CN221191569U - Electronic grade nitrogen trifluoride purification system - Google Patents

Electronic grade nitrogen trifluoride purification system Download PDF

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Publication number
CN221191569U
CN221191569U CN202323087089.3U CN202323087089U CN221191569U CN 221191569 U CN221191569 U CN 221191569U CN 202323087089 U CN202323087089 U CN 202323087089U CN 221191569 U CN221191569 U CN 221191569U
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nitrogen trifluoride
electronic grade
liquid
separator
pipeline
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CN202323087089.3U
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陈朝琦
陈宏权
曾律宪
陈佳佳
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Nantong Zhanding Material Technology Co ltd
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Nantong Zhanding Material Technology Co ltd
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Abstract

The utility model relates to an electronic grade nitrogen trifluoride purifying system, which comprises: cooling the reactor for receiving crude nitrogen trifluoride gas; a liquid nitrogen refrigeration device having a liquid nitrogen tank for supplying liquid nitrogen to the cooling reactor and an evaporator; the separator is connected with the cooling reactor, receives materials in the cooling reactor, and performs solid-liquid separation on the materials; the separator is also connected with the evaporator, and the evaporator is used for receiving the liquid material after solid-liquid separation and evaporating and separating to obtain nitrogen trifluoride gas; and the purification tower is connected with the evaporator and is used for purifying the nitrogen trifluoride gas to obtain electronic grade nitrogen trifluoride. According to the utility model, impurities in the crude nitrogen trifluoride gas are solidified and liquefied by a liquid nitrogen refrigeration technology, then the impurities are removed by solid-liquid separation, then the liquid nitrogen trifluoride gas is separated from liquid nitrogen, and then the nitrogen trifluoride gas is purified, so that the impurities in the nitrogen trifluoride gas are greatly reduced, and the operation is simple and convenient.

Description

Electronic grade nitrogen trifluoride purification system
Technical Field
The utility model relates to the technical field of gas purification, in particular to an electronic grade nitrogen trifluoride purification system.
Background
Nitrogen trifluoride (NF 3) is an important high-purity chemical that is widely used in the semiconductor industry for cleaning semiconductor devices. In the semiconductor device manufacturing process, NF 3 with high purity is used as an oxidizing agent of gallium oxide (Ga 2O3), and fluorine ions form highly volatile fluorides with the metal surface in the reaction, thereby facilitating the cleaning and maintenance of the semiconductor device. In order to meet the requirements of semiconductor manufacturing for high purity NF 3, efficient purification of industrially produced NF 3 is required. Currently, some purification techniques have been applied to practical production, such as methods of adsorbent adsorption, molecular sieve separation, and membrane separation.
The following patent publications describe the production and purification of NF 3:
US4,091,081 discloses a process for the production of NF 3 by direct fluorination of ammonium bifluoride at temperatures above 260°f and below 400°f. The ratio HF/NH 3 is kept between 2 and 2.5. Purification was achieved by passing the reaction product through a demister pad and then through a KOH aqueous scrubber. The remaining HF and unreacted F 2 are removed in a scrubber. After washing, the temperature of the stream is reduced to form condensed water, and the stream is further purified by a molecular sieve dryer.
US4,156,598 describes a process for the production of NF 3 by direct fluorination of ammonium bifluoride. Purification of the gaseous reactant stream comprises passing the gaseous reactant stream through a demister pad to remove entrained ammonium fluoride or ammonium bifluoride and then through a bath of salts that form HF and F 2, for example, a bath of aqueous KOH. Or sodium fluoride is used instead of KOH, but F 2 cannot be removed by this method. To extend the life of the adsorber column, N 2F2 was removed to a level below 0.03 volume percent prior to absorbing N 2 O and water.
However, the purification of the nitrogen trifluoride has the problems of high operation difficulty, complex operation process and the like.
Disclosure of Invention
The utility model aims to provide an electronic grade nitrogen trifluoride purifying system based on a liquid nitrogen refrigeration technology, which can effectively reduce the concentration of impurities in an NF 3 gas phase and improve the purity of NF 3.
In order to solve the technical problems, the utility model adopts the following technical scheme:
An electronic grade nitrogen trifluoride purification system comprising:
cooling the reactor for receiving crude nitrogen trifluoride gas;
The liquid nitrogen refrigerating device is provided with a liquid nitrogen tank and an evaporator, and the liquid nitrogen tank is used for providing liquid nitrogen for the cooling reactor, so that nitrogen trifluoride in the cooling reactor is liquefied and impurities are solidified, and materials containing solid impurities, liquid nitrogen trifluoride and liquid nitrogen are obtained;
The separator is connected with the cooling reactor, receives materials in the cooling reactor, and performs solid-liquid separation on the materials to obtain solid materials containing solid impurities and liquid materials containing liquid nitrogen trifluoride and liquid nitrogen;
The separator is also connected with the evaporator, and the evaporator is used for receiving the liquid material after the solid-liquid separation, evaporating and separating to obtain nitrogen trifluoride gas and nitrogen in sequence;
And the purification tower is connected with the evaporator and is used for receiving the nitrogen trifluoride gas and purifying the nitrogen trifluoride gas to obtain electronic grade nitrogen trifluoride.
In some embodiments, the liquid nitrogen refrigeration device further comprises a compressor connected between the cooling reactor and the liquid nitrogen tank, the compressor is connected with the cooling reactor through a first pipeline, the compressor is connected with the liquid nitrogen tank through a second pipeline, and the compressor is further connected with the evaporator through a third pipeline.
In some embodiments, the liquid nitrogen refrigeration unit further comprises an expansion valve connected between the separator and the evaporator, the expansion valve being connected to the separator by a fourth conduit, the expansion valve being connected to the evaporator by a fifth conduit.
In some embodiments, the separator is connected to the cooling reactor through a sixth pipeline, and valves are respectively disposed on the first pipeline, the second pipeline, the third pipeline, the fourth pipeline, and the sixth pipeline.
In some embodiments, the purification column is a membrane separation column or an adsorption column.
In some embodiments, the adsorption tower is filled with an adsorbent, and the adsorbent is a copper oxide adsorbent.
In some embodiments, the pressure in the cooling reactor is controlled to be between 10 and 50 kilopascals.
In some embodiments, the separator is a filtration separator or a centrifugal separator.
In some embodiments, the separator is provided with a discharge opening for discharging the solid material.
In some embodiments, the electronic grade nitrogen trifluoride purification system further comprises a nitrogen trifluoride formation reactor coupled to the cooling reactor; and/or, the electronic grade nitrogen trifluoride purification system further comprises a gas storage tank, and the gas storage tank is connected with the purification tower.
In some embodiments, the nitrogen trifluoride generating reactor is connected with a first raw material pipe for conveying ammonia gas and a second raw material pipe for conveying fluorine gas.
Due to the application of the technical scheme, compared with the prior art, the utility model has the following advantages:
According to the purification system disclosed by the utility model, impurities in the crude nitrogen trifluoride gas are solidified and liquefied by a liquid nitrogen refrigeration technology, then the impurities are removed by solid-liquid separation, then the liquid nitrogen trifluoride gas is separated from liquid nitrogen, and the nitrogen trifluoride gas is further purified, so that the impurities in the nitrogen trifluoride gas are greatly reduced, and the operation is simple and convenient. Furthermore, the separated nitrogen can be reused, and the cost is low.
Drawings
FIG. 1 is a schematic diagram of an electronic grade nitrogen trifluoride purification system in accordance with a representative embodiment of the present utility model;
FIG. 2 is a flow chart of a method of purifying electronic grade nitrogen trifluoride using the electronic grade nitrogen trifluoride purification system of FIG. 1;
In the figure: 10. a nitrogen trifluoride generating reactor; 20. cooling the reactor; 30. a liquid nitrogen refrigerating device; 301. a liquid nitrogen tank; 302. an evaporator; 303. a compressor; 304. an expansion valve; 40. a separator; 401. a discharge port; 50. a purifying column;
101. A first pipe; 102. a second pipe; 103. a third conduit; 104. a fourth conduit; 105. a fifth pipe; 106. a sixth conduit; 107. a seventh pipe; 108. a first raw material pipe; 109. and a second raw material pipe.
Detailed Description
The embodiment of the disclosure reduces the impurity concentration in the NF 3 gas phase by utilizing a liquid nitrogen refrigeration technology so as to realize the efficient purification of the electronic grade NF 3. The method is mainly characterized in that liquid nitrogen is added into the NF 3 gas phase, so that NF 3 and the liquid nitrogen coexist at low temperature, and the refrigeration effect of the liquid nitrogen is utilized to reduce the impurity concentration in the gas phase, thereby realizing the efficient purification of NF 3. The purification method disclosed by the embodiment of the disclosure has the effects of simply, conveniently, economically and effectively improving the purity of NF 3.
The traditional method for preparing NF 3 gas can be basically divided into a chemical synthesis method and an electrolytic method, and the chemical synthesis method is a more classical method for preparing nitrogen trifluoride (NF 3) gas by reacting ammonia (NH 3) with fluorine (F 2); in addition, an electrolysis method can be used for preparing NF 3 gas by taking NH 4 F-xHF (or adding a small amount of KF) as an electrolyte system.
According to the embodiment of the disclosure, the NF 3 gas is prepared by adopting ammonia (NH 3) and fluorine (F 2) to carry out chemical reaction so as to obtain a NF 3 gas crude product.
The utility model is further described with reference to the drawings and specific examples in the specification:
referring to the electronic grade nitrogen trifluoride purification system shown in fig. 1, comprising:
a nitrogen trifluoride production reactor 10 for reacting a raw material gas ammonia gas with fluorine gas to produce a crude nitrogen trifluoride gas;
a cooling reactor 20 connected to the nitrogen trifluoride generating reactor 10 and for receiving crude nitrogen trifluoride gas;
The liquid nitrogen refrigerating device 30 is provided with a liquid nitrogen tank 301 and an evaporator 302, wherein the liquid nitrogen tank 301 is used for providing liquid nitrogen for the cooling reactor 20 so as to liquefy nitrogen trifluoride and solidify impurities in the cooling reactor 20, and a material containing solid impurities, liquid nitrogen trifluoride and liquid nitrogen is obtained;
A separator 40 connected to the cooling reactor 20, the separator 40 receiving the material in the cooling reactor 20 and performing solid-liquid separation on the material to obtain a solid material containing solid impurities and a liquid material containing liquid nitrogen trifluoride and liquid nitrogen;
The separator 40 is also connected with an evaporator 302, and the evaporator 302 is used for receiving the liquid material after solid-liquid separation and evaporating and separating to sequentially obtain nitrogen trifluoride gas and nitrogen;
And a purification column 50 connected to the evaporator 302, the purification column 50 being configured to receive the nitrogen trifluoride gas and purify the nitrogen trifluoride gas to obtain electronic grade nitrogen trifluoride.
In some embodiments, liquid refrigeration device 30 further comprises a compressor 303 connected between cooling reactor 20 and liquid nitrogen tank 302, and an expansion valve 304 connected between separator 40 and evaporator 302, compressor 303 being connected to cooling reactor 20 by first conduit 101, compressor 303 being connected to liquid nitrogen tank 301 by second conduit 102, compressor 303 being further connected to evaporator 302 by third conduit 103; an expansion valve 304 is connected to the separator 40 via a fourth conduit 104, and the expansion valve 304 is connected to the evaporator 302 via a fifth conduit 105.
The separator 40 is connected to the cooling reactor 20 via a sixth pipe 106, the cooling reactor 20 is connected to the nitrogen trifluoride generating reactor 10 via a seventh pipe 107, and valves are provided in the first pipe 101, the second pipe 102, the third pipe 103, the fourth pipe 104, the sixth pipe 106, and the seventh pipe 107, respectively. A first raw material pipe 108 for transporting ammonia gas and a second raw material pipe 109 for transporting fluorine gas are connected to the nitrogen trifluoride production reactor 10.
Separator 40 may be a filter separator or a centrifugal separator. The separator 40 is provided with a discharge opening 401 for discharging solid material.
In some embodiments, the electronic grade nitrogen trifluoride purification system further comprises a gas storage tank coupled to purification column 50.
The purification column 50 may be an adsorption column or a membrane separation column, and uses a technique such as adsorbent or membrane separation to separate and remove impurities in the gas phase. For example, NF 3 may be passed into an adsorption column, and impurities therein may be removed by an adsorbent filled in the adsorption column. The adsorbent may be a copper oxide adsorbent.
The purification of nitrogen trifluoride is carried out by using the above-mentioned electronic grade nitrogen trifluoride purification system, see fig. 2, and the method comprises the steps of:
Step S1, a reaction gas generation step:
In a nitrogen trifluoride production reactor 10 for producing nitrogen trifluoride gas, a predetermined amount of ammonia gas (NH 3) and fluorine gas (F 2) are mixed in a desired molar ratio and introduced into the nitrogen trifluoride production reactor 10, and reacted in the nitrogen trifluoride production reactor 10 to produce a crude nitrogen trifluoride gas. The temperature and pressure within nitrogen trifluoride formation reactor 10 are maintained at suitable reaction conditions.
Step S2, cooling and removing impurities:
Crude nitrogen trifluoride gas generated in the nitrogen trifluoride generating reactor 10 is led into the cooling reactor 20, and liquid nitrogen in the liquid nitrogen tank 301 is led into the cooling reactor 20 through the compressor 303, so that the crude nitrogen trifluoride gas is mixed with the liquid nitrogen, and impurities in the nitrogen trifluoride gas are formed into liquid state and mixed to solidify, thus obtaining a material containing solid impurities, liquid nitrogen trifluoride and liquid nitrogen; wherein the pressure in the cooling reactor 20 is controlled to be 10 to 50 kilopascals.
Then, introducing the material containing the solid impurities, the liquid nitrogen trifluoride and the liquid nitrogen into a separator 40 for solid-liquid separation to obtain the solid material containing the solid impurities and the liquid material containing the liquid nitrogen trifluoride and the liquid nitrogen; the solid material exits the separator 40.
Step S3, a purification step:
The liquid material containing liquid nitrogen trifluoride and liquid nitrogen is introduced into the evaporator 302, and the two gases are separated under the preset temperature condition by utilizing the difference of the vaporization temperature of the liquid nitrogen trifluoride and the liquid nitrogen trifluoride. The separated nitrogen gas is used as liquid nitrogen to enter the liquid nitrogen tank 301 or the cooling reactor 20 through the compressor 303; the nitrogen trifluoride gas is introduced into the purification column 50, and impurities in the gas phase are separated and removed using a technique such as an adsorbent or membrane separation.
In this step, the liquid material is passed through expansion valve 304 prior to entering evaporator 302, so that the nitrogen trifluoride can be more easily discharged from evaporator 302.
The electronic grade nitrogen trifluoride purifying system is simple in equipment, simple and convenient to operate, capable of recycling liquid nitrogen and low in cost.
The above embodiments are only for illustrating the technical concept and features of the present utility model, and are intended to enable those skilled in the art to understand the present utility model and to implement the same, but are not intended to limit the scope of the present utility model, and all equivalent changes or modifications made according to the spirit of the present utility model should be included in the scope of the present utility model.

Claims (10)

1. An electronic grade nitrogen trifluoride purification system comprising:
cooling the reactor for receiving crude nitrogen trifluoride gas;
A liquid nitrogen refrigeration device having a liquid nitrogen tank for supplying liquid nitrogen to the cooling reactor and an evaporator;
the separator is connected with the cooling reactor, receives materials in the cooling reactor, and performs solid-liquid separation on the materials;
The separator is also connected with the evaporator, and the evaporator is used for receiving the liquid material after the solid-liquid separation and evaporating and separating to obtain nitrogen trifluoride gas;
and the purification tower is connected with the evaporator and is used for purifying the nitrogen trifluoride gas to obtain electronic grade nitrogen trifluoride.
2. The electronic grade nitrogen trifluoride purification system as recited in claim 1, wherein: the liquid nitrogen refrigerating device further comprises a compressor connected between the cooling reactor and the liquid nitrogen tank, the compressor is connected with the cooling reactor through a first pipeline, the compressor is connected with the liquid nitrogen tank through a second pipeline, and the compressor is further connected with the evaporator through a third pipeline.
3. The electronic grade nitrogen trifluoride purification system as recited in claim 2, wherein: the liquid nitrogen refrigerating device further comprises an expansion valve connected between the separator and the evaporator, the expansion valve is connected with the separator through a fourth pipeline, and the expansion valve is connected with the evaporator through a fifth pipeline.
4. An electronic grade nitrogen trifluoride purification system as claimed in claim 3, wherein: the separator is connected with the cooling reactor through a sixth pipeline, and valves are respectively arranged on the first pipeline, the second pipeline, the third pipeline, the fourth pipeline and the sixth pipeline.
5. The electronic grade nitrogen trifluoride purification system as recited in claim 1, wherein: the purification tower is a membrane separation tower or an adsorption tower; and/or the pressure in the cooling reactor is controlled to be 10-50 kilopascals.
6. The electronic grade nitrogen trifluoride purification system as recited in claim 5, wherein: the adsorption tower is filled with an adsorbent, and the adsorbent is a copper oxide adsorbent.
7. The electronic grade nitrogen trifluoride purification system as recited in claim 1, wherein: the separator is a filtering separator or a centrifugal separator.
8. The electronic grade nitrogen trifluoride purification system as recited in claim 1 or 7, wherein: and a discharge port is arranged on the separator.
9. The electronic grade nitrogen trifluoride purification system as claimed in any one of claims 1-7, wherein: the electronic grade nitrogen trifluoride purifying system also comprises a nitrogen trifluoride generating reactor, and the nitrogen trifluoride generating reactor is connected with the cooling reactor; and/or, the electronic grade nitrogen trifluoride purification system further comprises a gas storage tank, and the gas storage tank is connected with the purification tower.
10. The electronic grade nitrogen trifluoride purification system as recited in claim 9, wherein: the nitrogen trifluoride generating reactor is connected with a first raw material pipe for conveying ammonia gas and a second raw material pipe for conveying fluorine gas.
CN202323087089.3U 2023-11-15 2023-11-15 Electronic grade nitrogen trifluoride purification system Active CN221191569U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202323087089.3U CN221191569U (en) 2023-11-15 2023-11-15 Electronic grade nitrogen trifluoride purification system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202323087089.3U CN221191569U (en) 2023-11-15 2023-11-15 Electronic grade nitrogen trifluoride purification system

Publications (1)

Publication Number Publication Date
CN221191569U true CN221191569U (en) 2024-06-21

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Country Status (1)

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CN (1) CN221191569U (en)

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