Constant-pressure continuous reaction device for laboratory

Abstract

The utility model discloses a constant-pressure continuous reaction device for a laboratory, which relates to the technical field of chemical reaction devices and comprises a gas source bottle, a reaction kettle and a sample introduction bottle which are sequentially arranged, the reaction kettle is provided with a first gas inlet, a gas outlet, a liquid inlet and a charging hole; a liquid outlet and a second gas inlet are formed in the sample injection bottle; a first gas pipeline is arranged between the gas source bottle and the reaction kettle, one end of the first gas pipeline is connected with the gas outlet end of the gas source bottle, and the other end is connected with the first gas inlet; a second gas pipeline and a liquid conveying pipeline are arranged between the reaction kettle and the sample injection bottle, one end of the second gas pipeline is connected with the gas outlet, and the other end is connected with the second gas inlet; one end of the liquid conveying pipeline is connected with the liquid outlet, the other end of the liquid conveying pipeline is connected with the liquid inlet, and a peristaltic pump is installed on the liquid conveying pipeline. According to the utility model, through specific reaction equipment, reaction liquid can be effectively added in a constant-pressure process of a system, namely, gas-liquid two-phase, micro-pressure and continuous reaction can be met at the same time.

Description

Technical Field

[0001] This utility model relates to the field of chemical reaction apparatus technology, and more specifically, to a laboratory constant pressure continuous reaction apparatus. Background Technology

[0002] In organic synthesis reactions, some gas-liquid two-phase reactions are often involved. These reactions can be achieved by purging or pressurizing. However, purging leads to waste of gaseous raw materials and accelerated solvent evaporation, so pressurization is preferred for gas-liquid reactions. Common pressurization devices are metal autoclaves, which are bulky and difficult to operate in the laboratory stage.

[0003] In actual organic synthesis, the reaction rate is controlled by adding the raw materials in one go or by dropping them. However, for some raw materials that are unstable in the solvent and involve two phases of gas and liquid, it is not possible to pressurize and drop them.

[0004] Therefore, in order to solve the above problems, a miniaturized pressurized continuous reaction device that can be disassembled in the laboratory is needed. Utility Model Content

[0005] In view of this, the purpose of this utility model is to provide a laboratory constant pressure continuous reaction device to solve the problems existing in the prior art.

[0006] To achieve the above objectives, the technical solution of this utility model is as follows:

[0007] A laboratory constant-pressure continuous reaction apparatus includes a gas source bottle, a reaction vessel, and a sample injection bottle arranged sequentially.

[0008] The reactor is equipped with a first air inlet, an air outlet, a liquid inlet, and a feed inlet;

[0009] The sample bottle is provided with a liquid outlet and a second air inlet;

[0010] A first gas pipeline is provided between the gas source cylinder and the reaction vessel. One end of the first gas pipeline is connected to the gas outlet of the gas source cylinder, and the other end is connected to the first gas inlet.

[0011] A second gas pipeline and a liquid delivery pipeline are provided between the reaction vessel and the sample bottle. One end of the second gas pipeline is connected to the gas outlet and the other end is connected to the second gas inlet. One end of the liquid delivery pipeline is connected to the liquid outlet and the other end is connected to the liquid inlet. A peristaltic pump is installed on the liquid delivery pipeline.

[0012] Furthermore, it also includes a temperature control system, which is provided with a circulating liquid inlet and a circulating liquid outlet;

[0013] The outer periphery of the reactor is provided with a first jacket, and the upper side of the first jacket is provided with a first circulating liquid inlet and the lower side is provided with a first circulating liquid outlet.

[0014] The sample vial is provided with a second jacket around its outer periphery. The upper side of the second jacket is provided with a second circulating liquid inlet, and the lower side is provided with a second circulating liquid outlet.

[0015] The circulating fluid outlet is connected to the first circulating fluid inlet and the second circulating fluid inlet via a first circulating fluid pipe, and the circulating fluid inlet is connected to the first circulating fluid outlet and the second circulating fluid outlet via a second circulating fluid pipe.

[0016] Furthermore, a magnetic stirrer is provided at the bottom of the reaction vessel; the magnetic stirrer, the peristaltic pump, and the sample bottle are all fixed on an iron frame.

[0017] Furthermore, the first gas pipeline, the second gas pipeline, the infusion pipeline, the first circulating fluid pipeline, and the second circulating fluid pipeline are all latex pipelines.

[0018] Furthermore, the reactor is also equipped with a pressure gauge and a thermometer.

[0019] Furthermore, the first air inlet and outlet are connected to the interior of the reactor via a three-way valve.

[0020] Furthermore, the reactor is a glass pressure reactor.

[0021] The beneficial effects of this utility model are as follows:

[0022] The reaction apparatus provided by this invention solves the problem of continuous flow reaction in the laboratory under pressure. It can ensure the effective addition of reaction liquid during constant pressure in the system. It can simultaneously meet the requirements of gas-liquid two-phase, micro-pressure, and continuous reaction. The injection rate of the peristaltic pump can be adjusted according to the reaction rate and reaction temperature. After the liquid in the injection bottle has completely entered the reaction vessel, the peristaltic pump is turned off and the pressure is maintained to continue the reaction. The reaction can be stopped according to the actual situation. Attached Figure Description

[0023] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other embodiments can be obtained based on these drawings.

[0024] Figure 1 This is a schematic diagram of the structure of this utility model.

[0025] Figure 2This is a schematic diagram of the main structure of the reaction vessel in this utility model.

[0026] Figure 3 This is a top view of the reactor structure in this utility model.

[0027] Figure 4 This is a side view of the reactor structure in this utility model.

[0028] Explanation of reference numerals in the attached figures:

[0029] 1. Reactor; 1A. First air inlet; 1B. Air outlet; 1C. Liquid inlet; 1D. Feed inlet; 1E. Exhaust outlet;

[0030] 2. Sample inlet bottle; 2A. Liquid outlet; 2B. Second air inlet;

[0031] 3. Temperature control system; 3A. Circulating fluid inlet; 3B. Circulating fluid outlet;

[0032] 4. Peristaltic pump; 5. Gas source cylinder; 6. Magnetic stirrer; 7. Infusion pipeline; 8. First gas pipeline; 9. Second gas pipeline;

[0033] 10. First jacket; 10A. First circulating fluid inlet; 10B. First circulating fluid outlet;

[0034] 11. Second jacket; 11A. Second circulating fluid inlet; 11B. Second circulating fluid outlet;

[0035] 12. First circulating fluid pipeline; 13. Second circulating fluid pipeline; 14. Iron frame; 15. Pressure gauge; 16. Thermometer; 17. Three-way valve. Detailed Implementation

[0036] The structure provided by this utility model will be explained and described in detail below with reference to the accompanying drawings.

[0037] refer to Figures 1 to 4 As shown, this embodiment specifically discloses a laboratory constant pressure continuous reaction device, including a gas source bottle 5, a reaction vessel 1 and a sample injection bottle 2 arranged in sequence;

[0038] In this embodiment, the gas source cylinder 5 is a conventional high-pressure gas cylinder equipped with a pressure reducing valve; the reaction vessel 1 is a glass pressurized reaction vessel, and the sample inlet bottle 2 is also made of glass; the glass reaction vessel and sample inlet bottle are easy to clean; and the glass pressurized reaction vessel allows operators to directly observe the material state, color changes, reaction progress, etc. during the internal reaction process, which helps to identify problems and make adjustments in a timely manner; in addition, glass has good chemical stability and can resist the corrosion of many chemical substances, making it suitable for reactions in various corrosive media such as acids and alkalis, which can effectively prevent the reaction vessel from being corroded and affecting its service life, and at the same time prevent impurities caused by corrosion of the reaction vessel material from entering the reaction system, thus ensuring product quality.

[0039] Combination Figure 2 and Figure 3 As shown, the reactor 1 is provided with a first air inlet 1A, an air outlet 1B, a liquid inlet 1C, and a feed inlet 1D; wherein, the feed inlet 1D is a large-diameter feed inlet with internal threads, used for adding solid raw materials, etc.

[0040] The sample vial 2 is provided with a liquid outlet 2A and a second air inlet 2B. The liquid outlet 2A extends to the bottom of the sample vial 2, and the second air inlet 2B extends to the cap.

[0041] A first gas pipeline 8 is provided between the gas source cylinder 5 and the reaction vessel 1. One end of the first gas pipeline 8 is connected to the gas outlet of the gas source cylinder 5, and the other end is connected to the first gas inlet 1A.

[0042] A second gas pipeline 9 and a liquid delivery pipeline 7 are provided between the reaction vessel 1 and the sample bottle 2. One end of the second gas pipeline 9 is connected to the gas outlet 1B and the other end is connected to the second gas inlet 2B. One end of the liquid delivery pipeline 7 is connected to the liquid outlet 2A and the other end is connected to the liquid inlet 1C. A peristaltic pump 4 is installed on the liquid delivery pipeline 7.

[0043] In this embodiment, the gas source in the gas source bottle 5 is delivered to the reaction vessel 1 through the first gas pipeline 8, so that the reaction vessel 1 maintains a certain pressure. Then, the peristaltic pump 4 is turned on, and the mixture in the sample bottle 2 is added to the reaction vessel 1 at a uniform rate. Then, the injection rate is adjusted according to the reaction rate. After the liquid in the sample bottle 2 has completely entered the reaction vessel 1, the peristaltic pump 4 is turned off, and the pressure is maintained to continue the reaction. The reaction can be stopped according to the actual situation. The device provided in this embodiment can simultaneously meet the requirements of gas-liquid two-phase, micro-pressure, and continuous reaction.

[0044] In some embodiments, the laboratory constant pressure continuous reaction apparatus further includes a temperature control system 3, which is provided with a circulating liquid inlet 3A and a circulating liquid outlet 3B.

[0045] A first jacket 10 is provided on the outer periphery of the reactor 1. A first circulating liquid inlet 10A is provided on the upper side of the first jacket 10, and a first circulating liquid outlet 10B is provided on the lower side.

[0046] A second jacket 11 is provided on the outer periphery of the sample vial 2. A second circulating liquid inlet 11A is provided on the upper side of the second jacket 11, and a second circulating liquid outlet 11B is provided on the lower side.

[0047] The circulating fluid outlet 3B is connected to the first circulating fluid inlet 10A and the second circulating fluid inlet 11A through the first circulating fluid pipe 12, and the circulating fluid inlet 3A is connected to the first circulating fluid outlet 10B and the second circulating fluid outlet 11B through the second circulating fluid pipe 13.

[0048] In this embodiment, the temperature control system 3 can be a high and low temperature integrated machine, which is common in the prior art. The temperature control system 3 is used to heat and keep the reaction vessel 1 and / or sample bottle 2 for heating and keeping or cooling. The temperature conditions of the reaction device are controlled, making the reaction process safer and more efficient.

[0049] In some other embodiments, the temperature inside the reactor 1 or sample bottle 2 can also be controlled by directly installing a water body device outside the reactor 1 or sample bottle 2.

[0050] Continue to refer to Figure 1 As shown, a magnetic stirrer 6 is installed at the bottom of the reactor 1 (understandably, a stir bar is also installed inside the reactor 1). The magnetic stirrer 6 drives the stir bar to rotate inside the reactor 1, which enables the reactants to be fully mixed and flowed inside the reactor. Compared with traditional mechanical stirring, the magnetic stirrer does not need to be inserted into the reactor 1 through mechanical shaft sealing or other means, which reduces the risk of leakage at the seal and impurities entering the reactor 1. In addition, the magnetic stirrer 6 installed at the bottom operates more smoothly and generates less vibration, which is conducive to maintaining a stable environment inside the reactor.

[0051] Furthermore, the magnetic stirrer 6, the peristaltic pump 4, and the sample vial 2 are all fixed on the iron frame 14; by setting the iron frame 14 at the bottom of the magnetic stirrer 6, the peristaltic pump 4, and the sample vial 2, reliable support can be provided for the magnetic stirrer 6, the peristaltic pump 4, and the sample vial 2, ensuring the stable operation of each device.

[0052] In this embodiment, the first gas pipeline 8, the second gas pipeline 9, the infusion pipeline 7, the first circulating fluid pipeline 12, and the second circulating fluid pipeline 13 are all latex pipelines; they have excellent elasticity and flexibility, can easily bypass obstacles, and connect equipment in different locations; they also have good sealing performance, and can maintain a good sealing effect even under certain pressure changes, which can effectively prevent liquid or gas leakage in the pipeline; in addition, they have good chemical stability and can resist the corrosion of some acid and alkali solutions, organic solvents, etc.

[0053] In the illustrated embodiment, a pressure gauge 15 and a thermometer 16 are also provided on the reactor 1; by providing the pressure gauge 15 and the thermometer 16, the temperature and pressure inside the reactor 1 can be monitored in real time, ensuring that the reaction proceeds safely and effectively.

[0054] Combination Figure 1 and Figure 2 As shown, in some preferred embodiments, the reactor 1 is also provided with an exhaust port 1E. In the illustrated embodiment, the exhaust port 1E and the liquid inlet 1C are connected to the interior of the reactor 1 through a three-way valve 17. Furthermore, the first air inlet 1A and the air outlet 1B are also connected to the interior of the reactor 1 through a three-way valve 17. By connecting the two ports to the reactor 1 through the three-way valve 17, the flow direction and flow rate of the gas can be flexibly controlled, and the number of openings on the reactor 1 can be reduced. In addition, it can improve the safety of the device. When the pressure inside the reactor 1 is too high, some gas can be discharged from the air outlet 1E through the three-way valve 17 to reduce the pressure inside the reactor 1 and prevent safety accidents such as explosions.

[0055] In summary, in this invention, the gas and liquid flow directions are as shown by the arrows. The gas enters the reactor 1 from the gas source bottle 5 through port 1A and then enters the sample bottle 2 through port 1B, forming a pressure balance. The reaction liquid in the sample bottle 2 is transported to the reactor 1 from port 2A through port 1C by the peristaltic pump 4. The temperature control system 3 directs the circulating liquid from the circulating liquid outlet 3B through the second circulating liquid inlet 11A to the interlayer space of the sample bottle 2, i.e., into the second jacket 11, and then circulates it back to the temperature control system 3 through the second circulating liquid outlet 11B and the circulating liquid inlet 3A. The temperature control system 3 also directs the circulating liquid from the first circulating liquid inlet 10A to the interlayer space of the reactor 1, i.e., into the first jacket 10, and then circulates it back to the temperature control system 3 through the first circulating liquid outlet 10B.

[0056] How to use the laboratory constant-pressure continuous reaction apparatus of this utility model:

[0057] Based on the equipment setup, select a 1L reactor 1, use a vacuum pump to evacuate reactor 1 to -0.05MPa, open the pressure reducing valve on gas source cylinder 5, pressurize the pressure inside reactor 1 to 0.05MPa, close the pressure reducing valve, and test the sealing performance of the reaction device. If there is no significant pressure drop on the pressure gauge of reactor 1 within 20-30 minutes, it proves that the airtightness of the setup is good and the experiment can begin.

[0058] Based on the equipment setup, add raw material A and solvent C to sample vial 2, dissolve them, and then seal the sample vial; add raw material B or catalyst and solvent D to reactor 1, turn on magnetic stirrer 6, and seal reactor 1; set temperature control system 3 to the specified temperature, turn on circulation, and control the temperature of reactor 1 and sample vial 2 at the specified temperature T℃; open the pressure reducing valve on gas source cylinder 5, and fill the reactor 1 to the required pressure X MPa, and maintain the pressure; turn on peristaltic pump 4, and add the mixture in sample vial 2 to reactor 1 at a uniform rate. Adjust the injection rate according to the reaction rate and temperature. After the liquid in sample vial 2 has completely entered reactor 1, turn off peristaltic pump 4, maintain pressure, and continue the reaction. Stop the reaction as needed.

[0059] Among them, raw material A is easily soluble in solvent C;

[0060] Raw material B may or may not be soluble in solvent D;

[0061] Solvent D can be a single solvent or a mixture of multiple solvents;

[0062] Solvent C may be the same as solvent D or different from solvent D;

[0063] The required pressure X is the experimental pressure value and is within the pressure resistance range of reactor 1;

[0064] The reaction temperature T is the required temperature value for the experiment and is within the temperature range of reactor 1.

[0065] The following specific examples illustrate this:

[0066] Based on the equipment setup, a 500ml reaction vessel 1 was selected. The reaction vessel 1 is a glass pressure reaction vessel. A vacuum pump was used to evacuate the glass reaction vessel to -0.05MPa. The pressure reducing valve of the gas source bottle 5 was opened (at this time, the gas source in the gas source bottle 5 is nitrogen or other inert gas). The pressure inside the reaction vessel was increased to 0.05MPa. The pressure reducing valve was then closed. The airtightness of the reaction device was tested. If there was no significant pressure drop on the pressure gauge of the reaction vessel within 20 to 30 minutes, it proved that the airtightness of the setup was good and the experiment could begin.

[0067] Based on the equipment setup, operate inside a fume hood. Add compound 1 and isopropanol to sample vial 2, dissolve, and seal the vial. Add potassium hydroxide, water, and palladium on carbon catalyst to reactor 1, turn on the magnetic stirrer, and seal the reactor. Set the temperature control system 3 to 55℃, turn on the circulation, and control the temperature of reactor 1 and sample vial 2 at the specified temperature of 50-55℃. Open the pressure reducing valve of gas source bottle 5 (at this time, the gas source in gas source bottle 5 is hydrogen) to introduce hydrogen and fill the pressure in reactor 1 to 1.5MPa, and maintain the pressure. Turn on the peristaltic pump 4 and add the mixture in sample vial 2 dropwise to reactor 1 at a uniform rate. Adjust the injection rate according to the reaction rate and temperature. Reduce the injection rate when the temperature rises. After the liquid in sample vial 2 has completely entered reactor 1, turn off the peristaltic pump 4 and maintain the pressure to continue the reaction. When the pressure is constant and there is no significant drop, the reaction ends. Stop the reaction, perform post-processing, and it is ready.

[0068] The reaction formulas involved are shown below:

[0069]

[0070] In the description of this utility model, it should be understood that the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., indicating the orientation or positional relationship are based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this utility model and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this utility model.

[0071] In this utility model, unless otherwise explicitly specified and limited, the terms "installation," "connection," "joining," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0072] In the description of this specification, the references to terms such as "this embodiment," "an embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in a suitable manner in any at least one embodiment or example. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0073] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of indicated technical features. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one of that feature. In the description of this utility model, "a plurality of" means at least two, such as two, three, etc., unless otherwise explicitly specified.

[0074] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Any modifications, equivalent substitutions and simple improvements made on the substantive content of the present utility model should be included within the protection scope of the present utility model.

Claims

1. A laboratory constant-pressure continuous reaction apparatus, characterized in that, It includes a gas source bottle (5), a reaction vessel (1), and a sample injection bottle (2) arranged in sequence; The reactor (1) is provided with a first air inlet (1A), an air outlet (1B), a liquid inlet (1C), and a feed inlet (1D); The sample inlet (2) is provided with a liquid outlet (2A) and a second air inlet (2B); A first gas pipeline (8) is provided between the gas source cylinder (5) and the reaction vessel (1). One end of the first gas pipeline (8) is connected to the gas outlet of the gas source cylinder (5), and the other end is connected to the first gas inlet (1A). A second gas pipeline (9) and a liquid delivery pipeline (7) are provided between the reaction vessel (1) and the sample bottle (2). One end of the second gas pipeline (9) is connected to the gas outlet (1B) and the other end is connected to the second gas inlet (2B). One end of the liquid delivery pipeline (7) is connected to the liquid outlet (2A) and the other end is connected to the liquid inlet (1C). A peristaltic pump (4) is installed on the liquid delivery pipeline (7).

2. The laboratory constant-pressure continuous reaction apparatus according to claim 1, characterized in that, It also includes a temperature control system (3), which is provided with a circulating liquid inlet (3A) and a circulating liquid outlet (3B); The outer periphery of the reactor (1) is provided with a first jacket (10), and the upper side of the first jacket (10) is provided with a first circulating liquid inlet (10A) and the lower side is provided with a first circulating liquid outlet (10B). The outer periphery of the sample bottle (2) is provided with a second jacket (11), and the upper side of the second jacket (11) is provided with a second circulating liquid inlet (11A), and the lower side is provided with a second circulating liquid outlet (11B). The circulating fluid outlet (3B) is connected to the first circulating fluid inlet (10A) and the second circulating fluid inlet (11A) through the first circulating fluid pipe (12), and the circulating fluid inlet (3A) is connected to the first circulating fluid outlet (10B) and the second circulating fluid outlet (11B) through the second circulating fluid pipe (13).

3. The laboratory constant-pressure continuous reaction apparatus according to claim 2, characterized in that, A magnetic stirrer (6) is provided at the bottom of the reactor (1); the magnetic stirrer (6), the peristaltic pump (4) and the sample bottle (2) are all fixed on the iron stand (14).

4. The laboratory constant-pressure continuous reaction apparatus according to claim 2, characterized in that, The first gas pipe (8), the second gas pipe (9), the infusion pipe (7), the first circulating liquid pipe (12), and the second circulating liquid pipe (13) are all latex pipes.

5. The laboratory constant-pressure continuous reaction apparatus according to claim 1, characterized in that, The reactor (1) is also equipped with a pressure gauge (15) and a thermometer (16).

6. The laboratory constant-pressure continuous reaction apparatus according to claim 1, characterized in that, The first air inlet (1A) and air outlet (1B) are connected to the interior of the reactor (1) via a three-way valve (17).

7. The laboratory constant-pressure continuous reaction apparatus according to claim 1, characterized in that, The reactor (1) is a glass pressure reactor.

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