration ratio of acetyl sulfate and polystyrene. The morphological and thermal properties of the sulfonated polystyrene obtained by homogeneous sulfonation were studied by means of scanning electron microscopy, differential scanning calorimetry and thermogravimetry. The glass transition temperature of sulfonated polystyrene increases in relation to pure polystyrene and ∆Cp was evaluated in order to confirm the strong interactions among thẽ SO 3 H groups.

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Section: Introductionmentioning

confidence: 99%

“…Turbak 2 sulfonated polystyrene in a homogeneous phase reacting polystyrene with complexes of triethyl phosphate and sulfur trioxide as sulfonating agents in dichloroethane. Makowski et al 1 also prepared lightly sulfonated polystyrene by using acetyl sulfate complexes as sulfonation reagent in a solution of dichloroethane.…”

Section: Introductionmentioning

confidence: 99%

Synthesis in pilot plant scale and physical properties of sulfonated polystyrene

Martins¹,

Ruggeri²,

Paoli³

2003

J. Braz. Chem. Soc.

146

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“…These reagents produced dark-brown agglomerates because of charring and the probable formation of sulfones which gave rise to cross-linking between particles. These difficuties were obviated by using the S03/phosphate colnplex syste~il discovered by Turbalc (14).…”

Section: Sulfonating Agentmentioning

confidence: 99%

“…The drawback of this inethod appears to be the problem of avoiding coagulation and of limiting sulfonation to the surface of the particle. An attempt has been made to overconle these difficulties by use of a simple concurrent-flow fast-reaction apparatus, uhich allo~vs reduction of the reaction time to less than 10-I s. Also, sulfonation was carried out in an organic medium by the method of Turbal: (14) to avoid coagulation of the latex by sulfone formation. This lllethod is described in the first part of the paper.…”

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confidence: 99%

Preparation and Characterization of Sulfonated Polystyrene Latexes

Chan¹,

Goring²

1966

Can. J. Chem.

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ABSTRrZCT ?'he purpose of the \vork was the preparation of aqucous suspensions of model spherical particles stabilized by ionizable groups covalently bound to the surface. Starting material >\Ins a 80/20 styrene/divinylbenzene latex. 'The latex had an average particle diameter of 500 A a s determined in the electron microscope. The copolymer mas sulfonated in dichloroethane with a 3/1 SOx/triethylphosphate complex in a concurrent-flow fast-reaction apparatus and was purified by dialysis and ion exchange.'Three main fractions with neutralization eq~~ivalents, N, of 0.9, 1.8, and 2.7 tneq g-1 \\-ere prepared. Elemental analysis revealed that the varying N, in these fractions resulted fro111 the absorption of Ca2+ and R/IgZ+ ions which were tightly bound to the inner-lying sulfonic groups of the particles. Treatment with strong acid followed by ion exchange eliminated the bivalent ions and increased N,, but the titration pattern was markedly changed after such treatment. Sulfonation caused both the partial specihc volume and the refractive index increment to decrease. Electron micrographs showed that the latex particles were only slightly polydisperse and that there was little change in size and shape after sulfonation. Lightscattering measurements established the absence of aggregates in the sulfonated latex. Particle sizes, determined from the intrinsic viscosities, indicated some swelling of the particles in 1 il/I aqueous NaCI. The extent to which the sulfonated latex satisfies the criteria required of a model colloid to be used for a study of electroviscous behavior is discussed.

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“…For instance, Turbak was one of the first scientists who carried out the sulfonation of macromolecules such as polystyrene (PS) using triethyl phosphate and sulfur trioxide as sulfonating agents in dichloroethane 6. Polystyrene was also sulfonated by Makowski using acetyl sulfate complexes as sulfonating reagent in a solution of dichloroethane, which generates random functionalities along the polymer backbone without significant degradation or cross-linking of the reaction products 7 .…”

Section: Introductionmentioning

confidence: 99%