Device for refining electronic-grade ultra-pure ammonia by removing light component and heavy component through medium-pressure rectification

Abstract

The utility model belongs to the technical field of electronic chemical purification equipment, and discloses a device for refining electronic-grade ultra-pure ammonia by removing light and heavy components through medium-pressure rectification. The device comprises a light component removal tower subsystem and a heavy component removal tower subsystem. A light component removal tower kettle of the light component removal tower subsystem is provided with a first liquid phase extraction opening and a first gas phase extraction opening which are parallel to each other, and the first liquid phase extraction opening and the first gas phase extraction opening can be alternatively communicated with a feeding opening of a heavy component removal tower after being connected in parallel through a pipeline, so that a switchable feeding structure is formed. And the de-heavy tower subsystem is provided with a switchable product extraction structure comprising a first extraction opening and a second extraction opening. The condensing equipment can adopt a condenser and a reflux tank which are split, or adopt a reflux condenser which is integrated on the tower top and has a corner cut structure at the lower end of a heat exchange tube. According to the utility model, through the specific switchable feeding and extraction structure, the adaptability of the device to different raw materials and product requirements is enhanced.

Description

Technical Field

[0001] This utility model relates to the field of electronic chemical purification technology, specifically to a distillation apparatus for refining ultrapure ammonia, and particularly to a medium-pressure distillation apparatus for removing light and heavy substances with multiple switchable feed and discharge structures. Background Technology

[0002] Electronic-grade ultrapure ammonia is a key raw material in semiconductor manufacturing, requiring extremely high purity. Currently, industrial ammonia is mainly purified using distillation columns. However, existing distillation units have the following significant structural defects:

[0003] The existing distillation units suffer from a single, unreliable design and poor adaptability: The connection between the distillation column bottom and downstream equipment typically involves only a single liquid-phase feed pipe. When the feed composition changes, especially when the content of heavy components (such as water and oil) is high, this single liquid-phase feed method can easily lead to excessive load on downstream equipment and poor separation efficiency. Furthermore, product collection is usually fixed at the top reflux tank or the bottom of the column, lacking a design that allows for flexible adjustment of the collection location based on different product purity requirements.

[0004] The requirements for the interfaces between hot and cold media are high, and the supporting systems are complex: In order to achieve low-temperature separation, the condenser in the existing equipment must be connected to a low-temperature refrigerant (such as liquid nitrogen) delivery pipeline, and the reboiler needs to be connected to a high-temperature heat source pipeline. This type of dedicated medium piping system has a complex structure and high investment and maintenance costs.

[0005] The filling process poses a risk of contamination: existing equipment typically has a low product outlet pressure, requiring an additional booster pump for filling. The introduction of the booster pump increases the complexity of the equipment and the number of connection points, while its internal lubrication system poses a risk of introducing contaminants into the product pipeline.

[0006] Therefore, existing ultrapure ammonia distillation devices suffer from problems such as insufficient structural flexibility, complex supporting systems, and easy introduction of pollution risks, requiring an improved device structure to address these issues. Utility Model Content

[0007] This invention aims to overcome the structural defects of existing ultrapure ammonia distillation devices and provide a novel medium-pressure distillation apparatus for refining electronic-grade ultrapure ammonia by removing light and heavy components. By improving the structure of the tower, pipeline connections, and interfaces, this apparatus achieves flexible switching between feeding and extraction methods, simplifies the external media system, and optimizes the product output structure, thereby enhancing the adaptability, economy, and product protection performance of the apparatus.

[0008] To solve the above-mentioned technical problems, this utility model provides the following technical solution:

[0009] A medium-pressure distillation apparatus for refining electronic-grade ultrapure ammonia by removing light and heavy components includes a light component removal tower system and a heavy component removal tower system.

[0010] The light-light-removal tower subsystem includes a light-light-removal tower, a condensation device connected to the top of the light-light-removal tower, and a light-light-removal tower reboiler connected to the bottom of the light-light-removal tower; the bottom of the light-light-removal tower is provided with a first liquid phase outlet and a first gas phase outlet in parallel, and both outlets are equipped with valves;

[0011] The de-weighting tower subsystem includes a de-weighting tower, a condensation device connected to the top of the de-weighting tower, and a de-weighting tower reboiler connected to the bottom of the de-weighting tower; the de-weighting tower is connected to at least one product collection mechanism;

[0012] The first liquid phase outlet and the first gas phase outlet of the light phase removal tower are connected in parallel through pipelines, and one of them is connected to the feed inlet of the heavy phase removal tower; the product collection mechanism is connected to the inlet of a product cooler through a product pipeline.

[0013] In some embodiments, the condensation equipment in the light-weight removal tower subsystem consists of a light-weight removal tower condenser and a light-weight removal tower reflux tank that are interconnected; the gas phase inlet of the light-weight removal tower condenser is connected to the top of the light-weight removal tower, and its liquid phase outlet is connected to the inlet of the light-weight removal tower reflux tank; the liquid phase outlet of the light-weight removal tower reflux tank is connected to the top of the light-weight removal tower through a reflux pipe.

[0014] Alternatively, the condensing equipment in the light-light tower subsystem is a light-light tower reflux condenser integrated at the top of the light-light tower.

[0015] In some embodiments, the condensation equipment in the deweight removal tower subsystem comprises a deweight removal tower condenser and a deweight removal tower reflux tank that are interconnected; the gas phase inlet of the deweight removal tower condenser is connected to the top of the deweight removal tower, and its liquid phase outlet is connected to the inlet of the deweight removal tower reflux tank; the liquid phase outlet of the deweight removal tower reflux tank is connected to the top of the deweight removal tower via a reflux pipe; and the product collection mechanism is a collection outlet located on the deweight removal tower reflux tank.

[0016] Alternatively, the condensing equipment in the deweight removal tower subsystem is a deweight removal tower reflux condenser integrated at the top of the deweight removal tower.

[0017] In some embodiments, the product extraction mechanism includes a first extraction outlet and a second extraction outlet. The first extraction outlet is disposed on the reflux tank of the de-weighting tower or on the tower body of the de-weighting tower, and the second extraction outlet is disposed on the tower body of the de-weighting tower. The two extraction outlets are connected in parallel through valves and pipelines to form a switchable product extraction mechanism.

[0018] In some embodiments, when the condensing device is a light tower reflux condenser or a heavy tower reflux condenser, the lower end of the heat exchange tube inside the reflux condenser has a chamfered structure.

[0019] In some embodiments, the chamfered structure is a 45-degree chamfer.

[0020] In some embodiments, the light-removal tower condenser and the heavy-removal tower condenser, or the light-removal tower reflux condenser and the heavy-removal tower reflux condenser, are each provided with a circulating cooling water inlet and a circulating cooling water outlet.

[0021] In some embodiments, both the light-weight removal tower reboiler and the heavy-weight removal tower reboiler are provided with a hot water inlet and a hot water outlet.

[0022] In some embodiments, the bottom of the deweighting tower is connected to a bottom liquid discharge pipe leading to an industrial ammonia recovery system.

[0023] In some embodiments, the light-weight removal tower, the light-weight removal tower condenser, the light-weight removal tower reboiler, the heavy-weight removal tower, the heavy-weight removal tower condenser, the heavy-weight removal tower reboiler, and the connecting pipes are integrated and installed on a common base, forming a skid-mounted structure.

[0024] Compared with the prior art, the device provided by this utility model has the following significant advantages in its structure:

[0025] 1. Flexible structure and enhanced adaptability: An innovative parallel dual-sampling outlet with valves for both liquid and gas phases is installed in the bottom of the light component removal tower. This structure allows the material to enter the downstream heavy component removal tower in either liquid or gas phase, thus adapting to raw materials with different heavy component contents and improving the overall operational flexibility of the unit and its adaptability to raw material fluctuations.

[0026] 2. Diverse product extraction mechanisms for precise purification: The deweighting tower is equipped with dual-path or multi-path product extraction mechanisms that allow extraction from the reflux tank or from the side of the tower. This design allows operators to flexibly select the optimal extraction point based on real-time product purity monitoring results, avoiding areas rich in light or heavy components, thus providing a structural basis for more precise purity control at the device level.

[0027] 3. Simplified external medium interfaces and economical structure: All condensing equipment is equipped with circulating cooling water interfaces, and all reboilers are equipped with hot water interfaces. This standardized medium-temperature medium interface structure replaces the original complex low-temperature refrigerant and high-temperature steam interfaces, greatly simplifying the connection structure between the unit and the utility system, and reducing the construction and maintenance costs of supporting pipelines, insulation, and control systems.

[0028] 4. Integrated and modular construction for easy implementation: The entire unit can adopt a skid-mounted integrated structure, with all towers, heat exchangers, tanks, and connecting pipes pre-installed on a robust base. This modular construction facilitates factory prefabrication, overall transportation, and rapid on-site installation, reducing on-site installation workload and the risk of potential connection leaks, thus improving project quality and construction efficiency.

[0029] 5. Optimized Component Structure for Stable Performance: The optional integrated reflux condenser at the top of the tower features heat exchange tubes with a chamfered bottom design. This specific shape effectively increases the flow area at the tube openings, optimizes the downward flow path of the condensate, and helps maintain the stability of the gas-liquid two-phase flow at the top of the tower, thus structurally ensuring the reliability of continuous operation of the unit. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the device structure according to Embodiment 1 of the present invention, showing the use of a split condenser, a reflux tank, and a structure with dual-outlet feed and dual-path product extraction.

[0031] Figure 2 This is a schematic diagram of the device structure of Embodiment 2 of the present invention, showing the structure of the integrated reflux condenser at the top of the tower and the corresponding extraction method.

[0032] Explanation of the labels in the diagram:

[0033] 1-Light weight removal tower; 2-Light weight removal tower condenser; 3-Light weight removal tower reflux tank; 4-Light weight removal tower reboiler; 5-Heavy weight removal tower; 6-Heavy weight removal tower condenser; 7-Heavy weight removal tower reflux tank; 8-Heavy weight removal tower reboiler; 9-Product cooler; 10-Light weight removal tower reflux condenser; 11-Heavy weight removal tower reflux condenser; L1-First liquid phase outlet; V1-First gas phase outlet; P1-First outlet; P2-Second outlet. Detailed Implementation

[0034] The technical solution of this utility model will now be clearly and completely described with reference to the accompanying drawings and specific embodiments. Obviously, the described embodiments are only a part of the embodiments of this utility model, and not all of them.

[0035] Example 1

[0036] See Figure 1 This embodiment demonstrates the specific structure of an apparatus for medium-pressure distillation to remove light and heavy components and purify electronic-grade ultrapure ammonia.

[0037] The device mainly consists of a light tower removal subsystem and a heavy tower removal subsystem, which are connected by pipelines.

[0038] Lightweight tower subsystem construction:

[0039] Lightweight removal tower 1 is a vertical tower with a raw material inlet in its tower body.

[0040] The condenser 2 of the light-light weight removal tower is a shell-and-tube heat exchanger with a circulating cooling water inlet and outlet on its shell side. The vapor inlet pipe of the condenser 2 is connected to the vapor outlet flange at the top of the light-light weight removal tower 1.

[0041] The reflux tank 3 of the light-light weight removal tower is a vertical or horizontal container, with its inlet flange connected to the liquid phase outlet pipe of the condenser 2 of the light-light weight removal tower. The reflux tank 3 has an exhaust pipe interface at the top and a liquid phase outlet at the bottom. A reflux pipe connects this liquid phase outlet to the reflux port at the top of the light-light weight removal tower 1.

[0042] The reboiler 4 of the light-light-removal tower is a thermosiphon reboiler with a hot water inlet and outlet on its tube side. The material inlet and outlet of the reboiler 4 are connected to the corresponding interfaces of the bottom of the light-light-removal tower 1 via pipelines.

[0043] At the bottom of the light-duty removal tower 1, there are two parallel flanged outlets. One is the lower-positioned first liquid phase outlet L1, and the other is the upper-positioned first gas phase outlet V1. Both outlet pipes are equipped with shut-off valves or ball valves.

[0044] Structure of the weight-removing tower subsystem:

[0045] The detachment tower 5 is a vertical tower.

[0046] The condenser 6 of the heavy removal tower has the same structure as the condenser 2 of the light removal tower. Its shell side is circulated with cooling water, and its gas phase inlet is connected to the top of the heavy removal tower 5.

[0047] The reflux tank 7 of the heavy removal tower has the same structure as the reflux tank 3 of the light removal tower. Its inlet is connected to the liquid phase outlet of the condenser 6 of the heavy removal tower, and it has an exhaust port at the top and a liquid phase outlet at the bottom. A reflux pipe connects this outlet to the top of the heavy removal tower 5.

[0048] The reboiler 8 for the heavy removal tower has the same structure as the reboiler 4 for the light removal tower. Its tube side is filled with hot water and connected to the bottom of the heavy removal tower 5.

[0049] The pipeline from the first liquid phase outlet L1 of the light phase removal tower and the pipeline from the first gas phase outlet V1 merge through a tee fitting to form a main feed pipeline, which ultimately connects to the feed inlet flange in the middle of the heavy phase removal tower 5. Each branch pipe is equipped with a valve before merging.

[0050] A first product outlet P1 is located at the bottom of the reflux tank 7 of the de-weighting tower. Simultaneously, a second product outlet P2 is located somewhere in the rectification section of the de-weighting tower 5. Valves are installed on the outlet pipes of both the first and second product outlets P1 and P2, and they converge into a main product pipeline via a tee fitting.

[0051] Product cooler 9 is a water-cooled heat exchanger. Its inlet is connected to the above-mentioned main product pipeline, and its outlet is the high-pressure product outlet, which can be directly connected to the filling arm or cylinder.

[0052] The bottom of the bottom of the deweight removal tower 5 is equipped with a bottom liquid discharge pipe, which is connected to the industrial ammonia recovery system.

[0053] Example 2

[0054] See Figure 2 This embodiment demonstrates another construction variant, the main difference being the integrated design of the condensing device.

[0055] Lightweight tower subsystem construction variants:

[0056] The separate light-weight tower condenser 2 and light-weight tower reflux tank 3 were eliminated.

[0057] At the top of the light-light ...

[0058] Uncondensed gas is discharged from the exhaust port at the top of the reflux condenser 10 of the light-weight gas removal tower. The condensate drips directly back into the tower.

[0059] The dual-outlet structure of the light-removal tower bottom is the same as in Example 1.

[0060] Construction variants of the weightless tower subsystem:

[0061] Similarly, the separate de-weighting tower condenser 6 and de-weighting tower reflux tank 7 were eliminated.

[0062] At the top of the de-weighting tower 5, a de-weighting tower reflux condenser 11 is integrated and installed. Its internal heat exchange tubes also have the same lower end chamfer structure, and the shell side is circulated with cooling water.

[0063] In this embodiment, the product is primarily extracted from the second extraction port P2 on the top of the deweight removal tower 5. The top of the deweight removal tower 5 may also have another, higher exhaust / side extraction port for discharging trace amounts of light components.

[0064] The structure of the reboiler 8 of the deweight removal tower, the product cooler 9, and the kettle liquid pipeline is similar to that of Example 1.

[0065] Overall integrated structure:

[0066] In any of the above embodiments, all equipment (towers, tanks, heat exchangers) and the pipes, valves, and instruments connecting them can be fixedly mounted on a steel frame base, forming an integrated skid-mounted module. The circulating cooling water main and hot water main are also pre-laid on the base, with quick-connect interfaces for external connections.

[0067] The above description is merely a preferred embodiment of this utility model, but the protection scope of this utility model is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the technical scope disclosed in this utility model, based on the technical solution and inventive concept of this utility model, should be included within the protection scope of this utility model.

Claims

1. An apparatus for medium-pressure distillation to remove light and heavy components and purify electronic-grade ultrapure ammonia, characterized in that, This includes a light-tower removal subsystem and a heavy-tower removal subsystem; The light-removal tower subsystem includes a light-removal tower (1), a condensation device connected to the top of the light-removal tower (1), and a light-removal tower reboiler (4) connected to the bottom of the light-removal tower (1); the bottom of the light-removal tower (1) is provided with a first liquid phase outlet (L1) and a first gas phase outlet (V1) in parallel. The deweight removal tower subsystem includes a deweight removal tower (5), a condensation device connected to the top of the deweight removal tower (5), and a deweight removal tower reboiler (8) connected to the bottom of the deweight removal tower (5); the deweight removal tower subsystem is also equipped with a product collection mechanism; The first liquid phase outlet (L1) and the first gas phase outlet (V1) are connected in parallel through pipelines and then connected to the feed inlet of the deweight tower (5); the product extraction mechanism is connected to the inlet of a product cooler (9) through a product pipeline.

2. The apparatus according to claim 1, characterized in that, The condensation equipment in the light-light tower subsystem includes a light-light tower condenser (2) and a light-light tower reflux tank (3) that are interconnected. The gas phase inlet of the light-light tower condenser (2) is connected to the top of the light-light tower (1), and its liquid phase outlet is connected to the inlet of the light-light tower reflux tank (3). The liquid phase outlet of the light-light tower reflux tank (3) is connected to the top of the light-light tower (1) through a reflux pipe.

3. The apparatus according to claim 1, characterized in that, The condensing equipment in the light-light tower subsystem is a light-light tower reflux condenser (10) integrated at the top of the light-light tower (1).

4. The apparatus according to claim 1, characterized in that, The condensation equipment in the de-weighting tower subsystem includes a de-weighting tower condenser (6) and a de-weighting tower reflux tank (7) that are interconnected. The gas phase inlet of the de-weighting tower condenser (6) is connected to the top of the de-weighting tower (5), and its liquid phase outlet is connected to the inlet of the de-weighting tower reflux tank (7). The liquid phase outlet of the de-weighting tower reflux tank (7) is connected to the top of the de-weighting tower (5) through a reflux pipe.

5. The apparatus according to claim 1, characterized in that, The condensing equipment in the deweight removal tower subsystem is a deweight removal tower reflux condenser (11) integrated at the top of the deweight removal tower (5).

6. The apparatus according to claim 1, characterized in that, The product extraction mechanism includes a first extraction outlet (P1) and a second extraction outlet (P2). The first extraction outlet (P1) is located on the reflux tank (7) of the deweight removal tower or on the tower body of the deweight removal tower (5). The second extraction outlet (P2) is located on the tower body of the deweight removal tower (5). The first extraction outlet (P1) and the second extraction outlet (P2) are connected in parallel through a pipeline, and one of them is connected to the product pipeline.

7. The apparatus according to claim 3, characterized in that, The lower end of the heat exchange tube in the light tower reflux condenser (10) has a chamfered structure.

8. The apparatus according to claim 5, characterized in that, The lower end of the heat exchange tube inside the de-weighting tower reflux condenser (11) has a chamfered structure.

9. The apparatus according to claim 1, characterized in that, All condensing equipment in the light-weight removal tower subsystem and the heavy-weight removal tower subsystem are equipped with circulating cooling water interfaces; all reboilers are equipped with hot water interfaces.

10. The apparatus according to claim 1, characterized in that, The light-removal tower (1), the condensation equipment, the light-removal tower reboiler (4), the heavy-removal tower (5), the heavy-removal tower reboiler (8), and the connecting pipes are integrated on a common base to form a skid-mounted structure.

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