KR200316911Y1 - High-temperature and high-pressure parallel micro reactor for high-throughput screening - Google Patents

Abstract

The present invention relates to a parallel reactor, and more particularly, to a high temperature and high pressure parallel micro reactor capable of high speed performance evaluation.

To this end, the parallel reactor according to the present invention is a fixed frame, a plurality of reaction tanks installed in parallel to the fixed frame to accommodate the reactants, a gas injection unit for receiving the gas to be injected into the reactor, a solvent containing the solvent to be injected into the reactor It is characterized in that it comprises an injection unit, a stirrer which is installed on the movable frame to be movable up and down in the fixed frame and a controller for agitating the reactants in the reaction tank and connected to each reaction tank to control the internal pressure and temperature.

Description

HIGH-TEMPERATURE AND HIGH-PRESSURE PARALLEL MICRO REACTOR FOR HIGH-THROUGHPUT SCREENING}

The present invention relates to a parallel reactor, and more particularly, to a high temperature and high pressure parallel micro reactor capable of high speed performance evaluation.

High-speed performance evaluation is a part of high-speed research technique using combinatorial technology along with high density library preparation, high density library sample synthesis and high speed characterization. Combination technology is a high-speed research technique that enables the development of new materials inexpensively, quickly and successfully by making many combination research samples at a low cost and measuring and evaluating their characteristics and performance at high speed. It consists of applied research.

In order to develop high-performance, high-efficiency new materials such as advanced functional chemical materials, a number of experiments must be conducted under various reaction conditions.

In the conventional case, since the experiment was performed in a single reactor, and the reaction conditions were to be changed every time the reaction conditions were different, there was a disadvantage in that a long time was required to find an appropriate material.

In addition, in general, a single reactor requires a pressure regulator and a mass flow rate sensor to be installed in each line into which the reaction gas is injected, which is expensive to install, and in the case of using a plurality of reactors, each reactor is operated, controlled and checked separately. There was a complicated downside to doing this.

In addition, since a conventional single reactor has a capacity of 100 cc or more, the minimum amount of solvents and reactants required for the experiment is not small. Therefore, when a large number of experiments are required to develop a new material, the economic loss is large. It causes more problems with damage.

In addition, when only a single reactor is used in accordance with the reaction conditions of the conventional wide space is required, there is a disadvantage that can not be appropriate experiment in a narrow space.

The present invention has been proposed in view of the above problems, and an object of the present invention is to provide a high temperature and high pressure parallel micro reactor capable of high speed performance evaluation.

Another object of the present invention is to provide a parallel reactor that can simultaneously perform experiments of different conditions in a narrow space.

Another object of the present invention is to provide a parallel reactor with low installation cost and easy operation.

1 is a front view of a parallel reactor according to an embodiment of the present invention.

2 is an enlarged schematic cross-sectional view of the reactor of FIG.

3 is an enlarged cross-sectional view of the reactor and the stirrer of FIG.

Figure 4 is a perspective view of the combination of the reactor and agitator of Figure 1;

Figure 5 is a perspective view of the combined reactor and agitator of Figure 4 combined.

6 is a perspective view of the reactor of FIG.

7 is a plan view of the parallel reactor of FIG.

8 is a schematic rear view of a parallel reactor according to an embodiment of the present invention.

9 is a state diagram used in the parallel reactor of FIG.

<Description of the symbols for the main parts of the drawings>

10: fixed frame 12: moving frame

14: lifting device 20: reactor

22: container 24: holder

26: flange 27: first coupling portion

28: packing 30: reactant inlet

32: gas injection portion 34: solvent injection portion

40: stirrer 42: cover

44: gear 50: clip

52: second coupling portion 56: screw

60: control unit 62: temperature control unit

64: pressure controller 66: speed controller

68: pressure gauge 69: vacuum gauge

70: temperature controller 72: heater

74: temperature sensor 80: pressure control unit

82: pressure transducer 84: solenoid valve

90: gas supply pipe 92: gas injection valve

94: vacuum valve 96: gas exhaust valve

100: electric motor

In order to achieve the above object, the parallel reactor according to the present invention is a fixed frame, a plurality of reaction vessels installed in parallel to the fixed frame to accommodate the reactants, reactant injection unit connected to the reaction tank to inject the reactants into the reaction tank It may include a control unit is installed in the movable frame to be elevated in the fixed frame, the agitator for stirring the reactants in the reaction tank and the reaction conditions in the reaction tank connected to each reaction tank.

The reactor may be detachably fixed to the receiving vessel in which the reactants are accommodated, and the reactor may be formed of a heat insulating material so as not to be affected by the external temperature.

The upper end of the reactor is provided with a flange, the lower end of the stirrer is provided with a cover corresponding to the flange, the flange and the cover may be coupled by a clip. A first coupling part is formed at one side of the flange, and a second coupling part coupled to the first coupling part may be formed at the clip.

A packing may be installed between the cover and the flange to maintain an airtight state.

Each of the reactors may be provided with a heater for heating the reactor and a temperature sensor for measuring the temperature therein, the gas injection portion of the reactant injection portion to adjust the pressure of the reaction vessel PRESSURE TRANSDUCER AND SOLENOID VALVE CAN BE CONNECTED.

The stirrers may be driven by one electric motor, and gears are installed on an upper end of each stirrer, and the respective gears may be engaged with each other when the electric motors are driven.

The control unit may be composed of a temperature control unit for controlling the temperature inside each reactor, and a pressure control unit for controlling the pressure therein.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

First, in adding reference numerals to the components of each drawing, it should be noted that the same components and the like have the same reference numerals as much as possible even if displayed on different drawings. In addition, in the following description of the present invention, if it is determined that a detailed description of a related known function or configuration may unnecessarily obscure the subject matter of the present invention, the detailed description thereof will be omitted.

Meanwhile, the parallel reactor according to the present invention has been described as being used in, for example, a polymerization reaction, but is not limited thereto.

1 is a front view of a parallel reactor according to an embodiment of the present invention, FIG. 2 is an enlarged schematic cross-sectional view of the reactor of FIG. 1, and FIG. 8 is a schematic rear view of a parallel reactor according to an embodiment of the present invention.

As shown in Figure 1, the parallel reactor according to an embodiment of the present invention, the fixed frame 10, the moving frame 12, the lifting device 14, the reaction vessel 20, the reactant injection unit 30, the stirrer 40, a clip 50, a control unit 60, a temperature control unit 70, a pressure control unit 80, a gas supply pipe 90, and an electric motor 100.

The fixed frame 10 is a basic frame that becomes the skeleton of the reactor, the reaction vessel 20 is installed in parallel.

The moving frame 12 is a frame installed to be moved up and down by a predetermined stroke with respect to the fixed frame 10, the agitator 40 is installed in parallel.

The lifting device 14 uses a pneumatic lifting device as a device for moving the moving frame 12 up and down with respect to the fixed frame 10.

The reaction vessel 20 is a place where the reactions are received by receiving the reactants injected from the outside, the container 22, the holder 24, the flange 26, the first coupling portion 27, the packing 28 It is composed.

The reactor 20 is formed of a heat insulating material so as not to be affected by the external temperature, in particular, the temperature of the reaction tank 20 disposed on the side, can be formed in a round shape in consideration of the ease of processing, to reduce the volume, etc. Both sides can be cut.

The container 22 is a container in which the reactants are directly received and is detachably fixed to the reactor 20.

As shown in FIG. 2, the container 22 is fixed to the reactor 20 by the holder 24. It is preferable to use a glass vial for the container 22, and in consideration of spatial and economic aspects, it is preferable to use a glass bottle having a capacity of 10 cc to 50 cc.

The holder 24 is a means for fixing the container 22 to the reactor 20 to prevent rotation of the container 22 under high temperature and high pressure reaction such as a polymerization reaction, and resistant to high temperature and high pressure and chemicals. It is preferably formed of a material such as Teflon.

The flange 26 is a lug portion formed at an upper end of the reactor 20 for connection between the reactor 20 and the stirrer 40, and is coupled to the second coupling part 52 formed in the clip 50. The first coupling portion 27 is formed.

The packing 28 is a means for mounting to maintain an airtight state between the cover 42 and the flange 26, and is provided between the reactor 20 and the stirrer 40.

6 is a perspective view of the reactor of FIG. 1.

As shown in Figure 6, in the parallel reactor according to an embodiment of the present invention, the packing 28 is inserted into the top of the reactor 20 with a rubber ring, considering the high temperature and high pressure and chemical resistance Viton rubber ring was used.

The reactant injector 30 is a part for injecting reactants into the reactor 20, and includes a gas injector 32 and a solvent injector 34.

The gas injection unit 32 is installed at one side of the reaction tank 20 to inject the reaction gas into the reaction tank 20, and the solvent injection unit 34 is installed at one side of the stirrer 40. It is a part for injecting a reaction solvent into the reactor 20.

The stirrer 40 is a device installed in the moving frame 12 to agitate the reactants in the reaction vessel 20, it is composed of a cover 42, a gear 44, a magnet drive is included therein.

The cover 42 is formed at a lower end of the stirrer 40 to connect the stirrer 40 and the reaction tank 20, and is formed in a shape corresponding to the flange 26.

The gear 44 is provided on the stirrer 40 as a part for transmitting the power of the electric motor 100 to the stirrer 40.

7 is a plan view of the parallel reactor of FIG.

As shown in FIG. 7, the gear 44 is interlocked so that the plurality of stirrers 40 are simultaneously operated by one electric motor 100.

4 is a perspective view of a combination of the reaction tank and the stirrer of Figure 1, Figure 5 is a perspective view of a combination of the reaction vessel and agitator of Figure 4 combined.

As shown in FIGS. 4 and 5, the clip 50 is a fixture used to fix the flange 26 and the cover 42, and includes a second coupling part 52 and a screw groove 54. And a screw 56.

The second coupling portion 52 is a portion that is coupled to the first coupling portion 27 of the flange 26 to increase the fixing force. The first coupling portion 27 is formed as a groove portion, and the second coupling portion 52 is formed as a protrusion inserted into the groove portion, but may be formed in the opposite shape.

The screw 56 is fastened to the screw groove 54 to fix the flange 26 and the cover 42 by the clip 50.

The control unit 60 is a part for controlling the reaction conditions of the respective reaction tank 20, the temperature control unit 60, the pressure control unit 60, the speed control unit 60, the pressure gauge 68, the vacuum gauge 69 It is composed of

The temperature control unit 60 and the pressure control unit 60 are portions that control the temperature and the pressure inside the reactor 20, respectively, and are installed at one side of the fixed frame 10.

The temperature control unit 60 and the pressure control unit 60 are designed to input and confirm the temperature and pressure set values of the corresponding reaction tanks 20, respectively, by a computer program or manually.

The speed control unit 60 is a part for controlling the rotational speed of the agitator 40, is installed on one side of the fixed frame 10, it can be controlled by a computer or manually.

The pressure gauge 68 is a part capable of checking the pressure inside the gas supply pipe 90, and the vacuum gauge 69 is a part capable of checking an internal pressure of a vacuum tube (not shown). ) It is installed on one side.

The temperature control unit 70 is a part for adjusting the temperature inside each reactor 20 according to the operation of the temperature control unit 60, it is composed of a heater 72 and a temperature sensor 74.

3 is an enlarged cross-sectional view of the reactor and the stirrer of FIG.

As shown in Figures 2 and 3, the heater 72 is a means for heating the reactor 20, in the present invention, four cartridge heaters 72 are arranged 90 symmetrically from the center.

The temperature sensor 74 is a portion for detecting the temperature inside the reaction vessel 20, using a thermocouple, in order to reduce the temperature difference according to the thickness of the receiving container 22 to the receiving container 22 as much as possible Installed closely.

The pressure regulator 80 is a portion for adjusting the pressure in each reactor 20 according to the operation of the pressure controller 60, it is composed of a pressure transducer 82 and a solenoid valve 84.

8 is a schematic rear view of a parallel reactor according to an embodiment of the present invention.

As shown in FIG. 8, the pressure transducer 82 detects a pressure change in the reactor 20 and returns the pressure control unit 60 to the pressure controller 60, and is connected to each reactor 20.

The solenoid valve 84 is a part for adjusting the gas filled in the gas supply pipe 90 to supply the respective reaction tank 20, is connected to the gas supply pipe 90 and the pressure transducer 82 have.

The gas supply pipe 90 is a gas-filled pipe for supplying a reaction gas to the reactor 20, and is configured to supply gas to a plurality of reactors 20 using a single gas supply pipe 90. .

Hereinafter, a process of using a parallel reactor according to the present invention will be described with reference to the drawings.

9 is a state diagram used in the parallel reactor of FIG.

As shown in Figure 9, the parallel reactor according to the present invention is the bar is moved after the moving frame 12 is fixed to the stirrer 40 and the reactor 20 by the clip 50, the reaction proceeds , By dividing the steps into a starting point of the state in which the reactor 20 and the stirrer 40 are not coupled.

In the first step (S10), the lifting device 14 is operated to raise the movable frame 12 by the stroke distance.

In the second step (S20), the receiving vessel 22 is fixed to the reaction vessel 20.

In the third step (S30), the lifting device 14 is operated to lower the movable frame 12 such that the flange 26 of the reactor 20 and the cover 42 of the agitator 40 abut.

In the fourth step S40, the flange 26 and the cover 42 are fixed with the clip 50.

In a fifth step S50, the inside of the reaction tank 20 is vacuum cleaned.

In the sixth step (S60), the reactor 20 is filled with nitrogen.

The seventh step S70, the fifth step and the sixth step are repeated three to four times.

In the eighth step (S80), while reacting nitrogen in the reaction tank 20, a reactant such as a solvent or a catalyst is injected into the solvent injection unit 34.

In a ninth step (S90), a vacuum is applied to the reactor 20 to remove nitrogen in the reactor.

In the tenth step S100, the reaction gas is injected into the reaction tank 20 at a predetermined temperature and pressure.

In an eleventh step S110, the electric motor 100 is driven to rotate the stirrers 40 at a predetermined rotation speed.

In the twelfth step (S120), after completion of the reaction, the pressure in each reactor 20 is reduced to atmospheric pressure.

In a thirteenth step S130, the clip 50 is released and the movable frame 12 is raised.

In the fourteenth step (S140), the container 22 is separated from the reactor 20.

Since the reaction gas is a gas such as ethylene or propylene in the tenth step S100, the reaction gas is dissolved in the solvent injected in the eighth step S80. In this case, the internal pressure of the gas supply pipe 90 is displayed on the pressure gauge 68.

The pressure inside each reactor 20 is confirmed by the pressure transducer 82 and transmitted to the pressure control unit 64.

When the pressure decreases as the reaction proceeds by rotating the stirrer 40 in the eleventh step S110, the pressure transducer 82 senses it and transmits it to the pressure controller 64. Accordingly, when the solenoid valve 84 is opened, and the desired pressure is reached, the pressure transducer 82 senses it and transmits it to the pressure control unit 64 to close the solenoid valve 84 to close the pressure in the reactor 20. Keep it constant.

The above embodiments are intended to specifically illustrate the present invention, and do not limit the scope of the present invention. In addition, it can be seen that all simple modifications or changes of the present invention are included in the scope of the present invention.

According to the parallel reactor according to the present invention as described above, it is possible to provide a parallel reactor capable of easy operation and high-speed performance evaluation by simultaneously connecting a plurality of reactors and reacting at the same time.

In addition, in the conventional single reactor, in order to detect the amount of reaction gas, an expensive and large-area pressure regulator (MASS FLOW SENSOR) has to be installed for each line into which the reaction gas is injected. The reactor uses an inexpensive, narrow-area pressure transducer and solenoid valve, which is very advantageous in terms of economy and space.

In addition, the use of a small capacity container is inserted into a plurality of reactors connected in parallel with the conventional single reactor, so that the number of experiments can be performed simultaneously with a small amount of reactants, thereby reducing environmental problems. .

In addition, the container is detachably fixed to the reactor, so to clean the reactor, only take out the container and wash it, simply shake off the lower part of the stirrer and perform the next experiment immediately. have.

In addition, the parallel reactor according to the present invention provides a combined reactor that is stably fixed even under a high temperature and high pressure environment inside the reactor by connecting the stirrer and the reactor using a clip having a separate coupling portion.

In addition, since the reaction tank is composed of a heat insulating material, heat transfer between adjacent reactors is prevented, thereby obtaining an accurate reaction result.

Claims (12)

Fixed frame; A plurality of reactors installed in parallel on the fixed frame to accommodate reactants; A reactant injection unit connected to the reactor to inject the reactants into the reactor; An agitator installed in the movable frame to be movable up and down on the fixed frame to agitate the reactants in the reactor; And A parallel reactor connected to each reactor, the controller comprising a reaction condition inside the reactor. The parallel reactor according to claim 1, wherein the reactor is detachably fixed to a receiving container in which the reactants are accommodated. The parallel reactor according to claim 2, wherein the reactor is formed of a heat insulating material so as not to be influenced by an external temperature. The parallel reactor of claim 1, wherein a flange is provided at an upper end of the reactor, and a cover corresponding to the flange is provided at a lower end of the agitator, and the flange and the cover are coupled by a clip. The parallel reactor of claim 4, wherein a first coupling part is formed at one side of the flange, and the second coupling part is coupled to the first coupling part. The parallel reactor according to claim 5, wherein a packing is provided between the cover and the flange to maintain an airtight state. The parallel reactor according to claim 1, wherein each reactor is provided with a heater for heating the reactor and a temperature sensor for measuring a temperature therein. The parallel reactor of claim 1, wherein a pressure converter and a solenoid valve for controlling the pressure of the reactor are connected to the gas injection part into which the gas is injected. The parallel reactor of Claim 1, wherein the stirrers are driven by one electric motor. The parallel reactor of claim 9, wherein gears are provided on an upper end of each stirrer, and the gears interlock with each other when the electric motor is driven. The parallel reactor according to claim 1, wherein the control unit comprises a temperature control unit for controlling a temperature inside each reactor and a pressure control unit for controlling a pressure therein. The parallel reactor of claim 11, wherein the controller further comprises a speed controller configured to control the rotational speed of the stirrers.