Supporting Information and the ORCID identification number(s) for the author(s) of this article can be found under: https://doi.Scheme1.(a) Synthesisofm odified lignin (L-COOH)from KL and MHHPA. (b) Curing reaction of L-COOH and PEG-epoxy and illustration of transesterification reaction within the crosslinkednetwork.
SynopsisBy use of a modified, small-bore, capihry extrusion rheometer (MCER) with an Tnstron tensile testing machine, the flow and set-up properties of thermosetting plastics and rubbers were characterized. The majority of the experiments were performed with diallyl phthalate, where the rate of curing was also followed by infrared determination of the reduction in unssturation as the polymerization-curing proceeded. Phenol-formaldehyde was also characterized. Finally, the curing of ethylene-propylene and ethylenevinyl acetate copolymer rubbers with peroxide was studied and correlated with the type of peroxide used. The MCER data are shown to be of practical use for predicting the time-temperature-pressure relationships for processing thermosetting plastics and rubbers. Moreover, the history of the curing, as obtained by analysis of the continuously extruded strand, is also of theoretical interest for studying reaction kinetics and for evaluating the effectiveness of various curing systems. It is predicted the MCER will be widely used for studying the curing of thermosetting plastics and rubbers. 1911 1912 SALYER, HEYD, BRODBECK, IIARTZEL, BROWN tion as the polymerization proceeded. A second thermosetting polymer, phenol-formaldehyde, was also analyzed. Finally, the curing of ethylenepropylene and ethylene-vinyl acetate copolymer rubbers with peroxide was studied, and the results were correlated with the type of peroxide used. EQUIPMENTThe Monsanto capillary extrusion rheonieter, MCER (Fig. l), shown schematically in Figure 2, contains an insulated, electrically heated steel cylinder supported on a steel framework. The cylinder is insulated by two transite disks ( I ) , a cylinder of high temperature insulating wool (S), and an outer jacket of asbestos tubing (2). Four narrow-banded cylindrical heaters (4) , manufactured by the Watlow Electric Manufacturing Company, supply heat to the steel cylinder. A thin aluminum sleeve (5), inserted between the steel cylinder and the heaters, improves heat transfer and alleviates thermal gradients. To prevent burn-out of the heaters, a 1/2-in. dead air space separated the heaters and the asbestos tubing insulation. The tempered steel cylinder (6) is 8:/8 in. long, 2 in. in diam-Fig. 1. Monsanto capillary extrusion rheometer in position in Instron testing machine.
This report was prepared m an account of GoTremment sponsored work. Neither the United Stales, nor the Commission, nor any person acting on behaif of tte CJommlssloffi A. Maltes any wananty or representation, expressed or Implied, with respect to the accuracy, completeness, or asefatoess of the information cont^ned in Ms report, or that the ase of any information, apparatus, method, or process disclosed in this report may not infringe privately owned tights: or B. Mstimes any Eabilittes with respect to the use of, or for damages resulting from the use of say information, appiratus, method, or process disclosed in this report. As ased in the above, "person acting on behalf of the Commission" Includes any employee or contractor of toe Commission, or employee of such contractor, to the extent that sttch employee or contractor of the Commission, or employee of such contractor prepares. disseraiaates, or provides access to, any information pursuant to Ms employment or contract with the Commission, or Ms employment with such ctmtractor.
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