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

[0036]The current invention offers a way of monitoring the evolution of stimuli responsiveness in a continuous way, during polymer synthesis. ‘Polymer synthesis’ includes any type of reaction in which a polymer is produced or modified. An example of the latter is when a polymer is first made and then specific functional groups are attached to it, such as charge groups (e.g. sulfate, quaternary amines, carboxylate, etc.), oligomers, grafted polymers, etc. In its simplest form the present invention is already a high throughput screening platform. In its enhanced form, described below, the present invention becomes a ‘high throughput squared’ platform, and may challenge and even disrupt ongoing high throughput developments that use expensive, robotic, multi-reactor approaches for mere end product analysis.

[0039]With its broad range of monitoring applicability now secured, the present invention is a ‘2nd generation ACOMP’ as it faces wholly new challenges; moving beyond monitoring to reaction control in order to produce polymers of desired characteristics, and extending the ACOMP platform to monitor, understand and control, the stimuli-responsiveness of polymers. These latter include polymers whose properties change with changing environmental factors, such as temperature, light, pH, solvent quality, presence of specific molecules, etc. The potential applications of these materials make them an exciting interface between chemical and biomolecular engineering, chemistry, materials science, and physics.

[0041]The present inventor aims to create a paradigm shift in polymer science, in which online monitoring and control become powerful adjuncts to polymer discovery, development and production, and for understanding stimuli responsive behavior in polymer solutions. Importantly, information-rich ACOMP results also provide a more complete database, and are available for polymer scientists in the broader community involved in modeling and reaction engineering. It is expected that the present invention will also quickly have real economic impact on polymer industries, yielding practical new materials and process monitoring and control that enhance savings of energy, petroleum, and other non-renewable resources, plant and labor time, and lead to better safety, and less greenhouse gas emissions and environmental pollution per kilogram of product.

[0043]The multi-purpose platform of the present invention allows different time-dependent processes in polymer and colloid solutions to be monitored, and also can be used to automatically map characteristics of multi-component solutions in equilibrium or quasi-equilibrium, such as automatic determination of phase diagrams, and combines sophisticated, interconnected optical detection methods, and a fully integrated multi-detector GPC.

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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