CN221309949U - Purification system of electronic grade sulfur hexafluoride - Google Patents

Purification system of electronic grade sulfur hexafluoride Download PDF

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CN221309949U
CN221309949U CN202323320413.1U CN202323320413U CN221309949U CN 221309949 U CN221309949 U CN 221309949U CN 202323320413 U CN202323320413 U CN 202323320413U CN 221309949 U CN221309949 U CN 221309949U
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sulfur hexafluoride
gas
purification system
electronic grade
membrane
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陈朝琦
王勇
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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 a purification system of electronic grade sulfur hexafluoride, which comprises pretreatment equipment; the filtering device is connected with the pretreatment equipment and is used for receiving the materials from the dryer and filtering and removing granular impurities; the compression device is connected with the gas filtering device and used for receiving and compressing materials from the gas filtering device; the membrane separation device is connected with the compression device and is used for receiving the materials from the compression device and performing membrane separation to remove gas impurities; and the post-treatment equipment is connected with the membrane separation device and is used for receiving materials from the membrane separation device and carrying out adsorption, condensation and pyrolysis treatment. The purification system of the utility model combines a filtering device, a membrane separation technology, pretreatment equipment and post-treatment equipment which simultaneously comprise heating, cooling and other devices, and ensures that the purity of sulfur hexafluoride reaches an electronic grade through multistage separation and purification.

Description

Purification system of electronic grade sulfur hexafluoride
Technical Field
The utility model relates to the technical field of gas purification, in particular to a purification system of electronic grade sulfur hexafluoride.
Background
Sulfur hexafluoride is a colorless, odorless, nontoxic and incombustible stable gas, and has octahedral molecular structure, small bonding distance and high bonding energy, so that the sulfur hexafluoride has high stability, and at temperature not higher than 180 deg.c, it has compatibility with electric structural material and similar nitrogen. Are often used for new generation ultra-high voltage dielectric materials and gas insulators for electronics and radar waveguides. Electronic grade sulfur hexafluoride (purity over 99.999%) is one type of electronic gas. High purity sulfur hexafluoride is an ideal electron etchant and is used in a large number of microelectronics technologies. The current domestic sulfur hexafluoride products execute GB/T12022-2006 standard, and only can meet industrial requirements (switches, circuit breakers and the like), but cannot purify sulfur hexafluoride into electronic grade (> 99.999%) gas.
CN102330109a provides a method for producing sulfur hexafluoride by electrolytic synthesis, sulfur is directly added into a fluorine-producing electrolytic cell to prepare KHF2-HF-S mixture, and when this mixture is melted by electrolysis, the fluorine produced immediately reacts with sulfur in the electrolyte to produce sulfur hexafluoride. The crude sulfur hexafluoride gas, though purified, has a small amount of water, N 2、O2、CF4、CO2, CO and other impurities, and must be further refined to reach the electronic grade.
CN101955164a discloses a method for producing and purifying sulfur hexafluoride, which is mainly composed of a reactor, a pyrolysis tower, a washing tower, an adsorption drying tower, a booster pump, a primary rectifying tower, a secondary rectifying tower, a vaporizer, a high-temperature heat processor, a bypass pipeline and a recovery pipeline which are connected with a fluorine gas feeding pipe and a molten sulfur feeding pipe in sequence through connecting pipelines, and is assembled integrally. The purification method has high energy consumption, and sulfur hexafluoride products with the content of at least 99.8 percent meeting the purity requirement are obtained from the top of the secondary rectifying tower and do not reach the electronic grade level.
Disclosure of utility model
The utility model aims to provide an electronic grade sulfur hexafluoride purification system which has no chemical change, better selectivity, stronger adaptability and lower energy consumption.
In order to solve the technical problems, the utility model adopts the following technical scheme:
A purification system of electronic grade sulfur hexafluoride comprises pretreatment equipment, a gas filtering device, a compression device, a membrane separation device and post-treatment equipment. The pretreatment equipment comprises a heater, a condenser, a filter and a dryer which are sequentially connected along the gas travelling direction, and is used for receiving the crude sulfur hexafluoride gas and providing the treatment effects of heating, cooling, filtering, drying and the like for the crude sulfur hexafluoride gas; the gas filtering device is connected with the dryer and is used for receiving materials from the dryer and filtering to remove granular impurities; the compression device is connected with the gas filtering device and is used for receiving materials from the gas filtering device and compressing the materials into high-pressure gas; the membrane separation device is connected with the compression device and is used for receiving the materials from the compression device and performing membrane separation to remove gas impurities; the post-treatment equipment is connected with the membrane separation device and comprises an adsorption device, a cooling device and a pyrolysis device which are sequentially connected, and the post-treatment equipment is used for receiving materials from the membrane separation device and carrying out adsorption, condensation and pyrolysis treatment to obtain purified sulfur hexafluoride gas.
Preferably, the condensing tower is filled with silica gel for absorbing water, and the silica gel can be regenerated and used by heating to remove the water.
Preferably, the pretreatment device further comprises a gas moisture meter connected with the dryer, the gas moisture meter is connected with the gas filtering device through an output pipeline, and the gas moisture meter is also connected with the inlet of the heater through a loop pipeline.
Further preferably, the pretreatment apparatus further comprises a three-way valve connected to the gas moisture meter, and the three-way valve is further connected to the inlet of the heater through the loop pipe and to the gas filtering device through the output pipe.
Preferably, the gas filtration device is one or a combination of a plurality of mechanical filters, activated carbon filters, particle filters, microporous filters.
Preferably, the gas filtration device has a filtration pore size of 0.2 to 0.5 microns.
Preferably, the filter material inside the gas filter device is polypropylene filter material or polytetrafluoroethylene filter material.
Further preferably, the gas filtering device is a multi-stage filtering device formed by sequentially connecting a plurality of filters in series, and the filtering pore diameter of the multi-stage filtering device is gradually reduced according to the gas travelling direction.
Preferably, the membrane separation device is one or more membrane separators, the membrane separators are hollow fiber membrane separators, and the hollow fiber membranes in the hollow fiber membrane separators are polymer membranes, silicon-based inorganic membranes or nano-membranes.
Further preferably, the hollow fiber membrane is a polyamide membrane, a polytetrafluoroethylene membrane, or a sulfoxide membrane.
Further preferably, the membrane separation device is a multistage membrane separation device formed by sequentially connecting a plurality of membrane separators in series.
Preferably, the adsorption device comprises one or more adsorption columns, and the adsorbent in the adsorption columns is activated carbon and/or molecular sieve.
Preferably, the cooling device is a cooler capable of cooling the material from the adsorption device below the dew point.
Preferably, the pyrolysis device is a heating device capable of heating the material from the cooling device to separate sulfur hexafluoride gas.
Preferably, valves are respectively arranged on a pipeline for connecting the dryer and the gas filtering device, a pipeline for connecting the gas filtering device and the compression device and a pipeline for connecting the membrane separation device and the adsorption device.
Preferably, the purification system of the electronic grade sulfur hexafluoride further comprises sulfur hexafluoride generating equipment or a sulfur hexafluoride crude product storage tank, and the sulfur hexafluoride generating equipment or the sulfur hexafluoride crude product storage tank is connected with the heater through a pipeline provided with a valve.
Preferably, the purification system of the electronic grade sulfur hexafluoride further comprises a steam trap and a gas storage tank, the pyrolysis device is connected with the steam trap through a pipeline provided with a valve, and the steam trap is connected with the gas storage tank through a pipeline provided with a valve. The steam trap may further remove moisture, including small amounts of water vapor that may be mixed in during collection, to avoid impact on the clean gas.
Due to the application of the technical scheme, compared with the prior art, the utility model has the following advantages:
The purification system of the utility model combines a filtering device, a membrane separation technology, pretreatment equipment and post-treatment equipment which simultaneously comprise heating, cooling and other devices, and ensures that the purity of sulfur hexafluoride reaches an electronic grade through multistage separation and purification.
Drawings
FIG. 1 is a schematic diagram of the overall structure of a purification system for electronic grade sulfur hexafluoride in an embodiment;
Fig. 2 is a schematic structural diagram of a pretreatment device of a purification system of electronic grade sulfur hexafluoride in an embodiment;
FIG. 3 is a schematic diagram of a gas filtering device of a purification system of electronic grade sulfur hexafluoride in an embodiment;
Fig. 4 is a schematic structural diagram of a post-treatment device of a purification system of electronic grade sulfur hexafluoride according to an embodiment;
FIG. 5 is a schematic flow chart of a method for purifying sulfur hexafluoride using the purification system of the electronic grade sulfur hexafluoride of this embodiment;
In the figure: 1. a pretreatment device; 11. a heater; 12. a condenser; 13. a filter; 14. a dryer; 15. a gas moisture meter; 16. a three-way valve; 17. an output pipe; 18. a loop conduit; 2. a gas filtering device; 21. a first microporous filter; 22. a second microporous filter; 3. a compression device; 4. a membrane separation device; 41. a first membrane separator; 42. a second membrane separator; 5. a post-treatment device; 51. an adsorption device; 511. a first adsorption column; 512. a second adsorption column; 52. a cooling device; 53. a pyrolysis device; 61. a first valve; 62. a second valve; 63. a third valve; 64. and a fourth valve.
Detailed Description
The following description of the embodiments of the present utility model will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The volume content of sulfur hexafluoride in the sulfur hexafluoride crude product treated in the following examples is 95%, wherein the impurities include nitrogen, carbon monoxide, carbon dioxide, water, sulfur fluoride, fluorine sulfur oxide, and the like.
Referring to fig. 1, the purification system of electronic grade sulfur hexafluoride comprises a pretreatment device 1, a gas filtering device 2, a compression device 3, a membrane separation device 4 and a post-treatment device 5.
As shown in fig. 2 in particular, the pretreatment apparatus 1 comprises a heater 11, a condenser 12, a filter 13, a dryer 14, a gas moisture meter 15 and a three-way valve 16 which are connected in this order in the gas traveling direction, and the three-way valve 16 is also connected to an inlet of the heater 11 through a return line 18 and to the gas filtering device 2 through an output line 17. The heater 11 is used for heating the sulfur hexafluoride crude product to a certain temperature, usually between 380 ℃ and 420 ℃, so as to improve vapor pressure and volatility of the sulfur hexafluoride crude product and facilitate removal of part of moisture and impurities. The condenser 12 is used to cool the material from the heater 11 (heated sulfur hexafluoride steam) through the condenser 12 to gradually condense the material into a liquid state, and part of the moisture and other impurities are separated from the sulfur hexafluoride during the process, so that the sulfur hexafluoride is removed. The condenser 12 of this embodiment is internally filled with silica gel for adsorbing water, and the silica gel can be regenerated by heating to remove water. The filter 13 filters the cooled liquid sulfur hexafluoride through a filter screen or other filters to remove tiny particles and impurities. Dryer 14 provides further moisture and some other detrimental components to sulfur hexafluoride by adding a quantity of desiccant, and in other embodiments dryer 14 may provide further moisture and some other detrimental components to sulfur hexafluoride by exposing sulfur hexafluoride to high temperature dry air. The gas moisture meter 15 may be a gas moisture meter 15 conventionally used in the art, and may be used for detecting the moisture content of sulfur hexafluoride gas after heating, condensing, filtering and drying. Through the design of the three-way valve 16 and the loop pipeline 18, the next process can be selected according to the test structure of the gas moisture tester 15, or the gas moisture tester is led back to the heater 11 for pretreatment again, and the next process is carried out until the water content is smaller than a certain value. In this embodiment, the water content is less than 1% as the qualification, and if the water content does not meet the qualification standard, the gas is returned to the heater 11 through the loop pipe 18 for pretreatment again. In this embodiment, filter 13 is selected from the group consisting of carbon filters, and in other embodiments, other filters conventionally used in the art may be selected.
As shown in fig. 3, the gas filtering device 2 in this embodiment is a two-stage filtering device formed by serially connecting a first microporous filter 21 and a second microporous filter 22 with a pore size of 0.2-0.5 μm, and the pore size of the first microporous filter 21 is larger than that of the second microporous filter 22. In other embodiments, one or more other existing filters may be used, such as mechanical filters, activated carbon filters, particulate filters, etc., as may be practically desired. When the multi-stage filter device formed by sequentially connecting a plurality of filters in series is adopted, the filter aperture of the multi-stage filter device is gradually reduced according to the gas advancing direction, so that the effects of gradually removing impurities with different sizes and avoiding filter blockage can be achieved. The gas filtering device 2 has therein a filtering material capable of removing particulate impurities mixed in sulfur hexafluoride gas, such as polypropylene filtering material or polytetrafluoroethylene filtering material.
The compression device 3 in this embodiment is a compressor conventionally used in the art, and is disposed between the second microporous filter 22 and the membrane separation device 4, and is configured to receive the material from the gas filtration device 2 and compress the material into a high-pressure gas that meets the requirements of the membrane separation device 4.
The membrane separation device 4 in this embodiment is a two-stage membrane separation device formed by connecting a first membrane separator 41 and a second membrane separator 42 in series. In other embodiments, one or more other existing membrane separators may be used as is practical. The membrane separator in the embodiment is a hollow fiber membrane separator, which contains a hollow fiber membrane component and has the characteristics of high packing density of polymer membrane fibers, strong transmembrane pressure difference resistance, high membrane gas permeability and the like. The hollow fiber membranes in the hollow fiber membrane separator may be polymer membranes, silica-based inorganic membranes, or nanomembranes conventionally used in the art.
As shown in fig. 4, the post-treatment device 5 includes an adsorption device 51, a cooling device 52 and a pyrolysis device 53, which are sequentially connected, and are configured to receive the material from the membrane separation device 4 and perform adsorption, condensation and pyrolysis treatment to obtain purified sulfur hexafluoride gas. The adsorption device 51 in this embodiment is composed of a first adsorption column 511 and a second adsorption column 512 connected in series, the first adsorption column 511 being connected to the second membrane separator 42, and the second adsorption column 512 being connected to the cooling device 52. The first adsorption column 511 and the second adsorption column 512 are respectively filled with different adsorbents for adsorbing part of impurities and moisture in sulfur hexafluoride gas, and the adsorbents selected may be adsorbents conventionally used in the art, such as activated carbon and molecular sieves. The cooling device 52 is a cooler conventionally used in the art to cool sulfur hexafluoride gas from the second adsorption column 512 below its dew point and to separate a portion of the moisture and impurities. The pyrolysis device 53 may be a heater capable of heating sulfur hexafluoride gas from the cooler to a temperature to further separate sulfur hexafluoride gas from impurities and moisture by thermal decomposition.
In this embodiment, the heater 11 in the pretreatment apparatus 1 is connected to the sulfur hexafluoride crude storage tank through a pipe provided with a first valve 61, a second valve 62 is provided on a pipe for connecting the three-way valve 16 and the first microporous filter 21, a third valve 63 is provided on a pipe for connecting the second microporous filter 22 and the compression device 3, and a fourth valve 64 is provided on a pipe for connecting the second membrane separator 42 and the first adsorption column 511.
In this embodiment, the purification system of electronic grade sulfur hexafluoride further includes a steam trap and a gas storage tank, the pyrolysis device 53 is connected to the steam trap through a pipeline with a valve, and the steam trap is connected to the gas storage tank through a pipeline with a valve.
The purification system of the electronic grade sulfur hexafluoride is adopted to purify sulfur hexafluoride, and referring to fig. 5, the method comprises the following steps:
Step S101 is pretreatment of a sulfur hexafluoride gas crude product. The sulfur hexafluoride gas crude product sequentially passes through the heater 11, the condenser 12, the filter 13, the dryer 14 and the gas moisture meter 15, if the water content measured by the gas moisture meter 15 is less than 1%, the step S102 is entered, and if the water content measured by the gas moisture meter 15 is more than or equal to 1%, the crude product is led back to the heater 11 through the loop pipeline 18 for pretreatment again.
Step S102 is to remove particulate impurities in sulfur hexafluoride gas. In this step, sulfur hexafluoride gas in step S101 is sequentially passed through the first microporous filter 21 and the second microporous filter 22 to remove impurities such as fine particles and dust, thereby not only further removing impurities, but also prolonging the service life of the membrane filtration device.
Step S103 is compressing gas. The sulfur hexafluoride gas in the step S102 is compressed to a certain pressure by the compression device 3 to adapt to the subsequent membrane separation.
Step S104 is to separate sulfur hexafluoride by membrane technology. In this step, sulfur hexafluoride gas in step S103 is sequentially passed through the first membrane separator 41 and the second membrane separator 42 to separate and extract high-purity sulfur hexafluoride gas by utilizing the principle of selective permeation, and other gases are discharged (including N 2、CO2、O2, CO, etc.) from other outlets of the membrane separators.
Step S105 is post-processing and collecting canning. In this step, sulfur hexafluoride gas in step S104 sequentially passes through the first adsorption column 511, the second adsorption column 512, the cooling device 52, the pyrolysis device 53, and finally enters the gas storage tank after passing through the steam trap.
After the purification system and the purification method are adopted to purify the sulfur hexafluoride gas crude product, the purity of the sulfur hexafluoride gas can reach an electronic level, the purification system does not relate to a rectifying device, and the whole operation energy consumption is obviously lower.
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. A purification system for electronic grade sulfur hexafluoride, comprising:
the pretreatment equipment comprises a heater, a condenser, a filter and a dryer which are sequentially connected along the gas travelling direction;
The gas filtering device is connected with the dryer and is used for receiving materials from the dryer and filtering to remove granular impurities;
The compression device is connected with the gas filtering device and is used for receiving and compressing materials from the gas filtering device;
the membrane separation device is connected with the compression device and is used for receiving materials from the compression device and performing membrane separation to remove gas impurities;
And the post-treatment equipment is connected with the membrane separation device and comprises an adsorption device, a cooling device and a pyrolysis device which are sequentially connected, and is used for receiving materials from the membrane separation device and carrying out adsorption, condensation and pyrolysis treatment to obtain purified sulfur hexafluoride gas.
2. The purification system of electronic grade sulfur hexafluoride of claim 1 wherein: the pretreatment equipment further comprises a gas moisture tester connected with the dryer, the gas moisture tester is connected with the gas filtering device through an output pipeline, and the gas moisture tester is also connected with the inlet of the heater through a loop pipeline.
3. The purification system of electronic grade sulfur hexafluoride of claim 2 wherein: the pretreatment equipment further comprises a three-way valve connected with the gas moisture tester, wherein the three-way valve is also connected with the inlet of the heater through the loop pipeline and connected with the gas filtering device through the output pipeline.
4. The purification system of electronic grade sulfur hexafluoride of claim 1 wherein: the gas filtering device is one or a combination of a plurality of mechanical filters, active carbon filters, particle filters and microporous filters; the filtering aperture of the gas filtering device is 0.2-0.5 micron; and/or the filter material inside the gas filter device is polypropylene filter material or polytetrafluoroethylene filter material.
5. The purification system of electronic grade sulfur hexafluoride of claim 1 or 4 wherein: the gas filtering device is a multi-stage filtering device formed by sequentially connecting a plurality of filters in series, and the filtering aperture of the multi-stage filtering device is gradually reduced according to the gas advancing direction.
6. The purification system of electronic grade sulfur hexafluoride of claim 1 wherein: the membrane separation device is one or more membrane separators, the membrane separators are hollow fiber membrane separators, and hollow fiber membranes in the hollow fiber membrane separators are polymer membranes, silicon-based inorganic membranes or nano-membranes.
7. The purification system of electronic grade sulfur hexafluoride of claim 6 wherein: the hollow fiber membrane is a polyamide membrane, a polytetrafluoroethylene membrane or a sulfoxide membrane;
And/or the membrane separation device is a multistage membrane separation device formed by sequentially connecting a plurality of membrane separators in series.
8. The purification system of electronic grade sulfur hexafluoride of claim 1 wherein: the adsorption device comprises one or more adsorption columns, and the adsorbent in the adsorption columns is activated carbon and/or molecular sieve.
9. The purification system of electronic grade sulfur hexafluoride of claim 1 wherein: the cooling device is a cooler capable of cooling the material from the adsorption device to below a dew point; and/or the pyrolysis device is a heating device capable of heating and separating sulfur hexafluoride gas from the material of the cooling device; and/or valves are respectively arranged on the pipeline for connecting the dryer and the gas filtering device, the pipeline for connecting the gas filtering device and the compression device and the pipeline for connecting the membrane separation device and the adsorption device.
10. The purification system of electronic grade sulfur hexafluoride of claim 1 wherein: the purification system of the electronic grade sulfur hexafluoride further comprises sulfur hexafluoride generating equipment or a sulfur hexafluoride crude product storage tank, wherein the sulfur hexafluoride generating equipment or the sulfur hexafluoride crude product storage tank is connected with the heater through a pipeline provided with a valve; and/or the purification system of the electronic grade sulfur hexafluoride further comprises a steam trap and a gas storage tank, wherein the pyrolysis device is connected with the steam trap through a pipeline provided with a valve, and the steam trap is connected with the gas storage tank through a pipeline provided with a valve.
CN202323320413.1U 2023-12-06 2023-12-06 Purification system of electronic grade sulfur hexafluoride Active CN221309949U (en)

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CN202323320413.1U CN221309949U (en) 2023-12-06 2023-12-06 Purification system of electronic grade sulfur hexafluoride

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CN202323320413.1U CN221309949U (en) 2023-12-06 2023-12-06 Purification system of electronic grade sulfur hexafluoride

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