Investigation of factors affecting isolation of needle-shaped particles in a vacuum-agitated filter drier through non-invasive measurements by Raman spectrometry

Peter Hamilton, David Littlejohn, Alison Nordon, Jan Sefcik, Paul Slavin, John Andrews, Paul Dallin

Research output: Contribution to journalArticle

10 Citations (Scopus)

Abstract

The effects of pressure filtration and vacuum agitated drying on cellobiose octaacetate (COA) particles in methanol slurries were studied by making Raman measurements through the glass wall at the side of a filter drier beneath the oil jacket. The change in intensity of methanol peaks in the spectra allowed the removal of the solvent from the particle bed to be monitored. Also, drying curves for COA generated from the Raman measurements gave an indication of the changing physical status of the particle bed during continuous or intermittent agitation. The intensity of the Raman signal for COA depended on the bulk density of the particle bed, which changed due to aggregation and attrition that occurred during solvent removal and particle motion induced by agitation during vacuum drying. Loss on drying (LOD) measurements of samples removed at the end of the pressure filtration and vacuum agitated drying stages established the degree of wetness and confirmed the end point of drying (<0.5% w/w solvent), respectively. Dynamic image analysis confirmed that minimum attrition of COA was achieved when (a) the majority of the methanol was removed during pressure filtration at 0.5bar N2 and (b) intermittent agitation was applied during the vacuum drying stage.

LanguageEnglish
Pages878-885
Number of pages8
JournalChemical Engineering Science
Volume101
Early online date27 May 2013
DOIs
Publication statusPublished - 1 Sep 2013

Fingerprint

needles
Needles
Spectrometry
drying
isolation
Drying
Vacuum
filters
vacuum
agitation
spectroscopy
Methanol
beds
comminution
methyl alcohol
jackets
slurries
Slurries
particle motion
image analysis

Keywords

  • Raman spectrometry
  • cellobiose octaacetate
  • image analysis
  • agitation time
  • particle properties
  • particle filtration–drying

Cite this

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title = "Investigation of factors affecting isolation of needle-shaped particles in a vacuum-agitated filter drier through non-invasive measurements by Raman spectrometry",
abstract = "The effects of pressure filtration and vacuum agitated drying on cellobiose octaacetate (COA) particles in methanol slurries were studied by making Raman measurements through the glass wall at the side of a filter drier beneath the oil jacket. The change in intensity of methanol peaks in the spectra allowed the removal of the solvent from the particle bed to be monitored. Also, drying curves for COA generated from the Raman measurements gave an indication of the changing physical status of the particle bed during continuous or intermittent agitation. The intensity of the Raman signal for COA depended on the bulk density of the particle bed, which changed due to aggregation and attrition that occurred during solvent removal and particle motion induced by agitation during vacuum drying. Loss on drying (LOD) measurements of samples removed at the end of the pressure filtration and vacuum agitated drying stages established the degree of wetness and confirmed the end point of drying (<0.5{\%} w/w solvent), respectively. Dynamic image analysis confirmed that minimum attrition of COA was achieved when (a) the majority of the methanol was removed during pressure filtration at 0.5bar N2 and (b) intermittent agitation was applied during the vacuum drying stage.",
keywords = "Raman spectrometry , cellobiose octaacetate , image analysis, agitation time, particle properties, particle filtration–drying",
author = "Peter Hamilton and David Littlejohn and Alison Nordon and Jan Sefcik and Paul Slavin and John Andrews and Paul Dallin",
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AU - Hamilton, Peter

AU - Littlejohn, David

AU - Nordon, Alison

AU - Sefcik, Jan

AU - Slavin, Paul

AU - Andrews, John

AU - Dallin, Paul

N1 - Notice: This is the author's version of a work that was accepted for publication in Chemical Engineering Science. Changes resulting from the publishing process, such as peer review, editing, corrections, structural formatting, and other quality control mechanisms may not be reflected in this document. Changes may have been made to this work since it was submitted for publication. A definitive version was subsequently published in Chemical Engineering Science, [101, 20 Sept., (2013)] DOI: 10.1016/j.ces.2013.05.035

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Y1 - 2013/9/1

N2 - The effects of pressure filtration and vacuum agitated drying on cellobiose octaacetate (COA) particles in methanol slurries were studied by making Raman measurements through the glass wall at the side of a filter drier beneath the oil jacket. The change in intensity of methanol peaks in the spectra allowed the removal of the solvent from the particle bed to be monitored. Also, drying curves for COA generated from the Raman measurements gave an indication of the changing physical status of the particle bed during continuous or intermittent agitation. The intensity of the Raman signal for COA depended on the bulk density of the particle bed, which changed due to aggregation and attrition that occurred during solvent removal and particle motion induced by agitation during vacuum drying. Loss on drying (LOD) measurements of samples removed at the end of the pressure filtration and vacuum agitated drying stages established the degree of wetness and confirmed the end point of drying (<0.5% w/w solvent), respectively. Dynamic image analysis confirmed that minimum attrition of COA was achieved when (a) the majority of the methanol was removed during pressure filtration at 0.5bar N2 and (b) intermittent agitation was applied during the vacuum drying stage.

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