Parallel reactor with internal sensing and method of using same

Abstract

Devices and methods for controlling and monitoring the progress and properties of multiple reactions are disclosed. The method and apparatus are especially useful for synthesizing, screening, and characterizing combinatorial libraries, but also offer significant advantages over conventional experimental reactors as well. The apparatus generally includes multiple vessels for containing reaction mixtures, and systems for controlling the stirring rate and temperature of individual reaction mixtures or groups of reaction mixtures. In addition, the apparatus may include provisions for independently controlling pressure in each vessel, and a system for injecting liquids into the vessels at a pressure different than ambient pressure. In situ monitoring of individual reaction mixtures provides feedback for process controllers, and also provides data for determining reaction rates, product yields, and various properties of the reaction products, including viscosity and molecular weight. Computer-based methods are disclosed for process monitoring and control, and for data display and analysis.

1 - 162 . (canceled)  
     
     
         163 . A system for parallel processing of reaction mixtures, wherein the system comprises: 
 vessels for receiving the reaction mixtures, said vessels being sealed against fluid communication with one another and adapted for containing the reaction mixtures at pressures greater than about 10 psig;    a chamber enclosing the vessels, the chamber being fillable with a suitable gas for minimizing contamination of the reaction mixtures;    a robotic material handling system for loading the vessels with chemical reaction materials;    a stirring system adapted to agitate the reaction mixtures; and    a temperature control system adapted to control the temperature of the vessels.    
     
     
         164 . The system of  claim 163  wherein the temperature control system is operable to maintain a first group of the vessels at a different temperature than a second group of the vessels.  
     
     
         165 . The system of  claim 163  wherein the chamber is substantially impermeable to entry of a contaminant gas.  
     
     
         166 . The system of  claim 163  wherein the stirring system comprises stirrers engageable with the reaction mixtures and a drive for rotating the stirrers to stir the reaction mixtures.  
     
     
         167 . The system of  claim 166  wherein at least one stirrer comprises a spindle having a first end and a second end and a stirring blade attached to the first end of the spindle, the second end of the spindle being magnetically coupled to the drive.  
     
     
         168 . The system of  claim 166  wherein at least one stirrer is a magnetic stirring bar, and wherein the drive comprises an array of electromagnets for producing rotating magnetic fields around the stirring bar.  
     
     
         169 . The system of  claim 163  further comprising an injection system for introducing chemical reaction materials into the vessels.  
     
     
         170 . The system of  claim 169  wherein the injection system is operable to introduce chemical reaction materials into the vessels when the vessels are at a pressure different than ambient pressure.  
     
     
         171 . The system of  claim 163  further comprising at least two reactor modules, each of said reactor modules comprising at least one of said vessels.  
     
     
         172 . The system of  claim 163  further comprising pressure sensors for measuring the pressure inside the vessels.  
     
     
         173 . The system of  claim 163  wherein the robotic handling system is inside the chamber.  
     
     
         174 . The system of  claim 173  wherein the robotic handling system comprises a moveable fluid delivery probe.  
     
     
         175 . The system of  claim 163  wherein the vessels contain the reaction mixtures at pressures ranging between about 10 psig and about 500 psi.  
     
     
         176 . The system of  claim 175  wherein the vessels contain the reaction mixtures at pressures ranging between about 10 psig and about 300 psi.  
     
     
         177 . A method of parallel processing of reaction mixtures comprising: 
 using a robotic material handling system to load chemical reaction materials into a plurality of vessels, said vessels being sealed against fluid communication with one another and adapted for containing the reaction mixtures at pressures greater than about 10 psig;    substantially enclosing the vessels in a chamber;    filling the chamber with a suitable gas for minimizing contamination of the reaction vessels;    agitating the reaction mixtures; and    controlling the temperature of at least some of the vessels.    
     
     
         178 . The method of  claim 177  wherein the step of controlling the temperature of at least some of the vessels comprising maintaining a first group of the vessels at a different temperature than a second group of the vessels.  
     
     
         179 . The method of  claim 177  wherein the step of filling the chamber with a suitable gas comprises pressurizing the chamber with the gas to a pressure greater than atmospheric.  
     
     
         180 . The method of  claim 177  wherein the step of agitating the reaction mixtures comprises stirring the reaction mixtures.  
     
     
         181 . The method of  claim 180  wherein the stirring step comprises rotating a plurality of stirrers engageable with the reaction mixtures.  
     
     
         182 . The method of  claim 181  wherein at least one of said stirrers comprises a spindle having a first end and a second end and a stirring blade attached to the first end of the spindle, and wherein the rotating step comprises using a drive system coupled to the second end of the spindle to rotate said at least one stirrer.  
     
     
         183 . The method of  claim 181  wherein at least one of said stirrers comprises a magnetic stirring bar, and wherein the stirring step comprises using an array of electromagnets to produce rotating magnetic fields around said magnetic stirring bar.  
     
     
         184 . The method of  claim 177  further comprising injecting chemical reaction materials into the vessels.  
     
     
         185 . The method of  claim 184  wherein the injecting step comprises using the robotic handling system to move a fluid delivery probe from a first vessel to a second vessel.  
     
     
         186 . The method of  claim 184  wherein the injecting step comprises injecting chemical reaction materials into the vessels when the vessels are at a pressure different than ambient pressure.  
     
     
         187 . The method of  claim 177  further comprising measuring the pressure inside the vessels.  
     
     
         188 . The method of  claim 177  further comprising allowing the reaction mixtures to react in the vessels at pressures ranging between about 10 psig and about 500 psi.  
     
     
         189 . The method of  claim 188  further comprising allowing the reaction mixtures to react in the vessels at  
       at pressures ranging between about 10 psig and about 300 psi