Characterization of Biomass-Derived Rigid Polyurethane Foam by Pyrolysis GCMS and Thermogravimetric Analysis
 

Characterization of Biomass-Derived Rigid Polyurethane Foam by Pyrolysis GCMS and Thermogravimetric Analysis

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This presentation describes a Shimadzu study, where a novel biomass-based rigid polyurethane foam (RPUF) was compared against a control sample of commercially available petroleum-based RPUF, using the ...

This presentation describes a Shimadzu study, where a novel biomass-based rigid polyurethane foam (RPUF) was compared against a control sample of commercially available petroleum-based RPUF, using the complementary techniques of thermogravimetric analysis and pyrolysis GC/MS.

Costs of polyurethane foams (PUF) are rising, as they are primarily derived from petroleum-based products whose price is tied directly to the cost of crude oil. PUFs are used widely throughout the automotive, insulation and housing industries, prompting recent advances in their production, using less expensive and renewable biomass.

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Characterization of Biomass-Derived Rigid Polyurethane Foam by Pyrolysis GCMS and Thermogravimetric Analysis Characterization of Biomass-Derived Rigid Polyurethane Foam by Pyrolysis GCMS and Thermogravimetric Analysis Presentation Transcript

  • Characterization of Biomass-DerivedRigid Polyurethane Foam by Pyrolysis GCMSand Thermogravimetric AnalysisCourtney Taylor, Shimadzu Scientific Instruments, Inc.Columbia, Md., USA
  • 2 / 16IntroductionPolyurethane foams (PUF), in both structural andnon-structural forms, are commonly used throughout theautomotive, insulation and housing industries.These PUFs are primarily derived from petroleum-basedproducts whose price is tied directly to the cost of crude oil.Due to these rising costs, manufacturers are looking foralternatives. Recent advances in the production of PUFs,using less expensive and renewable biomass, makes thismaterial a viable alternative.
  • 3 / 16Various biomass feed stocks were investigated to this end,with some being more promising than others. In thisinvestigation we: Compare a novel biomass-based rigid polyurethane foam (RPUF)against a control sample of commercially available petroleum-basedRPUF Use the complementary techniques of thermogravimetric analysis andpyrolysis GC/MS View slide
  • 4 / 16Methodology This study used a Shimadzu GCMS-QP2010SE coupledwith a PY-3030D Double Shot Pyrolizer and a ShimadzuTGA-50 thermogravimetric analyzer to characterize thesamples. All samples for the TGA portion of this study weremeasured at programmed temperature rates of 2 °C, 5 °C,10 °C and 20 °C/min. for kinetics analysis. Sample weights were kept between 2-4 mg. View slide
  • 5 / 16Rigid PUF samples were prepared in the lab with variousratios of glycerol and other biomass-related components.A control sample of commercial manufacture was obtainedand used to develop the pyrolysis GCMS method.This sample was analyzed at various temperatures in thepyrolizer to determine the optimal conditions (see Figure 1).
  • 6 / 16GCMS Analytical ConditionsGC ConditionsMS ConditionsPy-3030D Temp 500 CInjector Temp 300 CFlow Mode Constant Linear Velocity 39 cm/secSplit Ratio 100:1Oven Program 30 C (1 min) → 20 C/min → 275 C (12 min)Column ZB-5HT 30 M X 0.24 mm X 0.25 µm (Phenomenex Inc.)Interface Temp 280 CSource Temp 200 CScan Range 45-500 m/zTune type Normal
  • 7 / 16Pyrolysis Scan of Commercial PUFFigure 1A temperature of 500 °C was found to give the bestpyrolysis-GCMS results and was used as the test conditionfor all samples.
  • 8 / 16Figure 2 shows a comparison of the three prepared sampleswith different glycerol content and the commercial control.BioPUFs vs. CommercialFigure 2
  • 9 / 16The control shows early eluting peaks as manufacturingblowing agents, followed by DEG and various species relatedto diisocyanate.The lab samples show no blowing agents were used, and theDEG peak is replaced by crude glycerine. All samples containcomponents related to diisocyanate (see Figure 2).
  • 10 / 16TGA KineticsTGA kinetics analysis was performed by the Ozawa method. The heating rates used were: 2 °C, 5 °C, 10 °C and 20 °C/min. Sample weights were kept between 2-4 mg and were sliced from arepresentative cross-section. All runs used a nitrogen purge at 40 ml/min. As seen in thethermograms, different formulations show slightly different curves andthe kinetics analysis was performed on the primary weight loss (seeFigures 3-6).
  • 11 / 16TGA Kinetics Analysis Commercial PUFFigure 3
  • 12 / 16Kinetics 4 PUFFigure 4
  • 13 / 16Kinetics C4 PUFFigure 5
  • 14 / 16Kinetics 5 PUFFigure 6
  • 15 / 16ConclusionPyrolysis GCMS and thermogravimetric analysis can provideuseful information regarding various formulations ofbiomass-derived rigid polyurethane foams.In this study, some difficulties encountered included relativelybusy GCMS chromatograms and less than stable TGAkinetics runs. Further investigations will include a moredetailed pyrolysis EGA analysis and better care will be takenregarding sample morphology in TGA runs.
  • 16 / 16Thank you for viewing this presentation. Should you have anyquestions or require additional information about ourresearch, products or services, please visit our Support page:www.ssi.shimadzu.com/support/@shimadzussiFollow us on Twitter