CN114715862A - Nitrogen trifluoride purification process - Google Patents

Nitrogen trifluoride purification process Download PDF

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Publication number
CN114715862A
CN114715862A CN202210308640.3A CN202210308640A CN114715862A CN 114715862 A CN114715862 A CN 114715862A CN 202210308640 A CN202210308640 A CN 202210308640A CN 114715862 A CN114715862 A CN 114715862A
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China
Prior art keywords
air
nitrogen trifluoride
filter
cold
heat exchanger
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CN202210308640.3A
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Inventor
李磊
宋佳良
李宗政
吴建魁
马亮
王继军
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Kaifeng In New Clean Energy Technology Co ltd
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Kaifeng In New Clean Energy Technology Co ltd
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Priority to CN202210308640.3A priority Critical patent/CN114715862A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00Nitrogen; Compounds thereof
    • C01B21/082Compounds containing nitrogen and non-metals and optionally metals
    • C01B21/083Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms
    • C01B21/0832Binary compounds of nitrogen with halogens
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25BREFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B9/00Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point
    • F25B9/002Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the refrigerant
    • F25B9/004Compression machines, plants or systems, in which the refrigerant is air or other gas of low boiling point characterised by the refrigerant the refrigerant being air
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02CCAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00Capture or disposal of greenhouse gases
    • Y02C20/30Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

The invention relates to the technical field of nitrogen trifluoride purification equipment, in particular to a nitrogen trifluoride purification process for reducing energy consumption.

Description

Nitrogen trifluoride purification process
Technical Field
The invention relates to the technical field of nitrogen trifluoride purification equipment, in particular to a process for purifying nitrogen trifluoride by using cold air instead of liquid nitrogen.
Background
Nitrogen trifluoride (nitrogen trifluoride) has the formula NF3Is colorless at normal temperatureOdorless gas with stable properties, which is a strong oxidant. Nitrogen trifluoride is used as an excellent plasma etching gas in the microelectronics industry, is cracked into active fluorine ions during ion etching, and the fluorine ions have excellent etching rate and selectivity (for silicon oxide and silicon) to silicon and tungsten compounds, and high-purity nitrogen trifluoride does not leave any residue on the surface of an etching object during etching, is a very good cleaning agent, and is widely applied to chip manufacturing and high-energy lasers. NF3The synthesis method of (1) comprises 2 chemical methods and electrolytic methods, but crude NF3 gas prepared by either chemical method or electrolytic method contains N2、O2、F2、HF、NO2、NHF2、N2F2And the like. According to NF3The impurities can be classified into class 2, having a boiling point lower than NF, unlike the boiling points of the components of the impurities3The component (A) is called a highly volatile impurity, also called a light component such as N2、O2、F2(ii) a Boiling point higher than NF3The component (B) is called low volatility impurity, also called heavy component, such as HF, NO2、NHF2、N2F2. According to NF3The main purification methods include cold trap method, adsorption method and modified adsorption method (see the modern chemical industry published in 2004, 4 months, 24, 4 th stage, 51-53)
At present, nitrogen trifluoride is purified mainly by a cold trap method, and specifically, a crude product of nitrogen trifluoride is introduced into a cold trap soaked in liquid nitrogen, high-boiling-point products such as nitrogen trifluoride are liquefied in the cold trap at the temperature of-150 ℃, low-boiling-point impurities are emptied from an outlet, the cold trap is naturally heated, and nitrogen trifluoride is recovered at the temperature of about-100 ℃ to realize the purification of nitrogen trifluoride gas.
In order to meet the requirement of a cold trap method for purifying nitrogen trifluoride on liquid nitrogen, a low-temperature liquid nitrogen storage tank and a liquid filling system are required to be equipped. The dangerous angle of liquid nitrogen transportation, the transportation carbon discharges highly, and cryogenic liquids are stored, vaporization factor of safety is lower, the cold-trap heat transfer is gone on in liquid nitrogen gasification period, and alternating stress strikes great to heat transfer system, and is strict to the cold-trap material requirement, and the processing degree of difficulty is great, and heat exchanger life is shorter, and factor of safety is lower.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a nitrogen trifluoride purification process for cooling by replacing liquid nitrogen with low-temperature cold air.
The invention is realized by the following technical scheme: a process for purifying nitrogen trifluoride comprising the steps of:
step 1: filtering, namely conveying the raw material air to a filtering device for filtering to remove granular impurities such as dust in the air;
and 2, step: preparing cold air, namely pressurizing the clean air prepared in the step 1 through a compression end of a turbo-charging expander, cooling the air through heat exchange equipment, and conveying the cooled air to an expansion end of the turbo-charging expander for adiabatic expansion to obtain the cold air;
and step 3: purification, namely introducing the cold air prepared in the step 2 into a cold trap, and conveying a crude product of nitrogen trifluoride into the cold trap, wherein the cold trap comprises an air inlet end and an air outlet end;
and 4, step 4: and collecting waste gas, absorbing heat by cold air in the purification process, and discharging the cold air with the increased temperature after absorbing heat from the air outlet end of the cold trap and then recovering.
Further, the filtering device in the step 1 comprises a first filter and a second filter, wherein the first filter adopts a self-cleaning filter, and the second filter adopts a molecular sieve adsorber.
Further, a supercharger and an air conditioner are arranged between the first filter and the second filter.
Furthermore, the number of the molecular sieve adsorbers is two, the two molecular sieve adsorbers are connected with the output end of the cold trap through a conveying pipeline, and a heater is arranged on the conveying pipeline.
Further, the heat exchange equipment in the step 2 comprises a first heat exchanger and a second heat exchanger, and the second heat exchanger adopts a plate heat exchanger.
Further, the air outlet end of the cold trap is connected with a second heat exchanger.
The invention has the beneficial effects that: the use of liquid nitrogen in the cold trap method when providing cold volume with this to replace nitrogen trifluoride purification in the cold trap after refrigerating to the air, guarantee the purification operation temperature in the cold trap through using air conditioning, reduce the investment of the storage device of liquid nitrogen, reduce the danger of liquid nitrogen transportation, reduce the transportation and reduce carbon and discharge, the liquid nitrogen is increased in the container internal pressure when meetting the high fever, leads to equipment fracture and explosion easily, and the continuity and the security that utilize air conditioning to replace production are higher.
Drawings
FIG. 1 is a flow diagram of a prior art nitrogen trifluoride cold trap purification process;
FIG. 2 is a block flow diagram of a nitrogen trifluoride purification process of the present invention;
FIG. 3 is a schematic diagram of the apparatus for purifying nitrogen trifluoride according to the present invention.
Wherein: 1-self-cleaning filters; 2-a supercharger; 3-an air conditioner; 4-a molecular sieve adsorber; 5-the compression end of the turbo-charged expansion machine; 6, a first heat exchanger; 7-heat exchanger II; 8-the expansion end of the turbocharger; 9-cold trap; 10-a heater.
Detailed Description
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
As shown in fig. 2-3, a nitrogen trifluoride purification process comprises the steps of:
step 1: filtering, conveying raw air to a filtering device for filtering, removing impurities in the air, wherein the filtering device comprises a first filter and a second filter, the first filter adopts a self-cleaning filter 1 for filtering dust and other granular impurities in the air, the second filter adopts a molecular sieve adsorber 4 for further filtering carbon dioxide, hydrocarbon and moisture in the air to ensure the cleanliness of the air, a supercharger 2 for providing power for conveying the air and an air conditioner 3 for cooling the pressurized high-temperature gas are arranged between the first filter and the second filter, the filtered air is pressurized by the supercharger 2 and then conveyed to the air conditioner 3 for cooling, the pressurized gas is cooled to room temperature, and the air conditioner 3 is used for primarily cooling the high-temperature high-pressure gas treated by the supercharger 2, in the cooling process, partial water vapor in the air is condensed and then discharged, so that the cooling effect can be achieved, the moisture in the air can be reduced, the air subjected to primary cooling is conveyed into the molecular sieve adsorbers 4 for secondary filtration after being processed by the air conditioner 3, the moisture, carbon dioxide and a part of hydrocarbon in the air are removed, the number of the molecular sieve adsorbers 4 is two, the two molecular sieve adsorbers 4 are both connected with the output end of the cold trap 9 through conveying pipelines, the two molecular sieve adsorbers 4 are alternately used, when one molecular sieve adsorber 4 is used for adsorption, the other molecular sieve adsorber 4 is heated by the recovered gas and then is subjected to backwashing, and the alternate use of the two molecular sieve adsorbers 4 can ensure that the filtering effect of the molecular sieve is kept optimal;
and 2, step: preparing cold air, namely pressurizing the clean air prepared in the step 1 through a compression end 5 of a turbo-charging expansion machine, increasing the temperature after pressurization, cooling the pressurized gas through heat exchange equipment, conveying the cooled air to an expansion end of a turbo supercharger 2, performing adiabatic expansion to obtain cold air, reducing the temperature of the gas to-178 ℃ by using the turbo supercharger, and using the cold air as cold source gas for purifying nitrogen trifluoride, wherein the heat exchange equipment comprises a first heat exchanger 6 and a second heat exchanger 7, and the second heat exchanger 7 adopts a plate heat exchanger;
and step 3: purifying, namely introducing cold air prepared in the step 2 into a cold trap 9 through an air inlet end, conveying a crude product of nitrogen trifluoride into the cold trap 9, wherein the cold trap 9 comprises an air inlet end and an air outlet end, the cold air enters the cold trap 9 through the air inlet end to cool and purify the crude product of nitrogen trifluoride, the cold air replaces liquid nitrogen to provide cold energy for purifying the crude product of nitrogen trifluoride in the purification process, the cold air is introduced into the cold trap through the air inlet end to cool the temperature in the cold trap during operation, the crude product of nitrogen trifluoride is conveyed into the cold trap through a feed pipeline to be purified when the temperature in the cold trap is reduced to-178 ℃, impurities in the purification operation are removed through a impurity discharge pipeline at the upper part of the cold trap to obtain pure nitrogen trifluoride liquid, the pure nitrogen trifluoride liquid is discharged from a pipeline below the cold trap and then collected, and heat absorption waste gas after the purification operation is discharged from the air outlet end;
and 4, step 4: collecting waste gas, recovering the waste gas after the temperature of the cold gas is raised after the cold gas absorbs heat in the purification process and then the waste gas is discharged from the gas outlet end of the cold trap 9, connecting the gas outlet end of the cold trap 9 with the second heat exchanger 7, wherein the temperature of the recovered waste gas is-30 ℃, and the waste gas is used as a refrigerant of the second heat exchanger 7 when passing through the second heat exchanger 7, further absorbing heat when passing through the second heat exchanger to provide partial cold energy for the heat exchange operation of the second heat exchanger, increasing the temperature of the waste gas to 30-40 ℃, the temperature of the waste gas is raised so as to reduce the energy consumed by the heater, the waste gas passing through the second heat exchanger 7 is conveyed to the heater 10 for heating after the temperature is raised through a conveying pipeline, the heated high-temperature gas is used for carrying out back flushing operation on the molecular sieve adsorber 4 which is not subjected to filtering operation, the energy consumption can be saved by utilizing the recovered gas, meanwhile, the recovered gas is purer, and the adsorption capacity of the molecular sieve adsorber can be improved after high-temperature washing.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (6)

1. A purification process of nitrogen trifluoride is characterized in that: the method comprises the following steps:
step 1: filtering, namely conveying the raw material air to filtering equipment for filtering to remove impurities in the air;
step 2: preparing cold air, namely pressurizing the clean air prepared in the step 1 through a compression end of a turbo-charging expansion machine, cooling the air through heat exchange equipment, and conveying the cooled air to an expansion end of a turbo-charger for adiabatic expansion to obtain cold air;
and step 3: and (3) purification, namely introducing the cold gas prepared in the step (2) into a cold trap, and conveying the crude product of the nitrogen trifluoride into the cold trap, wherein the cold trap comprises a gas inlet end and a gas outlet end.
2. The process of purifying nitrogen trifluoride according to claim 1, characterized in that: the filtering device in the step 1 comprises a first filter and a second filter, wherein the first filter adopts a self-cleaning filter, and the second filter adopts a molecular sieve adsorber.
3. The process of purifying nitrogen trifluoride according to claim 2, characterized in that: and a supercharger and an air conditioner are arranged between the first filter and the second filter.
4. The process of purifying nitrogen trifluoride according to claim 2, characterized in that: the number of the molecular sieve absorbers is two, the two molecular sieve absorbers are connected with the output end of the cold trap through a conveying pipeline, and a heater is arranged on the conveying pipeline.
5. The process of purifying nitrogen trifluoride according to claim 1, characterized in that: the heat exchange equipment in the step 2 comprises a first heat exchanger and a second heat exchanger, wherein the second heat exchanger adopts a plate heat exchanger.
6. The process of purifying nitrogen trifluoride according to claim 5, characterized in that: and the air outlet end of the cold trap is connected with the second heat exchanger.
CN202210308640.3A 2022-03-28 2022-03-28 Nitrogen trifluoride purification process Pending CN114715862A (en)

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Application Number Priority Date Filing Date Title
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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1450202A (en) * 2003-04-30 2003-10-22 中国船舶重工集团公司第七一八研究所 Technological method and equipment for preparing nitrogen trifluoride gas
JP2005142377A (en) * 2003-11-07 2005-06-02 Mitsubishi Heavy Ind Ltd Recycle system for cleaning gas
CN104061757A (en) * 2014-07-07 2014-09-24 开封空分集团有限公司 Liquid oxygen and liquid nitrogen preparation device and method
CN204006965U (en) * 2014-07-07 2014-12-10 开封空分集团有限公司 A kind of liquid oxygen and liquid nitrogen device for making
CN104296500A (en) * 2014-10-14 2015-01-21 开封空分集团有限公司 Device and method for cryogenic separation and purification of nitrogen and liquid ammonia
CN108061428A (en) * 2018-01-12 2018-05-22 杭州特盈能源技术发展有限公司 A kind of purity nitrogen device for making and technique
CN111039267A (en) * 2019-12-29 2020-04-21 中船重工(邯郸)派瑞特种气体有限公司 Device and method for pre-purifying electrolytically prepared nitrogen trifluoride crude product
CN111170279A (en) * 2019-05-20 2020-05-19 上海海尔医疗科技有限公司 Novel oxygenerator
CN113893663A (en) * 2021-11-15 2022-01-07 中船重工(邯郸)派瑞特种气体有限公司 Nitrogen trifluoride production pollution discharge equipment and technological method

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1450202A (en) * 2003-04-30 2003-10-22 中国船舶重工集团公司第七一八研究所 Technological method and equipment for preparing nitrogen trifluoride gas
JP2005142377A (en) * 2003-11-07 2005-06-02 Mitsubishi Heavy Ind Ltd Recycle system for cleaning gas
CN104061757A (en) * 2014-07-07 2014-09-24 开封空分集团有限公司 Liquid oxygen and liquid nitrogen preparation device and method
CN204006965U (en) * 2014-07-07 2014-12-10 开封空分集团有限公司 A kind of liquid oxygen and liquid nitrogen device for making
CN104296500A (en) * 2014-10-14 2015-01-21 开封空分集团有限公司 Device and method for cryogenic separation and purification of nitrogen and liquid ammonia
CN108061428A (en) * 2018-01-12 2018-05-22 杭州特盈能源技术发展有限公司 A kind of purity nitrogen device for making and technique
CN111170279A (en) * 2019-05-20 2020-05-19 上海海尔医疗科技有限公司 Novel oxygenerator
CN111039267A (en) * 2019-12-29 2020-04-21 中船重工(邯郸)派瑞特种气体有限公司 Device and method for pre-purifying electrolytically prepared nitrogen trifluoride crude product
CN113893663A (en) * 2021-11-15 2022-01-07 中船重工(邯郸)派瑞特种气体有限公司 Nitrogen trifluoride production pollution discharge equipment and technological method

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