Arsine purification device

Abstract

The utility model relates to the technical field of arsine production, and discloses an arsine purification device which comprises a raw material crude arsine gas cylinder and a rectifying tower body, and the raw material crude arsine gas cylinder is communicated with the rectifying tower body through a pipeline matched with an automatic valve. A vacuum system, a helium feeding device and a tail gas treatment device are respectively communicated with a pipeline between the raw material crude arsine gas bottle and the rectifying tower body; the lower part of the rectifying tower body is communicated with a constant-temperature water tank, a cold trap recycling tank and a product arsine collecting tank respectively, the upper part of the rectifying tower body is communicated with a refrigerating unit through a heat exchanger, and the upper part of the rectifying tower body is sequentially communicated with a flow meter and the cold trap recycling tank through a tower plate heat exchanger. According to the utility model, after crude arsine purified by a traditional molecular sieve is rectified, most impurities such as C2 impurities, C3-C5 impurities, S compounds and the like in a product can be removed, so that the requirements of customers are met.

Description

Technical Field

[0001] The utility model relates to the technical field of arsine production, in particular to an arsine purification device. Background Art

[0002] At present, the purification process of arsine 6N products mostly uses 3A or 4A molecules for purification, which has good purification effects on certain impurity indicators such as water, and meets the needs of most electronic market customers. However, with the continuous updating and iteration of customer products, the traditional arsine product indicators no longer meet the gas needs of customers. For example, semiconductor customers have extremely low requirements for certain specific impurity contents (such as: COS ≤ 30ppb), and traditional purification processes can no longer meet customer needs. Utility Model Content

[0003] 1. Technical issues to be solved

[0004] In view of the deficiencies in the prior art, the utility model provides an arsine purification device, which solves the problem that the product obtained after purification in the prior arsine purification device easily contains impurities exceeding the standard and cannot meet the use requirements of customers.

[0005] (II) Technical solution

[0006] To achieve the above purpose, the utility model is implemented through the following technical solutions: an arsine purification device, comprising a raw material crude arsine gas cylinder and a distillation tower body, the raw material crude arsine gas cylinder is connected to the distillation tower body through a pipeline with an automatic valve, the pipeline between the raw material crude arsine gas cylinder and the distillation tower body is also connected with a vacuum system, a helium feeding device and an exhaust gas treatment device, the exhaust gas treatment device can inhale the residual gas in the pipeline; the lower part of the distillation tower body is connected with a constant temperature water tank, the lower part of the distillation tower body is also connected with a cold trap recovery tank and a product arsine collection tank, the lower part of the distillation tower body is controlled by a liquid level transmitter interlocking with a regulating valve to control the collection and switching of the cold trap recovery tank and the product arsine collection tank, the upper part of the distillation tower body is connected with a refrigeration unit through a heat exchanger, and the upper part of the distillation tower body is sequentially connected with a flow meter and a cold trap recovery tank through a plate heat exchanger.

[0007] Preferably, the helium delivery device can deliver high-pressure helium and low-pressure helium into the entire purification pipeline.

[0008] Preferably, a safety valve is arranged in the pipeline between the plate heat exchanger and the cold trap recovery tank, and the gas outlet end of the safety valve is connected to the tail gas treatment device.

[0009] Preferably, a pressure transmitter is arranged on the pipeline between the flow meter and the plate heat exchanger through a valve, and the pressure transmitter is connected to the constant temperature water tank through a pressure interlocking controller.

[0010] Preferably, two groups of temperature transmitters are symmetrically arranged on the constant temperature water tank, and the temperature transmitters can control and shut down the electric heating system in the constant temperature water tank.

[0011] Preferably, one-way valves are provided between the helium feeding device and the tail gas treatment device and the pipeline, and manual diaphragm valves are arranged at the connection points between the pressure transmitter and the distillation pipeline.

[0012] (III) Beneficial effects

[0013] The utility model has the following beneficial effects:

[0014] (1) The arsine purification device, through the helium delivery device and vacuum system, can detect whether there is leakage in the entire distillation pipeline, purge and replace the residual gas in the pipeline, and then evacuate the pipeline, effectively preventing the residual gas in the pipeline from affecting the subsequent distillation and purification of crude arsine. At the same time, through the exhaust gas treatment device, the residual exhaust gas in the pipeline and the helium used for replacement can be uniformly collected and treated before being discharged.

[0015] (2) The arsine purification device is provided with a liquid level transmitter and a regulating valve, so that during the distillation and purification process, when the liquid level in the distillation tower body rises to a preset value, the valve corresponding to the cold trap recovery tank is opened to recover the arsine obtained by the distillation and purification. At the same time, the arsine obtained in the cold trap recovery tank is tested and analyzed. If the purity is qualified, the valve corresponding to the cold trap recovery tank is closed, and the product arsine collection tank is opened to collect the arsine that meets the purity requirements. The flow meter is provided to control the flow of the entire distillation and purification process in conjunction with the pneumatic regulating valve. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a schematic diagram of the process structure of the utility model;

[0017] Figure 2 It is a schematic diagram of the structure of the utility model.

[0018] In the figure: 1. Crude arsine gas cylinder; 2. Distillation tower; 3. Vacuum system; 4. Helium delivery device; 5. Tail gas treatment device; 6. Refrigeration unit; 7. Heat exchanger; 8. Plate heat exchanger; 9. Safety valve; 10. Cold trap recovery tank; 11. Flow meter; 12. Pressure transmitter; 13. Pressure interlocking controller; 14. Constant temperature water tank; 15. Liquid level transmitter; 16. Temperature transmitter; 17. Product arsine collection tank. DETAILED DESCRIPTION

[0019] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0020] See also Figure 1 The utility model provides a technical solution: an arsine purification device, comprising a raw material crude arsine gas cylinder 1 and a distillation tower body 2, the raw material crude arsine gas cylinder 1 is connected to the distillation tower body 2 through a pipeline with an automatic valve, the raw material crude arsine gas cylinder 1 and the distillation tower body 2 are also connected to a vacuum system 3, a helium feeding device 4 and an exhaust gas treatment device 5 respectively on the pipeline between the raw material crude arsine gas cylinder 1 and the distillation tower body 2, and the exhaust gas treatment device 5 can inhale the residual gas in the pipeline; the lower part of the distillation tower body 2 is connected to a constant temperature water tank 14, the lower part of the distillation tower body 2 is also connected to a cold trap recovery tank 10 and a product arsine collection tank 17 respectively, the lower part of the distillation tower body 2 is controlled by a liquid level transmitter 15 interlocking with a regulating valve to control the collection switching of the cold trap recovery tank 10 and the product arsine collection tank 17, the upper part of the distillation tower body 2 is connected to a refrigeration unit 6 through a heat exchanger 7, and the upper part of the distillation tower body 2 is connected to a flow meter 11 and the cold trap recovery tank 10 in sequence through a plate heat exchanger 8.

[0021] The utility model can detect whether there is leakage in the entire distillation pipeline, purge and replace residual gas in the pipeline and perform vacuuming through the helium feeding device 4 and the vacuum system 3, effectively avoiding the residual gas in the pipeline from affecting the subsequent distillation and purification of crude arsine. Meanwhile, the tail gas treatment device 5 can be used to uniformly collect and treat the residual tail gas in the pipeline and the helium used for replacement and then discharge them. Through the liquid level transmitter and the regulating valve, when the liquid level in the distillation tower body 2 rises to a preset value during the distillation and purification process, the valve corresponding to the cold trap recovery tank 10 is opened to recover the arsine obtained by the distillation and purification at this time. Meanwhile, the arsine obtained in the cold trap recovery tank 10 is detected and analyzed. If the purity is qualified, the valve corresponding to the cold trap recovery tank 10 is closed, and the product arsine collection tank 17 is opened to collect the arsine that meets the purity requirement. Through the flow meter 11, the flow rate of the entire distillation and purification process can be controlled in conjunction with the pneumatic regulating valve.

[0022] Reference Figure 2As shown, in this embodiment, the helium delivery device 4 can deliver high-pressure helium and low-pressure helium into the entire purification pipeline. By delivering high-pressure helium into the pipeline, the entire pipeline can be tested for helium pressure maintenance to detect whether there is leakage in the pipeline; the low-pressure helium introduced can purge and replace the pipeline to avoid residual gas in the pipeline causing subsequent distillation and purification to obtain the purity of the product arsine.

[0023] In this embodiment, a safety valve 9 is arranged in the pipeline between the plate heat exchanger 8 and the cold trap recovery tank 10, and the gas outlet end of the safety valve 9 is connected to the tail gas treatment device 5. Figure 2 As shown, by providing a safety valve 9, when the gas pressure in the pipeline is too high, the pipeline can be depressurized and the gas can be discharged to the exhaust gas treatment device 5 for treatment.

[0024] Reference Figure 2 As shown, in this embodiment, a pressure transmitter 12 is arranged on the pipeline between the flow meter 11 and the plate heat exchanger 8 through a valve, and the pressure transmitter 12 is connected to the constant temperature water tank 14 through the pressure interlocking controller 13. The pressure transmitter 12 can be used to detect the air pressure of the pipeline of the entire distillation tower body 2. When the pressure value exceeds the preset value, the electric heating gear of the constant temperature water tank 14 can be reduced through the pressure interlocking controller 13 to avoid excessive tower pressure, thereby causing safety hazards.

[0025] In this embodiment, two groups of temperature transmitters 16 are symmetrically arranged on the constant temperature water tank 14 , and the temperature transmitters 16 can control and shut down the electric heating system in the constant temperature water tank 14 .

[0026] Reference Figure 2 As shown, in this embodiment, a one-way valve is provided between the helium feeding device 4 and the tail gas treatment device 5 and the pipeline, and a manual diaphragm valve is arranged at the connection between the pressure transmitter 12 and the distillation pipeline. By manually opening or closing the manual diaphragm valve, in which the diaphragm in the valve body is in a closed state, medium contamination or cross infection between the pressure transmitter 12 and the pipeline can be avoided.

[0027] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions. The sentence "includes an element defined by ... does not exclude the existence of other identical elements in the process, method, article or device including the element".

[0028] 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. An arsine purification device, comprising a raw material crude arsine gas cylinder and a distillation tower body, characterized in that: The raw material crude arsine gas cylinder is connected to the distillation tower body through a pipeline with an automatic valve. The pipeline between the raw material crude arsine gas cylinder and the distillation tower body is also connected with a vacuum system, a helium delivery device and an exhaust gas treatment device, respectively, and the exhaust gas treatment device can inhale the residual gas in the pipeline; the lower part of the distillation tower body is connected with a constant temperature water tank, and the lower part of the distillation tower body is also connected with a cold trap recovery tank and a product arsine collection tank, respectively. The lower part of the distillation tower body controls the collection and switching of the cold trap recovery tank and the product arsine collection tank through a liquid level transmitter interlocking with a regulating valve, the upper part of the distillation tower body is connected with a refrigeration unit through a heat exchanger, and the upper part of the distillation tower body is sequentially connected with a flow meter and a cold trap recovery tank through a plate heat exchanger.

2. The arsine purification device according to claim 1, characterized in that: The helium delivery device can deliver high-pressure helium and low-pressure helium into the entire purification pipeline.

3. An arsine purification device according to claim 1 or 2, characterized in that: A safety valve is arranged in the pipeline between the plate heat exchanger and the cold trap recovery tank, and the gas outlet end of the safety valve is in communication with the tail gas treatment device.

4. The arsine purification device according to claim 3, characterized in that: A pressure transmitter is arranged on the pipeline between the flow meter and the plate heat exchanger through a valve, and the pressure transmitter is connected to the constant temperature water tank through a pressure interlocking controller.

5. The arsine purification device according to claim 4, characterized in that: Two groups of temperature transmitters are symmetrically arranged on the constant temperature water tank, and the temperature transmitters can control and shut down the electric heating system in the constant temperature water tank.

6. The arsine purification device according to claim 5, characterized in that: One-way valves are provided between the helium feeding device and the tail gas treatment device and the pipeline, and manual diaphragm valves are arranged at the connection points between the pressure transmitter and the distillation pipeline.

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