CN113072080A - Method and device for preparing electronic grade ultra-pure ammonia by flash evaporation - Google Patents
Method and device for preparing electronic grade ultra-pure ammonia by flash evaporation Download PDFInfo
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- CN113072080A CN113072080A CN202110498013.6A CN202110498013A CN113072080A CN 113072080 A CN113072080 A CN 113072080A CN 202110498013 A CN202110498013 A CN 202110498013A CN 113072080 A CN113072080 A CN 113072080A
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- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
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- C01C1/02—Preparation, purification or separation of ammonia
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Abstract
The invention relates to the field of special gas production, and particularly discloses a method and a device for preparing electronic grade ultrapure ammonia by flash evaporation, wherein liquid ammonia is treated in a mode of carrying out reduced pressure flash evaporation for multiple times, light component impurities in the liquid ammonia are separated, and finally, gas phase substances subjected to reduced pressure flash evaporation are purified and condensed to obtain the electronic grade ultrapure ammonia; the corresponding preparation equipment comprises a flash tank and a plurality of subsequent reprocessing flash mechanisms, and the gas phase recovery mechanism is arranged to reprocess and utilize the intermediate product, so that the waste of materials is reduced, and the utilization rate of raw materials is improved.
Description
Technical Field
The invention relates to the field of special gas production, in particular to the technical field of ammonia preparation, and particularly relates to a method and a device for preparing electronic grade ultra-pure ammonia by flash evaporation.
Background
The electronic grade ultra-pure ammonia industry belongs to the electronic gas in special gas, and belongs to ultra-clean high-purity electronic chemicals. The method is mainly applied to manufacturing high-quality nitride, namely gallium nitride (GaN) and silicon nitride (Si3N4), wherein the former is the basis for manufacturing light emitting diodes, and the latter is widely applied to manufacturing solar cells (photovoltaics), Integrated Circuits (ICs) and Liquid Crystal Displays (LCDs).
Electronic grade ultra-pure ammonia is used as one of key basic chemical materials in the manufacturing process of integrated circuits, and is mainly used for the processes of cleaning, etching, doping and depositing of chips. The purity and cleanliness of ultra-clean high-purity electronic chemicals have very important influence on the yield, electrical performance and reliability of integrated circuits.
Therefore, the purity requirement of the ultra-pure ammonia is higher and higher, and the national standard of the ultra-pure ammonia is from 99.9995% (5N5), 99.99994% (6N4, blue ammonia) to 99.99999% (7N, white ammonia) of market demand.
In many existing patents and factory production processes, the adopted process routes are basically similar, and industrial-grade liquid ammonia is subjected to low-temperature vaporization, filtration and oil removal, adsorption and water removal, rectification, terminal purification and other processes in a permutation and combination manner to gradually obtain high-concentration ammonia. But the technical process is complex, and the processes of temperature swing adsorption and the like need regeneration, so that the energy consumption is overlarge; a drying adsorption device is arranged before rectification, so that new particle impurities and the like are easily brought in, and the fluctuation of the product quality is caused.
Therefore, the existing preparation process of electronic grade ultrapure ammonia still has a space for optimization and improvement, so that not only the extraction precision needs to meet higher requirements, but also the extraction process needs to be correspondingly simplified. Therefore, a more reasonable technical scheme needs to be provided, and the defects in the prior art are overcome.
Disclosure of Invention
In order to solve the defects of the prior art mentioned in the above, the invention provides a method and a device for preparing electronic grade ultra-pure ammonia by flash evaporation, wherein the light components in the raw material liquid ammonia are removed by adopting the processes of flash evaporation, pressurization and preheating treatment, the removal of the light components can be realized to the maximum extent by circulating treatment, and finally the ultra-pure ammonia is obtained by purification and condensation liquefaction treatment.
In order to achieve the purpose, the invention specifically adopts the technical scheme that:
a method for preparing electronic grade ultra-pure ammonia by flash evaporation comprises the following steps:
liquid ammonia is used as a raw material, and the raw material is subjected to reduced pressure flash evaporation to obtain a saturated gas phase and a saturated liquid phase;
collecting saturated liquid phase, pressurizing to 1.35-3.2 MPa, preheating after pressurizing to raise the temperature of the saturated liquid phase, carrying out decompression flash evaporation again before the liquid phase temperature reaches the saturation temperature of saturated vapor pressure, wherein the pressure during decompression flash evaporation is less than 1 MPa; circularly performing the pressurizing, preheating and pressure-reducing flash evaporation operation steps to ensure that the number of times of pressure-reducing flash evaporation reaches three times at least;
collecting saturated gas phase subjected to circulating reduced pressure flash evaporation treatment, purifying, and condensing and liquefying to obtain the electronic grade ultra-pure ammonia.
According to the preparation method disclosed by the invention, the liquid ammonia raw material is subjected to multiple times of reduced pressure flash evaporation, light components in the liquid ammonia raw material are continuously removed, the gas phase is subjected to purification treatment, and finally the gas phase after flash evaporation is purified to obtain the electronic grade ultra-pure ammonia with extremely high purity; and after the first reduced-pressure flash tank and the second reduced-pressure flash tank, the obtained gas phase can be further processed for preparing products such as crude ammonia or ammonia water.
Further, in the present invention, the pressure of the saturated liquid phase for pressurization treatment influences the effect of the subsequent decompression flash evaporation, and is optimized and one of the following feasible options is provided: the pressure was increased to 1.5MPa while pressurizing the saturated liquid phase. When the scheme is adopted, the pressure is reduced to below 1MPa during the subsequent pressure reduction flash evaporation, and the gas phase and the liquid phase can be separated to a higher degree.
Further, the intermediate product obtained after each vacuum flash evaporation treatment comprises a gas phase and a liquid phase, wherein the liquid phase is used for subsequent reprocessing to obtain ammonia with higher purity, and the gas phase can be exported and recycled, and specifically, one of the gas phase recycling modes is given as follows: and collecting gas phases obtained after the first decompression flash evaporation and the second decompression flash evaporation and carrying out condensation treatment to obtain crude ammonia. When the scheme is adopted, crude ammonia can be treated and then used as raw material liquid ammonia to carry out reduced pressure flash evaporation again for preparing ultra-pure ammonia, and the utilization rate of raw materials is improved.
Further, another way of treating the gas phase of the intermediate product is as follows: collecting gas phases obtained after the first decompression flash evaporation and the second decompression flash evaporation, and obtaining ammonia water through water absorption treatment. The ammonia water can be used for other industrial production, and the waste of raw materials is reduced.
The above disclosure describes a method for preparing electronic grade ultra-pure ammonia, and the present invention also discloses a device for preparing ultra-pure ammonia, specifically described as follows:
a device for preparing electronic grade ultra-pure ammonia by flash evaporation comprises a primary flash evaporation tank, wherein a feed inlet of the primary flash evaporation tank is communicated with a raw material conveying mechanism; the discharge hole of the flash tank is sequentially communicated with at least two reprocessing flash mechanisms, and each reprocessing flash mechanism comprises a pressurizing assembly, a preheating assembly and a flash evaporation assembly; the output end of the last flash evaporation assembly is connected with the terminal purification assembly, the condensation liquefaction assembly and the storage assembly.
According to the preparation device disclosed above, primary flash evaporation is performed through the primary flash tank, the liquid ammonia raw material is processed to obtain a saturated gas phase and a saturated liquid phase, wherein the saturated liquid phase is sent to the processing flash evaporation mechanism to be subjected to circulating flash evaporation processing, and finally, the electronic grade ultra-pure ammonia can be obtained.
Furthermore, the preparation equipment of the invention sets a special export mechanism for the intermediate product to process, and the following feasible options are provided: and when the number of the reprocessing flash evaporation mechanisms is more than two, gas phase conveying structures are arranged from the second flash evaporation assembly to the last flash evaporation assembly and communicated to the terminal purification assembly. When adopting such scheme, the ammonia that finally carries out purification condensation and obtain is handled through cubic flash distillation at least, has fully removed light component impurity, and the purification degree improves greatly, can satisfy actual demand.
Still further, for the special export processing of the intermediate product, the invention optimizes the preparation device and puts out one feasible choice as follows: the first-stage flash tank and/or the first reprocessing flash mechanism are communicated with the gas phase recovery mechanism. The gas phase recovery mechanism is used for collecting the saturated gas phase subjected to the reduced pressure flash evaporation treatment and carrying out retreatment, and the retreated product is used for repeatedly preparing ammonia or used for producing other industrial products, so that the utilization rate of raw materials can be improved, and the waste of the raw materials is reduced.
Further, the weather recovery mechanism employed in the present invention may be configured in a variety of ways, not exclusively limited thereto, optimized and one of the possible options: the gas phase recovery mechanism comprises a recovery condensation component and a crude ammonia storage component. When adopting such scheme, carry out condensation process and obtain crude ammonia product to the saturated gaseous phase of collecting, crude ammonia product can be used as the liquid ammonia raw materials and carry out decompression flash distillation to improve the utilization ratio of raw materials.
Further, the vapor phase recovery mechanism is not limited to the above one, and another possible option is exemplified here: the gas phase recovery mechanism comprises a gas phase absorption assembly, an ammonia water storage assembly and a tail gas separation treatment assembly; the tail gas separation processing assembly is communicated with the ammonia cooler assembly, and the output end of the ammonia cooler assembly is communicated to the first-stage flash tank. When adopting such scheme, can follow and handle in the saturation gas phase and obtain the aqueous ammonia, carry out the separation processing with tail gas simultaneously and can obtain the liquid ammonia raw materials through ammonia cooler subassembly processing, improved the utilization ratio of raw materials.
Still further, the solution that the flash evaporation component can adopt is not limited only, and the flash evaporation component disclosed in the above technical solution is optimized, and one of the feasible options is as follows: the flash evaporation assembly comprises a pressure reducing valve assembly and a flash evaporation tank which are communicated in sequence.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the liquid ammonia is treated in a way of carrying out reduced pressure flash evaporation for multiple times, light component impurities in the liquid ammonia are separated, and finally, the gas phase substance subjected to reduced pressure flash evaporation is purified and condensed to obtain electronic grade ultrapure ammonia; the corresponding preparation equipment can reprocess and utilize the intermediate product, thereby reducing the waste of materials and improving the utilization rate of raw materials.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only show some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic flow diagram of the preparation of electronic grade ultra-pure ammonia.
FIG. 2 is a schematic diagram of the components of an apparatus for producing electronic grade ultra-pure ammonia.
FIG. 3 is a schematic diagram of the components of another apparatus for producing electronic grade ultra-pure ammonia.
Detailed Description
The invention is further explained below with reference to the drawings and the specific embodiments.
It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. Specific structural and functional details disclosed herein are merely illustrative of example embodiments of the invention. This invention may, however, be embodied in many alternate forms and should not be construed as limited to the embodiments set forth herein.
Example 1
Aiming at the current situations that the existing preparation process of the electronic grade ultrapure ammonia is complex and the preparation effect is not ideal enough, the embodiment optimizes the preparation process of the electronic grade ultrapure ammonia and provides a scheme capable of overcoming the problems in the prior art.
Specifically, the technical solution disclosed in this embodiment is as follows:
as shown in fig. 1, a method for preparing electronic grade ultra-pure ammonia by flash evaporation comprises the following steps:
s01: liquid ammonia is used as a raw material, and the raw material is subjected to reduced pressure flash evaporation to obtain a saturated gas phase and a saturated liquid phase;
s02: collecting saturated liquid phase, pressurizing to 1.35-3.2 MPa, preheating after pressurizing to raise the temperature of the saturated liquid phase, carrying out decompression flash evaporation again before the liquid phase temperature reaches the saturation temperature of saturated vapor pressure, wherein the pressure during decompression flash evaporation is less than 1 MPa;
s03: repeating S02, and circularly performing the pressurizing, preheating and pressure-reducing flash evaporation operation steps to minimize the number of times of pressure-reducing flash evaporation to three times;
s04: collecting saturated gas phase subjected to circulating reduced pressure flash evaporation treatment, purifying, and condensing and liquefying to obtain the electronic grade ultra-pure ammonia.
According to the preparation method disclosed by the invention, the liquid ammonia raw material is subjected to multiple times of reduced pressure flash evaporation, light components in the liquid ammonia raw material are continuously removed, the gas phase is subjected to purification treatment, and finally the gas phase after flash evaporation is purified to obtain the electronic grade ultra-pure ammonia with extremely high purity; and after the first reduced-pressure flash tank and the second reduced-pressure flash tank, the obtained gas phase can be further processed for preparing products such as crude ammonia or ammonia water.
Preferably, the number of times of the reduced-pressure flash is set to be four in the embodiment, and the reduced-pressure flash comprises primary flash, secondary flash, tertiary flash and terminal flash. After three-stage flash evaporation, the purity of the flash-evaporated gas-phase ammonia reaches more than 4N7, and 5N 5-grade ultra-pure ammonia can be prepared after terminal purification; after terminal flash evaporation, the purity of the flash-evaporated gas-phase ammonia reaches above 5N7, and 6N4, even 7N-grade ultra-pure ammonia can be prepared by terminal purification.
In this embodiment, the pressure of the saturated liquid phase for pressurization affects the effect of the subsequent decompression flash, and is optimized and one of the following feasible options is provided: the pressure was increased to 1.5MPa while pressurizing the saturated liquid phase. When the scheme is adopted, the pressure is reduced to below 1MPa during the subsequent pressure reduction flash evaporation, and the gas phase and the liquid phase can be separated to a higher degree.
Preferably, in this embodiment, the pressure of each flash evaporation may be controlled and adjusted, for example, the pressure value of the raw material used in the first-stage flash evaporation may be 1.35MPa, or may be a higher value; before the second-stage flash evaporation, the third-stage flash evaporation and the terminal flash evaporation, the pressure of the saturated liquid phase is increased to 1.5-3.2 MPa after pressurization treatment, and the pressure can be specifically adjusted according to factors such as the actual amount of saturated liquid phase substances.
Preferably, the pressure in the flash tank can be adjusted to be reduced to 0.3MPa to 1MPa when the second-stage, third-stage and final-stage reduced-pressure flash evaporation is carried out.
The intermediate product obtained after each pressure reduction flash evaporation treatment comprises a gas phase and a liquid phase, wherein the liquid phase is used for subsequent reprocessing to obtain ammonia with higher purity, and the gas phase can be recycled after being output, specifically, the embodiment adopts one of the gas phase recycling modes: collecting gas phases obtained after the first-stage reduced pressure flash evaporation and the second-stage reduced pressure flash evaporation, and condensing to obtain crude ammonia. When the scheme is adopted, crude ammonia can be treated and then used as raw material liquid ammonia to carry out reduced pressure flash evaporation again for preparing ultra-pure ammonia, and the utilization rate of raw materials is improved.
In some embodiments, another intermediate gas phase treatment may be used: collecting gas phases obtained after the first decompression flash evaporation and the second decompression flash evaporation, and obtaining ammonia water through water absorption treatment. The ammonia water can be used for other industrial production, and the waste of raw materials is reduced.
Example 2
The above example 1 discloses a method for preparing electronic grade ultra-pure ammonia, and this example also discloses a device for preparing ultra-pure ammonia, which is specifically described as follows:
as shown in FIG. 2, the device for preparing electronic grade ultra-pure ammonia by flash evaporation comprises a primary flash evaporation tank, wherein a feed inlet of the primary flash evaporation tank is communicated with a raw material conveying mechanism; the discharge hole of the flash tank is sequentially communicated with at least two reprocessing flash mechanisms, and each reprocessing flash mechanism comprises a pressurizing assembly, a preheating assembly and a flash evaporation assembly; the output end of the last flash evaporation assembly is connected with the terminal purification assembly, the condensation liquefaction assembly and the storage assembly.
According to the preparation device disclosed above, primary flash evaporation is performed through the primary flash tank, the liquid ammonia raw material is processed to obtain a saturated gas phase and a saturated liquid phase, wherein the saturated liquid phase is sent to the processing flash evaporation mechanism to be subjected to circulating flash evaporation processing, and finally, the electronic grade ultra-pure ammonia can be obtained.
Preferably, set up special feedstock equipment in this embodiment, feedstock equipment can add liquid ammonia in the one-level flash tank, also can add gaseous ammonia in the one-level flash tank after the condensation liquefaction.
In this embodiment, the preparation apparatus is provided with a special export mechanism for processing the intermediate product, and the following possible options are mentioned here: and when the number of the reprocessing flash evaporation mechanisms is more than two, gas phase conveying structures are arranged from the second flash evaporation assembly to the last flash evaporation assembly and communicated to the terminal purification assembly. When adopting such scheme, the ammonia that finally carries out purification condensation and obtain is handled through cubic flash distillation at least, has fully removed light component impurity, and the purification degree improves greatly, can satisfy actual demand.
Preferably, the number of flash evaporation mechanisms in the treatment is set to three in this embodiment, corresponding to that in embodiment 1.
Wherein, the pressurizing assembly comprises a pressurizing pump, and the preheating assembly comprises a preheater. The pressurizing assembly and the preheating assembly are communicated in sequence, and the saturated liquid phase obtained after decompression flash evaporation is pressurized and preheated and then sent into a flash tank of the next stage.
For the specific export process of the intermediate product, this embodiment optimizes the production device and presents one possible choice as follows: the first-stage flash tank and/or the first reprocessing flash mechanism are communicated with the gas phase recovery mechanism. The gas phase recovery mechanism is used for collecting the saturated gas phase subjected to the reduced pressure flash evaporation treatment and carrying out retreatment, and the retreated product is used for repeatedly preparing ammonia or used for producing other industrial products, so that the utilization rate of raw materials can be improved, and the waste of the raw materials is reduced.
The weather recovery mechanism may be configured in a variety of ways, not exclusively, and the present embodiment is optimized and uses one of the possible options: the gas phase recovery mechanism comprises a recovery condensation component and a crude ammonia storage component. When adopting such scheme, carry out condensation process and obtain crude ammonia product to the saturated gaseous phase of collecting, crude ammonia product can be used as the liquid ammonia raw materials and carry out decompression flash distillation to improve the utilization ratio of raw materials.
In other embodiments, the vapor phase recovery mechanism is not limited to the above one, and is optimized and another possible option is presented: as shown in fig. 3, the gas phase recovery mechanism includes a gas phase absorption assembly, an ammonia water storage assembly and a tail gas separation treatment assembly; the tail gas separation processing assembly is communicated with the ammonia cooler assembly, and the output end of the ammonia cooler assembly is communicated to the first-stage flash tank. When adopting such scheme, can follow and handle in the saturation gas phase and obtain the aqueous ammonia, carry out the separation processing with tail gas simultaneously and can obtain the liquid ammonia raw materials through ammonia cooler subassembly processing, improved the utilization ratio of raw materials.
Preferably, the gas-phase absorption assembly comprises an absorption tower, and the off-gas separation treatment assembly comprises a melamine off-gas separation device.
Preferably, the flash unit in this embodiment also employs a flash tank.
Preferably, in order to achieve better decompression flash effect, the scheme that the flash evaporation component can adopt is not limited, and the embodiment optimizes the flash evaporation component disclosed in the technical scheme, such as one feasible option: the flash evaporation assembly comprises a pressure reducing valve assembly and a flash evaporation tank which are communicated in sequence.
The above embodiments are just exemplified in the present embodiment, but the present embodiment is not limited to the above alternative embodiments, and those skilled in the art can obtain other various embodiments by arbitrarily combining with each other according to the above embodiments, and any other various embodiments can be obtained by anyone in light of the present embodiment. The above detailed description should not be construed as limiting the scope of the present embodiments, which should be defined in the claims, and the description should be used for interpreting the claims.
Claims (10)
1. A method for preparing electronic grade ultra-pure ammonia by flash evaporation is characterized by comprising the following steps:
liquid ammonia is used as a raw material, and the raw material is subjected to reduced pressure flash evaporation to obtain a saturated gas phase and a saturated liquid phase;
collecting saturated liquid phase, pressurizing to 1.35-3.2 MPa, preheating after pressurizing to raise the temperature of the saturated liquid phase, carrying out decompression flash evaporation again before the liquid phase temperature reaches the saturation temperature of saturated vapor pressure, wherein the pressure during decompression flash evaporation is less than 1 MPa; circularly performing the pressurizing, preheating and pressure-reducing flash evaporation operation steps to ensure that the number of times of pressure-reducing flash evaporation reaches three times at least;
collecting saturated gas phase subjected to circulating reduced pressure flash evaporation treatment, purifying, and condensing and liquefying to obtain the electronic grade ultra-pure ammonia.
2. The flash evaporation process for preparing electronic grade ultra-pure ammonia according to claim 1, wherein: the pressure was increased to 1.5MPa while pressurizing the saturated liquid phase.
3. The flash evaporation process for preparing electronic grade ultra-pure ammonia according to claim 1, wherein: and collecting gas phases obtained after the first decompression flash evaporation and the second decompression flash evaporation and carrying out condensation treatment to obtain crude ammonia.
4. The flash evaporation process for preparing electronic grade ultra-pure ammonia according to claim 1, wherein: collecting gas phases obtained after the first decompression flash evaporation and the second decompression flash evaporation, and obtaining ammonia water through water absorption treatment.
5. An apparatus for flash evaporation preparation of electronic grade ultra-pure ammonia, which is used in the method for preparing the ultra-pure ammonia according to any one of claims 1 to 4, and is characterized in that: the device comprises a primary flash tank, wherein a feed inlet of the primary flash tank is communicated with a raw material conveying mechanism; the discharge hole of the flash tank is sequentially communicated with at least two reprocessing flash mechanisms, and each reprocessing flash mechanism comprises a pressurizing assembly, a preheating assembly and a flash evaporation assembly; the output end of the last flash evaporation assembly is connected with the terminal purification assembly, the condensation liquefaction assembly and the storage assembly.
6. The apparatus for flash evaporation of ultra-pure ammonia of electronic grade according to claim 5, wherein: and when the number of the reprocessing flash evaporation mechanisms is more than two, gas phase conveying structures are arranged from the second flash evaporation assembly to the last flash evaporation assembly and communicated to the terminal purification assembly.
7. The apparatus for flash evaporation of ultra-pure ammonia of electronic grade according to claim 5 or 6, characterized in that: the first-stage flash tank and/or the first reprocessing flash mechanism are communicated with the gas phase recovery mechanism.
8. The apparatus for flash evaporation of ultra-pure ammonia of electronic grade according to claim 7, wherein: the gas phase recovery mechanism comprises a recovery condensation component and a crude ammonia storage component.
9. The apparatus for flash evaporation of ultra-pure ammonia of electronic grade according to claim 7, wherein: the gas phase recovery mechanism comprises a gas phase absorption assembly, an ammonia water storage assembly and a tail gas separation treatment assembly; the tail gas separation processing assembly is communicated with the ammonia cooler assembly, and the output end of the ammonia cooler assembly is communicated to the first-stage flash tank.
10. The apparatus for flash evaporation of ultra-pure ammonia of electronic grade according to claim 5, wherein: the flash evaporation assembly comprises a pressure reducing valve assembly and a flash evaporation tank which are communicated in sequence.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114506859A (en) * | 2022-02-18 | 2022-05-17 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation method of high-purity deuterated ammonia |
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2021
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114506859A (en) * | 2022-02-18 | 2022-05-17 | 中船(邯郸)派瑞特种气体股份有限公司 | Preparation method of high-purity deuterated ammonia |
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