A negative pressure sampling device

Abstract

The utility model discloses a kind of negative pressure sampling devices, negative pressure sampling device includes the sampling tube of insertion to be sampled reation kettle and the pipeline outside to be sampled reation kettle, pipeline is provided with main cut-off valve, sight glass, balance valve, sampling valve, sampling bottle, gas source main valve, protection valve and vacuum vent valve, one end of sampling tube inserts the bottom of reation kettle, another end of sampling tube is communicated main cut-off valve, main cut-off valve is communicated with sight glass and sampling valve respectively by first tee, another end of sight glass is communicated with balance valve and gas source main valve respectively by second tee, sampling valve is communicated with sampling bottle and balance valve respectively by third tee, gas source main valve is communicated with protection valve and vacuum vent valve respectively by fourth tee.The negative pressure sampling device provided in the application can ensure sampling under negative pressure, reduces the operation process, and does not need to stop the reaction during sampling, effectively avoids the leakage of materials and pollution to the environment, while ensuring the safety of operators.

Description

Technical Field

[0001] This utility model relates to the field of chemical and pharmaceutical equipment technology, specifically to a negative pressure sampling device. Background Technology

[0002] In chemical production processes, chemical synthesis reactors are pressurized, requiring multiple samplings of the material inside. Currently, the common practice is to install the sampling port directly on the reactor. To obtain the material inside the reactor and avoid introducing impurities, the material at the front end of the sampling pipe must first be drained into another container before sampling. However, this existing technology has the following drawbacks:

[0003] 1. **Operational Inconvenience:** The additional material discharge step prolongs sampling time, consumes significant manpower, and reduces production efficiency. 2. **Material Waste:** Material discharged from the front end of the pipe cannot be recycled, directly causing waste. This is especially true for high-value materials, where long-term accumulation significantly increases production costs. 3. **Poor Safety:** For toxic, strongly odorous, highly toxic, or even extremely toxic materials, leaks are highly likely during sampling. Operators are directly exposed to toxic substances; inhaling harmful gases or contact with materials can lead to poisoning. The operation is difficult and dangerous, making it difficult to guarantee employee safety. 4. **Environmental Pollution:** Toxic gases released during sampling or leaked materials pollute the operating environment, damaging the surrounding ecosystem and posing a serious environmental pollution risk.

[0004] Therefore, there is an urgent need in this field for a negative pressure sampling device that is simple in structure, easy to operate, and can achieve closed sampling without interrupting the reaction, thereby avoiding material waste, reducing the risk of environmental pollution, and protecting the physical and mental health of operators. Utility Model Content

[0005] To solve the above-mentioned technical problems, this utility model provides a negative pressure sampling device, including a sampling tube inserted into a reaction vessel to be sampled and a pipeline outside the reaction vessel. The pipeline is equipped with a main shut-off valve, a sight glass, a balance valve, a sampling valve, a sampling bottle, a gas source main valve, a protection valve, and a vacuum venting valve. The sampling tube is a bottom-insertion tube, with one end inserted into the bottom of the reaction vessel and the other end connected to the main shut-off valve. The main shut-off valve is connected to the sight glass and the sampling valve through a first three-way valve. The other end of the sight glass is connected to the balance valve and the gas source main valve through a second three-way valve. The sampling valve is connected to the sampling bottle and the balance valve through a third three-way valve. The gas source main valve is connected to the protection valve and the vacuum venting valve through a fourth three-way valve.

[0006] In one specific embodiment, the sight glass is a transparent cavity tube used to observe the flow state of materials, and the interior of the sight glass contains a suspended ball.

[0007] In one specific embodiment, the suspended ball has a hollow structure and is made of PTFE or PP material. The suspended ball is disposed inside the sight glass and is used to indicate the liquid level inside the sight glass.

[0008] In one specific embodiment, the sampling bottle is used to collect samples, and the outside of the sampling bottle is provided with a sampling cover.

[0009] In one specific embodiment, the sampling cover is a cylinder or cuboid, the surrounding material of the sampling cover is glass or acrylic resin, and the top and bottom surfaces of the sampling cover are made of stainless steel, titanium or Hastelloy.

[0010] In one specific embodiment, one end of the protective valve is connected to a protective gas source, wherein the protective gas is selected from nitrogen, carbon dioxide, or an inert gas.

[0011] In one specific embodiment, the sampling tube, sight glass, and tubing are made of a material selected from stainless steel, Hastelloy, titanium, PP, PVC, PTFE, or fiberglass.

[0012] In one specific embodiment, the main shut-off valve, balancing valve, sampling valve, gas source main valve, protection valve, and vacuum venting valve are selected from one of the following: ball valve, solenoid valve, or diaphragm valve.

[0013] In one specific embodiment, the third tee is a T-type tee, and the vertical inner diameter of the T-type tee is consistent with the inner diameter of the sampling bottle connector, and the vertical inner diameter is greater than the horizontal inner diameter.

[0014] A second aspect of this application provides a sampling method for a negative pressure sampling device, the method being based on the aforementioned negative pressure sampling device, the method comprising the following steps:

[0015] (1) Pretreatment: Close all valves, connect the protective gas source to the protective valve, open the main shut-off valve, the main gas source valve, and the protective valve, use the protective gas to push the residual material in the sampling tube back into the reactor, and purge until bubbles emerge from the outlet of the sampling tube in the reactor.

[0016] (2) Pressure setting: Adjust the pressure of the reactor to 0.03-0.08 MPa;

[0017] (3) Pipeline cleaning: Open the main shut-off valve, the main gas source valve and the vacuum vent valve. When the material enters the sight glass and the suspension ball floats to the top of the sight glass, close the main gas source valve. Then open the protection valve and the main gas source valve to push the material in the sight glass back into the reactor. Repeat 2-3 times to clean the inside of the sampling tube.

[0018] (4) Sampling: Open the main shut-off valve, the main gas supply valve and the vacuum vent valve. The material enters the sight glass. When the suspension ball floats to the top of the sight glass, close the main gas supply valve. Then open the balance valve, the sampling valve and the main gas supply valve at the same time. Then open the vacuum vent valve. The material enters the sampling bottle due to gravity and is sampled. After sampling, close the sampling valve, the balance valve and the vacuum vent valve. Then open the main shut-off valve and the protection valve to push the residual material back into the reactor.

[0019] (5) Post-processing: Repeat step (4) to clean the pipeline, then seal the sampling bottle to complete the sampling.

[0020] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0021] 1. The negative pressure sampling device provided by this utility model has a simple structure and is easy to operate. With the sampling tube inserted into the bottom, there is no need to discharge the material in the reaction vessel to other containers, which reduces a lot of operation steps. The entire sampling process does not require complicated operations. It is only necessary to use protective gas to draw negative pressure on the reaction vessel to achieve fast and safe sampling.

[0022] 2. The negative pressure sampling device provided by this utility model can achieve closed sampling, thereby avoiding material leakage. During the sampling process, there is no need to take measures to stop the material reaction, improving the efficiency and smoothness of sampling.

[0023] 3. The negative pressure sampling device provided by this utility model can effectively reduce material waste. The material in the sampling pipe does not need to be discharged from the system for separate collection and processing. Only by using protective gas to purge the sampling pipe can the residual material be removed. This will not cause material waste or environmental pollution. It eliminates safety hazards and will not cause environmental pollution, effectively improving the safety of sampling operations. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the overall structure of the negative pressure sampling device provided by this utility model;

[0025] In the diagram, 1-Reaction vessel; 2-Sampling tube; 3-Main shut-off valve; 4-Suspension ball; 5-Sight glass; 6-Balancing valve; 7-Sampling valve; 8-Sampling bottle; 9-Gas source main valve; 10-Protection valve; 11-Vacuum venting valve. Detailed Implementation

[0026] The technical solution of this utility model will be clearly and completely described below. Obviously, the described embodiments are only some, not all, of the embodiments of this utility model. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this utility model. Unless otherwise specified, the materials, instruments, and reagents used in the following embodiments can be obtained commercially. Unless otherwise specified, the technical means used in the embodiments are conventional means well known to those skilled in the art.

[0027] The structures, proportions, sizes, etc., shown in the accompanying drawings of this specification are only for illustrative purposes to aid those skilled in the art and are not intended to limit the implementation of this utility model. Therefore, they have no substantial technical significance. Any modifications to the structure, changes in proportions, or adjustments to size, without affecting the effects and objectives of this utility model, should still fall within the scope of the technical content disclosed in this utility model. Furthermore, the terms such as "upper," "lower," "left," "right," "middle," and "one" used in this specification are merely for clarity of description and are not intended to limit the scope of implementation of this utility model. Changes or adjustments to their relative relationships, without substantially altering the technical content, should also be considered within the scope of implementation of this utility model.

[0028] Example 1

[0029] like Figure 1 As shown in the figure, this embodiment illustrates a negative pressure sampling device, including a sampling tube 2 inserted into the reactor 1 to be sampled and a pipeline outside the reactor 1 to be sampled. The pipeline is equipped with a main shut-off valve 3, a sight glass 5, a balance valve 6, a sampling valve 7, a sampling bottle 8, a gas source main valve 9, a protection valve 10, and a vacuum venting valve 11. The pipeline connects the aforementioned components and also provides support.

[0030] Sampling tube 2 is a bottom insertion tube. One end of sampling tube 2 is vertically inserted into the bottom of reactor 1, and the other end of sampling tube 2 is connected to the main shut-off valve 3. The main shut-off valve 3 is the main switch of the entire negative pressure sampling device, which can quickly cut off the connection between reactor 1 and external pipelines to avoid material leakage after sampling.

[0031] The main shut-off valve 3 is connected to the sight glass 5 and the sampling valve 7 via the first three-way valve. The sight glass 5 is a transparent cavity tube used to observe the flow state of the material. The inside of the sight glass 5 contains a suspended ball 4. The suspended ball 4 is a hollow structure made of PTFE or PP material, which is corrosion resistant and has a density less than that of the material. The suspended ball 4 is used to indicate the liquid level in the sight glass 5 and can float with the liquid level of the material. The operator can directly observe whether the material in the sight glass 5 is full.

[0032] The other end of the sight glass 5 is connected to the balance valve 6 and the main gas valve 9 via the second three-way valve. The balance valve 6 is used to balance the pressure between the sampling bottle 8 and the sight glass 5 to avoid the material flow being obstructed due to pressure difference. At the same time, it can release the tail gas in the sampling bottle 8 (such as volatile gases sometimes), which can prevent the pressure in the sampling bottle 8 from being too high.

[0033] The sampling valve 7 is connected to the sampling bottle 8 and the balance valve 6 via a third tee. The third tee is a T-type tee, and the vertical inner diameter of the T-type tee is consistent with the inner diameter of the connector of the sampling bottle 8 to ensure that there is no material retention. In addition, the vertical inner diameter is larger than the horizontal inner diameter to reduce the flow resistance of the material and avoid blockage.

[0034] The main gas valve 9 is connected to the protection valve 10 and the vacuum vent valve 11 via a fourth three-way valve. One end of the protection valve 10 is connected to a protective gas source, which is selected from nitrogen, carbon dioxide, or an inert gas. The protective gas is used to purge the pipeline, push back residual materials, and avoid the risk of explosion. The vacuum vent valve 11 is used to extract negative pressure in the pipeline and assist material flow.

[0035] The sampling bottle 8 is used to collect samples, and the outside of the sampling bottle 8 is equipped with a sampling cover. The sampling cover is cylindrical or cuboid, and the surrounding material of the sampling cover is glass or acrylic resin. The top and bottom surfaces of the sampling cover are made of stainless steel, titanium or Hastelloy, which can prevent the sampling bottle 8 from accidentally breaking and causing material leakage.

[0036] The selection of materials and valves can be based on the characteristics of the material. The materials for sampling tube 2, sight glass 5, and piping are selected from stainless steel, Hastelloy, titanium, PP, PVC, PTFE, or fiberglass. For highly corrosive materials (such as hydrochloric acid and nitric acid), PTFE (acid and alkali resistant) or Hastelloy (oxidation resistant) are selected; for common organic solvents, stainless steel or PP are selected; for high-temperature systems, titanium or fiberglass (resistant to high-temperature deformation) is preferred. The main shut-off valve 3, balancing valve 6, sampling valve 7, main gas supply valve 9, protection valve 10, and vacuum venting valve 11 are selected from ball valves, solenoid valves, or diaphragm valves. Ball valves are selected for manual operation (rapid switching); solenoid valves are selected for automated production lines (remote control possible); for high-viscosity materials (such as resins), diaphragm valves are selected (to prevent valve core sticking).

[0037] This embodiment also illustrates the sampling method of this negative pressure sampling device, including the following steps:

[0038] (1) Pretreatment: Close all valves, connect the protective gas source to the protective valve 10, open the main shut-off valve 3, the main gas source valve 9, and the protective valve 10, and use the protective gas to push the residual material in the sampling tube 2 back into the reactor 1, and purge until bubbles emerge from the outlet of the sampling tube 2 in the reactor 1.

[0039] (2) Pressure setting: Adjust the pressure of reactor 1 to 0.03-0.08 MPa;

[0040] (3) Pipeline cleaning: Open the main shut-off valve 3, the gas source main valve 9 and the vacuum venting valve 11. The material enters the sight glass 5. When the suspension ball 4 floats to the top of the sight glass 5, close the gas source main valve 9. Then open the protection valve 10 and the gas source main valve 9 to push the material in the sight glass 5 back into the reactor 1. Repeat 2-3 times to clean the inside of the sampling tube 2.

[0041] (4) Sampling: Open the main shut-off valve 3, the gas source main valve 9 and the vacuum vent valve 11. The material enters the sight glass 5. When the suspension ball 4 floats to the top of the sight glass 5, close the gas source main valve 9. Then open the balance valve 6, the sampling valve 7 and the gas source main valve 9 at the same time. Then open the vacuum vent valve 11. The material enters the sampling bottle 8 due to gravity and is sampled. After sampling, close the sampling valve 7, the balance valve 6 and the vacuum vent valve 11. Then open the main shut-off valve 3 and the protection valve 10 to push the residual material back into the reactor 1.

[0042] (5) Post-processing: Repeat step (4) to clean the pipeline, then seal the sampling bottle 8 to complete the sampling.

[0043] In summary, the above embodiments are merely preferred embodiments of the present utility model and are not intended to limit the scope of protection of the present utility model. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the scope of protection of the present utility model.

Claims

1. A negative pressure sampling device, characterized in that, The system includes a sampling tube inserted into the reactor to be sampled and pipelines outside the reactor. The pipelines are equipped with a main shut-off valve, a sight glass, a balance valve, a sampling valve, a sampling bottle, a gas source main valve, a protection valve, and a vacuum venting valve. The sampling tube is a bottom-insertion tube, with one end inserted into the bottom of the reactor and the other end connected to the main shut-off valve. The main shut-off valve is connected to the sight glass and the sampling valve via a first three-way valve. The other end of the sight glass is connected to the balance valve and the gas source main valve via a second three-way valve. The sampling valve is connected to the sampling bottle and the balance valve via a third three-way valve. The gas source main valve is connected to the protection valve and the vacuum venting valve via a fourth three-way valve.

2. The negative pressure sampling device according to claim 1, characterized in that, The sight glass is a transparent cavity tube used to observe the flow state of materials, and a suspended ball is contained inside the sight glass.

3. The negative pressure sampling device according to claim 2, characterized in that, The suspended ball has a hollow structure and is made of PTFE or PP material. The suspended ball is placed inside the sight glass to indicate the liquid level inside the sight glass.

4. The negative pressure sampling device according to claim 1, characterized in that, The sampling bottle is used to collect samples, and the outside of the sampling bottle is equipped with a sampling cover.

5. The negative pressure sampling device according to claim 4, characterized in that, The sampling cover is cylindrical or cuboid, with the surrounding material of the sampling cover being glass or acrylic resin, and the top and bottom surfaces of the sampling cover being stainless steel, titanium, or Hastelloy.

6. The negative pressure sampling device according to claim 1, characterized in that, One end of the protective valve is connected to a protective gas source, and the protective gas is selected from nitrogen, carbon dioxide or an inert gas.

7. The negative pressure sampling device according to claim 1, characterized in that, The sampling tube, sight glass, and tubing are made of one of the following materials: stainless steel, Hastelloy, titanium, PP, PVC, PTFE, or fiberglass.

8. The negative pressure sampling device according to claim 1, characterized in that, The main shut-off valve, balancing valve, sampling valve, gas source main valve, protection valve, and vacuum venting valve are selected from one of the following types: ball valve, solenoid valve, or diaphragm valve.

9. The negative pressure sampling device according to claim 1, characterized in that, The third tee is a T-type tee, and the vertical inner diameter of the T-type tee is the same as the inner diameter of the sampling bottle connector, and the vertical inner diameter is greater than the horizontal inner diameter.

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