Phase separation studies in RIM polyurethanes catalyst and hard segment crystallinity effects

R. E. Camargo; Chris Macosko; M. Tirrell; S. T. Wellinghoff

doi:10.1016/0032-3861(85)90243-5

Phase separation studies in RIM polyurethanes catalyst and hard segment crystallinity effects

R. E. Camargo, Chris Macosko, M. Tirrell, S. T. Wellinghoff

Chemical Engineering and Materials Science

Research output: Contribution to journal › Article › peer-review

52 Scopus citations

Abstract

Polyurethanes were prepared from pure 4,4′-diphenylmethane diisocyanate (MDI), 1,4-butane diol (BDO) or 1,2-ethane diol (EDO) and α,ω-hydroxyl poly(propylene oxide) (PPO) by reaction injection moulding (RIM). Hard segment (MDI + BDO or EDO) level was 45-50 wt%. The PPO had about 20% ethylene oxide copolymerized in at the chain ends to provide 80% primary OH end groups. M_n was varied from 2000 to 4000. Dibutyl tin dilaurate catalyst and mould temperature were varied. Dynamic mechanical, wide-angle X-ray, differential scanning calorimeter, molecular weight and tensile elongation measurements were made on the RIM polyurethanes. At low reaction rates (low catalyst or temperature) highly crystalline, well phase separated but low molecular weight polymers were produced. At high catalyst or temperature levels more poorly phase separated but high molecular weight, tough polymers resulted. Higher M_n PPO gave better phase separation and EDO gave higher melting temperatures. Preventing hard segment crystallinity by substituting asymmetric MDI or glycols resulted in phase compatibility.

Original language	English (US)
Pages (from-to)	1145-1154
Number of pages	10
Journal	Polymer
Volume	26
Issue number	8
DOIs	https://doi.org/10.1016/0032-3861(85)90243-5
State	Published - Aug 1985

Bibliographical note

Funding Information:
This work was supported by Industry University Cooperative funding from the National Science Foundation, Grant NSF-CPE-8118-232, the General Motors Corporation and the Union Carbide Corporation. The authors are also indebted to Drs D. Spence and J. Ferrarini from Rubicon Chemicals, R. Lloyd from Texaco Chemicals, J. O'Connors from Olin Corp. and R. Gerkin and L. Lawler from Union Carbide for providing us with the raw chemicals used in this work. Invaluable assistance by K. Dulin, J. Horns and J. Andrews in sample preparation and characterization is acknowledged. One of the authors (R.E.C.) would also like to thank the 3M Company for fellowship support through this project.

Keywords

crystalline hard segments
molecular weight
phase separation
polymerization rate
polyurethane
reaction injection moulding

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title = "Phase separation studies in RIM polyurethanes catalyst and hard segment crystallinity effects",

abstract = "Polyurethanes were prepared from pure 4,4′-diphenylmethane diisocyanate (MDI), 1,4-butane diol (BDO) or 1,2-ethane diol (EDO) and α,ω-hydroxyl poly(propylene oxide) (PPO) by reaction injection moulding (RIM). Hard segment (MDI + BDO or EDO) level was 45-50 wt%. The PPO had about 20% ethylene oxide copolymerized in at the chain ends to provide 80% primary OH end groups. Mn was varied from 2000 to 4000. Dibutyl tin dilaurate catalyst and mould temperature were varied. Dynamic mechanical, wide-angle X-ray, differential scanning calorimeter, molecular weight and tensile elongation measurements were made on the RIM polyurethanes. At low reaction rates (low catalyst or temperature) highly crystalline, well phase separated but low molecular weight polymers were produced. At high catalyst or temperature levels more poorly phase separated but high molecular weight, tough polymers resulted. Higher Mn PPO gave better phase separation and EDO gave higher melting temperatures. Preventing hard segment crystallinity by substituting asymmetric MDI or glycols resulted in phase compatibility.",

keywords = "crystalline hard segments, molecular weight, phase separation, polymerization rate, polyurethane, reaction injection moulding",

author = "Camargo, {R. E.} and Chris Macosko and M. Tirrell and Wellinghoff, {S. T.}",

note = "Funding Information: This work was supported by Industry University Cooperative funding from the National Science Foundation, Grant NSF-CPE-8118-232, the General Motors Corporation and the Union Carbide Corporation. The authors are also indebted to Drs D. Spence and J. Ferrarini from Rubicon Chemicals, R. Lloyd from Texaco Chemicals, J. O'Connors from Olin Corp. and R. Gerkin and L. Lawler from Union Carbide for providing us with the raw chemicals used in this work. Invaluable assistance by K. Dulin, J. Horns and J. Andrews in sample preparation and characterization is acknowledged. One of the authors (R.E.C.) would also like to thank the 3M Company for fellowship support through this project.",

year = "1985",

month = aug,

doi = "10.1016/0032-3861(85)90243-5",

language = "English (US)",

volume = "26",

pages = "1145--1154",

journal = "Polymer",

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T1 - Phase separation studies in RIM polyurethanes catalyst and hard segment crystallinity effects

AU - Camargo, R. E.

AU - Macosko, Chris

AU - Tirrell, M.

AU - Wellinghoff, S. T.

N1 - Funding Information: This work was supported by Industry University Cooperative funding from the National Science Foundation, Grant NSF-CPE-8118-232, the General Motors Corporation and the Union Carbide Corporation. The authors are also indebted to Drs D. Spence and J. Ferrarini from Rubicon Chemicals, R. Lloyd from Texaco Chemicals, J. O'Connors from Olin Corp. and R. Gerkin and L. Lawler from Union Carbide for providing us with the raw chemicals used in this work. Invaluable assistance by K. Dulin, J. Horns and J. Andrews in sample preparation and characterization is acknowledged. One of the authors (R.E.C.) would also like to thank the 3M Company for fellowship support through this project.

PY - 1985/8

Y1 - 1985/8

N2 - Polyurethanes were prepared from pure 4,4′-diphenylmethane diisocyanate (MDI), 1,4-butane diol (BDO) or 1,2-ethane diol (EDO) and α,ω-hydroxyl poly(propylene oxide) (PPO) by reaction injection moulding (RIM). Hard segment (MDI + BDO or EDO) level was 45-50 wt%. The PPO had about 20% ethylene oxide copolymerized in at the chain ends to provide 80% primary OH end groups. Mn was varied from 2000 to 4000. Dibutyl tin dilaurate catalyst and mould temperature were varied. Dynamic mechanical, wide-angle X-ray, differential scanning calorimeter, molecular weight and tensile elongation measurements were made on the RIM polyurethanes. At low reaction rates (low catalyst or temperature) highly crystalline, well phase separated but low molecular weight polymers were produced. At high catalyst or temperature levels more poorly phase separated but high molecular weight, tough polymers resulted. Higher Mn PPO gave better phase separation and EDO gave higher melting temperatures. Preventing hard segment crystallinity by substituting asymmetric MDI or glycols resulted in phase compatibility.

AB - Polyurethanes were prepared from pure 4,4′-diphenylmethane diisocyanate (MDI), 1,4-butane diol (BDO) or 1,2-ethane diol (EDO) and α,ω-hydroxyl poly(propylene oxide) (PPO) by reaction injection moulding (RIM). Hard segment (MDI + BDO or EDO) level was 45-50 wt%. The PPO had about 20% ethylene oxide copolymerized in at the chain ends to provide 80% primary OH end groups. Mn was varied from 2000 to 4000. Dibutyl tin dilaurate catalyst and mould temperature were varied. Dynamic mechanical, wide-angle X-ray, differential scanning calorimeter, molecular weight and tensile elongation measurements were made on the RIM polyurethanes. At low reaction rates (low catalyst or temperature) highly crystalline, well phase separated but low molecular weight polymers were produced. At high catalyst or temperature levels more poorly phase separated but high molecular weight, tough polymers resulted. Higher Mn PPO gave better phase separation and EDO gave higher melting temperatures. Preventing hard segment crystallinity by substituting asymmetric MDI or glycols resulted in phase compatibility.

KW - crystalline hard segments

KW - molecular weight

KW - phase separation

KW - polymerization rate

KW - polyurethane

KW - reaction injection moulding

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SN - 0032-3861

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ER -

Phase separation studies in RIM polyurethanes catalyst and hard segment crystallinity effects

Abstract

Bibliographical note

Keywords

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