A high vacuum line operating system

Abstract

The present invention provides a high vacuum line operating system, comprising a vacuum main pipeline, a first right-angle plug valve, a second right-angle plug valve, a third right-angle plug valve, a fourth right-angle plug valve, a first T-type one-way three-way pipeline plug valve, a second T-type one-way three-way pipeline plug valve, a third T-type one-way three-way pipeline plug valve, a fourth T-type one-way three-way pipeline plug valve, a cold hydrazine, a bellows, a vacuum oil pump, a thermocouple vacuum gauge, a balloon and an inert gas bottle. The present invention can not only introduce inert gas, but also perform multiple operations at the same time, such as transferring a solvent alone, transferring two solvents at the same time, transferring a solvent to three reaction bottles at the same time, and performing vacuuming and solvent transfer operations at the same time.

Description

Technical Field

[0001] The invention belongs to the technical field of solvent transfer, and in particular relates to a high vacuum line operating system. Background Art

[0002] At present, the main anhydrous and oxygen-free laboratory operation technologies for air-sensitive compounds are: Schlenk technology, glove box technology, and high vacuum line technology. The basic principles of Schlenk technology and glove box technology are based on using inert gas to displace the air in the device, while high vacuum line technology uses vacuuming to displace the air in the device. The advantages of high vacuum line technology are: better dehydration and deoxygenation effects, quantitative preservation of reaction products, and the amount of reaction substances operated can be trace, which is more suitable for operating compounds that are particularly sensitive to air. However, the existing conventional high vacuum line system cannot introduce inert gas after the reaction vessel is evacuated, and the function is relatively simple; the interfaces can only be connected through the main pipeline. When the solvent is transferred in vacuum, the main pipeline must be occupied. At this time, the high vacuum line system cannot perform other operations and can only transfer one solvent at the same time. Summary of the invention

[0003] The technical problem to be solved by the present invention is to provide a high vacuum line operating system in view of the above-mentioned deficiencies in the prior art, wherein the high vacuum line operating system can not only introduce inert gas but also perform multiple operations simultaneously.

[0004] In order to solve the above technical problems, the technical solution adopted by the present invention is: a high vacuum line operating system, including a vacuum main pipeline, one end of the vacuum main pipeline is connected to the side wall branch of the first right-angle plug valve, the bottom branch of the first right-angle plug valve is connected to the cold hydrazine, the side wall of the cold hydrazine is connected to the side wall branch of the second right-angle plug valve, and the bottom branch of the second right-angle plug valve is connected to the vacuum oil pump through a bellows; the other end of the vacuum main pipeline is connected to the bottom branch of the first T-type one-way three-way pipeline plug valve, the side wall branch at one end of the first T-type one-way three-way pipeline plug valve is connected to the electric thermocouple vacuum gauge, the side wall branch at the other end of the first T-type one-way three-way pipeline plug valve is connected to the side wall branch of the third right-angle plug valve, and at the other end of the first T-type one-way three-way pipeline plug valve A connecting opening for connecting to a balloon is provided on the tube wall of the side wall branch pipe, and the bottom branch pipe of the third right-angle stopcock valve is connected to an inert gas bottle; the side wall of the vacuum main pipeline is respectively connected to the side wall branch pipe of the second T-type one-way three-way pipeline stopcock valve, the side wall branch pipe of the third T-type one-way three-way pipeline stopcock valve, the side wall branch pipe of the fourth T-type one-way three-way pipeline stopcock valve and the side wall branch pipe of the fourth right-angle stopcock valve in sequence; the other side wall branch pipe of the second T-type one-way three-way pipeline stopcock valve is connected to the bottom branch pipe of the third T-type one-way three-way pipeline stopcock valve, the other side wall branch pipe of the third T-type one-way three-way pipeline stopcock valve is connected to the bottom branch pipe of the fourth T-type one-way three-way pipeline stopcock valve, and the other side wall branch pipe of the fourth T-type one-way three-way pipeline stopcock valve is connected to the bottom branch pipe of the fourth right-angle stopcock valve.

[0005] Preferably, the end of the bottom branch pipe of the second T-type one-way three-way pipe plug valve is integrally connected with a first external ground joint, the end of the bottom branch pipe of the fourth T-type one-way three-way pipe plug valve is integrally connected with a second external ground joint, the end of the bottom branch pipe of the third T-type one-way three-way pipe plug valve is integrally connected with a first internal ground joint, and the end of the bottom branch pipe of the fourth right-angle plug valve is integrally connected with a second internal ground joint.

[0006] Preferably, the first external ground joint, the second external ground joint, the first internal ground joint and the second internal ground joint are all coated with high vacuum ester.

[0007] Preferably, the side wall branch at one end of the first T-type one-way three-way pipeline plug valve is connected to the thermocouple vacuum gauge through a glass ground joint; the connecting opening opened on the tube wall of the side wall branch at the other end of the three-way pipeline plug valve is connected to the balloon through a glass ground joint; the bottom branch at the lower end of the first right-angle plug valve is connected to the cold hydrazine through a glass ground joint; the side wall of the cold hydrazine is connected to the side wall branch of the second right-angle plug valve through a glass ground joint.

[0008] Preferably, each of the ground glass joints is coated with high vacuum ester.

[0009] Preferably, both ends of the bellows are provided with vacuum quick-release connectors, which are respectively connected to the bottom branch pipe at the lower end of the first right-angle stopcock valve and the vacuum oil pump.

[0010] Preferably, the connection between the vacuum main pipeline and the side wall branch of the first right-angle plug valve is integrally formed; the connection between the vacuum main pipeline and the bottom branch of the first T-type one-way three-way pipeline plug valve is integrally formed; the side wall of the vacuum main pipeline is respectively integrally formed with the side wall branches of the second T-type one-way three-way pipeline plug valve, the third T-type one-way three-way pipeline plug valve, the fourth T-type one-way three-way pipeline plug valve and the fourth right-angle plug valve; the other side wall branch of the second T-type one-way three-way pipeline plug valve is integrally formed with The connection of the bottom branch pipe of the third T-type one-way three-way pipeline plug valve is integrally formed, the connection of the other side wall branch pipe of the third T-type one-way three-way pipeline plug valve to the bottom branch pipe of the fourth T-type one-way three-way pipeline plug valve is integrally formed, the connection of the other side wall branch pipe of the fourth T-type one-way three-way pipeline plug valve to the bottom branch pipe of the fourth right-angle plug valve is integrally formed; the connection of the side wall branch pipe at the other end of the three-way pipeline plug valve and the side wall branch pipe of the third right-angle plug valve is integrally formed.

[0011] Preferably, the materials of the first T-type one-way three-way pipeline plug valve, the second T-type one-way three-way pipeline plug valve, the third T-type one-way three-way pipeline plug valve, the fourth T-type one-way three-way pipeline plug valve, the first right-angle plug valve, the second right-angle plug valve, the third right-angle plug valve and the fourth right-angle plug valve are all high borosilicate glass; and each plug valve is coated with high vacuum ester.

[0012] Preferably, it is characterized in that the high vacuum line operating system is fixed on a bracket.

[0013] Compared with the prior art, the present invention has the following advantages:

[0014] 1. The main components of the present invention are integrally formed. The materials of each plug valve are high borosilicate glass. Each ground joint is coated with high vacuum ester. The vacuum degree can be below 0.1Pa, which is much lower than the vacuum degree of anhydrous and oxygen-free operating systems such as double-row pipes (vacuum degree greater than 100Pa). This system is better for dehydration and deoxygenation in anhydrous and oxygen-free experiments.

[0015] 2. In the present invention, inert gas can be introduced into the vacuum reaction device through the connected balloon, which overcomes the disadvantage that the traditional high vacuum line cannot introduce inert gas.

[0016] 3. The present invention can connect each interface to the main vacuum pipeline or to the adjacent interface by adjusting each stopcock valve, so that multiple operations can be performed simultaneously, such as transferring one solvent alone, transferring two solvents at the same time, transferring one solvent to three reaction bottles at the same time, and performing vacuuming and solvent transfer operations at the same time.

[0017] The present invention is further described in detail below with reference to the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a structural schematic diagram of the present invention.

[0019] Figure 2 This is the application scenario of embodiment 2 of the present invention.

[0020] Figure 3 This is the application scenario of embodiment 3 of the present invention.

[0021] Figure 4 This is the application scenario of embodiment 4 of the present invention.

[0022] Figure 5 This is the application scenario of embodiment 5 of the present invention.

[0023] Description of reference numerals:

[0024] 1—vacuum main pipeline; 2—first right angle plug valve;

[0025] 3—cold hydrazine; 4—first T-type one-way three-way pipeline cock valve;

[0026] 5—Second right-angle plug valve; 6—Bellows;

[0027] 7—vacuum oil pump; 8—thermocouple vacuum gauge;

[0028] 9—third right-angle plug valve; 10—balloon;

[0029] 11—Vacuum quick-release connector; 12—Inert gas bottle;

[0030] 13—Second T-type one-way three-way pipeline plug valve; 14—Third T-type one-way three-way pipeline plug valve;

[0031] 15—the fourth T-type one-way three-way pipeline cock valve; 16—the fourth right-angle cock valve;

[0032] 17—first external ground joint; 18—second external ground joint;

[0033] 19—first internal ground joint; 20—second internal ground joint;

[0034] 21—Stand. DETAILED DESCRIPTION Example 1

[0035] The high vacuum line operating system of the present invention is as follows: Figure 1 As shown, it includes a vacuum main pipeline 1, one end of which is connected to the side wall branch of the first right-angle plug valve 2, the bottom branch of the first right-angle plug valve 2 is communicated with the cold hydrazine 3, the side wall of the cold hydrazine 3 is communicated with the side wall branch of the second right-angle plug valve 5, and the bottom branch of the second right-angle plug valve 5 is connected to the vacuum oil pump 7 through a bellows 6; the other end of the vacuum main pipeline 1 is connected to the bottom branch of the first T-type one-way three-way pipeline plug valve 4, the side wall branch at one end of the first T-type one-way three-way pipeline plug valve 4 is connected to the electric thermocouple vacuum gauge 8, the side wall branch at the other end of the first T-type one-way three-way pipeline plug valve 4 is connected to the side wall branch of the third right-angle plug valve 9, and a connection opening for connecting a balloon 10 is opened on the pipe wall of the side wall branch at the other end of the first T-type one-way three-way pipeline plug valve 4 mouth, the bottom branch of the third right-angle plug valve 9 is connected to the inert gas bottle 12; the side walls of the vacuum main pipeline 1 are respectively connected to the side wall branches of the second T-type one-way three-way pipeline plug valve 13, the side wall branches of the third T-type one-way three-way pipeline plug valve 14, the side wall branches of the fourth T-type one-way three-way pipeline plug valve 15 and the side wall branches of the fourth right-angle plug valve 16 in sequence; the other side wall branch of the second T-type one-way three-way pipeline plug valve 13 is connected to the bottom branch of the third T-type one-way three-way pipeline plug valve 14, the other side wall branch of the third T-type one-way three-way pipeline plug valve 14 is connected to the bottom branch of the fourth T-type one-way three-way pipeline plug valve 15, and the other side wall branch of the fourth T-type one-way three-way pipeline plug valve 15 is connected to the bottom branch of the fourth right-angle plug valve 16.

[0036] In the present invention, the end of the bottom branch pipe of the second T-type one-way three-way pipeline plug valve 13 is integrally connected with a first external ground joint 17, the end of the bottom branch pipe of the fourth T-type one-way three-way pipeline plug valve 15 is integrally connected with a second external ground joint 18, the end of the bottom branch pipe of the third T-type one-way three-way pipeline plug valve 14 is integrally connected with a first internal ground joint 19, and the end of the bottom branch pipe of the fourth right-angle plug valve 16 is integrally connected with a second internal ground joint 20.

[0037] In the present invention, the first external ground joint 17, the second external ground joint 18, the first internal ground joint 19 and the second internal ground joint 20 are all coated with high vacuum ester.

[0038] In the present invention, the side wall branch pipe at one end of the first T-type one-way three-way pipeline plug valve 4 is connected to the thermocouple vacuum gauge 8 through a glass ground joint; the connecting opening opened on the pipe wall of the side wall branch pipe at the other end of the three-way pipeline plug valve 4 is connected to the balloon 10 through a glass ground joint; the bottom branch pipe at the lower end of the first right-angle plug valve 2 is connected to the cold hydrazine 3 through a glass ground joint; the side wall of the cold hydrazine 3 is connected to the side wall branch pipe of the second right-angle plug valve 5 through a glass ground joint.

[0039] In the present invention, each of the glass ground joints is coated with high vacuum ester.

[0040] In the present invention, both ends of the bellows 6 are provided with vacuum quick-release connectors 11, which are respectively connected to the bottom branch pipe at the lower end of the first right-angle cock valve 2 and the vacuum oil pump 7.

[0041] In the present invention, the connection between the vacuum main pipeline 1 and the side wall branch of the first right-angle plug valve 2 is integrally formed; the connection between the vacuum main pipeline 1 and the bottom branch of the first T-type one-way three-way pipeline plug valve 4 is integrally formed; the side wall of the vacuum main pipeline 1 is respectively connected to the side wall branches of the second T-type one-way three-way pipeline plug valve 13, the third T-type one-way three-way pipeline plug valve 14, the fourth T-type one-way three-way pipeline plug valve 15 and the fourth right-angle plug valve 16 are integrally formed; the other side wall branch of the second T-type one-way three-way pipeline plug valve 13 The connection between the pipe and the bottom branch of the third T-type one-way three-way pipeline plug valve 14 is integrally formed, the connection between the other side wall branch of the third T-type one-way three-way pipeline plug valve 14 and the bottom branch of the fourth T-type one-way three-way pipeline plug valve 15 is integrally formed, and the connection between the other side wall branch of the fourth T-type one-way three-way pipeline plug valve 15 and the bottom branch of the fourth right-angle plug valve 16 is integrally formed; the connection between the side wall branch at the other end of the three-way pipeline plug valve 4 and the side wall branch of the third right-angle plug valve 9 is integrally formed.

[0042] In the present invention, the materials of the first T-type one-way three-way pipeline plug valve 4, the second T-type one-way three-way pipeline plug valve 13, the third T-type one-way three-way pipeline plug valve 14, the fourth T-type one-way three-way pipeline plug valve 15, the first right-angle plug valve 2, the second right-angle plug valve 5, the third right-angle plug valve 9 and the fourth right-angle plug valve 16 are all high borosilicate glass; each plug valve is coated with high vacuum ester.

[0043] In the present invention, the high vacuum line operating system is fixed on the bracket 21. Example 2

[0044] This embodiment provides an application scenario of the high vacuum line operating system of embodiment 1, such as Figure 2 As shown, the operation method of transferring a solvent under vacuum conditions (the solvent gas in the solvent storage bottle B is transferred to the reaction bottle A) is as follows:

[0045] S1, close the fourth T-shaped one-way three-way pipeline cock valve 15 and the fourth right-angle cock valve 16 at the idle interface;

[0046] S2, insert the cold hydrazine 3 into the Doerr bottle filled with liquid nitrogen, and after sufficient cooling, open the vacuum oil pump 7, the first right-angle stopcock valve 2 and the second right-angle stopcock valve 5, and the high vacuum line operating system starts to evacuate;

[0047] S3, after applying vacuum ester evenly on the ground joints of the reaction bottle A and the solvent storage bottle B, they are connected to the first outer ground joint 17 and the first inner ground joint 19 respectively, and the second T-type one-way three-way pipeline cock valve 13 and the third T-type one-way three-way pipeline cock valve 14 are adjusted to make the first outer ground joint 17 and the first inner ground joint 19 connected to the vacuum main pipeline 1, and the Teflon cock on the reaction bottle A is opened to evacuate the reaction bottle A;

[0048] S4, adjust the first T-type one-way three-way pipeline cock valve 4 to connect the thermocouple vacuum gauge 8 with the vacuum main pipeline 1, measure the vacuum degree in the system, and start transferring the solvent when the vacuum degree reaches about 1Pa;

[0049] S5, when transferring the solvent, the reaction bottle A is cooled with liquid nitrogen, and the second T-shaped one-way three-way pipeline cock valve 13 is adjusted to connect to the first internal ground joint 19, and the third T-shaped one-way three-way pipeline cock valve 14 is closed at the same time;

[0050] S6, open the Teflon stopcock on the solvent storage bottle B, and the solvent gas inside the solvent storage bottle B quickly enters the reaction bottle A along the channel. Since the reaction bottle A is cooled by liquid nitrogen at an extremely low temperature, the solvent gas is quickly cooled into the reaction bottle A;

[0051] S7. When the amount of cooled solvent in reaction bottle A reaches the required volume, close the Teflon stopcocks on reaction bottle A and solvent storage bottle B;

[0052] S8. Since reaction bottle A is cooled by liquid nitrogen, the solvent gas transferred at an extremely low temperature is frozen into a solid. Therefore, after the dissolved transfer is completed, the reaction bottle A is removed and quickly placed in an ethanol bath at room temperature to thaw the solvent in the reaction bottle A. At this point, the solvent transfer under vacuum conditions is completed.

[0053] If inert gas needs to be introduced into reaction bottle A, after the solvent is thawed, evenly apply vacuum ester to the ground joint of reaction bottle A, connect it to the first external ground joint 17, adjust the second T-type one-way three-way pipe stopcock valve 13, so that the first external ground joint 17 is connected to the vacuum main pipeline 1, and evacuate the interface of reaction bottle A. At this time, the third T-type one-way three-way pipe stopcock valve 14, the fourth T-type one-way three-way pipe stopcock valve 15, and the fourth right-angle stopcock valve 16 are in a closed state; since the reaction bottle A is in a vacuum state, there is no need to open the Teflon stopcock of reaction bottle A at this time.

[0054] When the vacuum degree of the system reaches about 1Pa, start to introduce inert gas into the reaction bottle A: close the first right-angle stopcock valve 2 to prevent the inert gas from being sucked into the vacuum oil pump 7; open the third right-angle stopcock valve 9 to allow the inert gas to pass into the balloon 10, and when the balloon 10 is full, close the third right-angle stopcock valve 9; adjust the first T-type one-way three-way pipeline stopcock valve 4 to connect the vacuum main pipeline 1 with the balloon; at this time, the vacuum main pipeline 1 is in a vacuum state, and the gas in the balloon 10 will automatically fill into the vacuum main pipeline 1; open the Teflon stopcock on the reaction bottle A, and at this time the inert gas is introduced into the reaction bottle A, close the Teflon stopcock of the reaction bottle A, and the inert gas is introduced. When the inert gas is introduced into the reaction bottle A, since the pressure inside and outside the system is the same, at this time, the interface between the reaction bottle A and the first external ground joint 17 should be fixed with a clip to prevent the reaction bottle from falling off. Example 3

[0055] This embodiment provides an application scenario of the high vacuum line operating system of embodiment 1, such as Figure 3 As shown, the operation method of transferring two different solvents at the same time under vacuum conditions (the solvent gas in the solvent storage bottle B is transferred to the reaction bottle A, and the solvent gas in the solvent storage bottle D is transferred to the reaction bottle C) is as follows:

[0056] The operation steps of transferring the solvent gas in the solvent storage bottle B to the reaction bottle A in this embodiment are the same as the operation steps of transferring the solvent gas in the solvent storage bottle B to the reaction bottle A in Example 2;

[0057] While the solvent gas in the solvent storage bottle B is transferred to the reaction bottle A, the solvent gas in the solvent storage bottle D can be transferred to the reaction bottle C. The specific method is as follows:

[0058] During the process of transferring the solvent in reaction bottle B to reaction bottle A, reaction bottle A and solvent storage bottle B are disconnected from the vacuum line system. Therefore, according to the method in Example 2, reaction bottle C and solvent storage bottle D are operated to transfer the solvent. At this time, reaction bottle C and solvent storage bottle D, reaction bottle A and solvent storage bottle B will not interfere with each other. Example 4

[0059] This embodiment provides an application scenario of the high vacuum line operating system of embodiment 1, such as Figure 4 As shown, a solvent is transferred to three reaction bottles at the same time under vacuum conditions (the solvent gas in the solvent storage bottle D is transferred to the reaction bottles A, E and C at the same time). Operation method:

[0060] S1, the second T-type one-way three-way pipeline plug valve 13, the third T-type one-way three-way pipeline plug valve 14, the fourth T-type one-way three-way pipeline plug valve 15, and the fourth right-angle plug valve 16 are in the closed state;

[0061] S2, insert the cold hydrazine 3 into the Doerr bottle filled with liquid nitrogen, and after sufficient cooling, open the vacuum oil pump 7 and the first right-angle stopcock valve 2 and the second right-angle stopcock valve 5, and the high vacuum line operating system starts to evacuate;

[0062] S3, after applying vacuum ester evenly on the ground joints of reaction bottle A, reaction bottle E, reaction bottle C and solvent storage bottle D, they are respectively connected to the first outer ground joint 17, the first inner ground joint 19, the second outer ground joint 18, and the second inner ground joint 20, and the second T-type one-way three-way pipeline cock valve 13, the third T-type one-way three-way pipeline cock valve 14, the fourth T-type one-way three-way pipeline cock valve 15, and the fourth right-angle cock valve 16 are adjusted to make the first outer ground joint 17, the first inner ground joint 19, the second outer ground joint 18, and the second inner ground joint 20 connected to the vacuum main pipeline 1, and the Teflon cocks on the reaction bottle A, the reaction bottle E, and the reaction bottle C are opened to evacuate the reaction bottle A, the reaction bottle E, and the reaction bottle C;

[0063] S4, adjust the first T-type one-way three-way pipeline cock valve 4 to connect the thermocouple vacuum gauge 8 with the vacuum main pipeline 1, measure the vacuum degree in the system, and start transferring the solvent when the vacuum degree reaches about 1Pa;

[0064] S5. When transferring the solvent, the reaction flask A, the reaction flask E and the reaction flask C are cooled with liquid nitrogen, and the second T-type one-way three-way pipeline cock valve 13, the third T-type one-way three-way pipeline cock valve 14 and the fourth T-type one-way three-way pipeline cock valve 15 are adjusted to connect the first inner ground joint 19, the second outer ground joint 18 and the second inner ground joint 20 respectively, and the fourth right-angle cock valve 16 is closed at the same time;

[0065] S6. Open the Teflon stopcock on the solvent storage bottle D, and the solvent gas inside the solvent storage bottle D quickly enters the reaction bottle A, the reaction bottle E, and the reaction bottle C along the channel. Since the reaction bottles A, the reaction bottles E, and the reaction bottles C are cooled by liquid nitrogen at extremely low temperatures, the solvent gas is quickly cooled into the reaction bottles A, the reaction bottles E, and the reaction bottles C;

[0066] S7. When the amount of cooled solvent in the reaction bottle reaches the required volume, close the Teflon stopcocks on the reaction bottle A, reaction bottle E, reaction bottle C and solvent storage bottle D;

[0067] S8. Since reaction flask A, reaction flask E, and reaction flask C are cooled by liquid nitrogen, the solvent gas transferred at an extremely low temperature is frozen into a solid. Therefore, after the dissolved transfer is completed, reaction flask A, reaction flask E, and reaction flask C are removed respectively, and quickly placed in an ethanol bath at room temperature to thaw the solvents in reaction flask A, reaction flask E, and reaction flask C. At this point, the solvent transfer under vacuum conditions is completed. Example 5

[0068] This embodiment provides an application scenario of the high vacuum line operating system of embodiment 1, such as Figure 5 As shown, one ground joint is evacuated to pass inert protective gas while the other two ground joints transfer solvent under vacuum (reaction bottle A is evacuated at the first outer ground joint, reaction bottle C and solvent storage bottle D transfer solvent gas at the second outer ground joint 18 and the second inner ground joint 20). Operation method:

[0069] S1, close the third T-type one-way three-way pipeline cock valve 14 at the idle interface;

[0070] S2, insert the cold hydrazine 3 into the Doerr bottle filled with liquid nitrogen, and after sufficient cooling, open the vacuum oil pump 7 and the first right-angle stopcock valve 2 and the second right-angle stopcock valve 5, and the high vacuum line operating system starts to evacuate;

[0071] S3, after applying vacuum ester evenly to the ground joints of the reaction bottle C and the solvent storage bottle D, they are connected to the second outer ground joint 18 and the second inner ground joint 20 respectively, and the fourth T-type one-way three-way pipe cock valve 15 and the fourth right-angle cock valve 16 are adjusted to make the second outer ground joint 18 and the second inner ground joint 20 connected to the vacuum main pipeline 1, and the Teflon cock on the reaction bottle C is opened to evacuate the reaction bottle C;

[0072] S4, adjust the first T-type one-way three-way pipeline cock valve 4 to connect the thermocouple vacuum gauge 8 with the vacuum main pipeline 1, measure the vacuum degree in the system, and start transferring the solvent when the vacuum degree reaches about 1Pa;

[0073] S5, when transferring the solvent, the reaction bottle C is cooled with liquid nitrogen, and the fourth T-shaped one-way three-way pipeline cock valve 15 is adjusted to connect to the second internal ground joint 20, and the fourth right-angle cock valve 16 is closed at the same time;

[0074] S6, open the Teflon stopcock on the solvent storage bottle D, and the solvent gas inside the solvent storage bottle D quickly enters the reaction bottle C along the channel. Since the reaction bottle C is cooled by liquid nitrogen at an extremely low temperature, the solvent gas is quickly cooled into the reaction bottle C;

[0075] S7. When the amount of cooled solvent in the reaction bottle reaches the required volume, close the Teflon stopcocks on the reaction bottle C and the solvent storage bottle D;

[0076] S8. Since reaction bottle C is cooled by liquid nitrogen, the solvent gas transferred at an extremely low temperature is frozen into a solid. Therefore, after the dissolved transfer is completed, the reaction bottle C is removed and quickly placed in an ethanol bath at room temperature to thaw the solvent in the reaction bottle C. At this point, the solvent transfer under vacuum conditions is completed.

[0077] During the process of transferring the solution to the reaction bottle C, since the reaction bottle C and the solvent storage bottle D are disconnected from the vacuum line system, the inert gas can be introduced into the reaction bottle A at the same time: after evenly applying vacuum ester to the ground joint of the reaction bottle A, connect it to the first external ground joint 17, adjust the second T-type one-way three-way pipe stopcock valve 13 to connect the first external ground joint 17 with the vacuum main pipeline 1, and at the same time open the Teflon stopcock on the reaction bottle A to evacuate the reaction bottle A. At this time, the third T-type one-way three-way pipe stopcock valve 14 is in a closed state.

[0078] When the vacuum degree of the system reaches about 1Pa, start to introduce inert gas into the reaction bottle A: close the first right-angle stopcock valve 2 to prevent the inert gas from being sucked into the vacuum oil pump 7; open the third right-angle stopcock valve 9 to allow the inert gas to pass into the balloon 10, and when the balloon is full, close the third right-angle stopcock valve 9; adjust the first T-type one-way three-way pipeline stopcock valve 4 to connect the vacuum main pipeline 1 with the balloon 10; at this time, the vacuum line system is in a vacuum state, and the gas in the balloon 10 will automatically fill the vacuum line system and the reaction bottle A; after the ventilation is completed, close the Teflon stopcock of the reaction bottle A, and the inert gas is introduced. When the inert gas is introduced into the reaction bottle A, since the pressure inside and outside the system is the same, the interface between the reaction bottle A and the first external ground joint 17 should be fixed with a clip to prevent the reaction bottle from falling off.

[0079] The above is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent change made to the above embodiment according to the technical essence of the invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. A high vacuum line operating system, characterized in that: The invention comprises a vacuum main pipeline (1), one end of which is connected to a side wall branch of a first right-angle plug valve (2), the bottom branch of the first right-angle plug valve (2) is communicated with a cold hydrazine (3), the side wall of the cold hydrazine (3) is communicated with a side wall branch of a second right-angle plug valve (5), and the bottom branch of the second right-angle plug valve (5) is connected to a vacuum oil pump (7) via a bellows (6); the other end of the vacuum main pipeline (1) is connected to a bottom branch of a first T-type one-way three-way pipeline plug valve (4), one end of the side wall branch of the first T-type one-way three-way pipeline plug valve (4) is connected to an electric thermocouple vacuum gauge (8), the other end of the side wall branch of the first T-type one-way three-way pipeline plug valve (4) is connected to a side wall branch of a third right-angle plug valve (9), and a connecting balloon (10) is provided on the pipe wall of the side wall branch of the other end of the first T-type one-way three-way pipeline plug valve (4). The bottom branch of the third right-angle plug valve (9) is connected to the inert gas bottle (12); the side wall of the vacuum main pipeline (1) is respectively connected to the side wall branch of the second T-type one-way three-way pipeline plug valve (13), the side wall branch of the third T-type one-way three-way pipeline plug valve (14), the side wall branch of the fourth T-type one-way three-way pipeline plug valve (15) and the side wall branch of the fourth right-angle plug valve (16); the other side wall branch of the second T-type one-way three-way pipeline plug valve (13) is connected to the bottom branch of the third T-type one-way three-way pipeline plug valve (14), the other side wall branch of the third T-type one-way three-way pipeline plug valve (14) is connected to the bottom branch of the fourth T-type one-way three-way pipeline plug valve (15), and the other side wall branch of the fourth T-type one-way three-way pipeline plug valve (15) is connected to the bottom branch of the fourth right-angle plug valve (16).

2. A high vacuum line operating system according to claim 1, characterized in that: The end of the bottom branch pipe of the second T-shaped one-way three-way pipeline plug valve (13) is integrally connected to a first external ground joint (17), the end of the bottom branch pipe of the fourth T-shaped one-way three-way pipeline plug valve (15) is integrally connected to a second external ground joint (18), the end of the bottom branch pipe of the third T-shaped one-way three-way pipeline plug valve (14) is integrally connected to a first internal ground joint (19), and the end of the bottom branch pipe of the fourth right-angle plug valve (16) is integrally connected to a second internal ground joint (20).

3. A high vacuum line operating system according to claim 2, characterized in that: The first external ground joint (17), the second external ground joint (18), the first internal ground joint (19) and the second internal ground joint (20) are all coated with high vacuum ester.

4. A high vacuum line operating system according to claim 1, characterized in that: A side wall branch pipe at one end of the first T-shaped one-way three-way pipe cock valve (4) is connected to the thermocouple vacuum gauge (8) via a glass ground joint; a connecting opening provided on the pipe wall of the side wall branch pipe at the other end of the first T-shaped one-way three-way pipe cock valve (4) is connected to the balloon (10) via a glass ground joint; a bottom branch pipe at the lower end of the first right-angle cock valve (2) is connected to the cold hydrant (3) via a glass ground joint; and a side wall of the cold hydrant (3) is connected to a side wall branch pipe of the second right-angle cock valve (5) via a glass ground joint.

5. A high vacuum line operating system according to claim 4, characterized in that: Each of the glass ground joints is coated with high vacuum ester.

6. A high vacuum line operating system according to claim 1, characterized in that: Both ends of the bellows (6) are provided with vacuum quick-release connectors (11), which are respectively connected to the bottom branch pipe at the lower end of the first right-angle cock valve (2) and the vacuum oil pump (7).

7. A high vacuum line operating system according to claim 1, characterized in that: The connection between the vacuum main pipeline (1) and the side wall branch of the first right-angle plug valve (2) is integrally formed; the connection between the vacuum main pipeline (1) and the bottom branch of the first T-shaped one-way three-way pipeline plug valve (4) is integrally formed; the connection between the side wall of the vacuum main pipeline (1) and the side wall branches of the second T-shaped one-way three-way pipeline plug valve (13), the third T-shaped one-way three-way pipeline plug valve (14), the fourth T-shaped one-way three-way pipeline plug valve (15) and the fourth right-angle plug valve (16) are integrally formed; the other side wall branch of the second T-shaped one-way three-way pipeline plug valve (13) is integrally formed with the bottom branch of the first T-shaped one-way three-way pipeline plug valve (4). The connection of the bottom branch pipe of the third T-shaped one-way three-way pipeline plug valve (14) is integrally formed, the connection of the other side wall branch pipe of the third T-shaped one-way three-way pipeline plug valve (14) to the bottom branch pipe of the fourth T-shaped one-way three-way pipeline plug valve (15) is integrally formed, and the connection of the other side wall branch pipe of the fourth T-shaped one-way three-way pipeline plug valve (15) to the bottom branch pipe of the fourth right-angle plug valve (16) is integrally formed; the connection of the other end side wall branch pipe of the first T-shaped one-way three-way pipeline plug valve (4) and the side wall branch pipe of the third right-angle plug valve (9) is integrally formed.

8. A high vacuum line operating system according to any one of claims 1 to 7, characterized in that: The materials of the first T-shaped one-way three-way pipeline plug valve (4), the second T-shaped one-way three-way pipeline plug valve (13), the third T-shaped one-way three-way pipeline plug valve (14), the fourth T-shaped one-way three-way pipeline plug valve (15), the first right-angle plug valve (2), the second right-angle plug valve (5), the third right-angle plug valve (9) and the fourth right-angle plug valve (16) are all high borosilicate glass; and the inside of each plug valve is coated with high vacuum ester.

9. A high vacuum line operating system according to claim 8, characterized in that: The high vacuum line operating system is fixed on the bracket (21).

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