Methods and instrumentation for during-synthesis monitoring of polymer functional evolution

Abstract

A method of monitoring the evolution of polymer and/or colloid stimuli responsiveness during synthesis of polymers and/or colloids, including postpolymerization modifications on natural and synthetic polymers, includes providing a reactor in which the polymers and/or colloids are synthesized; and providing a means of monitoring the stimuli responsiveness of the polymers and/or colloids during said synthesis. Preferably, the method also includes monitoring the evolution of the characteristics of the polymers and/or colloids during said synthesis. Preferably, evolution of polymer and/or colloid stimuli responsiveness is correlated to the evolution of the properties of the polymers and/or colloids themselves. Also, preferably the conditions of the fluid in the reactor in which the synthesis occurs is determined. The determination can be by detection, choice of materials and temperature conditions, for example, and combinations thereof. The method and instrumentation disclosed can lead to optimization and control of processes and synthetic and modification strategies leading to polymers and colloids with desired stimuli responsiveness.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]Priority of U.S. Provisional Patent Application Ser. No. 61 / 059,050, filed 5 Jun. 2008, hereby incorporated herein by reference, is hereby claimed.[0002]U.S. patent application Ser. No. 11 / 865,589, filed 1 Oct. 2007, and International Application Number PCT / US2007 / 80116, filed 1 Oct. 2007, are hereby incorporated herein by reference.[0003]U.S. Provisional Patent Application Ser. No. 60 / 827,559, filed 29 Sep. 2006, and U.S. Provisional Patent Application Ser. No. 60 / 884,821, filed 12 Jan. 2007, are hereby incorporated herein by reference.[0004]This is not a continuation, continuation-in-part, or divisional of any patent application.STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT[0005]Not applicableREFERENCE TO A “MICROFICHE APPENDIX”[0006]Not applicableBACKGROUND OF THE INVENTION[0007]1. Field of the Invention[0008]The present invention relates to a ‘second generation of ACOMP’ (Automatic Continuous Online Monitoring of Pol...

AI Technical Summary

Benefits of technology

[0045]Simultaneous monitoring of polymer properties, such as mass and composition, and the onset of stimuli responsiveness during synthesis (including any postpolymerization modifications), such as phase transitions, micellization, conformational changes, microgelation, ability to interact with other substances, such as drugs, etc. The SG-ACOMP will be the only instrument of its kind in the world, able to determine at what point in synthesis, (including postpolymerization reactions and modifications of polymers and colloids extracted from natural products), polymers and copolymers become stimuli responsive, whether sharply or gradually; e.g. the effect of solvent type on LCST (lower critical solution temperature) of an evolving polymer and the relationship with polymer composition and molecular weight distributions could be determined. The transition at the LCST will be automatically detected, and the threshold characteristics of the polymer stimuli responsiveness can be quantified.

Problems solved by technology

The lack of on-line measurement of polymer properties is usually the main problem in closed-loop control of polymerization reactions.

The controllers employed in closed-loop methods use some on-line measurements, but none have had continuous or substantially continuous streams of co-conversion, molecular weight and other pertinent data available, precisely the type of massive data stream provided by ACOMP.

There are typically serious problems with drift and bias in the empirical and inferential models used for data interpretation, and fouling of in-situ probes.

Efforts to control Mw have been reported.59,78,85,86 Usually, the main difficulty in controlling Mw is the lack of on-line sensors.

Current methods for relating polymer characteristics to their stimuli responsiveness are cumbersome and inefficient.

The mere preparation of polymeric test products can be disproportionately time-consuming, and require such steps as precipitation, purification, freeze-drying, re-dissolution, dialysis, etc.

Spectroscopic or other detection of transitions can be made.114,115 These methods, however, have no means of determining when during synthesis the polymer's stimuli responsiveness begins to appear.

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