A filling device and a method of filling
By using nitrogen purging and carbonyl sulfide replacement in the filling device, the problems of high consumption and increased tail gas treatment costs during carbonyl sulfide filling are solved, achieving high-purity carbonyl sulfide filling and low-cost production.
Patent Information
- Application Number
- CN202310545072.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-05-15
- Publication Date
- 2026-02-06
- Estimated Expiration
- 2043-05-15
AI Technical Summary
In the carbonyl sulfide filling process, existing technologies consume a lot of carbonyl sulfide and increase the cost of the tail gas treatment system. They also make it difficult to effectively remove impurity gases from pipelines and product bottles, resulting in a decrease in product purity.
The filling device includes a distillation unit, a collection unit, a purging pipeline, and a tail gas removal system pipeline. The pipeline and product bottle are purged with inert nitrogen gas. Impurity gases are treated through the tail gas system. Carbonyl sulfide is replaced before and after filling to reduce the amount entering the tail gas system and is then returned to the distillation unit.
It reduces carbonyl sulfur consumption, lessens the burden on the exhaust gas treatment system, increases the purity of filled products to the 5N level, and lowers production costs.
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Figure CN116428514B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of industrial gas production, and in particular to a filling device and a filling method thereof. BACKGROUND
[0002] Carbon sulfide, also known as carbon oxysulfide, is an industrial gas widely used in the production of pesticides, medicines and other chemical products. For example, carbon sulfide is used as a fumigant for grains. The fumigant has good permeability and good toxic effect on many pests, and has moderate toxicity and is easy to degrade. In water, it can be decomposed into carbon disulfide and hydrogen sulfide, and when burned, it generates carbon monoxide and sulfur, which has less environmental pollution than other components.
[0003] In recent years, high-purity carbon sulfide has been found to have special effects in integrated circuit etching processes. Currently, in some integrated circuit production industries, chip etching production lines have been established using carbon oxysulfide as raw material. With the further opening up of the application range of carbon sulfide, the demand for carbon sulfide in the market has also gradually increased.
[0004] In the production process of carbon sulfide, a series of reactions and treatments are usually carried out first to obtain carbon sulfide, and then the obtained carbon sulfide product is filled into a product tank for transportation.
[0005] With the high-endization of the application field of carbon sulfide, the purity requirement of carbon sulfide has become higher. During the filling process, some impurity gases are usually present in the product bottle. Therefore, in order to improve the purity of carbon sulfide in the product bottle after filling, a gas purging (such as nitrogen) pipeline is usually provided. The pipeline and the product bottle are first purged by inert gas to remove gas impurities in the pipeline and the product bottle, and the purging gas is introduced into the tail gas treatment system. Then, before filling the carbon sulfide, the pipeline and the product bottle are purged by carbon sulfide, and the gas in the pipeline and the product bottle is discharged into the tail gas treatment system. The product bottle does not contain other gases, and then the filling is carried out. When carbon sulfide is used to purge the pipeline and the product bottle, the carbon sulfide tail gas is discharged into the tail gas treatment system, which is difficult to treat by conventional methods, thus increasing the treatment cost of the tail gas treatment system. In the above scheme, the use of carbon sulfide for purging increases the consumption of carbon sulfide, which also increases the cost. SUMMARY
[0006] In order to reduce the consumption of carbon sulfide due to filling and reduce the emission of carbon sulfide into the tail gas treatment system, thereby reducing the cost of the tail gas treatment system, the present application provides a filling device and a filling method. The filling device and the filling method can reduce the burden on the tail gas treatment system during filling, reduce the consumption of carbon sulfide during filling, improve the purity of the filled product, and have great practical production significance.
[0007] The application adopts the following technical scheme:
[0008] The filling device comprises a rectifying part, a collecting part, a purging pipeline and a tail gas system pipeline, a filling pipeline is connected between the rectifying part and the collecting part, one side of the filling pipeline and a feeding side of the collecting part are connected, the purging pipeline can be connected with the filling pipeline, a first pipeline and a second pipeline are connected on a discharging side of the collecting part; the first pipeline is connected between the collecting part and the tail gas system pipeline, the second pipeline is connected between the collecting part and the rectifying part, the purging pipeline, the tail gas system pipeline, the filling pipeline and the first pipeline and the second pipeline are respectively connected with opening and closing parts.
[0009] By adopting the above technical scheme, in workshop production, the rectifying part is usually a rectifying tower, the produced carbonyl sulfur product is fed into the rectifying part after multiple rectification and heavy component removal, and then is filled into the collecting part; the rectifying part flushes the product from the rectifying part into the collecting part through the filling pipeline. The purging pipeline is connected with the filling pipeline, the collecting part is connected with the first pipeline and the second pipeline, the purging pipeline first introduces a displacement gas such as nitrogen into the filling pipeline, when the purging pipeline is used to displace the gas, the gas flow sequentially passes through the filling pipeline, the collecting part and the first pipeline, and enters the tail gas system pipeline, so as to carry away the impurity gas in the pipeline and the collecting part, and improve the purity during the subsequent filling. After the purging pipeline is purged, the carbonyl sulfur is used to purge the pipeline, the carbonyl sulfur sequentially passes through the filling pipeline, the collecting part and the second pipeline, and the second pipeline is connected with the rectifying part, so that the purged carbonyl sulfur can enter the rectifying part, and the purging gas in the pipeline is carried away, and after the carbonyl sulfur purging is completed, the filling of the carbonyl sulfur can be performed.
[0010] After displacement by the purging pipeline and the carbonyl sulfur, the impurities in the collecting part can be reduced, the product quality can reach the level of 5N, and the purity is very high. Through the above scheme, the possibility of the carbonyl sulfur entering the tail gas treatment system is greatly reduced, so that the tail gas treatment is not easily burdened, and when the carbonyl sulfur purging pipeline is used, the carbonyl sulfur enters the rectifying part, and the consumption of the carbonyl sulfur is also reduced.
[0011] Optionally, a metering pump is connected to the filling pipeline.
[0012] By adopting the above technical scheme, the functions of conveying, metering and adjusting can be achieved at the same time by using the metering pump.
[0013] Optionally, the purging pipeline comprises a first purging pipeline and a second purging pipeline, the first purging pipeline and the second purging pipeline are connected with the filling pipeline, and the first purging pipeline is connected with the filling pipeline between the rectifying component and the metering pump; the second purging pipeline is connected with the filling pipeline between the metering pump and the collecting component.
[0014] By using the above technical scheme, the first purging pipeline can be used to purge the filling pipeline and the metering pump at the beginning to replace the impurity gas in the pipeline, and the second purging pipeline can be used to replace the impurity gas in the new collecting component after the metering pump is filled with the liquid-phase carbonyl sulfide product, thereby improving the adaptability of the filling device during use.
[0015] Optionally, the third purging pipeline is connected with the first purging pipeline or the second purging pipeline at an end away from the collecting component.
[0016] By using the above technical scheme, the third purging pipeline can be used for ventilation after purging, so that the carbonyl sulfide product in the second pipeline can flow back to the rectifying component, thereby further reducing the consumption of the carbonyl sulfide product.
[0017] Optionally, the filling pipeline is provided with a third pipeline and a fourth pipeline between the metering pump and the collecting component, the third pipeline is connected with the tail gas removal system pipeline, and the fourth pipeline is connected with the second pipeline.
[0018] By using the above technical scheme, the part of the filling pipeline between the metering pump and the collecting component can be cleaned by the second purging pipeline and the third pipeline, and the tail gas cleaned can be introduced into the tail gas removal system pipeline, and then the carbonyl sulfide in the second pipeline can flow back to the rectifying component when the carbonyl sulfide is used to replace the gas in the pipeline.
[0019] Optionally, the purging pipeline is connected with an LPN nitrogen pipeline.
[0020] In a second aspect, the application provides a filling method.
[0021] A filling method using the filling device in the above scheme, comprising the following steps:
[0022] (1) Purging the pipeline before filling; closing the opening and closing component of the second pipeline, and then purging through the purging pipeline; the nitrogen purging path is first into the filling pipeline, then into the collecting component, and then discharged to the tail gas removal system pipeline through the first pipeline, thereby discharging the impurity gas in the filling pipeline and the collecting component.
[0023] (2) filling; during the filling process, the first pipeline is kept in a closed state and the second pipeline is kept in an open state, the carbonyl sulfide in the rectifying part is filled into the collecting part through the filling pipeline, and the carbonyl sulfide gasified in the collecting part can enter the second pipeline and flow back to the rectifying part.
[0024] By adopting the above technical solution, the content of CO2 and other gases can be reduced during the filling process, and the quality of the carbonyl sulfide product obtained by filling can reach 5N.
[0025] Optionally, before filling, the filling product liquid fills the pump body of the metering pump.
[0026] By adopting the above technical solution, the cavitation of the metering pump can be effectively reduced, and the subsequent exhaust into the rectifying part is more beneficial.
[0027] In summary, the present application has at least one of the following beneficial effects:
[0028] 1. Before filling, nitrogen is blown through the blowing pipeline, so that the filling pipeline and the collecting part are replaced by nitrogen, and at this time, one end of the gas outlet is connected to the tail gas treatment pipeline. After the nitrogen replacement is completed, carbonyl sulfide is used to replace the nitrogen, and at this time, one end of the gas outlet is returned to the rectifying part, which can reduce the entry of carbonyl sulfide into the tail gas treatment system, causing additional burden to the tail gas treatment system, and can also reduce the consumption of carbonyl sulfide, thereby reducing the cost.
[0029] 2. By the filling method of the present application, the light component impurities in the collecting part can be reduced, the content of CO2 and other impurities in the filled product is greatly reduced, and the product quality of carbonyl sulfide can be improved to the level of 5N. BRIEF DESCRIPTION OF DRAWINGS
[0030] Figure 1 is a flowchart of an embodiment of the present application.
[0031] BRIEF DESCRIPTION OF DRAWINGS DETAILED DESCRIPTION
[0032] The following will be described in detail in combination with the accompanying drawings Figure 1 The present application will be further described in detail.
[0033] Example 1
[0034] The embodiment of the present application discloses a filling device, the filling device is used for filling product into a product tank in industrial gas production, and the present application does not limit the specific type of industrial gas. In order to facilitate description and understanding, the filled product is taken as an example of carbonyl sulfur.
[0035] Referring to Figure 1 The filling device comprises a rectifying part 1, a collecting part 2, a purging pipeline 3 and a tail gas system pipeline 4. The rectifying part 1 and the collecting part 2 are connected with a filling pipeline 5. The rectifying part 1 is a rectifying tower, and the carbonyl sulfur purified through multiple heavy-removing towers in the production process enters the rectifying part 1. In the rectifying part 1, the carbonyl sulfur is in liquid phase and located at the lower end of the rectifying part 1 by adjusting pressure, and part of impurity components are in gas phase and located at the upper end of the rectifying part 1.
[0036] The collecting part 2 is a product tank, and the liquid-phase carbonyl sulfur in the rectifying part 1 is filled into the collecting part 2, that is, the carbonyl sulfur can be stored and transported, and the collecting part 2 can be selected from a filling Y bottle. One end of the filling pipeline 5 is connected to a discharging position at the lower end of the rectifying part 1, and the other end of the filling pipeline 5 is connected to a feeding position of the collecting part 2. One side of the discharging position of the collecting part 2 is also connected with a first pipeline 6 and a second pipeline 7. One end of the first pipeline 6 away from the collecting part 2 is connected to the tail gas system pipeline 4, and one end of the second pipeline 7 away from the collecting part 2 is connected to a gas inlet position at the upper end of the rectifying part 1. The tail gas system pipeline 4 is connected with a tail gas treatment system in the workshop, such as a tail gas absorption tower, so as to discharge the tail gas into the tail gas treatment system for subsequent treatment and discharge.
[0037] The purging pipeline 3 is connected with the filling pipeline 5, the purging pipeline 3 is used for connecting a gas source of inert gas and is used for purging gas in the filling pipeline 5 and the collecting part 2, the purging pipeline 3 can use inert gas such as nitrogen, and nitrogen is used for purging in the embodiment. Before filling, the impurity gas components in the filling pipeline 5 and the collecting part 2 are removed through the purging pipeline 3, and then filling is performed.
[0038] The purge pipe 3, the tail gas removal system pipe 4, the filling pipe 5, and the first pipe 6 and the second pipe 7 are respectively connected with an opening and closing member 8, which can be a valve or the like device, as long as it can be used to realize the opening and closing device of the pipeline, and the control mode of the valve is not limited, the valve can be manually controlled to open and close, or can be controlled to open and close by using an electric control mode. Before filling, the purge pipe 3 is used to remove impurities from the pipe and the collecting member 2, and in the present application, the purge pipe 3 is connected to the LPN (LOW PRESSURE NITROGEN) nitrogen pipeline, which has the advantages of better stability and easier operation. Nitrogen enters the collecting member 2 from the filling pipe 5 and enters the tail gas removal system pipe 4 through the first pipe 6, so as to remove the impurity gas in the collecting member 2, and the number of purging times can be adaptively adjusted according to the actual situation, such as 1-3 times. During the purging process, the second pipe 7 is in a closed state, so that the nitrogen can be effectively purged.
[0039] When the nitrogen purging is completed, the liquid phase of carbonyl sulfur is filled. When filling, the first pipe 6 is closed, the second pipe 7 is opened, and the liquid phase of carbonyl sulfur enters the collecting member 2 through the filling pipe 5. In the collecting member 2, the liquid phase of carbonyl sulfur enters the collecting member 2, and part of the carbon-based sulfur will be gasified, and the gasified carbonyl sulfur can be returned to the rectifying member 1 through the second pipe 7, thereby reducing the consumption of carbonyl sulfur during filling. In the prior art, due to the pressure difference between the rectifying tower and the product tank during filling, dry ice or the like is used to cool the product tank in order to be able to fill. In the present application, the second pipe 7 is connected to the rectifying member 1 during filling, thereby balancing the pressure in the collecting member 2 to some extent, so that normal filling can be performed without the need for cooling, thereby reducing the cost. In a further embodiment, a filling metering pump 9 is installed on the filling pipe 5, which is more conducive to the transportation of carbon-based sulfur to the collecting member 2 during carbonyl sulfur filling.
[0040] In a further embodiment, the purging pipe 3 comprises a first purging pipe 31 and a second purging pipe 32, both of which are connected to the filling pipe 5. The first purging pipe 31 is connected to the filling pipe 5 between the metering pump 9 and the rectifying device 1, and the second purging pipe 32 is connected to the filling pipe 5 between the metering pump 9 and the collecting device 2. The first purging pipe 31 and the second purging pipe 32 are also provided with the on-off member 8, and the metering pump 9 is provided with valves at the front and rear positions. During the first filling, nitrogen is replaced through the first purging pipe 31, so that the impurity gas in the metering pump 9 can also be discharged and finally enters the tail gas removal system pipe 4. During the filling, the metering pump 9 is filled with liquid-phase carbonyl sulfur, so that after the collecting device 2 is replaced and the filling is performed again, the valves at the front and rear positions of the metering pump 9 are closed, and the collecting device 2 and the first pipe 6 are purged through the second purging pipe 32, so that the adaptability of the overall filling device is improved.
[0041] In a further embodiment, the collecting device 2 is further connected to a third purging pipe 10 at the outlet side, and the third purging pipe 10 is provided with a valve for opening and closing the third purging pipe 10. The third purging pipe 10 can be connected to the first purging pipe 31 or the second purging pipe 32, so that the purging gas can also enter the third purging pipe 10. The third purging pipe 10 can form a passage with the first pipe 6 and the second pipe 7. After the valve at the outlet of the collecting device 2 is closed and the second pipe 7 is closed, the gas in the first pipe 6 can be discharged into the tail gas removal system pipe 4 through the third purging pipe 10; or the first pipe 6 can be closed, and the second pipe 7 can be opened, so that the carbonyl sulfur gas in the second pipe 7 is discharged into the rectifying device 1.
[0042] In a further embodiment, the filling pipe 5 is provided with a third pipe 11 and a fourth pipe 12, which are located between the metering pump 9 and the collecting device 2. The third pipe 11 is connected to the tail gas removal system pipe 4, and the fourth pipe 12 is connected to the second pipe 7. When the second purging pipe 32 and the filling pipe 5 are in communication, and the valve at the inlet of the collecting device 2 is closed, nitrogen can enter the tail gas removal system pipe 4 through the third pipe 11, so that the filling pipe 5 is replaced with nitrogen.
[0043] When replacing the new collector 2 after filling, nitrogen purging is required. However, carbonyl sulfur from the previous filling will remain in the filling pipe 5. At this time, close the valves of the third pipe 11 and the feed inlet of the collector 2. First, discharge the carbonyl sulfur in the filling pipe 5 through the second purging pipe 32 from the fourth pipe 12 into the second pipe 7 and back to the distillation unit 1. After all the carbonyl sulfur in the filling pipe 5 between the metering pump 9 and the collector 2 has returned to the distillation unit 1, nitrogen is then used to purge the collector 2. This allows the carbonyl sulfur in the filling pipe 5 to be recovered before purging the new collector 2 with nitrogen, further reducing the consumption of carbonyl sulfur. In this application, carbonyl sulfide is refluxed into the distillation unit 1, and some nitrogen gas will also enter the distillation unit 1. The boiling point of carbonyl sulfide and the boiling point of nitrogen gas are quite different, so it is not easy to affect the purity of carbonyl sulfide. Alternatively, the gas inside the upper end of the distillation unit 1 can be passed into the deweighting tower for purification.
[0044] The principle of the filling process in this embodiment is as follows: Before filling, after the collection unit 2 is connected, nitrogen is first purged using the first purging pipe 31. The purging gas first enters the tail gas removal system pipe 4, thereby discharging the remaining gas in the pipe and the collection unit 2. Then, carbonyl sulfide is filled using the filling pipe 5. During filling, the exhaust gas is discharged into the distillation unit 1 through the second pipe 7, thereby enabling the recovery of carbonyl sulfide and reducing its consumption. After filling, carbonyl sulfide is discharged into the distillation unit 1 through the third purging pipe 10 via the second pipe 7. The carbonyl sulfide in the filling pipe 5 can be discharged into the second pipe 7 and then into the distillation unit 1 through the second purging pipe 32 and the fourth pipe 12.
[0045] Example 2
[0046] This embodiment provides a filling method using the filling device described in Embodiment 1 above. It mainly includes the following steps:
[0047] (1) Before filling, purge the pipeline; close the opening and closing part 8 of the second pipeline 7, and then purge through the purging pipeline 3. The nitrogen purging path is to first enter the filling pipeline 5, then enter the collection part 2, and then discharge through the first pipeline 6 to the exhaust gas system pipeline 4, thereby purging the impurity gas in the filling pipeline 5 and the collection part 2, and leaving only nitrogen.
[0048] (2) Filling; During the filling process, the first pipe 6 is kept closed and the second pipe 7 is kept open. During filling, the carbonyl sulfur in the distillation unit 1 enters the collection unit 2 through the filling pipe 5, and the vaporized carbonyl sulfur in the collection unit 2 can enter the second pipe 7 and flow back to the distillation unit 1.
[0049] (3) When the collecting device 2 is full, replace it with a new one and purge the new collecting device 2 with nitrogen. When replacing, close all the opening and closing devices 8 and then replace the collecting device 2 with a new one. When purging the new collecting device 2 with nitrogen, first control the valves so that the second purging pipeline 32, the filling pipeline 5, the fourth pipeline 12 and the second pipeline 7 are in communication, and the second purging pipeline 32 can discharge the residual carbonyl sulphur in the filling pipeline into the rectifying device 1 through the fourth pipeline 12 and the second pipeline 7 in turn. Then make the third purging pipeline 10 and the second pipeline 7 in communication, so as to discharge the residual carbonyl sulphur in the second pipeline 7 into the rectifying device 1. Finally, make the second purging pipeline 32, the filling pipeline 5, the collecting device 2 and the first pipeline in communication, and nitrogen can discharge the impurity gas in the collecting device 2 into the exhaust gas system pipeline 4 through the first pipeline 6, and then repeat the filling of step (2).
[0050] The above are preferred embodiments of the present application, and are not intended to limit the protection scope of the present application. Any equivalent changes made on the basis of the structure, shape and principle of the present application should be covered within the protection scope of the present application.
Claims
1. A filling device, characterized in that: The system includes a distillation unit (1), a collection unit (2), a purge pipe (3), and a tail gas removal system pipe (4). A filling pipe (5) is connected between the distillation unit (1) and the collection unit (2), and the filling pipe (5) is connected to the feed side of the collection unit (2). The purge pipe (3) can be connected to the filling pipe (5). A first pipe (6) and a second pipe (7) are connected to the discharge side of the collection unit (2). The first pipe (6) is connected between the collection unit (2) and the tail gas removal system pipe (4), and the second pipe (7) is connected between the collection unit (2) and the distillation unit (1). The purge pipe (3), the tail gas removal system pipe (4), the filling pipe (5), the first pipe (6), and the second pipe (7) are each connected to an opening and closing device (8). A metering pump (9) is connected to the filling pipe (5); The purge pipe (3) includes a first purge pipe (31) and a second purge pipe (32). Both the first purge pipe (31) and the second purge pipe (32) are connected to the filling pipe (5). The connection between the first purge pipe (31) and the filling pipe (5) is located between the distillation unit (1) and the metering pump (9). The connection between the second purge pipe (32) and the filling pipe (5) is located between the metering pump (9) and the collecting unit (2). The discharge side of the collection component (2) is also connected to a third purging pipe (10), and the end of the third purging pipe (10) away from the collection component (2) is connected to the first purging pipe (31) or the second purging pipe (32). The filling pipe (5) is connected to the metering pump (9) and the collecting device (2) by a third pipe (11) and a fourth pipe (12). The third pipe (11) is connected to the exhaust gas system pipe (4), and the fourth pipe (12) is connected to the second pipe (7).
2. The filling device according to claim 1, characterized in that: The purging pipe (3) is connected to the LPN nitrogen pipeline.
3. A filling method, using the filling device according to any one of claims 1-2, characterized in that: Includes the following steps: (1) Purge the pipeline before filling; close the opening and closing part (8) of the second pipeline (7), and then purge through the purging pipeline (3). The nitrogen purging path is to first enter the filling pipeline (5), then enter the collection part (2), and then discharge through the first pipeline (6) to the exhaust gas system pipeline (4), thereby purging the impurity gas in the filling pipeline (5) and the collection part (2); (2) Filling; During the filling process, the first pipe (6) is kept closed and the second pipe (7) is kept open. During filling, the carbonyl sulfur in the distillation unit (1) enters the collection unit (2) through the filling pipe (5), and the vaporized carbonyl sulfur in the collection unit (2) can enter the second pipe (7) and flow back to the distillation unit (1).
4. The filling method according to claim 3, characterized in that: Before filling, fill the pump body of the metering pump (9) with the product liquid to be filled.
Citation Information
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Carbonyl sulfide purification device and purification method thereof
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