Rectification purification system and method for producing high purity gas for electronic industry from industrial products

Abstract

The application discloses a rectification and purification system and method for preparing high-purity gas for electronic industry from industrial products, which comprises a booster pump, a heavy component removal tower, a light component removal tower, a first condensing unit, a refining tower and a second condensing unit; the application combines the booster rectification and the energy-saving three-effect rectification, thereby saving investment, reducing energy consumption, simplifying operation and ensuring high quality of products; compared with common rectification, the energy consumption can be saved by about 75%.

Description

Technical Field

[0001] This invention belongs to the field of high-purity gas preparation, and particularly relates to a distillation purification system and method for producing high-purity gases for the electronics industry from industrial products. Background Technology

[0002] With the rapid development of the information industry, the demands for semiconductor support materials—electronic gases—are increasing in variety, quantity, and performance, while simultaneously requiring lower prices. Therefore, it is imperative to develop new, low-cost electronic gas product preparation technologies that are widely applicable, have stable performance, and are energy-efficient. Thus, to adapt to the current development of the semiconductor industry, a new, low-cost process technology for producing electronic gas products using industrial products is being developed. Summary of the Invention

[0003] The purpose of this invention is to provide a distillation purification system and method for producing high-purity gases for the electronics industry from industrial products, so as to prepare high-purity gases for the electronics industry at low cost.

[0004] To achieve the above-mentioned objectives, the present invention adopts the following technical solution:

[0005] A distillation and purification system for producing high-purity gases for the electronics industry from industrial products, characterized in that the distillation and purification system comprises:

[0006] A booster pump is used to pressurize the raw material to be fed into the deweighting tower and to transport the pressurized raw material to the deweighting tower.

[0007] The heavy components removal tower is used to refine the raw material from the booster pump to remove the heavy components and send the light components out from the top of the tower; the bottom of the heavy components removal tower is equipped with a heavy components removal tower reboiler;

[0008] A light component removal tower is used to refine the feed from the first delivery pump to remove light components, and the bottom product is fed into a refining tower. The bottom of the light component removal tower is equipped with a light component removal reboiler, which is used to exchange heat between a portion of the bottom material of the light component removal tower and the light components from the top of the heavy component removal tower so as to boil and vaporize, and to partially condense the light components from the top of the heavy component removal tower.

[0009] The first condensation unit includes a first gas-liquid separator, a first water cooler, a storage tank, and a first transfer pump. The first gas-liquid separator is used to separate the light components from the top of the heavy component removal tower after condensation in the reboiler of the light component removal tower, and sends the separated gas phase from the top to the first water cooler and the separated liquid phase from the bottom to the storage tank. The first water cooler is used to condense the gas phase material from the first gas-liquid separator and send the condensed product to the storage tank. The storage tank is used to receive the liquid phase material from the first gas-liquid separator and the condensed product from the first water cooler. The first transfer pump is used to send a portion of the liquid phase material in the storage tank as top reflux to the heavy component removal tower and a portion as feed to the light component removal tower.

[0010] A refining column is used to refine the feed from the light component removal column to remove heavy components. The refining column has a reboiler at the bottom and a condenser at the top. The reboiler allows heat exchange between a portion of the bottom material and the light component from the top of the light component removal column for boiling and vaporization, and also partially condenses the light component from the top of the light component removal column. The condenser condenses the overhead gas from the refining column, and sends a portion of the condensate as overhead reflux and a portion as finished product.

[0011] The second condensation unit includes a second gas-liquid separator, a second water cooler, a separation tank, and a second transfer pump. The second gas-liquid separator tank is used to perform gas-liquid separation on the light components from the top of the light component removal tower after condensation in the reboiler of the refining tower. The separated gas phase is sent from the top to the second water cooler, and the separated liquid phase is sent from the bottom to the separation tank. The second water cooler is used to condense the gas phase material from the second gas-liquid separator and send the condensed product to the separation tank. The separation tank is used to receive the liquid phase material from the second gas-liquid separator and the condensed product from the second water cooler, and discharge the gas phase from the top. The second transfer pump is used to send the liquid phase material in the tank as top reflux into the light component removal tower.

[0012] According to the distillation and purification system of the present invention, preferably, the refining column is used to refine the feed from the light component removal column, and the removed heavy component is returned as feed to the booster pump.

[0013] In a preferred embodiment, the distillation purification system further includes a collection tank for receiving the product collected from the purification column; preferably, the top of the collection tank is provided with a gas phase sampling tube.

[0014] According to the distillation and purification system of the present invention, preferably, the top of the storage tank is provided with a safety valve to automatically release air after overpressure.

[0015] In some embodiments, the distillation and purification system is further provided with a bypass line for directly feeding material from the booster pump into the light-light ...

[0016] In another aspect of achieving the above-mentioned objectives, the present invention also provides a method for preparing high-purity gases for the electronics industry using the above-mentioned distillation and purification system.

[0017] In some embodiments, when the molar fraction of heavy component impurities in the raw material is less than 0.001, for example 0.0005, the raw material pressurized by the booster pump is directly fed into the light component removal tower.

[0018] According to the method of the present invention, preferably, the cold source for the first water cooler, the second water cooler, and the refining tower condenser is circulating water.

[0019] According to the method of the present invention, preferably, the heat source of the reboiler of the deweighting tower is low-pressure steam.

[0020] According to the method of the present invention, preferably, the raw material is industrial liquid chlorine, food-grade carbon dioxide, or 3N-grade HBr.

[0021] The present invention has the following advantages:

[0022] 1. The process of the present invention is a continuous distillation process, which can be used to produce most compressed liquefied gas products for the electronics industry and has a wide range of applications;

[0023] 2. In use, this invention employs inexpensive low-pressure steam as the heat source for the de-weighting tower and inexpensive circulating water as the cold source for the refining tower, resulting in low cost.

[0024] 3. This process combines pump-boosted distillation and energy-saving triple-effect distillation, which saves investment, reduces energy consumption, simplifies operation, and ensures high product quality. Under normal circumstances, triple-effect distillation can save 75% of energy compared with ordinary distillation.

[0025] 4. The discharged heavy and light components can still be recycled as low-grade industrial products;

[0026] 5. This process is a continuous, stable, and fully automated control process, which ensures product quality stability and batch-to-batch consistency, and improves product utilization. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the distillation and purification system of the present invention;

[0028] Figure 2 Based on Figure 1 A system diagram omitting the deweight removal tower;

[0029] The equipment labels in the diagram are explained as follows: Booster pump B-101; First delivery pump B-102; Second delivery pump B-103;

[0030] Heavy removal tower T-101; Light removal tower T-102; Refining tower T-103;

[0031] Heavy removal tower reboiler E-101; Light removal tower reboiler E-102; First water cooler E-103; Second water cooler E-104; Refining tower reboiler E-105; Refining tower condenser E-106.

[0032] Storage tank G-101; Separation tank G-102; Production tank G-103; First gas-liquid separator G-104; Second gas-liquid separator G-105;

[0033] The logistics numbering is explained as follows: ①-Raw materials; ②-T-101 Meter grate; ③-T-102 Feed; ④-T-102 Top grate; ⑤-T-103 Feed; ⑥-Product. Detailed Implementation

[0034] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.

[0035] It should be noted that the terms "first," "second," etc., in the specification, claims, and accompanying drawings of this invention are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such data can be interchanged where appropriate for the embodiments of the invention described herein. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion; for example, a process, method, system, product, or apparatus that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or apparatus.

[0036] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. The present invention will now be described in detail with reference to the embodiments.

[0037] like Figure 1As shown, the distillation and purification system of the present invention includes a booster pump B-101, a heavy removal tower T-101, a light removal tower T-102, a first condensation unit, a purification tower T-103, and a second condensation unit.

[0038] The booster pump B-101 is used to pressurize the raw material to be introduced into the deweighting tower T-101 and to transport the pressurized raw material to the deweighting tower.

[0039] The deweighting tower T-101 is used to refine the raw material from the booster pump to remove the heavy components and send the light components out from the top of the tower; the bottom of the deweighting tower is equipped with a deweighting tower reboiler E-101.

[0040] The light component removal tower T-102 is used to refine the feed from the first transfer pump B-102 to remove light components, and the bottom product is fed into the refining tower T-103. The bottom of the light component removal tower is equipped with a light component removal tower reboiler E-102, which is used to exchange heat between a portion of the bottom material of the light component removal tower and the light components from the top of the heavy component removal tower so as to boil and vaporize, and to partially condense the light components from the top of the heavy component removal tower.

[0041] The first condensation unit includes a first gas-liquid separator G-104, a first water cooler E-103, a storage tank G-101, and a first transfer pump B-102. The first gas-liquid separator G-104 is used to separate the light components from the top of the heavy component removal tower after condensation by the reboiler E-102, and to send the separated gas phase from the top to the first water cooler E-103 and the separated liquid phase from the bottom to the storage tank G-101. The first water cooler E-103 is used to... The gaseous material from the first gas-liquid separator is condensed, and the condensed product is sent to the storage tank; the storage tank G-101 is used to receive the liquid material from the first gas-liquid separator and the condensed product from the first water cooler, wherein the top of the storage tank G-101 is equipped with a safety valve to automatically vent air after overpressure; the first transfer pump B-102 is used to send part of the liquid material in the storage tank as top reflux to the heavy removal tower T-101 and part as feed to the light removal tower T-102.

[0042] The refining column T-103 is used to refine the feed from the light component removal column T-102 to remove heavy components, and preferably, the removed heavy components are fed back to the booster pump B-101 for recycling. The bottom of the refining column T-103 is provided with a reboiler E-105 and the top is provided with a condenser E-106. The reboiler E-105 is used to exchange heat between a portion of the bottom material of the refining column and the light components from the top of the light component removal column to achieve boiling vaporization and partial condensation of the light components from the top of the light component removal column. The condenser E-106 is used to condense the top gas of the refining column and send a portion of the condensate as top reflux and a portion of the condensate as the collected product. In some embodiments, the distillation purification system further includes a collection tank G-103 for receiving the collected product of the refining column. Preferably, the top of the collection tank G-103 is provided with a gas phase sampling pipe.

[0043] The second condensation unit includes a second gas-liquid separator G-105, a second water cooler E-104, a separation tank G-102, and a second transfer pump B-103. The second gas-liquid separator G-105 is used to perform gas-liquid separation on the light components from the top of the light component removal tower after condensation in the reboiler E-105 of the refining tower. The separated gas phase is sent from the top to the second water cooler E-104, and the separated liquid phase is sent from the bottom to the separation tank G-102. The second water cooler E-104 is used to condense the gas phase material from the second gas-liquid separator G-105 and send the condensed product to the separation tank G-102. The separation tank G-102 is used to receive the liquid phase material from the second gas-liquid separator and the condensed product from the second water cooler, and discharge the gas phase from the top. The second transfer pump B-103 is used to send the liquid phase material in the separation tank G-102 as top reflux into the light component removal tower T-102.

[0044] In one embodiment, the distillation and purification system further includes a bypass line, which allows the material from the booster pump B-101 to be directly fed into the light-weight removal tower T-102. That is, the heavy-weight removal tower T-101 is not used; the material from the booster pump is directly fed into the light-weight removal tower for processing. The processing flow can be as follows: Figure 2 As shown.

[0045] When the distillation and purification system of this invention is running, see [link to documentation]. Figure 1Raw material ① is pressurized by booster pump B-101 and enters from the bottom of the heavy component removal tower T-101. The reboiler E-101 of the heavy component removal tower is indirectly heated by inexpensive low-pressure steam, and the heavy components are discharged from the bottom of the tower (i.e., the bottom discharge ② of T-101). The gas stream from the top of the heavy component removal tower is directly fed into the reboiler E-102 of the light component removal tower as a heat source and is used to exchange heat indirectly with the bottom liquid of the light component removal tower T-102. This causes part of the bottom liquid to evaporate and form the rising gas phase of the tower, while the gas stream from the top of the heavy component removal tower itself is cooled and condensed. After being separated by the first gas-liquid separator G-104, the gas phase enters the first water cooler E-103 for further condensation. Both the gas phase and the liquid phase from the first gas-liquid separator enter the storage tank G-101. The condensate from storage tank G-101 is divided into two streams. One stream is pumped by the first transfer pump B-102 to the top of the heavy removal tower T-101 as the reflux liquid for that tower. The other stream (i.e., feed ③ to T-102) is the feed to the light removal tower T-102. This forms an energy-saving double-effect distillation process.

[0046] The bottom product of the light-light removal tower T-102 is used as feed to the refining tower T-103 ⑤, and enters directly into the upper part of the refining tower T-103; while the gas stream from the top of the light-light removal tower T-102 serves as the heat source for the bottom of the refining tower T-103, and is directly fed into the reboiler E-105 of the refining tower, where it indirectly exchanges heat with the bottom liquid of the refining tower T-103, causing part of the bottom liquid to evaporate and form rising gas phase. Meanwhile, the vapor stream from the top of the light component removal tower is condensed by a cooler and separated by the second gas-liquid separator G-105. The vapor portion then enters the second water cooler E-104 for further condensation before entering the separator G-102 for gas-liquid separation. The vapor phase (i.e., the top discharge ④ of T-102) is discharged as the light component of the light component removal tower T-102, while the liquid phase is sent to the top of T-102 as the reflux liquid from the top of the light component removal tower T-102 by the second transfer pump B-103. This completes a triple-effect distillation process, which can save approximately 75% of energy compared to ordinary distillation.

[0047] The bottom liquid of the refining tower T-103 contains a large amount of heavy components with a high content of the target product. It is directly sent to the booster pump for recovery. The gas phase from the top of the tower is condensed by the refining tower condenser E-106 and enters the collection tank G-103. Its liquid phase is divided into two streams. One stream is used as the top reflux liquid of the refining tower T-103, and the other stream is collected as the high-purity product ⑥ for the electronics industry. The equilibrium gas phase in the collection tank G-103 can be taken out for testing as an online test sample through the gas phase sampling tube.

[0048] Based on this invention, it can also be understood that if the raw materials of industrial products contain only a very small amount of liquid volatiles that are easy to remove, then the heavy matter removal tower T-101 can be omitted, and a different method can be used. Figure 2The double-effect distillation process shown in the diagram involves the discharge of the bottom liquid from the refining column T-103 (i.e., the T-103 bottom drain ⑦) without recirculation, which is controlled by the booster pump B-101.

[0049] The present invention is further illustrated below with reference to the embodiments:

[0050] Example 1

[0051] Using industrial liquid chlorine as raw material, and employing methods such as Figure 1 The distillation and purification system shown produces high-purity chlorine for the electronics industry. The physical and thermal constants during operation and the parameters of each distillation column are shown in Tables 1 and 2 below:

[0052] Table 1. Thermal Constancy:

[0053]

[0054]

[0055] Table 2 Parameters of each distillation column:

[0056]

[0057] Example 2

[0058] Using food-grade carbon dioxide as raw material, and employing methods such as Figure 1 The distillation and purification system shown produces high-purity carbon dioxide for the electronics industry. The physical and thermal constants during operation and the parameters of each distillation column are shown in Tables 3 and 4 below:

[0059] Table 3. Heat Balance Calculation:

[0060]

[0061]

[0062] Table 4. Distillation column parameters:

[0063]

[0064] Example 3

[0065] Using 3N grade HBr as raw material, and employing methods such as... Figure 1 The distillation and purification system shown produces 5N-grade HBr. The physical and thermal constants during operation and the parameters of each distillation column are shown in Tables 5 and 6 below:

[0066] Table 5. Heat Balance Calculation:

[0067]

[0068]

[0069] Table 6. Distillation column parameters:

[0070]

[0071] Example 4

[0072] Using industrial liquid chlorine (in industrial liquid chlorine products, the heavy components contain only trace amounts of saturated water, so the heavy components removal tower T-101 is omitted) as raw material, the following method is adopted: Figure 2 The distillation and purification system shown produces high-purity chlorine for the electronics industry. The physical and thermal constants during operation and the parameters of each distillation column are shown in Tables 7 and 8 below:

[0073] Table 7. Heat Balance Calculation:

[0074]

[0075] Table 8 Parameters of each distillation column:

[0076]

[0077] Based on the results of the various embodiments, the performance of the product purified by distillation in this invention can fully meet the national standards. Moreover, it is energy-saving and has a high recovery rate. Compared with conventional distillation, it not only simplifies the process and saves about 75% of energy, but also improves the recovery rate.

Claims

1. A distillation and purification system for producing high-purity gases for the electronics industry from industrial products, characterized in that, The distillation and purification system includes: A booster pump is used to pressurize the raw material to be introduced into the deweighting tower and to transport the pressurized raw material to the deweighting tower. The heavy components removal tower is used to refine the raw material from the booster pump to remove the heavy components and send the light components out from the top of the tower; the bottom of the heavy components removal tower is equipped with a heavy components removal tower reboiler; A light component removal tower is used to refine the feed from the first delivery pump to remove light components, and the bottom product is fed into a refining tower. The bottom of the light component removal tower is equipped with a light component removal reboiler, which is used to exchange heat between a portion of the bottom material of the light component removal tower and the light components from the top of the heavy component removal tower so as to boil and vaporize, and to partially condense the light components from the top of the heavy component removal tower. The first condensation unit includes a first gas-liquid separator, a first water cooler, a storage tank, and a first transfer pump. The first gas-liquid separator separates the light components from the top of the heavy component removal tower after condensation in the reboiler of the light component removal tower, and sends the separated gas phase from the top to the first water cooler and the separated liquid phase from the bottom to the storage tank. The first water cooler condenses the gas phase material from the first gas-liquid separator and sends the condensed product to the storage tank. The storage tank receives the liquid phase material from the first gas-liquid separator and the condensed product from the first water cooler. The first transfer pump sends a portion of the liquid phase material in the storage tank as top reflux to the heavy component removal tower and a portion as feed to the light component removal tower. A refining column is used to refine the feed from the light component removal column to remove heavy components. The refining column has a reboiler at the bottom and a condenser at the top. The reboiler allows heat exchange between a portion of the bottom material and the light component from the top of the light component removal column for boiling vaporization and partial condensation. The condenser condenses the overhead gas from the refining column, and discharges a portion of the condensate as overhead reflux and a portion as collected product. The second condensation unit includes a second gas-liquid separator, a second water cooler, a separation tank, and a second transfer pump. The second gas-liquid separator separates the light components from the top of the light component removal tower after condensation in the reboiler of the refining tower, sending the separated gas phase from the top to the second water cooler and the separated liquid phase from the bottom to the separation tank. The second water cooler condenses the gas phase material from the second gas-liquid separator and sends the condensed product to the separation tank. The separation tank receives the liquid phase material from the second gas-liquid separator and the condensed product from the second water cooler, discharging the gas phase from the top. The second transfer pump sends the liquid phase material in the separation tank as top reflux back to the light component removal tower.

2. The distillation and purification system according to claim 1, characterized in that, The refining tower is used to refine the feed from the light component removal tower and to return the removed heavy components as feed to the booster pump.

3. The distillation and purification system according to claim 1, characterized in that, The distillation and purification system is also equipped with a bypass pipeline for directly feeding the material from the booster pump into the light-light ...

4. The distillation purification system according to any one of claims 1-3, characterized in that, The distillation and purification system also includes a collection tank for receiving the product collected from the purification column.

5. The distillation and purification system according to claim 4, characterized in that, The top of the storage tank is equipped with a safety valve to automatically release air in case of overpressure.

6. A method for preparing high-purity gases for the electronics industry using the distillation purification system according to any one of claims 1-5.

7. The method according to claim 6, characterized in that, When the molar fraction of heavy component impurities in the raw material is less than 0.001, the raw material pressurized by the booster pump is directly fed into the light component removal tower.

8. The method according to claim 6, characterized in that, The cold source for the first water cooler, the second water cooler, and the refining tower condenser is circulating water.

9. The method according to claim 8, characterized in that, The heat source for the reboiler of the deweight removal tower is low-pressure steam.

10. The method according to any one of claims 6-9, characterized in that, The raw materials are industrial liquid chlorine, food-grade carbon dioxide, or 3N-grade HBr.

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