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  Continuous process for the production of combinatorial libraries of modified materialsUSPTO Application #: 20070122915Title: Continuous process for the production of combinatorial libraries of modified materials Abstract: A system is provided wherein a devolatilizing reactor is used to make combinatorial libraries of materials. Examples of suitable reactors include continuous high viscosity devolatilizers and continuous devolatilizing kneaders. (end of abstract) Agent: 3m Innovative Properties Company - St. Paul, MN, US Inventors: James M. Nelson, Ryan E. Marx, Jeffrey J. Cernohous, James R. McNerney USPTO Applicaton #: 20070122915 - Class: 436518000 (USPTO) Related Patent Categories: Chemistry: Analytical And Immunological Testing, Involving An Insoluble Carrier For Immobilizing Immunochemicals The Patent Description & Claims data below is from USPTO Patent Application 20070122915. Brief Patent Description - Full Patent Description - Patent Application Claims
CROSS REFERENCE TO RELATED APPLICATIONS [0001] This application is a continuation of U.S. patent application Ser. No. 10/211,219, filed Aug. 2, 2002, the disclosure of which is incorporated by reference in its entirety herein. FIELD OF THE INVENTION [0002] The present invention relates to a continuous process for the production of combinatorial libraries of modified materials. BACKGROUND INFORMATION [0003] A combinatorial approach for materials synthesis is aimed at using rapid synthesis and screening methods to build libraries of polymeric, inorganic or solid state materials. For example, advances in reactor technology have empowered chemists and engineers to rapidly produce large libraries of discrete organic molecules in the pursuit of new drug discovery, which have led to the development of a growing branch of research called combinatorial chemistry. Robotic driven parallel synthesizers consisting of arrays of small batch type reactors have been designed for such efforts (e.g., Chemspeed, Endeavor, Neptune, FlexChem, Reacto-Stations). These reactors synthesize milligram to gram quantities of materials, which can rapidly be screened or analyzed by various techniques including gas chromatography, FT-IR, and UV-Visible spectroscopy. [0004] The development and use of combinatorial methods to develop new polymeric materials is a topic of considerable current interest. A large portion of the current focus of this material-based research is the synthesis of block, graft, dendritic and functionalized polymers. For example, the production of copolymer emulsions at temperatures well below 100.degree. C. in a batch combinatorial chemistry system capable of evaluating 1,000 polymers/week has recently been demonstrated (see Fairley, P., "Symyx Makes `Living` Block Copolymer" Chemical Week 1999, 161, No. 17, 5 May, 1999, p. 13) [0005] An important consideration in making these arrays is that batch reactors suffer from poor heat transfer characteristics, which may have a detrimental effect on the materials produced in batch arrays. In addition, materials produced in small batch reactors still need to be scaled to an appropriate level for application testing and product qualification, requiring some process development and scale up understanding. SUMMARY OF THE INVENTION [0006] There exists a need for a readily scalable, economical method that can rapidly produce many combinatorial formulations in quantities appropriate for application development. The present invention provides a new method of preparing combinatorial libraries of chemically-modified materials in a high throughput fashion. It allows for library members to be continuously made and collected. It also allows the option of later determining the starting materials for a member by tracing back to the time when the starting materials would have been input. [0007] In one aspect the present invention provides a continuous method of making a combinatorial library of materials comprising providing a plug flow mixing apparatus having a high shear environment and devolatilization capabilities, continuously introducing into the mixing apparatus a composition containing at least one polymer that can be modified by a thermally-induced reaction into the reactor, exposing the composition to a high shear environment, and introducing or changing over time at least one variable affecting the properties of the at least one polymer that can be modified to produce a combinatorial library of materials. The composition may be exposed to a temperature of about 100.degree. C. to about 180.degree. C. while it is exposed to a high shear environment. The materials of the library may further be evaluated. [0008] The composition when introduced into the apparatus comprises 90 weight % solids or less. The composition may comprise at least one polymer that is temperature sensitive. [0009] The thermally-induced reaction may remove at least one protective group to expose a functional group. The exposed functional group may be capable of undergoing a grafting reaction. For example, the functional group may ethylenically or acetylenically unsaturated. An in situ chemical reaction may be caused to take place at the functional group. A library of graft polymers may be made. [0010] The thermally-induced reaction may comprise the elimination of isobutylene and water from methacrylic and acrylic esters to produce one or both of acid and anhydride functionalities. This reaction may be catalyzed, optionally by an acid. [0011] The thermally-induced reaction may comprise the elimination of trialkylsilanes from trialkylsiloxy end or side group containing polymers to produce a library of hydroxyl end or side group functional polymers. The thermally-induced reaction may comprise the elimination of trialkylsilanes from trialkylsilazane end or side group containing polymers to produce a library of amino end or sidegroup functional polymers. [0012] The thermally-induced reaction may comprise a deesterification reaction to produce a library of hydroxyl- or carboxylic acid-functionalized polymers. This reaction may be base-catalyzed. [0013] The thermally-induced reaction may comprise the elimination of N.sub.2 from acyl azides and subsequent rearrangement to form isocyanate functionality. [0014] The thermally-induced reaction may comprise the elimination of benzenesulfenic acid from poly(vinyl phenyl sulfoxide) to produce a library of polyacetylene-containing polymers. [0015] The thermally-induced reaction comprises the elimination of trialkylsilanes from trialkylsilthiane end or sidegroup containing polymers to produce a library of thiol end or sidegroup functional polymers. The thermally-induced reaction may comprise the elimination of trialkylsilanes from trialkylsilyl-substituted ethynyl monomers, such as 2-, 3- and 4-[(trimethylsilyl)-ethynyl]styrenes, to produce a library of ethynyl-containing sidegroup or end functionalized polymers. [0016] Variable that can be changed when conducting the method include concentration of starting material, type of starting material, pressure in the reactor, temperature profile in the reactor, amount of energy supplied to a reaction zone, type of energy supplied to a reaction zone, type of component mixing, degree of component mixing, residence time, type and amount of grafting agent, and where and when additional components are introduced into the reactor. Other variables include physical mixing of components and chemical reaction of components. The variables may be changed in a continuous manner or a stepwise manner. [0017] The mixing apparatus may comprises a high viscosity devolatilizer, such as a LIST apparatus. The mixing apparatus may be operated in series with one or more other continuous reactors. The ability to control feed flows, feed locations, and compositional variations in a devolatilizing reactor provides an opportunity to produce a variety of compositions in a continuous, economical, and scalable fashion. A major advantage of producing a combinatorial library of materials in a devolatilizing reactor is that different library components need only be separated in time. They do not need to be physically separated. As used herein: [0018] "actinic radiation" means electromagnetic radiation, preferably UV and IR; [0019] "axial mixing" means mixing in a direction parallel to the overall direction of flow in a reactor; Continue reading... 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