阅读说明：本技术 一种连续流反应装置 (Continuous flow reaction device ) 是由 王春 李嫣然 张海彬 卜春坡 何影 胡维洪 曾天宝 钟明 李正强 于 2020-08-25 设计创作，主要内容包括：本发明提供了一种连续流反应装置,包括机架,设置于机架上的温度控制器,设置于机架内的恒温槽,设置于恒温槽内与温度控制器电连接的加热装置,设置于机架上且至少有两个的第一入料口,与第一入料口通过第一管道连接的混合器,与混合器连接的微通道反应器,与微通道反应器连接的固定床反应器,与固定床连接用于输出反应生成物的第二管道；混合器及微通道反应器置于恒温槽内。通过本实例实施,可实现反应实验的研究,反应过程中的换热等效果,使用方便,可有效降低成本,并且,微通道反应器与固定床反应器配合,可进行催化剂的筛选和多相反应等,为进行连续工艺摸索、验证、催化剂筛选等提供了便利,增强连续流反应装置的实用性。(The invention provides a continuous flow reaction device, which comprises a rack, a temperature controller arranged on the rack, a thermostatic bath arranged in the rack, a heating device arranged in the thermostatic bath and electrically connected with the temperature controller, at least two first material inlet ports arranged on the rack, a mixer connected with the first material inlet ports through a first pipeline, a micro-channel reactor connected with the mixer, a fixed bed reactor connected with the micro-channel reactor, and a second pipeline connected with the fixed bed and used for outputting reaction products, wherein the first material inlet port is arranged on the rack; the mixer and the microchannel reactor are arranged in a constant temperature tank. Through this example implementation, can realize the research of reaction experiment, effects such as heat transfer in the reaction process, convenient to use can effectively reduce cost to, microchannel reactor and fixed bed reactor cooperation can carry out screening and heterogeneous reaction etc. of catalyst, for carrying out continuous process groping, verification, catalyst screening etc. provide convenience, reinforcing continuous flow reaction unit's practicality.)

1. A continuous flow reaction device, comprising: the device comprises a rack, a temperature controller arranged on the rack, a thermostatic bath arranged in the rack and used for containing liquid, a heating device arranged in the thermostatic bath and electrically connected with the temperature controller and used for heating the liquid, at least two first feeding ports arranged on the rack, a mixer connected with the first feeding ports through a first pipeline, a microchannel reactor connected with the mixer, a fixed bed reactor connected with the microchannel reactor, and a second pipeline connected with the fixed bed and used for outputting reaction products;

the mixer and the microchannel reactor are arranged in a constant temperature tank.

2. The continuous-flow reaction device of claim 1, wherein: the device comprises a fixed bed reactor, a first microchannel reactor, a second microchannel reactor, a mixer, a first three-way valve, a second three-way valve, a first micro-channel reactor, a second micro-channel reactor, a first three-way valve, a second three-way valve and a third three-way valve.

3. The continuous-flow reaction device of claim 2, wherein: the outside cover of fixed bed reactor is equipped with the outer tube, the interval sets up and vacuole formation between outer tube and the fixed bed reactor, be provided with on the outer tube and be connected the inlet that is used for leading-in liquid and be used for deriving the liquid outlet of liquid with the constant temperature tank, wherein, the inlet passes through the liquid pump and is connected with the constant temperature tank.

4. The continuous-flow reaction device of claim 3, wherein: and the liquid inlet and the liquid outlet are provided with temperature sensors which are electrically connected with a temperature controller and used for detecting temperature.

5. The continuous-flow reaction device of claim 4, wherein: the device still includes the condenser, be provided with the cavity in the condenser, be provided with the condensing medium entry and the condensing medium export that switch on with the cavity on the condenser, be provided with first condenser pipe in the cavity, the one end of first condenser pipe is connected with third pipeline, the other end and the second pipe connection that are used for exporting reaction product.

6. The continuous-flow reaction device of claim 5, wherein: the outside of condenser is provided with the second condenser pipe of being connected with the second pipeline, connect through third three-way valve between second pipeline, first condenser pipe and the second condenser pipe, third pipeline, first condenser pipe, second condenser pipe pass through fourth three-way valve and connect.

7. The continuous-flow reaction device of claim 6, wherein: the device comprises a fixed bed reactor, a first pipeline, a feeding port, a mixer, a first three-way valve, a first micro-channel reactor, a second three-way valve, a first pipeline, a first condensing pipe, a second condensing pipe, a fourth three-way valve, a third pipeline, a first condensing pipe and a second condensing pipe, wherein the first pipeline, the feeding port and the mixer, the first three-way valve, the mixer, the first micro-channel reactor and the second micro-channel reactor, the second three-way valve, the first three-way valve, the second three-way valve, the first condensing pipe and the second three-way valve are connected through clamping sleeves.

8. The continuous-flow reaction device of claim 7, wherein: the device also comprises a preheating ring which is arranged between the first pipeline and the mixer and is respectively connected with the first pipeline and the mixer, and the preheating ring is positioned in the thermostatic bath.

9. The continuous-flow reaction device of claim 8, wherein: be provided with check valve, relief valve and first pressure gauge on the first pipeline, the relief valve is located one side that first pan feeding mouth was kept away from to the check valve, first pressure gauge is located between check valve and the relief valve.

10. The continuous-flow reaction device of claim 9, wherein: and a second pressure gauge and a back pressure valve are arranged on the third pipeline, and the back pressure valve is positioned on one side of the second pressure gauge, which is far away from the condenser.

[ technical field ] A method for producing a semiconductor device

The invention relates to the technical field of chemical equipment, in particular to a continuous flow reaction device.

[ background of the invention ]

Continuous flow microreaction technology is known as a new reaction technology in the chemical and pharmaceutical industry. The continuous flow reaction device refers to a microchannel reactor, a microstructure reactor or a microfluid reaction device and the like, which can enable materials to perform a process in the flowing process, such as chemical reaction, process heat exchange, reaction product separation and the like.

However, the existing continuous-flow microreactor in the market is mainly imported, expensive, single in use function and poor in applicability, and the existing microchannel reactor is not suitable for heterogeneous reaction with a catalyst, so that experiments of a large number of catalytic reactions are limited, research and development of developers are hindered, and the requirements of the developers cannot be met.

Accordingly, the prior art is in need of improvement and development.

[ summary of the invention ]

The invention aims to provide a continuous flow reaction device, which is used for solving the problems of single function and poor applicability of the existing continuous flow microreactor and solving the problem that the existing continuous flow microreactor is not suitable for heterogeneous reaction with a catalyst and hinders developers.

The technical scheme of the invention is as follows: a continuous flow reaction device, comprising: the device comprises a rack, a temperature controller arranged on the rack, a thermostatic bath arranged in the rack and used for containing liquid, a heating device arranged in the thermostatic bath and electrically connected with the temperature controller and used for heating the liquid, at least two first feeding ports arranged on the rack, a mixer connected with the first feeding ports through a first pipeline, a microchannel reactor connected with the mixer, a fixed bed reactor connected with the microchannel reactor, and a second pipeline connected with the fixed bed and used for outputting reaction products;

the mixer and the microchannel reactor are arranged in a constant temperature tank.

Furthermore, the number of the microchannel reactors is two, namely a first microchannel reactor and a second microchannel reactor, the mixer is connected with the first microchannel reactor and the second microchannel reactor through a first three-way valve, and the fixed bed reactor is connected with the first microchannel reactor and the second microchannel reactor through a second three-way valve.

Further, fixed bed reactor's outside cover is equipped with the outer tube, the interval sets up and forms the cavity between outer tube and the fixed bed reactor, be provided with on the outer tube and be connected the inlet that is used for leading-in liquid and be used for deriving the liquid outlet of liquid with the thermostatic bath, wherein, the inlet passes through the liquid pump and is connected with the thermostatic bath.

Furthermore, the liquid inlet and the liquid outlet are provided with temperature sensors which are electrically connected with a temperature controller and used for detecting temperature.

Further, the device still includes the condenser, be provided with the cavity in the condenser, be provided with the condensing medium entry and the condensing medium export that switch on with the cavity on the condenser, be provided with first condenser pipe in the cavity, the one end of first condenser pipe is connected with the third pipeline that is used for exporting reaction products, the other end and second pipe connection.

Further, the outside of condenser is provided with the second condenser pipe of being connected with the second pipeline, connect through the third three way valve between second pipeline, first condenser pipe and the second condenser pipe, third pipeline, first condenser pipe, second condenser pipe pass through the fourth three way valve and connect.

Furthermore, the first pipeline, the feeding port and the mixer, the first three-way valve, the mixer, the first microchannel reactor and the second microchannel reactor, the second three-way valve, the first microchannel reactor, the second microchannel reactor and the fixed bed reactor, the third three-way valve, the second pipeline, the first condenser pipe and the second condenser pipe, and the fourth three-way valve, the third pipeline, the first condenser pipe and the second condenser pipe are all connected through clamping sleeves.

Further, the device also comprises a preheating ring which is arranged between the first pipeline and the mixer and is respectively connected with the first pipeline and the mixer, and the preheating ring is positioned in the thermostatic bath.

Further, a one-way valve, a safety valve and a first pressure gauge are arranged on the first pipeline, the safety valve is located on one side, away from the first feeding port, of the one-way valve, and the first pressure gauge is located between the one-way valve and the safety valve.

Further, a second pressure gauge and a back pressure valve are arranged on the third pipeline, and the back pressure valve is located on one side, far away from the condenser, of the second pressure gauge.

The invention has the beneficial effects that: compared with the prior art, the invention integrates the mixer, the fixed bed reactor, the temperature controller, the thermostatic bath, the heating device and the microchannel reactor into a whole, is convenient to use, and a developer can realize experimental research only by configuring a feed pump, and the heat exchange effect and other effects in the reaction process can effectively reduce the cost.

[ description of the drawings ]

FIG. 1 is a perspective view of a continuous flow reactor according to an embodiment of the present invention.

FIG. 2 is a partial structural view of a continuous flow reactor according to an embodiment of the present invention.

FIG. 3 is a top view of a fixed bed reactor in a continuous flow reactor apparatus according to an embodiment of the present invention.

FIG. 4 is a cross-sectional view of the fixed bed reactor of the continuous flow reactor apparatus of FIG. 3 taken along the direction A-A,

FIG. 5 is a schematic view of a frame of a continuous flow reactor apparatus according to an embodiment of the present invention.

[ detailed description ] embodiments

The invention is further described with reference to the following figures and embodiments.

FIGS. 1-5 are block diagrams of a continuous flow reactor apparatus according to an embodiment of the present invention.

The continuous flow reaction device comprises a frame 10, and a temperature controller 30, a constant temperature tank 13, a heating device (not shown in the figure), a mixer 90, a microchannel reactor, a fixed bed reactor 50, a second pipeline 45 and at least more than two feeding ports 20 which are arranged on the frame 10. Temperature controller 30, pan feeding mouth 20 are located the surface of frame 10, and thermostatic bath 13 is located frame 10 and is used for holding liquid, and heating device sets up in thermostatic bath 13 and is connected the heating device who is used for heating liquid with temperature controller 30 electricity, and blender 90 is connected through first pipeline 21 with pan feeding mouth 20, and fixed bed reactor 50 is connected with microchannel reactor, second pipeline 45 respectively, and blender 90 and microchannel reactor are arranged in thermostatic bath 13.

According to the invention, the mixer 90, the fixed bed reactor 50, the temperature controller 30, the thermostatic bath 13 and the heating device are integrated into a whole, so that the use is convenient, and a developer can realize the research of a reaction experiment and the effects of heat exchange and the like in the reaction process only by configuring a feed pump, so that the cost can be effectively reduced.

In addition, the present invention combines the microchannel reactor with the fixed bed reactor 50, which makes the continuous flow reactor of the present invention more applicable. Specifically, when a reaction experiment is performed between two gases or two liquids, or between a gas and a liquid, but the fixed bed reactor 50 is not required, and a solid reactant or a catalyst in the fixed bed reactor 50 does not affect the reaction between two gases or liquids or gas and liquid, the fixed bed reactor 50 is only equivalent to one pipeline, and a reaction product is led out. When one or two or more of the gas or liquid, or the gas and liquid reactants are reacted with a catalyst or a fixed reactant, the reactants can directly enter the fixed bed reactor 50 through the microchannel reactor to react, i.e., the microchannel reactor is equivalent to a pipe. In addition, when two gases or two liquids, or a gas and a liquid can be reacted in the microchannel reactor, the product generated by the reaction enters the fixed bed reactor 50 to continue reacting with the solid reactant. Therefore, the continuous flow reaction device can carry out catalyst screening and multiphase reaction, and provides convenience for units such as scientific research units, colleges and universities, research centers of fine chemical and pharmaceutical enterprises and the like or researchers to carry out continuous process exploration, verification, catalyst screening and the like.

Specifically, in the present embodiment, the heating device may be a heating coil, oil is preferably used as the liquid in the thermostatic bath 13, and the oil has a wide temperature range, but is not limited thereto, and water and the like may also be used. And two feeding ports 20 are arranged side by side and are used in cooperation with a liquid phase pump or a gas pump to realize the introduction of reactants (liquid or gas) from the feeding ports 20 into the continuous flow reaction device of the present invention.

When different reactants enter from the material inlet 20, the reactants enter the mixer 90 through the first pipeline 21 to be mixed to form a mixture, the mixture enters the microchannel reactor to react, or enters the fixed bed reactor 50 through the microchannel reactor to react with the solid reactants inside the fixed bed reactor or react under the action of the catalyst of the fixed bed reactor, and reaction products generated in the reaction process are collected through the second pipeline 45, so that the reaction experiment is completed. When the continuous flow reaction device is started to use, the temperature controller 30 is started to control the heating device to heat the liquid in the constant temperature tank 13 to the reaction temperature, and the mixer 90 and the microchannel reactor are heated to the temperature required by the reaction. Thus, when the reactants are mixed after passing through the mixer 90 and heated in the mixer 90, the mixture enters the microchannel reactor to fully react or is heated to the reaction temperature by the reactor, and enters the fixed bed reactor 50 to fully react with the solid reactants inside the fixed bed reactor or under the catalyst. Therefore, the reactants realize heat exchange through the constant temperature tank 13, and reach the reaction temperature to facilitate full reaction, thereby increasing the practicability of the continuous flow micro-reaction device.

Specifically, a check valve 22, a safety valve 24 and a first pressure gauge 23 are arranged on the first pipeline 21, the safety valve 24 is located on one side of the check valve 22 away from the feeding port 20, and the first pressure gauge 23 is located between the check valve 22 and the safety valve 24. The third pipe 70 is provided with a second pressure gauge 71 and a back pressure valve 72, and the back pressure valve 72 is located on a side of the second pressure gauge 71 away from the condenser 60. The check valve 22 prevents the reactant introduced from the inlet 20 from flowing backwards, the first pressure gauge 23 and the second pressure gauge 71 are used for detecting pressure, the pressure in the continuous flow reaction device is adjusted through the back pressure valve 72 and the safety valve 24, and a developer can adjust the speed of the fluid in the continuous flow reaction device by himself.

The microchannel reactor and the fixed bed reactor are preferably made of 316L stainless steel or stainless steel materials, have good heat resistance and wide working temperature range, have good corrosion resistance, do not rust, and have high heating and cooling speed, so that research personnel can operate homogeneous-phase and heterogeneous-phase organic chemical synthesis reaction experiments with the temperature of-30 ℃ to 200 ℃ and the pressure of 0-100 bar, but are not limited to liquid-liquid, liquid-solid, gas-liquid-solid and other reaction types, and the exploration is convenient. Wherein, the materials of the microchannel reactor and the fixed bed reactor can also be selected from special alloys, such as hastelloy, titanium alloy and the like, and are not limited herein.

In one embodiment, there are two microchannel reactors, namely a first microchannel reactor 41 and a second microchannel reactor 42, the mixer 90 is connected to the first microchannel reactor 41 and the second microchannel reactor 42 through a first three-way valve 44, and the fixed bed reactor 50 is connected to the first microchannel reactor 41 and the second microchannel reactor 42 through a second three-way valve 43. The invention adopts a first three-way valve 44 to connect the first microchannel reactor 41, the second microchannel reactor 42 and the mixer 90 together, and adopts a second three-way valve 43 to connect the first microchannel reactor 41, the second microchannel reactor 42 and the fixed bed reactor 50 together. Therefore, through the first three-way valve 44 and the second three-way valve 43, a developer can select to use the first microchannel reactor 41 or the second microchannel reactor 42 according to experimental requirements, and when the first microchannel reactor 41 and the second microchannel reactor 42 with different reaction channel sizes are configured, the requirements of the developer on the reaction volumes of different reactors in different reaction experiments can be met. Wherein, the volumes of the reaction channels in the first microchannel reactor 41 and the second microchannel reactor 42 can be respectively 6.5mL and 13mL, and the flux of the continuous flow reaction device can be realized at 0.1-20 mL/min. The volumes of the reaction channels within the first microchannel reactor 41 and the second microchannel reactor 42 are not limited herein.

In one embodiment, the fixed bed reactor 50 is a jacketed fixed bed reactor, and the temperature controller 30 can not only heat the liquid in the thermostatic bath 13 by the heating device, but also provide an external circulation of the heat transfer medium. Namely: an outer tube 51 is sleeved outside the fixed bed reactor 50, a cavity 56 is formed between the outer tube 51 and the fixed bed reactor 50 at intervals, a liquid inlet 54 for leading in liquid and a liquid outlet 52 for leading out the liquid are arranged on the outer tube 51, the liquid inlet 54 is connected with the constant temperature tank 13 through a liquid pump (not shown in the figure) to realize liquid leading-in, and the liquid pump is positioned below the temperature controller 30. Thus, when the connected flow reactor is started to be used, the liquid pump is started to operate, the liquid in the thermostatic bath 13 is introduced into the cavity 56 from the liquid inlet 54, and the liquid in the cavity 56 is filled and then flows back into the thermostatic bath 13 from the liquid outlet 52. Therefore, after liquid or gas enters the fixed bed reactor 50, the temperature is prevented from being reduced, the temperature cannot reach the reaction temperature, the reaction of reactants is not influenced, and the effects of heat preservation and heat exchange are achieved.

In addition, in an embodiment, the liquid inlet 54 and the liquid outlet 52 are provided with temperature sensors 53 electrically connected to the temperature controller 30 for detecting temperatures, so that the temperature of the cavity 56 can be monitored in real time by the temperature controller 30, and the temperature of the liquid in the thermostatic bath 13 can be maintained in real time by the heating device, which is convenient for developers to use.

In an embodiment, the continuous flow reactor further includes a condenser 60, a cavity (not shown) is disposed in the condenser 60, a condensing medium inlet 62 and a condensing medium outlet 61 are disposed on the condenser 60, the cavity is provided with a first condensing pipe (not shown), one end of the first condensing pipe is connected to the third pipe 70, and the other end of the first condensing pipe is connected to the second pipe 45. Wherein, condenser 60 preferentially adopts oil bath or water bath to realize the cooling, can get into the cavity with coolant liquid through external cold water machine of condensing medium entry 62 or running water etc. in the coolant liquid export 61 can be derived and take away the heat in the first condenser pipe with the coolant liquid, realizes the cooling effect. Therefore, when the reaction product is cooled to a safe temperature by the condenser 60 and is led out from the third pipeline 70, the reaction product can be conveniently collected by developers, and the phenomenon that the temperature of the reaction product is too high, so that the developers can not collect the reaction product or harm the developers is prevented.

In one embodiment, a second condensation pipe 65 is disposed outside the condenser 60, the second pipe 45 is connected to the first condensation pipe and the second condensation pipe 65 through a third three-way valve 63, and the first condensation pipe, the second condensation pipe 65 and the third pipe 70 are connected through a fourth three-way valve 64. Thus, the developer can select whether the first condensation pipe or the second condensation pipe 65 is needed in the reaction experiment through the third three-way valve 63 and the fourth three-way valve 64, namely, the water (oil) bath or air condensation mode is selected, so that the selection of the developer is widened, and the requirement of the developer is met.

In one embodiment, the connection between the pipes of the continuous flow reactor of the present invention is a ferrule connection. Namely: the first pipeline 21, the feeding port 20 and the mixer 90, the first three-way valve 44, the mixer 90, the first microchannel reactor 41 and the second microchannel reactor 42, the second three-way valve 43, the first microchannel reactor 41, the second microchannel reactor 42 and the fixed bed reactor 50, the third three-way valve 63, the second pipeline 45, the first condensation pipe and the second condensation pipe 65, and the fourth three-way valve 64, the third pipeline 70, the first condensation pipe and the second condensation pipe 65 are all connected by cutting sleeves. With the ferrule type connection, when the mixer 90, the first microchannel reactor 41, the second microchannel reactor 42, and the like are clogged or otherwise problematic, replacement of these components is facilitated, and connection between the respective components is facilitated.

In one embodiment, the continuous flow reactor further comprises a preheating ring 80 disposed between the first conduit 21 and the mixer 90 and connected to the first conduit 21 and the mixer 90, respectively, the preheating ring 80 being located within the thermostatic bath 13. For preheating the reactants to facilitate the reaction of the mixture at the reaction temperature in the first microchannel reactor 41 or the second microchannel reactor 42. Specifically, the preheating ring 80 is a pipe type and is disposed in a spiral shape.

While the foregoing is directed to embodiments of the present invention, it will be understood by those skilled in the art that various changes may be made without departing from the spirit and scope of the invention.