Spectroscopic examination of ethylene–propylene–norbornenic diene terpolymers

Tosi, Camillo; Ciampelli, F.; Cameli, N.

doi:10.1002/app.1972.070160401

Cited by 7 publications

References 13 publications

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Unsteady diffusion kinetics of Ziegler‐Natta heterogeneous catalyst polymerization, 4. Prediction of experimental results of propylene/ethylene/1‐hexadecene terpolymerization

1993

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The prediction, based on unsteady diffusion kinetics, of the enhancement of reactivity and incorporation of 1-hexadecene in its copolymerization with propylene on adding a small amount of ethylene (increase from 5,2 mol-Vo to 10,8 mol-Yo when 2% of ethylene was added, and to 16,l mol-Yo when 5% was added) was verified in the terpolymerization of propylene/l-hexadecene/ ethylene on a commercial Solvay-type 6-TiC1, catalyst. The catalyst efficiency was thus also increased. These augmentations originate from the increase in diffusion coefficient of 1 -hemdecene at the catalyst surface when the P P crystallinity decreases on introduction of ethylene. Calculation based on unsteady diffusion kinetics showed that the order of diffusion coefficients ethylene > propylene > 1-hexadecene is reversed as the monomer concentration increases when the monomers are not at their equilibrium concentration. Sequence distribution as determined by means of I3C NMR revealed a tendency of blocky structure rather than a Bernoullian one. The terpolymer compositions obtained by means of an IR method developed in this work conform rather well with the NMR results. Results in this work not only support the unsteady diffusion kinetics but also provide a new route to prepare olefinic copolymer rubbers with heterogeneous titanium catalysts. a) Part 3: cf. ref. '). b, Present address:

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Unsteady diffusion kinetics of Ziegler‐Natta heterogeneous catalyst polymerization, 4. Prediction of experimental results of propylene/ethylene/1‐hexadecene terpolymerization

1993

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Linear non‐conjugated dienes from biomass as termonomers in EPDM synthesis, 2. Comparison with 5‐ethylidene‐2‐norbornene termonomer

Dolatkhani¹,

Cramail²,

Deffieux³

1996

Macro Chemistry & Physics

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A comparative study of 5-ethylidene-2-norbornene (ENB) or 5,7-dimethylocta-l,6diene (5,7-DMO) as diene termonomer in ethylene-propylene-diene (EPDM) terpolymer synthesis is presented. The reactivities of the cyclic and linear non-conjugated dienes are first compared in homopolymerization in the presence of two conventional Ziegler-Natta catalytic systems: TiCl,, 1/3A1C13, 14MgC1, associated to AIEt,, and VOCl, (or VCI,) associated to AlEt,Cl. ENB polymerization yields a branched poly(ENB) in agreement with a predominant cationic reaction, whereas polymerization of 5,7-DMO proceeds exclusively by a Ziegler-Natta mechanism. In terpolymerization, ENB is much more reactive than 5,7-DMO and is incorporated more easily in the terpolymer. However, the high sensitivity of ENB toward acidic species also results in cationic side reactions and therefore limits the utilization of ENB to a low concentration range. We have shown that the productivity of vanadium catalysts, which are mainly used in industrial EPDM synthesis, is drastically reduced in the presence of ENB an 5,7-DMO, due to the rapid reduction of vanadium involving the diene.

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Functionalization of ethylene‐propylene‐diene terpolymer via the alder ene reaction

Thompson

Tzoganakis

Rempel

1998

Polymer Engineering & Sci

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An ethylene‐propylene‐diene rubber (EPDM), containing 5 wt% 5‐ethylidene‐2‐norbornene, was functionalized with maleic anhydride through the Alder Ene reaction at temperatures above 200°C in a co‐rotating twin screw extruder. Characterization of the maleated product included FT‐IR, 1H and 13C NMR, and GPC. The degree of functionalization was determined by infrared analysis and by the mechanical properties of an ionic network formed by neutralizing the maleated rubber with zinc oxide. Increased temperature and maleic anhydride reactant concentration were found to improve the extent of reaction. Several Lewis acid species (SnCl2•2H2O, RuCln•xH2O and AlCl3) were tested as catalysts, and they were found to have a small effect on the degree of functionalization. This effect improved with reduced acid concentration. Among the Lewis acids examined, AlCl3 gave rise to the greatest improvement of succinyl anhydride incorporation into the rubber.

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Spectroscopic examination of ethylene–propylene–norbornenic diene terpolymers

Cited by 7 publications

References 13 publications

Unsteady diffusion kinetics of Ziegler‐Natta heterogeneous catalyst polymerization, 4. Prediction of experimental results of propylene/ethylene/1‐hexadecene terpolymerization

Unsteady diffusion kinetics of Ziegler‐Natta heterogeneous catalyst polymerization, 4. Prediction of experimental results of propylene/ethylene/1‐hexadecene terpolymerization

Linear non‐conjugated dienes from biomass as termonomers in EPDM synthesis, 2. Comparison with 5‐ethylidene‐2‐norbornene termonomer

Functionalization of ethylene‐propylene‐diene terpolymer via the alder ene reaction

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