A sampling device and method for 2,2-difluoroethyl ester synthesis kettle

By designing a sampling device including a sampling cylinder, an intrasurveillance window, an isolation baffle, a trachea, a solenoid valve, a hydraulic cylinder and an ultrasonic sensor, the problem of residual materials and inability to adjust the sampling depth in the sampling device in the synthetic kettle is solved, and high-quality and representative sampling is achieved, ensuring accurate monitoring of the reaction process.

CN118758668BActive Publication Date: 2025-03-18临沂小篆新材料科技有限公司
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Patent Information

Application Number
CN202411158066.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-08-22
Publication Date
2025-03-18
Estimated Expiration
2044-08-22

AI Technical Summary

Technical Problem

The existing sampling device of 2,2-difluoroethyl ester synthesis kettle has residual material problems, which leads to sampling errors and cannot adjust the insertion height of the intubation tube, affecting the representativeness of the sample.

Method used

A sampling device including a sampling cylinder, an endoscope window, an isolation baffle, a trachea, a solenoid valve, a hydraulic cylinder and an ultrasonic sensor is designed. Through nitrogen cleaning and hydraulic cylinder driving the piston to move, the cleaning of the inner tube and the adjustment of the sampling depth is achieved.

Benefits of technology

Effectively prevent residual materials in the intubation cannula, ensure that the fresh reaction mixture is obtained at the beginning of each sampling, avoid sampling errors, increase product quality, and be able to sample from different locations in the synthetic kettle as needed, ensuring the representativeness of the sample.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to the technical field of sampling detection devices, and specifically discloses a sampling device and method for a 2,2-difluoroethyl ester synthesis reactor, including: a sampling barrel, a plurality of air holes connected to its inner cavity are opened at the top of the sampling barrel; an endoscope window is arranged at the front side of the sampling barrel; an isolation baffle is arranged in the middle of the inner cavity of the sampling barrel, and a sampling mechanism is arranged in the middle of the left side of the outer wall of the sampling barrel. The device can effectively prevent residual materials in the inner insert tube, ensure that fresh reaction mixture is obtained at the beginning of each sampling, so that the sampling result can more truly reflect the actual situation in the reaction system, increase product quality, and can adjust the height of the inner insert tube inserted into the inner cavity of the synthesis reactor, and can sample from different positions in the synthesis reactor as needed. This flexibility ensures that representative samples can be obtained even in the case of uneven mixing, and the entire reaction process can be monitored more accurately to avoid misleading data.
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Description

Technical Field

[0001] The invention relates to the technical field of sampling detection devices, and in particular to a sampling device and method for a 2,2-difluoroethyl ester synthesis kettle. Background Art

[0002] In the field of chemical synthesis and industrial production, 2,2-difluoroethyl ester, as an important organic compound, is widely used in industries such as medicine, pesticides and polymer materials. Due to its unique chemical properties, the preparation process of 2,2-difluoroethyl ester requires precise control of reaction conditions to ensure product quality and yield. Therefore, using a synthesis reactor as the main equipment for production and preparation can provide a closed and controllable environment to meet the strict requirements of parameters such as temperature, pressure and reaction time in the synthesis process of 2,2-difluoroethyl ester;

[0003] In the production process of 2,2-difluoroethyl ester, in order to ensure that the reaction proceeds as expected and reaches the required product quality standards, it is necessary to regularly sample and analyze the reaction mixture in the synthesis reactor. This step is crucial because it can help producers monitor the progress of the reaction and adjust the reaction conditions in time to avoid the formation of by-products or waste of raw materials. However, the existing sampling device of the 2,2-difluoroethyl ester synthesis reactor has some disadvantages, which may affect the accuracy and efficiency of sampling;

[0004] First, in chemical synthesis and industrial production, the preparation process of 2,2-difluoroethyl ester requires delicate operation and multiple sampling and analysis to ensure that the reaction proceeds as expected and reaches the required product quality standards. During the sampling process, some materials from the previous sampling may remain in the inner tube. These materials may not participate in the reaction or their properties may have changed. This situation will result in the acquisition of this part of "dead materials" at the beginning of each sampling. These residues will be counted in the new sample during sampling, resulting in the sampling concentration not being consistent with the concentration in the actual reaction system. This error will affect the judgment and control of the reaction process, and further affect the quality and yield of the final product.

[0005] Secondly, the sampling device of the prior art is usually unable to adjust the height of the inner tube inserted into the inner cavity of the synthesis reactor. In the synthesis reactor, the reactants at different positions may differ due to uneven mixing. If the sampling position is fixed, then in some cases the key reaction area may be missed, which may cause the sample taken to be unrepresentative and unable to accurately reflect the actual situation of the entire reaction system, thereby obtaining misleading data. Summary of the invention

[0006] The object of the present invention is to provide a sampling device and method for a 2,2-difluoroethyl ester synthesis reactor to solve the problems raised in the above background technology.

[0007] To achieve the above-mentioned purpose, the present invention provides the following technical solutions: a sampling device and method for a 2,2-difluoroethyl ester synthesis reactor, comprising: a sampling barrel, a plurality of air holes connected to its inner cavity are opened at the top of the sampling barrel; an endoscope window is arranged on the front side of the sampling barrel; an isolation baffle is arranged in the middle of the inner cavity of the sampling barrel; an air pipe is arranged at the top of the left side of the outer wall of the sampling barrel, and the right end of the air pipe is connected to the inner cavity of the isolation baffle; a first solenoid valve is arranged on the outer wall of the air pipe; a reflux pipe is arranged at the top of the right side of the outer wall of the sampling barrel, and the left end of the reflux pipe is connected to the inner cavity of the isolation baffle; a fourth solenoid valve is arranged on the outer wall of the reflux pipe; a sampling mechanism is arranged in the middle of the left side of the outer wall of the sampling barrel; a cleaning pipe is arranged on the right side of the outer wall of the sampling barrel side middle; the one-way valve is arranged on the outer wall of the cleaning tube; the connecting tube is arranged at the bottom end of the left side of the outer wall of the sampling tube; the third solenoid valve is arranged on the outer wall of the connecting tube; the sampling tube is arranged at the bottom end of the right side of the outer wall of the sampling tube; the spherical valve, the spherical valve is arranged on the outer wall of the sampling tube; the first hydraulic cylinder is arranged at the bottom end of the sampling tube, and the top end of the first hydraulic cylinder extends into the inner cavity of the sampling tube; the first piston is slidably adapted to be inserted in the middle part of the inner cavity of the sampling tube, and the middle part of the bottom end of the first piston is arranged at the top end of the first hydraulic cylinder; the second hydraulic cylinder is arranged at the top end of the sampling tube, and the bottom end of the second hydraulic cylinder extends into the inner cavity of the sampling tube; the second piston is slidably adapted to be inserted in the top of the inner cavity of the sampling tube, and the middle part of the top end of the second piston is arranged at the bottom end of the second hydraulic cylinder.

[0008] Preferably, in order to transport nitrogen into the inner cavity of the sampling tube, the left end of the connecting pipe is provided with: a nitrogen tank, and the left end of the connecting pipe is arranged in the inner cavity of the nitrogen tank; the tank cover is screwed to the top of the nitrogen tank; the air pump is screwed to the right side of the outer wall of the nitrogen tank, and the left end of the air pipe is arranged at the exhaust port of the air pump; one end of the air inlet pipe is arranged at the air inlet of the air pump, and the other end of the air inlet pipe extends into the inner cavity of the nitrogen tank.

[0009] Preferably, in order to extract 2,2-difluoroethyl ester in the synthesis kettle, the sampling mechanism includes: an inner tube, one end of the inner tube is arranged in the middle of the left side of the outer wall of the sampling tube; the second solenoid valve is arranged on the outer wall of the inner tube; the baffle is arranged on the right side of the outer wall of the inner tube; and the baffle is arranged at the other end of the inner tube.

[0010] Preferably, in order to adjust the sampling depth, the sampling mechanism also includes: a nut, which is screwed to the right side of the outer wall of the inner tube; an extension tube is arranged at the bottom end of the nut, and the extension tube can be slidably sleeved on the outer wall of the inner tube; and an ultrasonic sensor is arranged at the bottom end of the outer wall of the extension tube.

[0011] Preferably, the inner tube and the cleaning tube are both located below the isolation baffle, and the distances from the inner tube and the cleaning tube to the bottom end of the isolation baffle are both greater than the thickness of the first piston.

[0012] Preferably, the thickness of the first piston is greater than the inner diameter length of the inner insert tube and the cleaning tube.

[0013] Preferably, the volume of the sampling cylinder is larger than the volume of the inner cannula.

[0014] The present invention provides a sampling device and method for a 2,2-difluoroethyl ester synthesis reactor, which has the following beneficial effects:

[0015] 1. The present invention utilizes a nitrogen tank to store nitrogen, and the sampling tube can be cleaned by connecting a cleaning tube to an external cleaning pump.

[0016] 2. The present invention utilizes the first hydraulic cylinder to drive the first piston to move upward, so as to form a negative pressure between the bottom end of the first piston and the bottom end of the inner cavity of the sampling tube, thereby enabling the 2,2-difluoroethyl ester solution in the inner cavity of the synthesis reactor to flow into the inner cavity of the sampling tube through the inner insert tube. The first hydraulic cylinder drives the first piston to move downward, so that the 2,2-difluoroethyl ester solution between the bottom end of the first piston and the bottom end of the inner cavity of the sampling tube can be squeezed into the inner cavity of the sampling tube and discharged, thereby completing the sampling.

[0017] 3. The present invention utilizes an air pump to extract the nitrogen in the inner cavity of the nitrogen tank through the air inlet pipe and the air pipe, and discharges it into the inner cavity of the sampling tube. The first hydraulic cylinder pushes the first piston to move upward, and the second hydraulic cylinder pushes the second piston to move downward, so that the nitrogen in the inner cavity of the sampling tube can be squeezed into the inner cavity of the inner tube, thereby squeezing out the 2,2-difluoroethyl ester solution in the inner cavity of the inner tube to prevent residue in the inner tube.

[0018] 4. This device can effectively prevent residual materials in the inner tube, ensure that fresh reaction mixture is obtained at the beginning of each sampling, avoid sampling errors caused by "dead materials", make the sampling results more truly reflect the actual situation in the reaction system, increase product quality, and can adjust the height of the inner tube inserted into the inner cavity of the synthesis reactor, and can sample from different positions in the synthesis reactor as needed. This flexibility ensures that representative samples can be obtained even in the case of uneven mixing, more accurately monitor the entire reaction process, and avoid misleading data. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic diagram of the structure of the present invention;

[0020] Figure 2 An exploded view of the present invention;

[0021] Figure 3 It is a front cross-sectional view of the present invention;

[0022] Figure 4 for Figure 2 A magnified image of point A;

[0023] Figure 5 for Figure 2The enlarged view of point B;

[0024] Figure 6 for Figure 3 Enlarged view of point C;

[0025] Figure 7 for Figure 2 The enlarged view of point D;

[0026] Figure 8 for Figure 2 The enlarged view of point E;

[0027] Fig. 9 for Figure 2 Enlarged view of point F.

[0028] In the figure: 1. sampling tube; 2. air hole; 3. endoscope window; 4. isolation baffle; 5. air pipe; 6. first solenoid valve; 7. reflux pipe; 8. fourth solenoid valve; 9. sampling mechanism; 91. inner tube; 92. second solenoid valve; 93. baffle; 94. baffle; 95. nut; 96. extension tube; 97. ultrasonic sensor; 10. cleaning tube; 11. one-way valve; 12. connecting tube; 13. third solenoid valve; 14. sampling tube; 15. ball valve; 16. first hydraulic cylinder; 17. first piston; 18. second hydraulic cylinder; 19. second piston; 20. nitrogen tank; 21. tank cover; 22. air pump; 23. air inlet pipe. DETAILED DESCRIPTION

[0029] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] See also Figure 1-Figure 9The present invention provides a technical solution for a sampling device of a 2,2-difluoroethyl ester synthesis reactor, comprising: a sampling tube 1, an air hole 2, an endoscope window 3, an isolation baffle 4, an air pipe 5, a first electromagnetic valve 6, a reflux pipe 7, a fourth electromagnetic valve 8, a sampling mechanism 9, a cleaning pipe 10, a one-way valve 11, a connecting pipe 12, a third electromagnetic valve 13, a sampling pipe 14, a ball valve 15, a first hydraulic cylinder 16, a first piston 17, a second hydraulic cylinder 18, a second piston 19, a nitrogen tank 20, a tank cover 21, an air pump 22 and an air inlet pipe 23. The top of the sampling tube 1 is provided with a plurality of gas ports connected to its inner cavity. Hole 2, an endoscope window 3 is arranged on the front side of the sampling tube 1, through which the height of the 2,2-difluoroethyl ester solution in the inner cavity of the sampling tube 1 can be observed, an isolation baffle 4 is arranged in the middle of the inner cavity of the sampling tube 1, and the isolation baffle 4 can be used to separate the first piston 17 and the second piston 19, an air pipe 5 is arranged on the top left side of the outer wall of the sampling tube 1, and the right end of the air pipe 5 is connected to the inner cavity of the isolation baffle 4, a first solenoid valve 6 is arranged on the outer wall of the air pipe 5, the first solenoid valve 6 is the prior art, and no further description is given here, the first solenoid valve 6 is used to control the closing and opening of the air pipe 5, and the reflux pipe 7 is provided. It is placed at the top right side of the outer wall of the sampling tube 1, the left end of the reflux pipe 7 is connected to the inner cavity of the isolation baffle 4, the reflux pipe 7 is used to discharge the cleaning liquid, the fourth solenoid valve 8 is arranged on the outer wall of the reflux pipe 7, the fourth solenoid valve 8 is the prior art, and no further description is given here. The fourth solenoid valve 8 is used here to control the closing and opening of the reflux pipe 7, the sampling mechanism 9 is arranged in the middle of the left side of the outer wall of the sampling tube 1, the sampling mechanism 9 is used to extract 2,2-difluoroethyl ester, the cleaning pipe 10 is arranged in the middle of the right side of the outer wall of the sampling tube 1, and the external cleaning pump is connected through the cleaning pipe 10 to transport the cleaning liquid into the inner cavity of the sampling tube 1. The cleaning liquid, the cleaning pipe 10 is located below the isolation baffle 4, the one-way valve 11 is arranged on the outer wall of the cleaning pipe 10, the one-way valve 11 is a prior art, and no further description is given here, the connecting pipe 12 is arranged at the bottom end of the left side of the outer wall of the sampling cylinder 1, and the connecting pipe 12 is used to transport nitrogen into the inner cavity of the sampling cylinder 1, the third solenoid valve 13 is arranged on the outer wall of the connecting pipe 12, the third solenoid valve 13 is a prior art, and no further description is given here, the third solenoid valve 13 is used for closing and opening the air connecting pipe 12, the sampling tube 14 is arranged at the bottom end of the right side of the outer wall of the sampling cylinder 1, and the sampling tube 14 is used to discharge 2,2-difluoroethyl ester sample, a ball valve 15 is arranged on the outer wall of the sampling tube 14, the ball valve 15 is a prior art, and no further description is given here. The ball valve 15 is used here to control the closing and opening of the sampling tube 14, and a first hydraulic cylinder 16 is arranged at the bottom end of the sampling tube 1, and the top end of the first hydraulic cylinder 16 extends into the inner cavity of the sampling tube 1. The first hydraulic cylinder 16 is a prior art, and no further description is given here. The first hydraulic cylinder 16 is used here to drive the first piston 17 to move, and the first piston 17 can be slidably adapted and plugged into the middle part of the inner cavity of the sampling tube 1, and the middle part of the bottom end of the first piston 17 is arranged at the top end of the first hydraulic cylinder 16, and the distance between the inner insert tube 91 and the cleaning tube 10 to the bottom end of the isolation baffle 4 is greater than the thickness of the first piston 17, ensuring that the first piston 17 can move to the top of the inner insert tube 91 and the cleaning tube 10, and the thickness of the first piston 17 is greater than the inner diameter length of the inner insert tube 91 and the cleaning tube 10. The second hydraulic cylinder 18 is arranged at the top of the sampling tube 1, and the bottom of the second hydraulic cylinder 18 extends into the inner cavity of the sampling tube 1. The second hydraulic cylinder 18 is a prior art, and no further description is given here. The second hydraulic cylinder 18 is used to drive the second piston 19 to move. The second piston 19 can be slidably adapted and plugged into the top of the inner cavity of the sampling tube 1. The middle of the top of the second piston 19 is arranged at the bottom of the second hydraulic cylinder 18. The left end of the connecting pipe 12 is arranged in the inner cavity of the nitrogen tank 20. The nitrogen tank 20 is used to store nitrogen. The tank cover 21 is screwed to the top of the nitrogen tank 20. The air pump 22 is screwed to the right side of the outer wall of the nitrogen tank 20. The left end of the air pipe 5 is arranged at the exhaust port of the air pump 22. The air pump 22 is a prior art, and no further description is given here. The air pump 22 is used to extract nitrogen. One end of the air inlet pipe 23 is arranged at the air inlet of the air pump 22, and the other end of the air inlet pipe 23 extends into the inner cavity of the nitrogen tank 20.

[0031] As a preferred embodiment, further, the sampling mechanism 9 includes: an inner tube 91, a second solenoid valve 92, a baffle 93, a baffle 94, a nut 95, an extension tube 96 and an ultrasonic sensor 97. One end of the inner tube 91 is arranged in the middle of the left side of the outer wall of the sampling tube 1, and 2,2-difluoroethyl ester is transported to the inner cavity of the sampling tube 1 through the inner tube 91. The inner tube 91 is located below the isolation baffle 4. The volume of the sampling tube 1 is larger than the volume of the inner tube 91, ensuring that the nitrogen can be used to push all the residual 2,2-difluoroethyl ester in the inner tube 91 back into the synthesis reactor. The second solenoid valve 92 is arranged on the outer wall of the inner tube 91. The second solenoid valve 92 is a prior art and will not be described in detail here. The second solenoid valve 92 is used here to control To control the closing and opening of the inner tube 91, a baffle 93 is arranged on the right side of the outer wall of the inner tube 91, a baffle 94 is arranged at the other end of the inner tube 91, a nut 95 is screwed on the right side of the outer wall of the inner tube 91, and the rotational force generated by the rotation of the nut 95 can drive the extension tube 96 to move. The extension tube 96 is arranged at the bottom end of the nut 95, and the extension tube 96 can be slidably connected to the outer wall of the inner tube 91. An ultrasonic sensor 97 is arranged at the bottom end of the outer wall of the extension tube 96. The ultrasonic sensor 97 is a prior art and will not be described in detail here. The characteristic of ultrasonic wave propagation in a medium is utilized, and the distance is calculated by measuring the time difference from the emission to the reception of ultrasonic wave, so that the depth of the extension tube 96 inserted into the 2,2-difluoroethyl ester solution can be calculated.

[0032] The working principle includes the following steps:

[0033] Step 1: When in use, open the tank cover 21, fill a proper amount of nitrogen into the inner cavity of the nitrogen tank 20, connect the cleaning pipe 10 to the external cleaning pump, insert the bottom end of the extension pipe 96 from the top of the synthesis kettle into the inner cavity of the synthesis kettle, and ensure that the nut 95 is not inserted into the inner cavity of the synthesis kettle;

[0034] Step 2: When sampling of 2,2-difluoroethyl ester is required, the nut 95 is rotated according to the depth of sampling required. The rotational force generated by the rotation of the nut 95 drives the extension tube 96 to slide in the inner cavity of the synthesis reactor, and the ultrasonic sensor 97 is used to sense the depth of the bottom end of the extension tube 96 inserted into the inner cavity of the synthesis reactor in real time until it is inserted to a suitable depth.

[0035] Step 3, close the ball valve 15 and the second solenoid valve 92, open the third solenoid valve 13, start the first hydraulic cylinder 16, use the first hydraulic cylinder 16 to pull the first piston 17 downward, thereby causing the gas between the bottom end of the first piston 17 and the bottom end of the inner cavity of the sampling tube 1 to be discharged into the inner cavity of the nitrogen tank 20 through the connecting pipe 12, close the third solenoid valve 13, start the first hydraulic cylinder 16 to push the first piston 17 upward, thereby causing negative pressure to be formed between the bottom end of the first piston 17 and the bottom end of the inner cavity of the sampling tube 1, until the bottom end of the first piston 17 moves to the top of the inner insert 91, open the second solenoid valve 92, and under the action of negative pressure, the gas is discharged through the extension tube 96 and The inner insert 91 extracts the 2,2-difluoroethyl ester liquid in the inner cavity of the synthesis reactor and draws it into the inner cavity of the sampling cylinder 1, and stores it between the bottom end of the first piston 17 and the bottom end of the inner cavity of the sampling cylinder 1. After extracting an appropriate amount of 2,2-difluoroethyl ester, close the second solenoid valve 92, take the sampling bottle, align the sampling bottle with the bottom end of the sampling tube 14, open the ball valve 15, and start the first hydraulic cylinder 16 to pull the first piston 17 downward, so that the 2,2-difluoroethyl ester liquid stored in the inner cavity of the sampling cylinder 1 flows into the inner cavity of the sampling bottle through the sampling tube 14 until the first piston 17 moves to the bottom end of the inner cavity of the sampling cylinder 1, thereby completing the sampling, and closing the ball valve 15;

[0036] Step 4, open the first solenoid valve 6, start the air pump 22, the air pump 22 starts to transport the nitrogen stored in the inner cavity of the nitrogen tank 20 to the inner cavity of the sampling tube 1 through the air inlet pipe 23 and the air pipe 5, and at the same time start the second hydraulic cylinder 18, use the second hydraulic cylinder 18 to pull the second piston 19 upward until the second piston 19 moves to the top of the inner cavity of the sampling tube 1, and promotes that a proper amount of nitrogen is stored in the inner cavity of the sampling tube 1, close the air pump 22 and the first solenoid valve 6, open the second solenoid valve 92 and start the second hydraulic cylinder 18, and use the second hydraulic cylinder 18 to push the second piston 1 9 moves downward, opens the third solenoid valve 13, starts the first hydraulic cylinder 16, and uses the first hydraulic cylinder 16 to push the first piston 17 upward, thereby squeezing the nitrogen in the inner cavity of the sampling cylinder 1 into the inner cavity of the inner tube 91, so that the 2,2-difluoroethyl ester liquid remaining in the inner cavity of the sampling cylinder 1 is returned to the synthesis reactor. When the first piston 17 moves upward, the nitrogen in the inner cavity of the nitrogen tank 20 is transported to between the first piston 17 and the bottom end of the inner cavity of the sampling cylinder 1 through the connecting pipe 12, so as to prevent the residual 2,2-difluoroethyl ester liquid in the inner tube 91 from affecting the next sampling;

[0037] Step 5. When it is necessary to clean the sampling tube 1, start the external cleaning pump to transport the cleaning liquid to the bottom end of the first piston 17 and the bottom end of the inner cavity of the sampling tube 1 through the cleaning pipe 10 and the one-way valve. After the bottom end of the first piston 17 and the bottom end of the inner cavity of the sampling tube 1 are filled with the cleaning liquid, turn off the external cleaning pump, open the ball valve 15, and use the first hydraulic cylinder 16 to pull the first piston 17 downward, so that the cleaning liquid at the bottom end of the first piston 17 and the bottom end of the inner cavity of the sampling tube 1 is discharged through the sampling tube 14, and start again. The cleaning pump is started to transport the cleaning liquid to the space between the first piston 17 and the second piston 19 through the cleaning pipe 10, and the second hydraulic cylinder 18 is used to drive the second piston 19 to move upward until the cleaning liquid fills the space between the first piston 17 and the second piston 19. Then, the cleaning pump is closed, the fourth solenoid valve 8 is opened, the first hydraulic cylinder 16 is used to push the first piston 17 upward, and the second hydraulic cylinder 18 is used to push the second piston 19 downward, thereby squeezing the cleaning liquid into the inner cavity of the reflux pipe 7, thereby discharging the cleaning liquid and completing the cleaning.

[0038] In summary, the device can effectively prevent residual materials in the inner tube 91, ensure that a fresh reaction mixture is obtained at the beginning of each sampling, avoid sampling errors caused by "dead materials", and make the sampling results more truly reflect the actual situation in the reaction system, thereby increasing product quality. In addition, the height of the inner tube 91 inserted into the inner cavity of the synthesis reactor can be adjusted, and sampling can be performed from different positions in the synthesis reactor as needed. This flexibility ensures that representative samples can be obtained even in the case of uneven mixing, and the entire reaction process can be monitored more accurately to avoid misleading data.

[0039] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A sampling device for a 2,2-difluoroethyl ester synthesis reactor, characterized in that: include: A sampling tube (1), wherein a plurality of air holes (2) communicating with the inner cavity of the sampling tube (1) are formed at the top of the sampling tube (1); An endoscope window (3), wherein the endoscope window (3) is arranged on the front side of the sampling tube (1); An isolation baffle (4), wherein the isolation baffle (4) is arranged in the middle of the inner cavity of the sampling tube (1); An air pipe (5), the air pipe (5) being arranged at the top of the left side of the outer wall of the sampling tube (1), and the right end of the air pipe (5) being connected to the inner cavity of the isolation baffle (4); A first solenoid valve (6), the first solenoid valve (6) being arranged on the outer wall of the air pipe (5); A reflux pipe (7), the reflux pipe (7) being arranged at the top right side of the outer wall of the sampling tube (1), the left end of the reflux pipe (7) being connected to the inner cavity of the isolation baffle (4); a fourth solenoid valve (8), the fourth solenoid valve (8) being arranged on an outer wall of the return pipe (7); A sampling mechanism (9), the sampling mechanism (9) being arranged at the middle portion of the left side of the outer wall of the sampling tube (1); A cleaning tube (10), the cleaning tube (10) being arranged in the middle of the right side of the outer wall of the sampling tube (1); a one-way valve (11), wherein the one-way valve (11) is arranged on the outer wall of the cleaning pipe (10); A connecting pipe (12), wherein the connecting pipe (12) is arranged at the bottom end of the left side of the outer wall of the sampling tube (1); a third solenoid valve (13), the third solenoid valve (13) being arranged on an outer wall of the connecting pipe (12); A sampling tube (14), wherein the sampling tube (14) is arranged at the right bottom end of the outer wall of the sampling tube (1); A spherical valve (15), wherein the spherical valve (15) is arranged on the outer wall of the sampling tube (14); A first hydraulic cylinder (16), the first hydraulic cylinder (16) being arranged at the bottom end of the sampling cylinder (1), the top end of the first hydraulic cylinder (16) extending into the inner cavity of the sampling cylinder (1); A first piston (17), the first piston (17) being slidably adapted to be inserted into the middle of the inner cavity of the sampling tube (1), and the middle of the bottom end of the first piston (17) being arranged at the top end of the first hydraulic cylinder (16); A second hydraulic cylinder (18), the second hydraulic cylinder (18) being arranged at the top end of the sampling cylinder (1), and the bottom end of the second hydraulic cylinder (18) extending into the inner cavity of the sampling cylinder (1); A second piston (19), the second piston (19) is slidably adapted to be inserted into the top of the inner cavity of the sampling tube (1), and the middle of the top end of the second piston (19) is arranged at the bottom end of the second hydraulic cylinder (18); The left end of the connecting pipe (12) is provided with: A nitrogen tank (20), wherein the left end of the connecting pipe (12) is arranged in the inner cavity of the nitrogen tank (20); A tank cover (21), wherein the tank cover (21) is screwed to the top of the nitrogen tank (20); An air pump (22), the air pump (22) being screwed to the right side of the outer wall of the nitrogen tank (20), and the left end of the air pipe (5) being arranged at the exhaust port of the air pump (22); An air intake pipe (23), one end of the air intake pipe (23) being arranged at the air intake port of the air pump (22), and the other end of the air intake pipe (23) extending into the inner cavity of the nitrogen tank (20).

2. A sampling device for a 2,2-difluoroethyl ester synthesis reactor according to claim 1, characterized in that: The sampling mechanism (9) comprises: An inner cannula (91), one end of which is disposed at the middle of the left side of the outer wall of the sampling tube (1); a second solenoid valve (92), the second solenoid valve (92) being arranged on the outer wall of the inner insert tube (91); A baffle (93), the baffle (93) being arranged on the right side of the outer wall of the inner insert tube (91); A baffle (94) is arranged at the other end of the inner insert tube (91).

3. A sampling device for a 2,2-difluoroethyl ester synthesis reactor according to claim 2, characterized in that, The sampling mechanism (9) further comprises: A nut (95), wherein the nut (95) is screwed onto the right side of the outer wall of the inner insert tube (91); An extension tube (96), the extension tube (96) being arranged at the bottom end of the nut (95), and the extension tube (96) being slidably sleeved on the outer wall of the inner insert tube (91); An ultrasonic sensor (97), wherein the ultrasonic sensor (97) is arranged at the bottom end of the outer wall of the extension tube (96).

4. A sampling device for a 2,2-difluoroethyl ester synthesis reactor according to claim 3, characterized in that: The inner insert tube (91) and the cleaning tube (10) are both located below the isolation baffle (4), and the distances between the inner insert tube (91) and the cleaning tube (10) and the bottom end of the isolation baffle (4) are both greater than the thickness of the first piston (17).

5. A sampling device for a 2,2-difluoroethyl ester synthesis reactor according to claim 4, characterized in that: The thickness of the first piston (17) is greater than the inner diameter length of the inner insert tube (91) and the cleaning tube (10).

6. A sampling device for a 2,2-difluoroethyl ester synthesis reactor according to claim 5, characterized in that: The volume of the sampling tube (1) is greater than the volume of the inner insert tube (91).

7. A sampling method for a 2,2-difluoroethyl ester synthesis reactor, which is applied to a sampling device for a 2,2-difluoroethyl ester synthesis reactor as claimed in claim 6, characterized in that: The following steps are involved: Step 1: When in use, open the tank cover (21), fill an appropriate amount of nitrogen into the inner cavity of the nitrogen tank (20), connect the cleaning pipe (10) to an external cleaning pump, insert the bottom end of the extension pipe (96) from the top of the synthesis kettle into the inner cavity of the synthesis kettle, and ensure that the nut (95) is not inserted into the inner cavity of the synthesis kettle; Step 2: When sampling of 2,2-difluoroethyl ester is required, the nut (95) is rotated according to the depth required for sampling. The rotational force generated by the rotation of the nut (95) drives the extension tube (96) to slide in the inner cavity of the synthesis reactor, and the ultrasonic sensor (97) is used to sense in real time the depth of the bottom end of the extension tube (96) inserted into the inner cavity of the synthesis reactor until the extension tube (96) is inserted to a suitable depth. Step 3: close the ball valve (15) and the second solenoid valve (92), open the third solenoid valve (13), start the first hydraulic cylinder (16), use the first hydraulic cylinder (16) to pull the first piston (17) downward, thereby causing the gas between the bottom end of the first piston (17) and the bottom end of the inner cavity of the sampling tube (1) to be discharged into the inner cavity of the nitrogen tank (20) through the connecting pipe (12), close the third solenoid valve (13), start the first hydraulic cylinder (16) to push the first piston (17) upward, thereby causing negative pressure to be formed between the bottom end of the first piston (17) and the bottom end of the inner cavity of the sampling tube (1), until the bottom end of the first piston (17) moves to the top of the inner tube (91), open the second solenoid valve (92), and under the action of the negative pressure, the gas is discharged through the extension tube (96) and the inner insert tube (91) extract the 2,2-difluoroethyl ester liquid in the inner cavity of the synthesis reactor and draw it into the inner cavity of the sampling tube (1) and store it between the bottom end of the first piston (17) and the bottom end of the inner cavity of the sampling tube (1). After an appropriate amount of 2,2-difluoroethyl ester is extracted, the second solenoid valve (92) is closed, the sampling bottle is taken, the sampling bottle is aligned with the bottom end of the sampling tube (14), the ball valve (15) is opened, and the first hydraulic cylinder (16) is started to pull the first piston (17) downward, thereby allowing the 2,2-difluoroethyl ester liquid stored in the inner cavity of the sampling tube (1) to flow into the inner cavity of the sampling bottle through the sampling tube (14) until the first piston (17) moves to the bottom end of the inner cavity of the sampling tube (1), thereby completing the sampling and closing the ball valve (15); Step 4: Open the first solenoid valve (6) and start the air pump (22). The air pump (22) starts to transport the nitrogen stored in the inner cavity of the nitrogen tank (20) through the air inlet pipe (23) and the air pipe (5) to the inner cavity of the sampling tube (1). At the same time, start the second hydraulic cylinder (18). Use the second hydraulic cylinder (18) to pull the second piston (19) upward until the second piston (19) moves to the top of the inner cavity of the sampling tube (1) and causes an appropriate amount of nitrogen to be stored in the inner cavity of the sampling tube (1). Close the air pump (22) and the first solenoid valve (6), open the second solenoid valve (92) and start the second hydraulic cylinder (18). The second piston (19) is pushed downward by the second hydraulic cylinder (18), the third electromagnetic valve (13) is opened, the first hydraulic cylinder (16) is started, and the first piston (17) is pushed upward by the first hydraulic cylinder (16), thereby squeezing the nitrogen in the inner cavity of the sampling tube (1) into the inner cavity of the inner insert tube (91), thereby returning the 2,2-difluoroethyl ester liquid remaining in the inner cavity of the sampling tube (1) to the synthesis reactor. When the first piston (17) moves upward, the nitrogen in the inner cavity of the nitrogen tank (20) is transported to the space between the first piston (17) and the bottom end of the inner cavity of the sampling tube (1) through the connecting pipe (12), thereby preventing the inner insert tube (91) from leaking. The residual 2,2-difluoroethyl ester liquid in the tube (91) affects the next sampling; step 5, when it is necessary to clean the sampling tube (1), start the external cleaning pump to transport the cleaning liquid to the bottom end of the first piston (17) and the bottom end of the inner cavity of the sampling tube (1) through the cleaning tube (10) and the one-way valve. After the bottom end of the first piston (17) and the bottom end of the inner cavity of the sampling tube (1) are filled with the cleaning liquid, turn off the external cleaning pump, open the ball valve (15), and use the first hydraulic cylinder (16) to pull the first piston (17) downward, so that the cleaning liquid at the bottom end of the first piston (17) and the bottom end of the inner cavity of the sampling tube (1) passes through The sampling tube (14) is discharged, and the cleaning pump is started again to transport the cleaning liquid to the space between the first piston (17) and the second piston (19) through the cleaning tube (10), and the second piston (19) is driven to move upward by the second hydraulic cylinder (18) until the cleaning liquid fills the space between the first piston (17) and the second piston (19). Then, the cleaning pump is closed, the fourth solenoid valve (8) is opened, the first hydraulic cylinder (16) is used to push the first piston (17) upward, and the second hydraulic cylinder (18) is used to push the second piston (19) downward, thereby squeezing the cleaning liquid into the inner cavity of the reflux tube (7), thereby discharging the cleaning liquid and completing the cleaning.

Citation Information

Patent Citations

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