CN211636461U - Gas replacement and introduction synthesis reaction device - Google Patents
Gas replacement and introduction synthesis reaction device Download PDFInfo
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- CN211636461U CN211636461U CN202020065304.7U CN202020065304U CN211636461U CN 211636461 U CN211636461 U CN 211636461U CN 202020065304 U CN202020065304 U CN 202020065304U CN 211636461 U CN211636461 U CN 211636461U
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Abstract
The utility model relates to a chemical reaction technical field discloses a gas displacement that gas consumption is little and reaction rate is very fast, lets in synthetic reaction unit, include through pipeline sealing connection's reaction vessel, accuse pressure gas holder, air current controller, at least one take out/exhaust pump and at least one gas concentration sensor to and programmable logic controller. The gas concentration sensor is used for detecting the oxygen concentration value or the water vapor concentration value of the gas in the reaction container and the pressure control gas storage tank; the programmable logic controller is respectively connected with the gas flow controller and the gas concentration sensor communication interface; the gas concentration sensor feeds back the acquired oxygen concentration value or water vapor concentration value to the programmable logic controller, and compares the oxygen concentration value or water vapor concentration value with a preset value of the programmable logic controller; and if the oxygen concentration value or the water vapor concentration value is less than or equal to a preset value, automatically switching the working mode of gas replacement or gas introduction by the programmable logic controller.
Description
Technical Field
The utility model relates to a chemical reaction technical field, more specifically say, relate to a gas replacement, synthetic reaction unit who lets in.
Background
In organic synthesis reactions, strict anhydrous and anaerobic conditions are a necessary condition. Currently, there are two common methods: the glove box is characterized in that a closed inert atmosphere is created, and the whole reaction process or the weighing and feeding of the reaction are placed in the glove box; the other is the Schlenk technology, air in a reaction system is replaced by inert gas through the pumping and exchanging air control of a double-calandria.
However, in the two methods, the former method is limited by the volume of the glove box and is not suitable for large-scale synthesis reaction; the latter relies on the manual regulation and control many times of the double-calandria, except needing to equip the specialized gas supply system, still need to equip with the mechanical pump or diaphragm pump with drying, except that acid, absorbing organic gas, it is relatively tedious to set up, maintain, operate the complete set of apparatus; on the other hand, some synthesis reactions require the introduction of gaseous reactants at atmospheric pressure or slightly above, such as carbon monoxide, carbon dioxide, oxygen or hydrogen, and are currently often fed by bubbling small gas streams through or introducing gas bags.
However, the bubbling method consumes a large amount of energy, and causes certain pollution and danger when carbon monoxide or carbon dioxide is used; when oxygen or hydrogen is used, there is a risk of explosion. The air bag access mode has high safety, but causes gas-liquid two-phase reaction, gas can only be slowly dissolved in a reaction solvent to react, and the reaction speed is low and the efficiency is low.
Therefore, how to reduce the consumption of gas and improve the reaction efficiency is a technical problem that needs to be solved by those skilled in the art.
Disclosure of Invention
The to-be-solved technical problem of the utility model lies in, to the above-mentioned current reaction unit gas consumption of prior art big and the slow defect of reaction rate, provide a gas consumption little and the faster gas replacement of reaction rate, the synthetic reaction unit who lets in.
The utility model provides a technical scheme that its technical problem adopted is: a synthesis reaction apparatus for gas replacement and introduction is constructed, and the apparatus comprises:
a reaction vessel configured as a closed reaction vessel of a hollow structure for containing a compound to be reacted and a reaction solvent;
the pressure control gas storage tank is a closed gas bin with a hollow structure and is used for storing protective gas or reaction gas required by reaction; the gas outlet of the pressure-control gas storage tank is hermetically communicated with the gas flow controller and the reaction container through pipelines;
at least one pumping/exhausting pump, wherein the air inlet of the pumping/exhausting pump is hermetically communicated with the airflow controller, the reaction container and the pressure control air storage tank through pipelines,
the pumping/exhausting pump is used for pumping and exhausting air in the reaction container, the pressure-control air storage tank and the airflow controller in a gas replacement working mode, and is used for pumping protective or reaction gas in the pressure-control air storage tank into the reaction container in a flowing mode or a bubbling mode in a gas introducing reaction mode;
the detection end of the gas concentration sensor is arranged in a pipeline communicated with the reaction container or in the pressure control gas storage tank, and the gas concentration sensor is used for detecting the oxygen concentration value or the water vapor concentration value of the gas in the reaction container and the pressure control gas storage tank;
the programmable logic controller is respectively connected with the communication interfaces of the pumping/exhausting pump, the gas flow controller and the gas concentration sensor; wherein the content of the first and second substances,
the gas concentration sensor feeds back the acquired oxygen concentration value or water vapor concentration value to the programmable logic controller, and the oxygen concentration value or water vapor concentration value is compared with a preset value of the programmable logic controller;
and if the oxygen concentration value or the water vapor concentration value is less than or equal to the preset value, the programmable logic controller automatically switches the working mode of gas replacement or gas introduction.
In some embodiments, the gas concentration sensor comprises an oxygen concentration sensor and a water vapor concentration sensor,
the oxygen concentration sensor and the water vapor concentration sensor are respectively connected with the communication interface of the programmable logic controller;
the oxygen concentration sensor is used for detecting the oxygen concentration values of the reaction container and the pressure control gas storage tank,
the water vapor concentration sensor is used for detecting the water vapor concentration values of the reaction container and the pressure control gas storage tank.
In some embodiments, the airflow controller comprises a first three-way solenoid valve, a second three-way solenoid valve, a third three-way solenoid valve,
a first inlet of the first three-way electromagnetic valve is connected with an exhaust port of the pumping/exhausting pump through a pipeline;
the second inlet of the first three-way electromagnetic valve is connected with the reaction vessel through a pipeline,
the outlet of the first three-way electromagnetic valve is communicated to the atmosphere side,
a first inlet of the second three-way electromagnetic valve is connected with an air outlet of the pressure control air storage tank through a pipeline;
a second inlet of the second three-way electromagnetic valve is communicated with an outlet of the third three-way electromagnetic valve through a pipeline,
the outlet of the second three-way electromagnetic valve is communicated with the air inlet of the pumping/exhausting pump through a pipeline;
a first inlet of the third three-way electromagnetic valve is connected with the reaction container through a pipeline;
and a second inlet of the third three-way electromagnetic valve is connected with an air inlet of the pressure control air storage tank through a pipeline.
In some embodiments, the system further comprises at least one gas filter, wherein the gas filter is arranged between the outlet of the second three-way solenoid valve and the gas inlet of the pumping/exhausting pump;
the gas filter is arranged between the first inlet of the second three-way electromagnetic valve and the gas outlet of the pressure control gas storage tank;
the gas filter is arranged between the second inlet of the third three-way electromagnetic valve and the gas outlet of the pressure control gas storage tank;
the gas filter is used for preventing organic gas from entering the pressure control gas storage tank and the pumping/exhausting pump.
In some embodiments, the pressure control air storage tank comprises a pressure reducing valve, a one-way piston air valve and a pressure reducing piston one-way air valve pressure controller,
the air inlet of the pressure reducing valve is communicated with a high-pressure gas source through a pipeline, and the air outlet of the pressure reducing valve is communicated with the air inlet of the one-way piston air valve through a pipeline;
the exhaust port of the one-way piston air valve is communicated with the pressure control air storage tank through a pipeline;
the pressure control gas storage tank is communicated with the gas inlet of the pressure reducing piston type one-way gas valve pressure controller through a pipeline,
and an exhaust port of the pressure-reducing piston type one-way air valve pressure controller is communicated to the atmosphere side.
In some embodiments, a pressure gauge and an explosion-proof hole are arranged on the pressure-control air storage tank,
the pressure gauge is used for monitoring the air pressure of the pressure control air storage tank,
the explosion-proof hole is used for discharging overpressure gas of the pressure control gas storage tank.
In the gas replacement and introduction synthesis reaction device of the present invention, the gas replacement and introduction synthesis reaction device comprises a reaction vessel for holding a compound to be reacted, a pressure-controlled gas storage tank, at least one gas pumping/exhausting pump, at least one gas concentration sensor and a programmable logic controller. The reaction container, the pressure-controlled gas storage tank, the pumping/exhausting pump and the gas concentration sensor are connected through pipelines to form a closed system, and the gas concentration sensor is used for detecting the oxygen concentration value or the water vapor concentration value of gas in the pressure-controlled gas storage tank; the programmable logic controller is respectively connected with the gas flow controller and the communication interface of the gas concentration sensor; the gas concentration sensor feeds back the acquired oxygen or water vapor concentration value to the programmable logic controller, and compares the oxygen or water vapor concentration value with a preset value of the programmable logic controller; and if the oxygen concentration value or the water vapor concentration value is less than or equal to a preset value, automatically switching the working mode of gas replacement or gas introduction by the programmable logic controller. Compared with the prior art, the oxygen or water vapor concentration value obtained by the gas concentration sensor is compared with the preset value of the programmable logic controller, and when the oxygen concentration value or the water vapor concentration value is less than or equal to the preset value, the programmable logic controller outputs working signals for controlling the pumping/exhausting pump and the airflow controller, so that the synthetic reaction device can automatically switch the working mode of gas replacement or gas introduction.
Drawings
The invention will be further explained with reference to the drawings and examples, wherein:
FIG. 1 is a schematic structural diagram of an embodiment of a synthesis reaction apparatus for gas replacement and introduction according to the present invention;
FIG. 2 is a schematic connection diagram of an embodiment of a gas displacement synthesis reactor apparatus according to the present invention;
FIG. 3 is a schematic connection diagram of an embodiment of a synthesis reactor apparatus for introducing gas according to the present invention;
fig. 4 is a schematic structural diagram of an embodiment of the pressure-controlling gas storage tank of the present invention.
Detailed Description
In order to clearly understand the technical features, objects, and effects of the present invention, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Fig. 1 is the utility model provides a gas replacement, synthetic reaction device embodiment structural principle picture that lets in, fig. 2 is the utility model provides a schematic diagram is connected to a synthetic reaction device embodiment of gas replacement, fig. 3 is the utility model provides a schematic diagram is connected to a synthetic reaction device embodiment that gaseous lets in, fig. 4 is the utility model provides a accuse pressure gas holder structure schematic diagram of an embodiment. As shown in fig. 1 to 4, in the first and second embodiments of the gas replacement/introduction synthesis reaction apparatus of the present invention, the gas replacement/introduction synthesis reaction apparatus mainly includes a reaction vessel 10, a pressure-controlled gas storage tank 20, at least one pumping/exhausting pump 30, a gas flow controller 40, at least one gas concentration sensor 50, and a programmable logic controller 60.
The reaction vessel 10 is constituted as a closed reaction vessel of a hollow structure for containing a compound to be reacted and a reaction solvent.
The pressure-controlling gas storage tank 20 is a hollow sealed gas chamber for storing the protective gas or the reaction gas required by the reaction. Wherein, the pressure-resistant gas cabin is made of stainless steel, glass fiber reinforced plastics or engineering plastics with acid and alkali resistance and organic solvent attached inside, and a hollow cavity chamber of 500 ml to 25L is formed by a sealing ring in a whole or split way.
Specifically, the gas outlet 207 and the gas inlet 208 of the pressure-controlling gas holder 20 are in sealed communication with the reaction vessel 10 through the pipeline gas flow controller 40.
The gas flow controller 40 is used to control the communication of the reaction vessel 10, the pressure-controlling gas container 20 and the pumping/exhausting pump 30 with each other and with the outside.
Further, an air inlet of the pumping/exhausting pump 30 is communicated with the air flow controller 40, the reaction vessel 10 and the pressure-controlling air tank 20 through a pipeline.
In the gas replacement operation mode, the pumping/exhausting pump 30 is used for pumping and exhausting air in the reaction vessel 10, the pressure-controlling air storage tank 20 and the airflow controller 40; in the gas introduction operation mode, the pumping/exhausting pump 30 is used to introduce the protection or reaction gas in the pressure-controlling gas container 20 into the reaction vessel 10 in a flowing manner or in a bubbling manner.
The detection end of the gas concentration sensor 50 is disposed in the pipeline between the exhaust/suction pump 30 and the second three-way solenoid valve 402 or in the pressure-controlling gas tank 20, and is configured to detect an oxygen concentration value or a water vapor concentration value of the gas in the reaction vessel 10 and the pressure-controlling gas tank 20, and feed back the oxygen concentration value or the water vapor concentration value to the programmable logic controller 60.
The programmable logic controller 60, which is a core control component of the synthesis reaction apparatus, has instructions for performing operations such as logical operations, sequence control, timing, counting, and arithmetic operations, and controls the operation of the suction/exhaust pump 30 and the gas flow controller 40 through input/output of digital signals or analog signals.
Specifically, the signal output of the programmable logic controller 60 is connected to the controlled terminals of the pump/exhaust pump 30 and the flow controller 40.
The signal input of the programmable logic controller 60 is connected to the communication interface of the gas concentration sensor 50, and is configured to receive the oxygen concentration value or the water vapor concentration value obtained by the gas concentration sensor 50.
The gas concentration sensor 50 feeds back the acquired oxygen concentration value or water vapor concentration value to the programmable logic controller 60, and compares the acquired oxygen concentration value or water vapor concentration value with a preset value of the programmable logic controller 60.
If the oxygen concentration value or the water vapor concentration value is less than or equal to the preset value, the programmable logic controller 60 may automatically switch the working mode of gas replacement or gas introduction.
In some embodiments, the gas concentration sensor 50 includes an oxygen concentration sensor 501 and a water vapor concentration sensor 502.
Specifically, the oxygen concentration sensor 501 and the water vapor concentration sensor 502 are respectively connected to the plc 60 through communication interfaces.
The oxygen concentration sensor 501 is configured to detect oxygen concentration values of the reaction container 10 and the pressure-controlling gas tank 20, and the water vapor concentration sensor 502 is configured to detect water vapor concentration values of the reaction container 10 and the pressure-controlling gas tank 20, feed back the obtained oxygen concentration values and water vapor concentration values to the programmable logic controller 60, and compare the obtained oxygen concentration values and water vapor concentration values with preset values of the programmable logic controller 60.
In some embodiments, in order to improve the circulation effect of the air pumping and charging of the synthesis reaction device, a first three-way solenoid valve 401, a second three-way solenoid valve 402, and a third three-way solenoid valve 403 may be disposed in the gas flow controller 40. The control mode of the three-way electromagnetic valve is two-in one-out.
Specifically, a first inlet of the first three-way solenoid valve 401 is connected to an exhaust port of the suction/exhaust pump 30 through a pipe, a second inlet of the first three-way solenoid valve 401 is connected to the reaction vessel 10 through a pipe, and an outlet of the first three-way solenoid valve 401 is opened to the atmosphere side.
A first inlet of the second three-way electromagnetic valve 402 is connected with the air outlet 207 of the pressure-controlling air storage tank 20 through a pipeline, a second inlet of the second three-way electromagnetic valve 402 is communicated with an outlet of the third three-way electromagnetic valve 403 through a pipeline, and an outlet of the second three-way electromagnetic valve 402 is communicated with an air inlet of the pumping/exhausting pump 30 through a pipeline.
A first inlet of the third three-way electromagnetic valve 403 is connected with the reaction vessel 10 through a pipeline, and a second inlet of the third three-way electromagnetic valve 403 is connected with the air inlet 208 of the pressure control air storage tank 20 through a pipeline.
Illustratively, the programmable logic controller 60 adjusts the pumping/venting capacity of the pump/vent pump 30 by adjusting its PWM (pulse width modulation) signal, voltage or current magnitude, and controls the gas flow controller 40 to implement both gas displacement and gas venting modes of operation. Specifically, the mode of operation of gas displacement (shown in fig. 2) is divided into two phases:
in the first stage, the pumping/exhausting pump 30 is started by a button on the programmable logic controller 60, and then the first three-way electromagnetic valve 401 is controlled to be opened to the atmosphere side to close the communication with the closed reaction vessel 10; meanwhile, the connection of the second three-way electromagnetic valve 402 with the pressure control gas storage tank 20, the suction/exhaust pump 30 and the third three-way electromagnetic valve 403 is opened; the third three-way solenoid valve 403 is opened to connect the pressure control gas tank 20 and the second three-way solenoid valve 402, and the connection with the reaction vessel 10 is closed.
At this time, air in a part of the pipelines in the pressure control air tank 20 and the airflow controller 40 will be pumped away, so that a negative pressure difference is formed between the air tank 2 and the high pressure gas source, and the protection gas or the reaction gas is charged into the pressure control air tank 20 through the one-way piston gas valve 205.
It should be noted that the oxygen concentration and the water vapor concentration in the pressure-controlling gas storage tank 20 are respectively measured by the oxygen concentration sensor 501 and the water vapor concentration sensor 502 in real time and displayed on the liquid crystal panel of the programmable logic controller 60, and when the oxygen concentration and the water vapor concentration meet the requirements required by the specific reaction, the gas replacement working mode of the next stage can be switched by manual operation; the oxygen concentration and water vapor concentration values preset by the programmable logic controller 60 can also be automatically switched to the second gas replacement stage when the actual measurement value of the sensor is less than or equal to the preset value.
In the second stage of gas replacement, the pumping/exhausting pump 30 needs to be kept in an open state, the connection between the second three-way electromagnetic valve 402 and the pumping/exhausting pump 30 is opened, and the connection between the second three-way electromagnetic valve and the pressure control gas storage tank 20 is closed; the third three-way solenoid valve 403 is opened to connect with the second three-way solenoid valve 402, and the connection with the pressure-controlling gas tank 20 is closed.
At this time, the air in the reaction vessel 10 and the airflow controller 40 is pumped out by the pumping/exhausting pump 30. A timing switch integrated in the programmable logic controller 60 controls the third three-way electromagnetic valve 403 to close the connection with the second three-way electromagnetic valve 402 every 30 seconds, and opens the communication with the pressure control gas storage tank 20, so that the gas in the pressure control gas storage tank 20 is filled into the reaction container 10 and the gas flow controller 40 with negative pressure; the third three-way electromagnetic valve 403 is opened again to be connected with the second three-way electromagnetic valve 402 after a preset timing switch in the programmable logic controller 60 is switched on for 5 seconds, the connection with the pressure control gas storage tank 20 is closed, and gas extraction or gas charging of the reaction system is carried out in a circulating manner until an operator manually switches the working mode of the device; the oxygen concentration and water vapor concentration values may also be preset by the programmable logic controller 60 to automatically switch the device operating mode when the actual sensor measurements are less than or equal to the preset values.
During this process, the pressure in the pressure control reservoir 20 will decrease, but will automatically be replenished from the high pressure gas source through the one-way piston gas valve 205.
Wherein, a gas filter 70 is provided at the connection end of the gas flow controller 40 with the pressure-controlling gas tank 20 and the suction/discharge pump 30 to prevent organic gas from entering the above two components.
The oxygen concentration and the water vapor concentration in the reaction container 10 and the gas flow controller 40 are respectively measured by the oxygen concentration sensor 501 and the water vapor concentration sensor 502 in real time, and are displayed on the liquid crystal panel of the programmable logic controller 60, and when the oxygen concentration and the water vapor concentration meet the requirements required by specific reaction, the gas can be replaced and switched into a gas introduction working mode through a button. The oxygen concentration and water vapor concentration values may also be preset by the programmable logic controller 60, and automatically switched to the gas introduction mode when the actual sensor measurements are less than or equal to the preset values.
In the working principle of the gas introduction mode (shown in fig. 3), firstly, the programmable logic controller 60 controls the first three-way electromagnetic valve 401 to open, and gas is introduced into the closed reaction vessel 10 and is closed to be communicated with the atmosphere; then, the second two-way electromagnetic valve 402 is controlled to be opened to be communicated with the pressure control air storage tank 20, and the third three-way electromagnetic valve 403 is controlled to be closed to be communicated; meanwhile, the third three-way solenoid valve 403 is controlled to open the communication with the pressure control air tank 20 and close the communication with the second three-way solenoid valve 402. Thus, the reaction vessel 10, the pressure-controlling gas container 20, the pumping/exhausting pump 30 and the gas flow controller 40 constitute a closed system which is communicated with each other, and the pumping/exhausting pump 30 realizes the circulation flow of the gas, and if the pipeline for introducing the gas into the reaction vessel 10 extends to the position below the reaction liquid level, the specific reaction gas can be bubbled into the reaction system. The programmable logic controller 60 can regulate the amount of flow through by adjusting the PWM signal, voltage or current of the pump 30.
In some embodiments, at least one gas filter 70 is further included for preventing organic gas from entering the pressure-controlled gas tank 20 and the suction/discharge pump 30.
Specifically, the gas filter 70 is provided between the outlet of the second three-way solenoid valve 402 and the intake port of the suction/exhaust pump 30.
The gas filter 70 is disposed between the first inlet of the second three-way solenoid valve 402 and the gas outlet 207 of the pressure-controlling gas tank 20.
The gas filter 70 is arranged between the second inlet of the third three-way solenoid valve 403 and the gas outlet 208 of the pressure control gas storage tank 20.
In some embodiments, a pressure gauge 201 and an explosion-proof hole 202 are provided on the pressure-controlling gas storage tank 20,
the pressure gauge 201 is used for monitoring the air pressure of the pressure control air storage tank 20, and the explosion-proof hole 201 is used for discharging the air of the pressure control air storage tank 20.
Further, the pressure-controlling air storage tank 20 includes a pressure-reducing valve 204, a one-way piston air valve 205 and a pressure-reducing piston one-way air valve pressure controller 206.
Specifically, the air inlet of the pressure reducing valve 204 is communicated with a high-pressure air source through a pipeline, the air outlet of the pressure reducing valve 204 is communicated with the air inlet of the one-way piston air valve 205 through a pipeline, and the air outlet of the one-way piston air valve 205 is communicated with the pressure control air storage tank 20 through a pipeline.
The pressure control air storage tank 20 is communicated with the air inlet of the pressure reducing piston type one-way air valve pressure controller 206 through a pipeline,
the exhaust of the pressure reducing piston type one-way air valve pressure controller 206 is open to the atmosphere side.
Illustratively, high-pressure gas is input into the pressure control gas tank 20 through the pressure reducing valve 204 at 1.5 atm, when the internal pressure of the pressure control gas tank 20 is less than or equal to 1.1 atm, the piston in the one-way piston gas valve 205 moves to the left, the valve is opened, and the gas is injected into the pressure control gas tank 20 through the pressure reducing valve 204; when the internal pressure of the pressure control air storage tank 20 reaches 1.2 atmospheric pressure, the piston in the one-way piston air valve 205 moves rightwards, and the valve is closed.
If the internal pressure of the pressure control air storage tank 20 is greater than 1.3 atmospheres, the piston in the pressure reduction piston type one-way air valve pressure controller 206 moves rightwards, the valve is opened, the air in the tank is discharged, and the pressure is reduced; when the pressure in the pressure-controlling air storage tank 20 is restored to 1.2 atmospheres, the piston in the pressure-reducing piston type one-way air valve pressure controller 206 moves leftwards, and the valve is closed. The pressure control of the pressure control air storage tank 20 can be realized by selecting a one-way piston air valve 205 with proper air outlet pressure difference at the air inlet and the air outlet and a pressure control device 206 with a pressure reduction piston type one-way air valve.
When the air pressure in the pressure-controlling air storage tank 20 is greater than 1.4 atmospheres, the rubber film of the explosion-proof hole 202 is broken, so that the pressure in the pressure-controlling air storage tank 20 is rapidly reduced, and the system safety is ensured.
The first embodiment is as follows: the pressure control gas storage tank 20 of the synthesis reaction device is connected with a high-purity nitrogen (99.999%) steel cylinder, and a switch and a pressure reducing valve 204 of the steel cylinder are opened. A100 mL pre-dried double-necked flask was equipped with a spherical condenser tube connected to the above-mentioned apparatus (FIGS. two and three) and a constant-pressure dropping funnel with a ground opening sealed with a turnup plug, and 1.5g of magnesium chips and a magnetic stirrer were added in advance. The starting device automatically replaces the air in the reaction bottle with nitrogen in two stages, the working voltage of the pumping/exhausting pump 30 can be adjusted to be larger (24V), after the programmable logic controller 60 displays that the oxygen concentration is less than or equal to 50ppm and the water vapor concentration is less than or equal to 50ppm on a control panel, the working voltage of the pumping/exhausting pump 30 is adjusted to be larger than 6V, the device is switched to a gas introducing mode, 10mL of anhydrous ether is added from a constant-pressure dropping funnel, and a magnetic stirrer is started. A mixed solution of 6.5mL of n-bromobutane and 10mL of anhydrous ether was added to the dropping funnel. Adding 3-4 mL of mixed solution into a double-necked bottle to initiate reaction. After the reaction is gradually mild, slowly dropping the residual n-bromobutane ethyl ether mixed solution, and controlling the dropping speed. After the addition, 15mL of anhydrous ether was added, and the mixture was heated in a warm water bath under reflux for 15min to ensure complete reaction. Cooling in an ice-water bath, and dropwise adding a mixed solution of 4.5mL of acetone and 5mL of anhydrous ether under stirring; after the addition was complete, stirring was continued at room temperature for 15 min. The reaction was quenched by standard methods and worked up to give 6.42g of the product 2-methyl-2-hexanol in 91.8% yield.
Example two: the pressure control gas storage tank 20 of the device is connected with a high-purity carbon monoxide (99.99%) steel cylinder, and a switch and a pressure reducing valve 204 of the steel cylinder are opened. The device was inserted into one port of a 25mL pre-dried double-necked flask (see FIGS. two and three), the other port was closed with a plug, and 10mg of palladium chloride (PdCl) was pre-placed in the flask2) 270mg of copper chloride (CuCl)2) 164mg sodium acetate (NaOAc) and magnetic stirrer. The starting device automatically replaces the air in the reaction bottle with carbon monoxide in two stages, the working voltage of the pumping/exhausting pump can be adjusted to 12V at the moment, after the programmable logic controller 60 displays that the oxygen concentration is less than or equal to 100ppm and the water vapor concentration is less than or equal to 100ppm on the control panel, the working voltage of the pumping/exhausting pump 30 is adjusted to 6V, and the device is switched to a gas introducing mode. 10mL of methanol and 0.11mL of phenylacetylene were added to the reaction flask from the tip-off stopper, respectively, by means of a syringe, and the reaction was carried out for 2 hours by starting a magnetic stirrer and inserting a stainless steel vent line under the liquid surface to bubble. The product methyl phenyl propiolate 138mg is obtained by standard extraction and quenching reaction and post-treatment, and the yield is 86%.
Implement the utility model has the advantages of as follows:
1. simple to operate, only three interface, gas access mouth, gas outlet and air inlet after equipment shaping, only need be connected to the gas source during installation and insert corresponding inert gas or reaction gas to the gas access mouth, again with gas outlet and air inlet insert the reaction can.
2. The operation is simple, the equipment adopts visual setting and operation, and can flexibly adopt a semi-automatic mode and an automatic mode to operate according to the requirement.
3. The method is safe and reliable, and a pressure control gas storage tank is adopted, so that the total positive pressure of the reaction system does not exceed 1.3 atmospheric pressure under normal conditions; the miniature pumping/exhausting pump 30 is adopted, the total negative pressure of the reaction system is lower than 0.5 atmosphere, and the pressure bearing of the system is small.
4. The device has high anhydrous and anaerobic degree, all parts of the device are made of stainless steel, glass fiber reinforced plastic, polytetrafluoroethylene materials and hard glass, and are tightly connected through hard pipelines, so that the air tightness is guaranteed under the condition of small system pressure bearing; from the point of view of gas concentration sensing gas detection, the final anhydrous and oxygen-free level of the system can substantially reach the standard limit of the high purity gas used.
5. The reaction efficiency is high, and the operation time is saved by semi-automatic and automatic operation; control of the anhydrous and oxygen-free reaction conditions by the apparatus is an example-the key to the ability of such highly reactive metal salt carbanions to produce high yields; the closed bubble reaction mode of the apparatus is also a direct reason why the metalorganic reactions of example two can achieve higher yields than reported in the literature.
6. The economy is used to gas, compares in gaseous gas replacement or the reaction mode of letting in reaction vessel reequiped gas continuously, the utility model discloses a take out/the gas pump 30 realizes the gas cycle in the airtight system and uses, and the gas quantity is little.
While the embodiments of the present invention have been described with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and many modifications may be made by one skilled in the art without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (6)
1. A synthesis reaction apparatus for gas replacement and introduction, comprising:
a reaction vessel configured as a closed reaction vessel of a hollow structure for containing a compound to be reacted and a reaction solvent;
the pressure control gas storage tank is a closed gas bin with a hollow structure, the pressure control gas storage tank is used for storing protective gas or reaction gas required by reaction, and a gas outlet of the pressure control gas storage tank is communicated with the gas flow controller and the reaction container in a closed mode through a pipeline;
at least one pumping/exhausting pump, wherein the air inlet of the pumping/exhausting pump is hermetically communicated with the airflow controller, the reaction container and the pressure control air storage tank through pipelines,
the pumping/exhausting pump is used for pumping and exhausting air in the reaction container, the pressure-control air storage tank and the airflow controller in a gas replacement working mode, and is used for pumping protective or reaction gas in the pressure-control air storage tank into the reaction container in a flowing mode or a bubbling mode in a gas introducing reaction mode;
the detection end of the gas concentration sensor is arranged in a pipeline communicated with the reaction container or in the pressure control gas storage tank, and the gas concentration sensor is used for detecting the oxygen concentration value or the water vapor concentration value of the gas in the reaction container and the pressure control gas storage tank;
the programmable logic controller is respectively connected with the communication interfaces of the pumping/exhausting pump, the gas flow controller and the gas concentration sensor; wherein the content of the first and second substances,
the gas concentration sensor feeds back the acquired oxygen concentration value or water vapor concentration value to the programmable logic controller, and the oxygen concentration value or water vapor concentration value is compared with a preset value of the programmable logic controller;
and if the oxygen concentration value or the water vapor concentration value is less than or equal to the preset value, the programmable logic controller automatically switches the working mode of gas replacement or gas introduction.
2. The gas-displacement, gas-fed synthesis reaction apparatus according to claim 1,
the gas concentration sensor includes an oxygen concentration sensor and a water vapor concentration sensor,
the oxygen concentration sensor and the water vapor concentration sensor are respectively connected with the communication interface of the programmable logic controller;
the oxygen concentration sensor is used for detecting the oxygen concentration values of the reaction container and the pressure control gas storage tank,
the water vapor concentration sensor is used for detecting the water vapor concentration values of the reaction container and the pressure control gas storage tank.
3. The gas-displacement, gas-fed synthesis reaction apparatus according to claim 1,
the air flow controller comprises a first three-way electromagnetic valve, a second three-way electromagnetic valve and a third three-way electromagnetic valve,
a first inlet of the first three-way electromagnetic valve is connected with an exhaust port of the pumping/exhausting pump through a pipeline;
the second inlet of the first three-way electromagnetic valve is connected with the reaction vessel through a pipeline,
the outlet of the first three-way electromagnetic valve is communicated to the atmosphere side,
a first inlet of the second three-way electromagnetic valve is connected with an air outlet of the pressure control air storage tank through a pipeline;
a second inlet of the second three-way electromagnetic valve is communicated with an outlet of the third three-way electromagnetic valve through a pipeline,
the outlet of the second three-way electromagnetic valve is communicated with the air inlet of the pumping/exhausting pump through a pipeline;
a first inlet of the third three-way electromagnetic valve is connected with the reaction container through a pipeline;
and a second inlet of the third three-way electromagnetic valve is connected with an air inlet of the pressure control air storage tank through a pipeline.
4. A gas-displacement, gas-fed synthesis reaction apparatus according to claim 3,
the gas filter is arranged between the outlet of the second three-way electromagnetic valve and the gas inlet of the pumping/exhausting pump;
the gas filter is arranged between the first inlet of the second three-way electromagnetic valve and the gas outlet of the pressure control gas storage tank;
the gas filter is arranged between the second inlet of the third three-way electromagnetic valve and the gas outlet of the pressure control gas storage tank;
the gas filter is used for preventing organic gas from entering the pressure control gas storage tank and the pumping/exhausting pump.
5. The gas-displacement, gas-fed synthesis reaction apparatus according to claim 1,
the pressure control gas storage tank comprises a pressure reducing valve, a one-way piston gas valve and a pressure reducing piston type one-way gas valve pressure controller,
the air inlet of the pressure reducing valve is communicated with a high-pressure gas source through a pipeline, and the air outlet of the pressure reducing valve is communicated with the air inlet of the one-way piston air valve through a pipeline;
the exhaust port of the one-way piston air valve is communicated with the pressure control air storage tank through a pipeline;
the pressure control gas storage tank is communicated with the gas inlet of the pressure reducing piston type one-way gas valve pressure controller through a pipeline,
and an exhaust port of the pressure-reducing piston type one-way air valve pressure controller is communicated to the atmosphere side.
6. A gas-displacement, gas-fed synthesis reaction apparatus according to claim 5,
a pressure gauge and an explosion-proof hole are arranged on the pressure-control gas storage tank,
the pressure gauge is used for monitoring the air pressure of the pressure control air storage tank,
the explosion-proof hole is used for discharging overpressure gas of the pressure control gas storage tank.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111097347A (en) * | 2020-01-13 | 2020-05-05 | 厦门大学 | Gas replacement and introduction synthesis reaction device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111097347A (en) * | 2020-01-13 | 2020-05-05 | 厦门大学 | Gas replacement and introduction synthesis reaction device |
| CN111097347B (en) * | 2020-01-13 | 2024-03-15 | 光炁钧宏(厦门)科技服务有限公司 | Synthetic reaction device for gas replacement and ventilation |
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Effective date of registration: 20201020 Address after: Unit 28, area C, 7th floor, No.26 Zhenhai Road, Siming District, Xiamen City, Fujian Province 361000 Patentee after: Guangqi Junhong (Xiamen) Technology Service Co., Ltd Address before: Xiamen City, Fujian Province, 361005 South Siming Road No. 422 Patentee before: XIAMEN University |