Atmosphere-controllable sealing bottle plug

Abstract

The utility model relates to an atmosphere-controllable sealing bottle plug which can be used in a microwave instrument, in particular to a microwave single-die-cavity instrument suitable for micro-dose reaction. Specifically, the reaction container comprises a bottle plug, an air injection pipe sealing screw plug, an air injection pipe, an O-shaped sealing ring and a pressure relief plug structure, round holes are formed in the bottle plug, the air injection pipe sealing screw plug and the pressure relief plug structure, and the round holes are communicated with the air injection pipe, so that the interior of the reaction container is communicated with air outside a microwave resonant cavity. The other end of the gas injection pipe is connected with the three-way valve and the gas pump and is matched with the indication of the pressure sensor, so that the working condition environments such as gas injection, gas washing and gas release in the reaction container can be controlled on the premise of keeping the reaction container sealed, and the working condition environments in the reaction container can be independently realized or compositely realized according to the control; smooth and simplified experimental reaction of expensive, weak-polarity and other tiny-dose reactants is greatly met.

Description

Technical Field

[0001] The utility model relates to the field of container sealing, in particular to a sealing bottle stopper with controllable atmosphere. Background Art

[0002] For many chemical reactions, the microwave heating method has unparalleled advantages in improving the reaction rate, reducing side reactions, and increasing the yield compared to the traditional heating method. Single-mode microwave instruments are typical representatives. Single-mode microwave instruments exhibit significant advantages compared to traditional heating equipment and multi-mode microwave technologies due to their rapid and uniform heating ability, high thermal energy utilization rate, precise temperature control, operational flexibility, and significant improvement in the quality of experimental products. These characteristics not only accelerate the reaction rate, improve the automation and controllability of experiments, but also enhance the reproducibility of reactions, making them an indispensable tool in many fields such as organic synthesis, pharmaceutical chemistry, materials science, and analytical chemistry.

[0003] When performing chemical reactions in a single-mode microwave resonator cavity, the temperature required for the reaction often exceeds the boiling point of the experimental solvent. At the same time, the reaction process faces experimental requirements such as isolating water and oxygen, which require evacuating the vacuum or filling the entire reaction vessel with inert gas for atmosphere protection, or adjusting the gas in the reaction vessel before or during the reaction, performing operations such as pressurization and depressurization, or collecting and analyzing the components of the gas generated during or after the reaction. Therefore, while the reaction vessel needs to be strictly sealed to ensure airtightness, it is necessary to retain a controllable gas inlet and outlet channel and effectively prevent problems such as gas leakage caused by the influence or damage of the overall sealing performance under high temperature and high pressure. Due to the characteristics of microwave transmission and resonance, microwaves must be confined within a microwave resonator cavity made of metal material. Moreover, the physical size of a single-mode microwave resonator cavity is very small compared to multi-mode microwave instruments or other ordinary microwave instruments. It is very difficult to implement functions such as high-pressure sealing, gas injection and pressurization, pressure relief, gas washing, and vacuum pumping of the reaction vessel, which are easily achieved in the conventional size of ordinary instruments, on a single-mode microwave cavity instrument.

[0004] Therefore, our company independently developed a sealing bottle stopper with controllable atmosphere. This bottle stopper can be used in a single-mode microwave resonator cavity, and can meet the requirements of individual working conditions and combined working conditions such as high-pressure sealing, gas injection and pressurization, pressure relief, gas washing, and vacuum pumping inside the reaction vessel in the cavity. Moreover, under the above working conditions, the working conditions can be controllably adjusted or changed according to experimental requirements, greatly meeting the smoothness and simplification of experiments with expensive, weakly polar, and other small-dose reactants. Summary of the Invention

[0005] The technical problem to be solved by the present utility model is to provide a sealed bottle stopper for a reaction vessel that can be used in a single-mode microwave resonator, has a good airtightness, and has a gas passage at the same time.

[0006] An atmosphere-controlled sealed bottle stopper, characterized in that it includes a bottle stopper, an injection tube sealing plug, an injection tube, an O-ring, and a pressure relief plug. The bottle stopper and the injection tube sealing plug connect the injection tube to pass through the injection tube sealing plug. The bottle stopper is connected to the pressure relief plug, and the O-ring is installed in the groove at the lower part of the bottle stopper.

[0007] The main body of the bottle stopper is a cylindrical structure, with a stepped protrusion at the top, a flat-bottom threaded hole at the bottom, a first round hole at the center of the flat-bottom threaded hole, a threaded hole at the center position of the side surface of the larger-diameter cylinder, and a second round hole at the center of the threaded hole. The first round hole and the second round hole are connected and have the same aperture.

[0008] The cross-section of the injection tube sealing plug is T-shaped, composed of two co-centered cylinders with different diameters. The smaller-diameter cylinder has an external thread on the outside and a through-hole at the center. The injection tube passes through the through-hole at the center of the injection tube sealing plug.

[0009] One end of the injection tube nozzle has an end face, and a small round hole is at the center of the end face. The end face of the injection tube nozzle is located at the bottom surface of the external-threaded cylinder of the injection tube sealing plug, and is pressed by the external thread of the injection tube sealing plug against the bottom plane of the side threaded hole of the bottle stopper to maintain the connection. The communication holes in the center and side of the bottle stopper are connected to the injection tube through the small round hole at the center of the end face of the injection tube nozzle. The other end of the injection tube passes through the through-hole at the center of the injection tube sealing plug and penetrates the cavity wall of the microwave resonator.

[0010] The cross-section of the pressure relief plug is T-shaped, composed of two co-centered cylinders with different diameters. The larger-diameter cylinder is in the form of a thin sheet. The tail of the smaller-diameter cylinder has an external thread, and a third round hole is at the center. At the end position of the external thread close to the larger-diameter cylinder, a fourth round hole is provided from the surface of the cylinder towards the center of the circle. The third round hole and the fourth round hole are connected and have the same aperture.

[0011] The bottle stopper has a cross-section of "dry" type, composed of two cylinders with two different diameters.

[0012] The injection tube sealing plug and the pressure relief plug are in a vertical structure.

[0013] The injection tube sealing plug and the bottle stopper are in a vertical structure.

[0014] Technical effect:

[0015] It is used for the sealing of the reaction vessel inside the single-mode microwave resonator, and while ensuring the sealing, it can realize the atmosphere-controlled experimental conditions such as gas injection and pressurization, pressure relief, gas washing, and vacuum pumping in the reaction vessel as required.

[0016] According to different requirements of experimental conditions, when it is necessary to achieve a reaction state where the reaction temperature exceeds the boiling point of the solvent and the solvent still remains non-boiling, reducing gas or reaction-involved gas or inert gas can be continuously injected according to the numerical display of the pressure sensor to make the pressure in the reaction vessel exceed the initial atmospheric pressure, so as to reach the experimental conditions. In some reaction processes, it is necessary to increase the pressure value inside the reaction vessel. At this time, the gas injection function is turned on, and gas is injected according to the numerical display of the pressure sensor to increase the pressure inside the reaction vessel to reach the experimental conditions.

[0017] According to different requirements of experimental conditions, by pre-injecting reducing gas such as hydrogen or reaction-involved gas such as carbon dioxide, oxygen or inert gas such as nitrogen or argon, deflating, re-injecting the gas, and re-deflating, and repeatedly washing the gas in this way, it is possible to ensure that water and air are completely isolated in the reaction vessel and maintain a pure gas environment inside the reaction vessel.

[0018] According to different requirements of experimental conditions, an external vacuum pump can be used to perform a vacuum experiment on the sealed reaction vessel before or during the reaction, so as to ensure isolation of water, air or gases generated during the reaction and other atmosphere environments that interfere with the reaction, and ensure that the experiment is carried out in a vacuum environment.

[0019] After the high-pressure and high-temperature reaction is completed and the temperature inside the reaction vessel drops below the boiling point of the solvent or meets the requirements of safe experimental conditions, the pressure relief function needs to be turned on at this time. After the pressure inside the reaction vessel reaches the standard atmospheric pressure, the reaction vessel is opened to ensure the integrity of the experimental product, the safety of the experimental instruments and personnel. Specific implementation mode

[0020] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0021] The present invention provides an atmosphere-controllable sealed bottle stopper, which is characterized in that it includes a bottle stopper 1, an injection pipe sealing plug 2, an injection pipe 3, an O-ring 4, and a pressure relief plug 5.

[0022] The base 7 is placed in the microwave resonator cavity 8. The reaction vessel 6 is vertically placed on the base 7. The bottle stopper 1 is installed at the mouth of the reaction vessel 6. The lower half of the bottle stopper 1 is located inside the mouth of the reaction vessel 6. The lower half of the bottle stopper 1 has grooves, and an O-ring seal 4 is installed in the grooves. The O-ring seal 4 is in close contact with the inner wall of the reaction vessel 6 to play a sealing role. The top surface of the bottle stopper 1 is in contact with the bottom surface of the pressure sensor 9, and the pressure sensor 9 constantly feeds back the pressure value inside the reaction vessel 6. One end of the gas injection pipe 3 has an end face with a small round hole in the center. The gas injection pipe 3 passes through the central through hole of the gas injection pipe sealing plug 2. The end face of the gas injection pipe 3 is located at the bottom surface of the outer threaded cylindrical end of the gas injection pipe sealing plug 2 and is pressed against the bottom plane of the side threaded hole of the bottle stopper 1 by the external thread of the gas injection pipe sealing plug 2 to maintain the connection. The communication holes in the center and side of the bottle stopper 1 are connected to the gas injection pipe 3 through the small round hole in the center of the end face of the gas injection pipe 3. The other end of the gas injection pipe 3 passes through the gas injection pipe sealing plug 2 and the wall of the microwave resonator cavity 8 and is connected to an external three-way valve. The other end of the three-way valve is connected to an air pump or a gas cylinder. The three-way valve has three states: 0° is the normally closed state. At this time, neither the air pump or gas cylinder nor the gas injection pipe is connected to the outside. After rotating 90° counterclockwise, the outside is connected to the gas injection pipe 3. At this time, the air pump or gas cylinder is not connected to the gas injection pipe 3. After rotating 90° clockwise, the air pump or gas cylinder is connected to the gas injection pipe 3. At this time, the outside is not connected to the gas injection pipe 3. The pressure relief plug 5 is screwed into the central threaded hole at the bottom of the bottle stopper 1 by a threaded connection method. There are communication holes in the center of the stud and on the side of the root of the stud of the pressure relief plug 5. There is a 0.1 - 0.9 MM gap between the flat surface of the plug cap of the pressure relief plug 5 and the bottom surface of the bottle stopper 1.

[0023] When conducting an air isolation experiment, before the reaction starts, the three-way valve is rotated 90° clockwise and the air pump or gas cylinder is opened to pre-inject argon or other inert gases into the reaction vessel 6. When the value displayed by the pressure sensor 9 reaches 1 MPa, the three-way valve is returned to 0° and then rotated 90° counterclockwise. The connection between the air pump or gas cylinder and the gas injection pipe 3 is closed and the nitrogen injection state is stopped. At the same time, the outside is connected to the gas injection pipe 3. The relative pressure of the mixed gas inside the reaction vessel 6 will quickly become the same as the outside and become 0.0 MPa, and the pressure relief state automatically stops. After repeating the above operations multiple times to meet the experimental conditions inside the reaction vessel 6, normal experiments can be started. At this time, there is a 0.1 - 2.0 MM gap between the flat surface of the plug cap of the pressure relief plug 5 and the bottom surface of the bottle stopper 1.

[0024] When conducting a vacuum pumping experiment, before the reaction starts, the three-way valve is rotated 90° clockwise and a vacuum pump is opened to pump air from the reaction vessel 6. When the gauge of the vacuum pump reaches the limit, the three-way valve is returned to 0°. The connection between the vacuum pump and the gas injection pipe 3 is closed and the vacuum pumping state is stopped. After repeating the above operations multiple times to meet the experimental conditions inside the reaction vessel 6, normal experiments can be started. At this time, there is a 0.1 - 2.0 MM gap between the flat surface of the plug cap of the pressure relief plug 5 and the bottom surface of the bottle stopper 1.

[0025] Ordinary high-pressure and normal-temperature experiments often have requirements for the pressure value inside the reaction vessel 6. According to different experimental reactions and working conditions, air injection or air release is carried out. When injecting air or nitrogen according to the requirements of the experimental working conditions, the three-way valve is rotated 90° clockwise to open the air pump or gas cylinder to inject air or nitrogen into the reaction vessel 6. When the value displayed by the pressure sensor 9 reaches the experimental working condition, the three-way valve returns to 0° to stop air injection. During the process of the experimental reaction, when it is necessary to increase the pressure in the reaction vessel 6, the above operations are repeated multiple times, and air injection stops after reaching the requirements of the experimental working condition. After the experimental reaction is completed, before extracting the reactants, the three-way valve is rotated 90° counterclockwise to connect the outside with the injection pipe 3. When the value displayed by the pressure sensor 9 is 0.0 MPa, then the bottle stopper 1 is pulled out to avoid loss or damage caused by the reactants spraying out with the high-pressure environment. At this time, the gap between the flat surface of the plug nut of the pressure relief plug 5 and the bottom surface of the bottle stopper 1 is 0.1 - 2.0 mm.

[0026] The high-pressure and high-temperature experimental reaction is the same as the ordinary high-pressure and normal-temperature reaction in operation. However, during the reaction process, the high temperature will soften the flat surface of the plug nut of the pressure relief plug 5. At the same time, under the action of high pressure, the flat surface of the plug nut will bend upward, and the flat surface of the plug nut will be pressed tightly against the bottom surface of the bottle stopper 1 to achieve a sealing effect, effectively isolating the high-temperature and high-pressure water vapor, high-temperature and high-pressure acids, alkalis or organic corrosive gases in the reaction vessel 6, completely avoiding the high-temperature and high-pressure gases from passing through the center and side communication ports of the bottle stopper 1 to soften and corrode the injection pipe, thereby causing extreme situations such as the explosion of the experimental reaction bottle, leakage of reactants, damage to experimental equipment and even injury to people. At this time, the gap between the flat surface of the plug nut of the pressure relief plug 5 and the bottom surface of the bottle stopper 1 is 0.1 - 0.9 mm.

[0027] The present utility model provides an atmosphere-controllable sealing bottle stopper, which can be used inside a microwave instrument or other experimental instruments that require sealing. According to different experimental working conditions, it can cooperate with sensors such as pressure sensors, and can use functions such as high-pressure sealing, air injection and pressurization, pressure relief, gas washing, and vacuum pumping alone or in combination and controllably. Its technical feature is that the adjustable pressure relief plug will deform upward under a certain temperature and pressure reaction state to seal the "dry"-shaped cylindrical bottom end surface of the bottle stopper, blocking the gas passage to prevent air leakage. At the same time, it bears the huge pressure in the reaction system, sharing the pressure borne by the sealing plug of the injection pipe, making the sealing plug of the injection pipe hardly stressed, improving the pressure resistance performance of the whole system, and reducing the risk of air leakage caused by the softening of the injection pipe at high temperature and being pushed open and disassembled by high air pressure. Through experimental verification, it can work continuously for a long time at 5 MPa (50 atm, 50 bar).

[0028] Based on the above technical solutions, the present utility model can also be improved as follows.

[0029] Further, the communication holes in the center and on the side of the bottle stopper 1 are changed from 90° to other angles.

[0030] Furthermore, the communication holes at the center and side of the stud of the pressure relief plug 5 are changed from 90° to other angles.

[0031] Furthermore, the threaded connection and compression sealing method between the gas injection pipe 3, the bottle stopper 1, and the gas injection pipe sealing plug 2 can be changed to snap-type compression sealing or integral injection molding.

[0032] Furthermore, the lower half of the bottle stopper 1 has a groove and an O-ring 4, which can be changed to multiple grooves and multiple O-rings 4, and the O-ring 4 can be changed to other material seals.

[0033] Furthermore, the material of an atmosphere-controllable sealed bottle stopper is all PTFE, and part or all of the materials can be changed to other engineering plastics, such as PFA, TFM, PEEK, or non-metallic materials such as quartz, glass, and sapphire.

[0034] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention. Description of the Drawings

[0035] Figure 1 : Cross-sectional view of the bottle stopper structure cooperation

[0036] Figure 2 : Cross-sectional view showing the small hole structure indication

[0037] In the drawings, the list of components represented by each reference numeral is as follows:

[0038] 1. Bottle stopper, 2. Gas injection pipe sealing plug, 3. Gas injection pipe, 4. O-ring, 5. Pressure relief plug, 6. Reaction vessel, 7. Base, 8. Microwave resonator, 9. Pressure sensor, 101. Round hole, 102. Round hole, 501. Round hole, 502. Round hole.

Claims

1. An atmosphere-controlled sealed bottle stopper, characterized in that: The invention comprises a bottle stopper (1), a gas injection pipe sealing plug (2), a gas injection pipe (3), an O-type sealing ring (4), and a pressure relief plug (5); the bottle stopper (1) and the gas injection pipe sealing plug (2) are connected to the gas injection pipe (3); the gas injection pipe (3) passes through the gas injection pipe sealing plug (2); the bottle stopper (1) and the pressure relief plug (5) are connected; and the O-type sealing ring (4) is installed in a groove at the bottom of the bottle stopper (1).

2. The atmosphere-controlled sealed bottle stopper according to claim 1, characterized in that: The main body of the bottle stopper (1) is a cylindrical structure, with a step-shaped protrusion at the top and a flat-bottomed threaded hole at the bottom. A first circular hole (101) is arranged at the center of the flat-bottomed threaded hole. A threaded hole is arranged at the center of the side surface of the cylinder with a larger diameter, and a second circular hole (102) is arranged at the center of the threaded hole. The first circular hole (101) and the second circular hole (102) are connected and have the same hole diameter.

3. The atmosphere-controlled sealed bottle stopper according to claim 2, characterized in that: The gas injection pipe sealing plug (2) has a T-shaped cross section and is composed of two co-centric cylinders of one larger diameter and one smaller diameter. The cylinder with the smaller diameter is provided with an external thread on the outside and a through hole in the center. The gas injection pipe (3) passes through the through hole in the center of the gas injection pipe sealing plug (2).

4. The atmosphere-controlled sealed bottle stopper according to claim 1, characterized in that: The gas injection pipe (3) has an end face at one end thereof, and a small circular hole at the center of the end face; the end face of the gas injection pipe (3) is located at the bottom surface of the external threaded cylindrical end of the gas injection pipe sealing plug (2), and is pressed against the bottom plane of the side threaded hole of the bottle plug (1) by the external thread of the gas injection pipe sealing plug (2) to maintain the connection; the connecting holes at the center and side of the bottle plug (1) are connected to the gas injection pipe (3) through the small circular hole at the center of the end face of the gas injection pipe (3); the other end of the gas injection pipe (3) passes through the central through hole of the gas injection pipe sealing plug (2) and passes through the cavity wall of the microwave resonance cavity (8).

5. The atmosphere-controlled sealed bottle stopper according to claim 1, characterized in that: The pressure relief plug (5) has a T-shaped cross section and is composed of two cylinders with a larger diameter and a smaller diameter that are co-centered. The cylinder with the larger diameter is in the form of a thin sheet. An external thread is provided at the tail of the cylinder with the smaller diameter, and a third circular hole (501) is provided at the center. A fourth circular hole (502) is provided from the surface of the cylinder toward the center of the circle at the end position of the external thread close to the cylinder with the larger diameter. The third circular hole (501) and the fourth circular hole (502) are connected and have the same hole diameter.

6. The atmosphere-controlled sealed bottle stopper according to claim 1, characterized in that: The bottle stopper (1) has a "dry" cross-section and is composed of two cylinders, one large and one small in diameter.

7. The atmosphere-controlled sealed bottle stopper according to claim 1, characterized in that: The gas injection pipe sealing plug (2) and the pressure relief plug (5) are in a vertical structure.

8. The atmosphere-controlled sealed bottle stopper according to claim 1, characterized in that: The gas injection pipe sealing plug (2) and the bottle plug (1) are in a vertical structure.

Images