KR-102960062-B1 - AUTOMATIC CONTINUOUS REACTOR USING PHASE SEPARATION OF REACTION SOLUTION AND AUTOMATIC CONTINUOUS REACTION METHOD USING THE SAME

KR102960062B1KR 102960062 B1KR102960062 B1KR 102960062B1KR-102960062-B1

Abstract

An automatic continuous reactor utilizing layer separation of a reaction solution according to the present invention comprises: a reaction vessel for receiving a reaction solution; an upper piping section including a solvent inlet installed at the top of the reaction vessel for injecting the reaction solution, a gas inlet for injecting an inert gas into the reaction vessel to form internal pressure, and a gas outlet for discharging internal gas; a discharge pipe extending from the top to the bottom of the reaction vessel, comprising a first discharge port provided at the bottom inside the reaction vessel and a second discharge port provided at the top outside the reaction vessel; at least one sensor installed in the discharge pipe for detecting a change in the characteristics of the discharged reaction solution; and a discharge shut-off valve installed upstream of the sensor in the discharge pipe for opening and closing the discharge pipe in response to a detection signal output based on the change in characteristics detected by the sensor, wherein the lower reaction solution with a higher specific gravity is discharged first through the first discharge port due to the differential pressure between the pressure inside the reaction vessel and the second discharge port, and the detection signal is output according to the detection of the boundary surface between the lower reaction solution and the upper reaction solution with a lower specific gravity.

Inventors

이한기
이상근
김민규
김상호

Assignees

주식회사 케이씨인더스트리얼

Dates

Publication Date: 20260507
Application Date: 20251202

Claims (20)

In an automatic continuous reactor utilizing layer separation of the reaction solution, A reaction vessel for holding a reaction solution; An upper piping section including a solvent inlet installed at the top of the reaction vessel for injecting a reaction liquid, a gas inlet for injecting an inert gas into the reaction vessel to form internal pressure, and a gas outlet for discharging internal gas; A first discharge port provided in the inner lower part of the reaction vessel and a second discharge port provided in the outer upper part of the reaction vessel, wherein a discharge pipe extending from the upper part to the lower part of the reaction vessel; At least one sensor installed in the discharge pipe to detect changes in the characteristics of the discharged reaction liquid; and It includes a discharge shut-off valve installed upstream of the sensor of the discharge pipe and opening and closing the discharge pipe in response to a detection signal output based on a characteristic change detected by the sensor, Due to the differential pressure between the pressure inside the reaction vessel and the second outlet, the lower reaction liquid with a heavier specific gravity is discharged first through the first outlet, and An automatic continuous reactor in which the above detection signal is output upon detection of the interface between the lower reaction layer and the upper reaction layer with a lighter specific gravity.
In paragraph 1, The above reaction vessel is made of a non-magnetic material, and An automatic continuous reactor, wherein an electromagnet capable of activation and deactivation is further coupled to the lower outer side of the reaction vessel to fix a magnetic metal catalyst to the bottom of the reaction vessel when the reaction liquid is discharged.
In paragraph 1, An automatic continuous reactor in which the bottom of the reaction vessel includes a ramp inclined toward the first outlet.
In paragraph 1, An automatic continuous reactor further comprising an orifice valve at the downstream end of the sensor of the discharge pipe to regulate the discharge flow rate to improve the sensing accuracy of the sensor.
In paragraph 1, An automatic continuous reactor further comprising, at the downstream end of the sensor of the discharge pipe, a backpressure regulator that maintains a constant pressure inside the discharge pipe and fills the section where the sensor is installed with a solution.
In paragraph 1, The sensor includes a specific gravity sensing sensor installed on the discharge pipe located outside the reaction vessel, wherein The above specific gravity sensing sensor detects a change in specific gravity at the interface between the lower reaction layer and the upper reaction layer, in an automatic continuous reactor.
In paragraph 1, The sensor comprises a conductivity sensing sensor installed on the discharge pipe located outside the reaction vessel, wherein An automatic continuous reactor in which the conductivity sensing sensor detects a change in conductivity at the interface between the lower reaction layer and the upper reaction layer.
In paragraph 1, The above sensor includes a specific gravity sensing sensor and a conductivity sensing sensor installed on the discharge pipe located outside the reaction vessel, An automatic continuous reactor in which the above-mentioned specific gravity sensing sensor and the above-mentioned conductivity sensing sensor are positioned at different heights along the discharge pipe.
In paragraph 1, An automatic continuous reactor further comprising an impeller provided inside the reaction vessel to stir the reaction liquid.
In paragraph 1, At the rear end of the sensor of the above discharge pipe The system further includes a first flow path switching valve that switches the flow path direction between a discharge flow path directed toward the second discharge port and a recovery flow path into which an inert gas is injected for the recovery of the upper reaction liquid, wherein The above-mentioned first Euro switching valve is, An automatic continuous reactor configured to recover the upper reaction liquid in the discharge pipe to the reaction vessel by the pressure of an injected inert gas, after the upper reaction liquid is detected by the sensor and the discharge shut-off valve is closed, then switched to the recovery flow path and the discharge shut-off valve is opened.
In Paragraph 10, The above upper piping part The apparatus further includes a second flow path switching valve for switching the flow path direction between a first flow path connected to the gas outlet and a second flow path connected to the gas inlet, and a third flow path switching valve for switching the flow path direction between the first flow path direction and a third flow path connected to the solvent inlet. The above-mentioned second Euro switching valve and third Euro switching valve are, An automatic continuous reactor configured such that, when recovering the upper layer reaction liquid remaining in the discharge pipe, the inside of the reaction vessel is opened in the direction of the first flow path so as to communicate with the gas outlet, thereby discharging the internal pressure of the reaction vessel.
In Paragraph 11, The apparatus further includes a control unit that controls the operation of the discharge shut-off valve, the first flow path switching valve, the second flow path switching valve, and the third flow path switching valve based on a detection signal received from the sensor, The above control unit controls the discharge shut-off valve to be closed when the boundary surface is detected by the sensor, and after the discharge shut-off valve is closed, to switch the first flow path switching valve to the recovery flow path direction to recover the upper reaction liquid remaining in the discharge pipe, to open the second flow path switching valve and the third flow path switching valve to the first flow path direction to lower the internal pressure of the reaction vessel, and to open the discharge shut-off valve.
In an automatic continuous reaction method utilizing layer separation of a reaction solution performed by a continuous reactor, (a) receiving a reaction solution into the reaction vessel through a solvent inlet of an upper piping section provided in the reaction vessel; (b) a step of forming pressure inside the reaction vessel by injecting an inert gas through a gas inlet provided in the upper piping section; (c) a step of discharging a lower reaction liquid with a heavy specific gravity through a first outlet provided at the lower inner part of the reaction vessel by utilizing the differential pressure between the pressure inside the reaction vessel and a second outlet provided at the upper outer part; (d) a step of detecting a change in the characteristics of the discharged reaction liquid by a sensor installed in a discharge pipe extending from the top to the bottom of the reaction vessel and including the first discharge port and the second discharge port; and (e) A method for automatic continuous reaction that includes the step of, when the sensor detects the interface between the lower reaction liquid and the upper reaction liquid with a lower specific gravity and outputs a detection signal, blocking a discharge shut-off valve installed upstream of the sensor of the discharge pipe in response to the detection signal to stop the discharge.
In Paragraph 13, Prior to step (c) above, The method further includes the step of activating an electromagnet at the bottom of the reaction vessel to fix a magnetic metal catalyst, and After the above (e) step, An automatic continuous reaction method comprising the additional step of deactivating the electromagnet to release the fixation of the catalyst.
In Paragraph 13, Prior to the above (b) step, An automatic continuous reaction method comprising the step of further including the step of discharging internal gas through a gas outlet provided in the upper piping section to bring the inside of the reaction vessel to an atmospheric pressure state.
In Paragraph 13, The above step (c) is, An automatic continuous reaction method performed by controlling the flow rate to a constant level through an orifice valve provided at the downstream end of the sensor of the discharge pipe.
In Paragraph 13, Steps (c) and (d) above are, An automatic continuous reaction method performed by maintaining a constant internal pressure through a backpressure regulator provided at the downstream end of the sensor of the discharge pipe, while filling the section where the sensor is installed with a solution.
In Paragraph 13, After step (a) above, An automatic continuous reaction method comprising the step of driving an impeller inside the reaction vessel to stir the reaction liquid.
In paragraph 15, After the above (e) step, A step of switching the flow direction of a first flow switching valve provided at the downstream end of the sensor of the discharge pipe from a discharge direction toward the second discharge port to a recovery flow direction in which an inert gas is injected for the recovery of the upper reaction liquid, and An automatic continuous reaction method comprising the additional step of opening the discharge shut-off valve and injecting an inert gas to recover the upper reaction liquid remaining in the discharge pipe into the reaction vessel.
In Paragraph 19, The step of recovering the upper reaction solution is, An automatic continuous reaction method performed by opening the second and third flow switching valves provided in the upper piping section in the direction of the first flow path communicating with the gas outlet, thereby releasing the internal pressure of the reaction vessel.

Description

AUTOMATIC CONTINUOUS REACTOR USING PHASE SEPARATION OF REACTION SOLUTION AND AUTOMATIC CONTINUOUS REACTION METHOD USING THE SAME The present invention relates to an automatic continuous reactor utilizing layer separation of a reaction solution and an automatic continuous reaction method using the same. Chemical reactions performed under high temperature and pressure conditions are widely utilized in industry and research, and post-processing of products, residual reactants, and catalysts is essential after the reaction is completed. In particular, in multiphase reaction systems with differences in specific gravity, component separation and recovery through phase separation are required after the reaction ends. However, conventional high-pressure reactors are designed to require dismantling after the reaction is complete to perform layer separation and subsequent processing, which has resulted in problems such as reactant loss due to exposure to the outside air during the repetitive assembly and disassembly process, operational risks under high temperature and pressure conditions, waste of time and energy, and reduced reproducibility due to inconsistencies in experimental conditions. For example, in phase-separating reactions such as deuterium substitution reactions, liquid phases with different specific gravities, such as D₂O (heavy water) and benzene, are produced. It was common practice to dismantle the reactor and transfer the mixture into a pipette or glass container to separate them. This method caused a decrease in the recovery rate of metal catalysts and some loss of the reaction solution, which significantly reduced the efficiency of the continuous reaction process. Furthermore, in conventional technology, the absence of an automated system capable of detecting or selectively discharging the components of the reaction solution meant that the entire process was performed manually, which acted as one of the major causes hindering the reliability of experimental results and productivity. FIG. 1 is a cross-sectional view showing an automatic continuous reactor using layer separation of a reaction solution according to one embodiment of the present invention. FIG. 2 is a drawing for explaining the configuration and operational use of an inclined ramp, a discharge port, and an electromagnet used in the reaction liquid discharge process according to one embodiment of the present invention. Figure 3 is an enlarged view of the sensor and valve configuration on the discharge pipe shown in Figure 1. FIG. 4 is a flowchart illustrating an automatic continuous reaction method using layer separation of a reaction liquid performed by an automatic continuous reactor according to another embodiment of the present invention. The present invention will be described in detail below with reference to the attached drawings. However, the present invention may be embodied in various different forms and is not limited to the embodiments described herein. Furthermore, the attached drawings are intended only to facilitate understanding of the embodiments disclosed in this specification, and the technical concept disclosed in this specification is not limited by the attached drawings. In order to clearly explain the present invention in the drawings, parts unrelated to the explanation have been omitted, and the size, form, and shape of each component shown in the drawings may be varied in various ways. Identical or similar parts throughout the specification are denoted by identical or similar reference numerals. Suffixes such as "module" and "part" for components used in the following description are assigned or used interchangeably solely for the sake of ease of drafting the specification, and do not inherently possess distinct meanings or roles. Furthermore, in describing the embodiments disclosed in this specification, detailed descriptions of related prior art have been omitted where it is determined that such detailed descriptions could obscure the essence of the embodiments disclosed in this specification. Throughout the specification, when it is stated that a part is "connected (connected, contacted, or coupled)" to another part, this includes not only cases where they are "directly connected (connected, contacted, or coupled)," but also cases where they are "indirectly connected (connected, contacted, or coupled)" with other members interposed therebetween. Furthermore, when it is stated that a part "includes (provides, or provides)" a certain component, this means that, unless specifically stated otherwise, it does not exclude other components but rather allows for additional "included (provided, or provided)" of other components. Terms indicating ordinal numbers, such as first, second, etc., used in this specification are used solely for the purpose of distinguishing one component from another and do not limit the order or relationship of the components. For example, the first component of the present invention may be