IP Library Granted Patent US 7,716,969
Granted Patent B2
US 7,716,969 · App. 11/865,589 · Granted May 18, 2010

Methods and devices for simultaneously monitoring colloid particles and soluble components during reactions

Assignees: The Administrators of the Tulane Educational Fund; Polymer Laboratories Ltd.
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Quick Facts
Patent No.
US 7,716,969
App. No.
11/865,589
Granted
May 18, 2010
Kind
B2
Abstract

A method and apparatus for continuously extracting liquid in at least two separate streams from a vessel, continuously diluting and/or conditioning a first stream in one or more stages, producing, as a result of the extraction, dilution and/or conditioning, the first stream consisting of a dispersion of particles to be characterized, and diluting and/or conditioning a second stream, the second stream consisting of soluble components; and subjecting the first and second streams to various characterizing measurements.

Claims (39)

1. A device for determining characteristics of a dispersion of particles and of soluble components of a liquid in a vessel, comprising:

an extracting means for continuously extracting a first stream and a second stream of the liquid from the vessel,

a first dilution/conditioning means for continually diluting and/or conditioning the first stream in one or more stages, whereby the diluted and/or conditioned first stream facilitates characterization of the dispersion of the particles, a second dilution/conditioning means for diluting and/or conditioning the second stream whereby the diluted and/or conditioned second stream facilitates characterization of the soluble components,

a particle characterizing means for characterizing the particles, and

a component characterizing means for characterizing the soluble components.

2. The device of claim 1 , wherein the liquid extracted from the vessel is from a polymerization reaction occurring in an emulsion or an inverse emulsion phase.

3. The device of claim 1 , further comprising a means for conducting packed column hydrodynamic chromatography on one of the streams.

4. The device of claim 1 further comprising a fractionation means for the soluble component stream, comprising at least one means from the group consisting of GPC, SEC, MALDI-TOF, field flow fractionation, and capillary hydrodynamic fractionation.

5. The device of claim 1 , further comprising a single tube for extracting the first stream from the vessel and a dividing means for subsequently dividing the first stream into at least a primary tributary stream and a secondary tributary stream.

6. The device of claim 5 , further comprising two or more tributary tubes or capillaries connected to the single tube.

7. The device of claim 1 , wherein the second stream further comprises solubilized components.

8. The device of claim 7 , wherein the second stream further comprises dissolved components of a polymer reaction from the group consisting of monomers, polymers, and polymer fragments, catalysts, initiators, chelating agents, stabilizing agents, surfactants, salts, and other small (non-polymeric) molecules.

9. The device of claim 7 , further comprising subjecting the second stream to at least one characterizing measurement.

10. The device of claim 9 , wherein the characterizing measurement is a polymer or monomer characterizing measurement.

11. The device of claim 1 , wherein the first stream contains a dispersion of particles.

12. The device of claim 11 , wherein the first stream is subjected to at least one characterizing measurement.

13. The device of claim 12 , wherein one of the characterizing measurements is a particle characterizing measurement.

14. The device of claim 13 , wherein the particle characterizing means includes at least one means from the group consisting of particle size measuring means, particle size distribution determining means, average of the particle size distribution determining means, particle number density measuring means, particle chemical composition determining means, particle shape and morphology determining means, particle structure measuring means.

15. The device of claim 13 , wherein the measurement is non-continuous.

16. A device for determining characteristics of a dispersion of particles and of soluble components of a liquid in a vessel in which a reaction, involving polymer and/or dispersed particles, occurs, comprising:

an extracting means for simultaneously extracting a first stream and a second stream of the liquid from the vessel, whereby the extraction is continuous,

a first dilution/conditioning means for continually diluting and/or conditioning the first stream in one or more stages, whereby the diluted and/or conditioned first stream facilitates characterization of the dispersion of the particles,

a second dilution/conditioning means for diluting and/or conditioning the second stream whereby the diluted and/or conditioned second stream facilitates characterization of the soluble components related to the reaction in the vessel, such as monomers, comonomers, polymer chains, and fragments of polymers,

a particle characterizing means for characterizing the dispersion of the particles, and

a component characterizing means for characterizing the soluble components.

17. The device of claim 16 , further comprising sample vials in which samples are collected for subsequent measurements of any type from the first stream prior to or subsequent to dilution and/or conditioning or from the second stream prior to or subsequent to dilution and/or conditioning.

18. A method of determining characteristics of a dispersion of particles and of soluble components of a liquid in a vessel, comprising:

continuously extracting a first stream and a second stream of the liquid from the vessel,

continually diluting and/or conditioning the first stream in one or more stages, whereby the diluted and/or conditioned first stream facilitates characterization of the dispersion of the particles,

diluting and/or conditioning the second stream whereby the diluted and/or conditioned second stream facilitates characterization of the soluble components,

characterizing the particles, and

characterizing the soluble components.

19. A method of determining characteristics of a dispersion of particles and of soluble components of a liquid in a vessel in which a reaction, involving polymer and/or dispersed particles, occurs, comprising:

simultaneously and continuously extracting a separate first stream and a separate second stream of the liquid from the vessel,

continually diluting and/or conditioning the first stream in one or more stages, whereby the diluted and/or conditioned first stream facilitates characterization of the dispersion of the particles,

diluting and/or conditioning the second stream whereby the diluted and/or conditioned second stream facilitates characterization of the soluble components related to the reaction in the vessel, such as monomers, comonomers, polymer chains, and fragments of polymers,

characterizing the particles, and

characterizing the soluble components.

20. The method of claim 19 , wherein the liquid in the vessel is a polymerization reaction occurring in an emulsion or inverse emulsion phase.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 1, 2016
From: AGILENT TECHNOLOGIES U.K. LIMITED
To: THE ADMINISTRATORS OF THE TULANE EDUCATIONAL FUND
Reel/Frame 038328/0715 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 31, 2011
From: POLYMER LABORATORIES LIMITED
To: AGILENT TECHNOLOGIES U.K. LIMITED
Reel/Frame 026052/0832 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 10, 2010
From: O'DONOHUE, STEPHEN J.; ANDERSON, ROBERT M.
To: POLYMER LABORATORIES, LTD.
Reel/Frame 024059/0130 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 24, 2009
From: REED, WAYNE F.; ALB, ALINA M.
To: THE ADMINISTRATORS OF THE TULANE EDUCATIONAL FUND
Reel/Frame 022444/0048 →
Continuity (3)
Provisional Application 6082755900 · Sep 29, 2006
Provisional Application 6088482100 · Jan 12, 2007
Related Publication 20080216563A1 · Sep 11, 2008