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Method of reacting two-phase solution changing in phase state with temperature change and apparatus for practicing the sameRelated Patent Categories: Colloid Systems And Wetting Agents; Subcombinations Thereof; Processes Of, Compositions Containing An Agent For Breaking (resolving) Or Inhibiting Colloid Systems; Processes Of Breaking (resolving) Or Inhibiting Colloid Systems (e.g., Gel Breaking Or Inhibiting, Coagulating, Flocculating); Processes Of Preparing The CompositionsMethod of reacting two-phase solution changing in phase state with temperature change and apparatus for practicing the same description/claimsThe Patent Description & Claims data below is from USPTO Patent Application 20070161713, Method of reacting two-phase solution changing in phase state with temperature change and apparatus for practicing the same. Brief Patent Description - Full Patent Description - Patent Application Claims
TECHNICAL FIELD [0001] The present invention relates to a method for making a two-phase solution of which the phase state changes as a result of temperature conversion react, of which the operability and reproducibility are excellent, as well as to an apparatus for implementing this. BACKGROUND TECHNOLOGY [0002] In a chemical process, in the case where a sequential mixture and separation operation can be carried out with ease, sequential work efficiency can be dramatically increased. Presently, it is known that change in temperature causes phase solving/phase separation in a solvent mixture that is formed of a combination of a solvent having a perfluoroalkyl group, and a general organic solvent (I. T. Horvath, J. Rabai, Science, 1994, 266, 72; J. A. Gladysz, Science, 1994, 266, 55). [0003] Japanese Unexamined Patent Publication H15 (2003)-62448 shows a combination of a cycloalkane and a polar solvent as an example of a solvent mixture where phase solving/phase separation is caused. Such solution phase solving and separation phenomena, where phase solving and phase separation can be made to repeat by slightly changing the temperature, can be applied to a wide range of chemical processes, from the micro and macro scale to the plant level. Recently, a method for making a number of processes progress simultaneously, where combinatorial chemistry or a high throughput process method is carried out in a tabletop apparatus, is used widely in many test and research institutions. [0004] FIG. 4 is a conceptual diagram illustrating the theory that solvent mixture causes phase solving/phase separation. (A) in FIG. 4 shows a state where single organic solvents or mixed organic solvents are separated. For example, a solvent that dissolves a reactive material is used as one solvent, and a solvent that dissolves a catalyst or a reaction adjuvant is used as the other solvent. (B) is a step where reaction progresses under such temperature conditions that the solvent is in a state where a uniform phase solving mixture solvent system. (C) shows the state of a separated solvent system where solvent phases of which the main components are solvents that form reversible solvent systems under the above described temperature conditions are separated into phases in which products are dissolved and catalysts or a reaction adjuvant are dissolved. Then, the phase in which the products are dissolved (product solution) is separated and taken out so as to be used for a desired application, while the phase in which reaction adjuvant dissolves (catalyst or reaction adjuvant solution) is recycled (D). [0005] One example of an automatic synthesizing method which uses the theory that such a solvent system causes phase solving/phase separation is described in reference to FIG. 3. That is to say, a material such as a reagent is injected into a reaction container 11 using a sampling apparatus 12 so that a two-phase solution (I) is gained. Next, reaction container 11 is heated, so that the two-phase solution becomes a uniform solution where reaction starts (II). After reaction has started and a predetermined period of time has passed, cooling is started (III). The solution in reaction container 11 automatically separates into phases when the temperature has been lowered to a predetermined temperature or lower (IV). Next, the product phase in reaction container 11 is extracted using an extraction apparatus 17 (V), and this product solution 16 is used for animal experimentation, which is an activity assay, or used for analysis (VI). According to a method for making a number of processes progress simultaneously, several tens to one hundred or more reaction systems, one of which is, for example, that shown in FIG. 3, are carried out in the same apparatus and under the same reaction conditions. [0006] However, it is structurally very troublesome to individually control the temperature of several tens to one hundred or more containers in a tabletop apparatus. Therefore, an apparatus where a block heater which can heat all of the several tens to one hundred or more containers simultaneously is built in is conventionally used. In this case, an automatic sampling operation is carried out on each sample sequentially and automatically, and after that, all the containers are simultaneously heated. In addition, after the solution has been converted into a uniform solution and reaction is complete, all the containers are cooled simultaneously. According to this method, the period of time that is required from the start of the automatic sampling operation to the start of the heating differs, depending on the container. After the automatic sampling, though the solution is in a two-phase state before the start of the reaction, in which, theoretically, no reaction occurs, in reality, a slight amount of reaction occurs even in the two-phase state, since there is contact between the phases in the interface portion. As described above, all of the process conditions are different, depending on the container, according to the conventional method, and it is impossible to carry out the process under the same conditions. This has caused many problems with reproducibility in chemical processes. [0007] Meanwhile, in the case where a multi-stage successive reaction process is carried out by repeating successive phase solving/phase separation, the temperature of the reaction containers should be increased or lowered at each stage, and thereby, the temperature of the solution changes, so that the phase structure of the solution changes. This causes a problem, such that control becomes difficult, particularly on a plant scale, where the capacity is large. In addition, when the temperature of the reaction containers on a plant scale is increased or lowered at each stage, a problem arises, such that the amount of use of utilities, such as electrical power and cooling water, becomes massive, increasing the cost for manufacture. [0008] Accordingly, an object of the present invention is to provide a method for making a two-phase solution of which the phase state changes as a result of temperature conversion react in a number of processes, where a chemical process can be carried out on a number of samples under the same conditions in one processing apparatus, and which is excellent in operativity and reproducibility, as well as an apparatus for implementing this. In addition, another object of the present invention is to provide a method for making a two-phase solution of which the phase state changes due to temperature conversion which is excellent in operativity and efficiency in production, as well as an apparatus for implementing this. [0009] (Non-Patent Document 1) I. T. Horvath, J. Rabai, Science, 1994, 266, 72; J. A. Gladysz, Science, 1994, 266, 55 [0010] (Patent Document 1) Japanese Unexamined Patent Publication H15 (2003)-62448 (claim 1) DISCLOSURE OF THE INVENTION [0011] Under these circumstances, the present inventors conducted diligent research, and as a result, discovered that phase separation automatically occurs when the temperature is lowered, while phase solving does not occur even when the temperature is increased, unless provided with certain physical stimulation, in a solvent mixture where phase solving and phase separation are repeated in a reversible manner, by changing the temperature; accordingly, the two-phase solution is maintained even when the uniform solution within the container is cooled without cooling the container that has been heated in order to make reaction occur, so that the two-phase solution is gained, and after that, the two-phase solution is kept within the container in this heated condition; accordingly, a multi-stage successive reaction process can be carried out while maintaining the temperature of the reaction container, even after the product solution has been removed from the two-phase solution, and as a result, excellent operativity and efficiency in production can be gained; furthermore, according to a method for making a number of processes progress simultaneously using these solvent properties, the respective samples can all be placed under the same conditions in the case where the respective steps of automatic sampling, stirring, inducing reaction and separating are carried out for the same period of time for all of the samples, even when there is a difference between the starting times of the operations that are carried out on the respective samples after a number of reaction containers have been simultaneously heated, so that excellent operativity and reproducibility can be achieved, and thus, the present invention was completed. [0012] That is to say, a first invention provides a method for carrying out a number of processes in a two-phase solution of which the phase state changes as a result of temperature conversion, which is a method for making a number of samples react under the same reaction conditions, wherein these samples are dissolved in a reaction solvent, where the phase state of the solution changes in a reversible manner between a two-phase solution state and a uniform solution state when the temperature fluctuates over or under a certain constant temperature, and processes are carried out sequentially in the respective steps: (A) the constant container heating step, where a number of reaction containers are simultaneously heated, and these reaction containers are maintained at a predetermined temperature; (B) the sample heating step, where samples are automatically put into the heated reaction containers, and the two-phase solution has a predetermined temperature; (C) the reaction step, where the samples that have been heated to the predetermined temperature are stirred, so that uniform solutions are gained, which are maintained in the same state for a predetermined period of time; and (D) the cooling step, where after a predetermined period of time has passed, the uniform solutions are cooled without cooling the reaction containers, so that two-phase solutions are gained within the reaction containers, and wherein the method is characterized in that the successive operation is carried out in such a manner that the period of time (t.sub.B) from the start of sampling to the start of stirring, and the period of time (t.sub.C) from the start of stirring to the start of cooling become the same for all of the samples. [0013] In addition, the present invention provides an apparatus for inducing a number of reaction processes in a two-phase solution where the phase state changes as a result of temperature conversion, having: a heating means for simultaneously heating a number of reaction containers and maintaining the temperature of the reaction containers at a predetermined temperature; an automatic sampling means for putting samples into the reaction containers; a stirring means for stirring the samples within the reaction containers; a cooling means for cooling uniform solutions within the reaction containers without cooling the reaction containers so that two-phase solutions are gained within the reaction containers; and a control means for controlling the time of the start of operation and the time of the stop of the operation in the respective operations: the sampling operation using the sampling means, the stirring operation using the stirring means, and the cooling operation using the cooling means. [0014] In addition, a second invention provides a method for making a two-phase solution of which the phase state changes as a result of temperature conversion react, characterized by having: a reaction step, where a material solution of which the reaction solvent is a solution of which the phase state changes in a reversible manner between a two-phase solution state and a uniform solution state when the temperature fluctuates over or under a certain constant temperature is stirred at a predetermined temperature within a reaction container, so that a uniform solution is gained and reaction occurs; and a cooling step, where the uniform solution is cooled without cooling the reaction container, so that a two-phase solution is gained within the reaction container. [0015] In addition, the present invention provides an apparatus for making a two-phase solution of which the phase state changes as a result of temperature conversion react, characterized by having: a heating means for heating a reaction container; a reaction container with a stimulation means for providing physical stimulation to a material solution within the reaction container so that a uniform solution is gained attached thereto; and a cooling means for cooling a uniform solution within the reaction container without cooling the reaction container. [0016] According to the first invention, a chemical process can be carried out on a number of samples under the same conditions in one processing apparatus. The configuration of the apparatus and the work process become simple, and the apparatus can operate automatically, making it excellent in productivity and reproducibility. In addition, according to the method for making a two-phase solution of which the phase state changes as a result of temperature conversion react of the second invention, cooling and reheating of one reaction container become unnecessary, and the temperature can be maintained constant, and therefore, efficiency in production greatly increases. In addition, after the completion of reaction in one process, the temperature of the reaction solution where the next reaction is to occur in the process becomes quickly constant (heated condition), and therefore, the period of time for the changing of the temperature can be greatly shortened in a multi-stage successive process or the like. BRIEF DESCRIPTION OF THE DRAWINGS [0017] FIG. 1 is a diagram illustrating the respective reaction steps in one sample in accordance with a method for causing reaction in a number of processes according to a first invention; [0018] FIG. 2(A) is a diagram showing the relationship between the time that has passed between the first sample (N=1) and the last sample (N=n), and the response steps in accordance with a method for causing reaction in a number of processes according to the first invention, and FIG. 2 (B) is a diagram showing the relationship between the time that has passed between the first sample (N=1) and the last sample (N=n), and the response steps in accordance with the prior art; [0019] FIG. 3 is a diagram illustrating the respective reaction steps in one sample in accordance with a method for causing reaction in a number of processes according to the prior art; and [0020] FIG. 4 is a schematic diagram illustrating the thesis that a solvent mixture causes phase solving/phase separation. BEST MODE FOR CARRYING OUT THE INVENTION [0021] First, the first invention is described. Continue reading about Method of reacting two-phase solution changing in phase state with temperature change and apparatus for practicing the same... Full patent description for Method of reacting two-phase solution changing in phase state with temperature change and apparatus for practicing the same Brief Patent Description - Full Patent Description - Patent Application Claims Click on the above for other options relating to this Method of reacting two-phase solution changing in phase state with temperature change and apparatus for practicing the same patent application. ###  How KEYWORD MONITOR works... a FREE service from FreshPatents1. Sign up (takes 30 seconds). 2. Fill in the keywords to be monitored. 3. Each week you receive an email with patent applications related to your keywords. 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