Device for preparing electronic-grade ammonia by liquid ammonia rectification process

Abstract

The utility model discloses a device for preparing electronic-grade ammonia by a liquid ammonia rectification process, which comprises a raw material buffer tank, a liquid ammonia rectification device and a liquid ammonia rectification device, a feed port of the rectifying tower is communicated with a discharge port of the raw material buffer tank through a feed pump; a material inlet of the reboiler is communicated with the tower kettle of the rectifying tower through a tower kettle circulating pump, and a material outlet of the reboiler is communicated with the tower kettle of the rectifying tower through a pipeline; a gas phase inlet of the condenser is communicated with a tower top gas phase outlet of the rectifying tower through a pipeline; an inlet of the reflux tank is communicated with a liquid phase outlet of the condenser through a pipeline, an outlet of the reflux tank is connected with an inlet of the reflux pump, and an outlet of the reflux pump is connected with a reflux inlet in the top of the rectifying tower; an inlet of the tower kettle extraction pump is connected with a tower kettle of the rectifying tower, an outlet of the tower kettle extraction pump is connected with an external treatment device, and all the systems are matched for use, so that the separation effect is improved, and the product purity is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to liquid ammonia rectification technical field, concretely is a kind of liquid ammonia rectification process preparation electronic grade ammonia device. BACKGROUND

[0002] Traditional ammonia rectification process exposes many short boards when coping with the ultra-high purity demand of electronic grade ammonia, and the core problem focuses on the difficulty of meeting the separation effect standard.

[0003] On the one hand, the design and operation of traditional rectification tower lack fine consideration, the internal structure is simple, the mass transfer and heat transfer efficiency of tray or packing is limited, and the subtle difference in volatility of ammonia and impurities cannot be fully utilized to achieve deep purification. For example, when processing liquid ammonia raw materials containing a small amount of water and hydrocarbon impurities, due to insufficient gas-liquid contact in the tower, impurities with similar volatility cannot be effectively separated, resulting in stagnant product purity. On the other hand, the traditional process controls the key parameters of rectification such as pressure and temperature in a rough way, the pressure fluctuates frequently, and the temperature control precision is insufficient, so that the boiling point difference between ammonia and impurities cannot be maximized in the rectification process, and efficient separation cannot be achieved. In addition, with the rapid advancement of electronic products towards miniaturization and high performance, the internal circuit structure becomes increasingly complex and precise, and the purity of electronic grade ammonia must reach 99.99% or even higher precision to avoid problems such as short circuit and signal interference caused by impurities, and to effectively ensure the excellent quality and stable performance of electronic products. SUMMARY

[0004] The utility model aims at providing a kind of liquid ammonia rectification process preparation electronic grade ammonia device, solve the problem of poor separation effect and low product purity of prior art liquid ammonia rectification.

[0005] In order to achieve the above-mentioned purpose, the main technical scheme adopted by the utility model includes: a kind of liquid ammonia rectification process preparation electronic grade ammonia device, comprising: raw material buffer tank, its feed inlet is connected with raw material conveying pipe;Rectification tower, its feed inlet is communicated with the raw material buffer tank discharge port by feed pump;Reboiler, its material inlet is communicated with the tower kettle of the rectification tower by tower kettle circulating pump, and the material outlet of the reboiler is communicated with the tower kettle of the rectification tower by pipeline;Condenser, its gas inlet is communicated with the overhead gas outlet of the rectification tower by pipeline;Reflux tank, its inlet is communicated with the liquid outlet of the condenser by pipeline, and the outlet of the reflux tank is connected with the inlet of reflux pump, and the outlet of the reflux pump is connected with the reflux port of the top of the rectification tower;And tower kettle production pump, its inlet is connected with the tower kettle of the rectification tower, and the outlet is connected with external processing device.

[0006] As a preferred technical scheme, the heating medium inlet of the reboiler is connected with the hot water supply device by the hot water input pipe, and the heating medium outlet is connected with the hot water recovery device by the hot water output pipe.

[0007] As a preferred technical scheme, the cooling medium inlet of the condenser is connected with the circulating water supply device through a cold water input pipe, and the cooling medium outlet is connected with the circulating water recovery device through a cold water output pipe.

[0008] As a preferred technical scheme, the internal liquid ammonia conveying temperature of the raw material conveying pipe connected with the raw material buffer tank feeding port is -12-14 DEG C, and the conveying pressure is 1.5-1.7 MPag.

[0009] As a preferred technical scheme, the internal operating pressure of the rectifying tower is controlled at 1.5-1.7 MPag.

[0010] The utility model at least has following beneficial effects:

[0011] The utility model provides a kind of electronic grade ammonia device of liquid ammonia rectification process preparation, by 99.9% low temperature liquid ammonia raw material is conveyed into raw material buffer tank in suitable state, then pressurized by feeding pump, with stable flow is conveyed to the inside of rectifying tower, rectifying tower internal operating pressure is accurately controlled at 1.6 MPag, under this pressure interval, according to the difference of ammonia and impurity volatility, tower kettle material realizes efficient separation under the synergistic effect of reboiler, during, reboiler extracts tower kettle material by tower kettle circulating pump, promotes the separation of ammonia and impurity, ammonia and other volatile components move to tower top, and impurity remains in tower kettle, the gas phase ammonia of rectifying tower top enters condenser by pipeline, the cooling medium inlet of condenser is connected with the cold water provided by circulating water supply device using cold water input pipe, and the cold water is used to condense tower top gas phase, and the liquid phase after condensation flows into reflux tank, part of liquid in reflux tank is transported back to reflux port in the top of rectifying tower by reflux pump, to maintain the gas-liquid balance in rectifying tower, strengthen rectification effect, ensure the stable output of high-purity ammonia, the cooperation of each system improves separation effect and improves product purity. BRIEF DESCRIPTION OF DRAWINGS

[0012] The drawings described herein are used to provide further understanding of the present application, and form part of the present application, the illustrative embodiments of the present application and the description thereof are used to explain the present application, and do not constitute improper limitation on the present application. In the drawings:

[0013] Figure 1 It is the process flow chart of the liquid ammonia rectification process preparation electronic grade ammonia device of the utility model.

[0014] Explanation of reference numerals:

[0015] 1, raw material buffer tank;2, feeding pump;3, rectifying tower;4, reboiler;401, hot water input pipe;402, hot water output pipe;5, condenser;501, cold water input pipe;502, cold water output pipe;6, reflux tank;7, tower kettle circulating pump;8, tower kettle extraction pump. Detailed Implementation

[0016] The following will describe in detail the implementation of this application with reference to the accompanying drawings and embodiments, so that the implementation process of how this application uses technical means to solve technical problems and achieve technical effects can be fully understood and implemented accordingly.

[0017] Example

[0018] Please refer to Figure 1 As shown, this embodiment provides a liquid ammonia distillation process for producing electronic-grade ammonia, comprising: a raw material buffer tank 1, whose inlet is connected to a raw material conveying pipe; a distillation column 3, whose inlet is connected to the outlet of the raw material buffer tank 1 via a feed pump 2; a reboiler 4, whose material inlet is connected to the reboiler of the distillation column 3 via a column bottom circulation pump 7, and whose material outlet is connected to the reboiler of the distillation column 3 via a pipe; a condenser 5, whose gas phase inlet is connected to the top gas phase outlet of the distillation column 3 via a pipe; a reflux tank 6, whose inlet is connected to the liquid phase outlet of the condenser 5 via a pipe, whose outlet is connected to the inlet of a reflux pump, and whose outlet is connected to the reflux port at the top of the distillation column 3; and a column bottom discharge pump 8, whose inlet is connected to the reboiler of the distillation column 3, and whose outlet is connected to an external processing device. The pump delivers 99.9% cryogenic liquid ammonia raw material into the raw material buffer tank 1 in a suitable state, and then pressurizes it via the feed pump 2 to stabilize the ammonia. A fixed flow rate is delivered to the interior of distillation column 3. The operating pressure inside distillation column 3 is precisely controlled at 1.6 MPa. Under this pressure range, based on the difference in volatility between ammonia and impurities, the bottom material achieves efficient separation with the synergistic effect of reboiler 4. During this process, reboiler 4 draws bottom material through bottom circulation pump 7 to promote the separation of ammonia and impurities. Volatile components such as ammonia move towards the top of the column, while impurities remain in the bottom. The vaporous ammonia at the top of distillation column 3 enters condenser 5 through a pipeline. The cooling medium inlet of condenser 5 is connected to the cold water supply device via cold water input pipe 501 to condense the vapor at the top of the column. The condensed liquid phase flows into reflux tank 6. A portion of the liquid in reflux tank 6 is pumped back to the reflux port at the top of distillation column 3 by reflux pump, thereby maintaining the gas-liquid balance inside distillation column 3, enhancing the distillation effect, and ensuring the stable production of high-purity ammonia. The coordinated use of various systems improves the separation effect and increases product purity.

[0019] The heating medium inlet of the reboiler 4 is connected to the hot water supply device through the hot water input pipe 401, and the heating medium outlet is connected to the hot water recovery device through the hot water output pipe 402. The reboiler 4 is heated by the hot water supply device and the hot water is recycled through the hot water recovery device, which reduces the additional energy consumption for heating.

[0020] The cooling medium inlet of the condenser 5 is connected with the circulating water supply device through the cold water input pipe 501, the cooling medium outlet is connected with the circulating water recovery device through the cold water output pipe 502, the condenser 5 uses the circulating water supply device to provide the cooling medium, and the cold water input pipe 501 and the cold water output pipe 502 realize the cooling circulation, so that the overhead gas phase condensation is completed in a low-cost and high-efficiency mode.

[0021] The internal liquid ammonia conveying temperature of the raw material conveying pipe connected with the raw material feeding port of the raw material buffer tank 1 is-12-14 DEG C, and the conveying pressure is 1.5-1.7 MPag, preferably, the internal liquid ammonia conveying temperature of the raw material conveying pipe is-13 DEG C, and the conveying pressure is 1.6 MPag, so that the liquid ammonia can enter the subsequent rectification process in the most suitable state, avoiding the premature gasification or crystallization caused by improper temperature and pressure, and improving the operation fluency and stability of the whole process.

[0022] The internal operation pressure of the rectification tower 3 is controlled at 1.5-1.7 MPag, preferably, the internal operation pressure of the rectification tower 3 is controlled at 1.6 MPag, so that the volatility difference between ammonia and other impurities can be better utilized, the ammonia can be preferentially gasified and rise to the top for condensation, and the impurities can be more left in the tower kettle, thereby improving the separation efficiency and helping to obtain high-purity electronic-grade ammonia.

[0023] Working principle:

[0024] The 99.9% low-temperature liquid ammonia raw material enters the raw material buffer tank 1 through the raw material conveying pipe, in the process, the raw material conveying pipe strictly controls the conveying temperature of the liquid ammonia to be-13 DEG C, and the conveying pressure is 1.6 MPag, the low-temperature and stable pressure condition ensures that the liquid ammonia enters the raw material buffer tank 1 in a suitable state, avoids premature gasification or crystallization and other abnormal phenomena, and ensures the stability of the subsequent process raw materials;

[0025] The liquid ammonia in the raw material buffer tank 1 is pressurized by the feed pump 2 and then conveyed to the feeding port of the rectification tower 3 at a stable flow rate, and the accurate conveying of the feed pump 2 ensures the continuity and stability of the feeding of the rectification tower 3;

[0026] The liquid ammonia entering the rectification tower 3 starts the rectification operation in the tower, and the internal operation pressure of the rectification tower 3 is accurately controlled at 1.6 MPag, under this pressure range, according to the difference in volatility between ammonia and impurities, the tower kettle material realizes efficient separation under the synergistic action of the reboiler 4;

[0027] The reboiler 4 extracts the tower kettle material through the tower kettle circulating pump 7, the heating medium inlet is introduced into the hot water provided by the hot water supply device through the hot water input pipe 401, the tower kettle material is partially gasified by heating, the gasified material is returned to the tower kettle of the rectifying tower 3 through the pipe from the material outlet of the reboiler 4, and a continuous gas-liquid circulating flow is formed, so as to promote the separation of ammonia and impurities, and the ammonia and other volatile components move to the top of the tower, and the impurities remain in the tower kettle;

[0028] The gaseous ammonia at the top of the rectifying tower 3 enters the condenser 5 through the pipe, the cooling medium inlet of the condenser 5 is connected to the circulating water supply device through the cold water input pipe 501, and the gaseous phase at the top of the tower is condensed;

[0029] The condensed liquid phase flows into the reflux tank 6, and part of the liquid in the reflux tank 6 is transported back to the reflux port at the top of the rectifying tower 3 through the reflux pump; the purpose of reflux is to maintain the gas-liquid balance in the rectifying tower 3, strengthen the rectification effect, and ensure the stable output of high-purity ammonia;

[0030] Another part of the liquid phase in the reflux tank 6 reaches the electronic grade ammonia purity standard: 99.99% and above, and is extracted as qualified products to enter the subsequent storage or use link;

[0031] A small amount of discharge liquid at the bottom of the rectifying tower 3 is extracted by the tower kettle extraction pump 8, the inlet of which is connected with the tower kettle of the rectifying tower 3, and the outlet is connected with an external treatment device; the external treatment device processes according to the composition and properties of the discharge liquid, such as recycling the liquid containing valuable components, and environmental protection treatment of the liquid containing pollution components, so as to realize the closed loop operation of the whole process;

[0032] In the whole process, the hot water after being used by the reboiler 4 is returned to the hot water recovery device through the hot water output pipe 402, so as to realize the recycling of the hot water and reduce the energy consumption;

[0033] The cold water after being used by the condenser 5 is returned to the circulating water recovery device through the cold water output pipe 502, so as to realize the recycling of the cooling medium, further improve the energy utilization efficiency, and ensure the economy and sustainability of the process.

[0034] The above description shows and describes several preferred embodiments of the utility model, but as before, it should be understood that the utility model is not limited to the form disclosed herein, and should not be regarded as excluding other embodiments, but can be used in various other combinations, modifications and environments, and can be modified by the above-mentioned teaching or related technical or knowledge within the scope of the utility model concept described herein. The modification and change made by the person skilled in the art without departing from the spirit and scope of the utility model shall be within the protection scope of the claims attached to the utility model.

Claims

1. An apparatus for producing electronic grade ammonia by a liquid ammonia rectification process, characterized by, The application relates to a distillation device for liquid ammonia, which comprises the following parts: a raw material buffer tank (1) with a raw material conveying pipe connected to the feeding port of the raw material buffer tank (1); a rectifying tower (3) with a feeding port communicated with the discharging port of the raw material buffer tank (1) through a feeding pump (2); a reboiler (4) with a material inlet communicated with the tower kettle of the rectifying tower (3) through a tower kettle circulating pump (7), and a material outlet communicated with the tower kettle of the rectifying tower (3) through a pipeline; a condenser (5) with a gas phase inlet communicated with the overhead gas phase outlet of the rectifying tower (3) through a pipeline; a reflux tank (6) with an inlet communicated with the liquid phase outlet of the condenser (5) through a pipeline, an outlet connected with the inlet of a reflux pump, and an outlet of the reflux pump connected with the reflux port of the top of the rectifying tower (3); a tower kettle discharging pump (8) with an inlet connected with the tower kettle of the rectifying tower (3) and an outlet connected with an external treatment device. The heating medium inlet of the reboiler (4) is connected with a hot water supply device through a hot water input pipe (401), and the heating medium outlet is connected with a hot water recovery device through a hot water output pipe (402).

2. The apparatus for producing electronic grade ammonia by a liquid ammonia rectification process according to claim 1, characterized in that: The cooling medium inlet of the condenser (5) is connected with a circulating water supply device through a cold water input pipe (501), and the cooling medium outlet is connected with a circulating water recovery device through a cold water output pipe (502).

3. The apparatus for producing electronic grade ammonia by a liquid ammonia rectification process according to claim 2, wherein: The internal liquid ammonia conveying temperature of the raw material conveying pipe connected with the feeding port of the raw material buffer tank (1) is -12-14 DEG C, and the conveying pressure is 1.5-1.7 MPa.

4. The apparatus for producing electronic grade ammonia by the process of rectifying liquid ammonia as claimed in claim 1, wherein: The internal operating pressure of the rectifying tower (3) is controlled to be 1.5-1.7 MPa.

5. The apparatus for producing electronic grade ammonia by the process of rectifying liquid ammonia as claimed in claim 1, wherein: ​

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