CN112978683A - Electronic-grade sulfur hexafluoride adsorption device and application - Google Patents
Electronic-grade sulfur hexafluoride adsorption device and application Download PDFInfo
- Publication number
- CN112978683A CN112978683A CN202110173728.4A CN202110173728A CN112978683A CN 112978683 A CN112978683 A CN 112978683A CN 202110173728 A CN202110173728 A CN 202110173728A CN 112978683 A CN112978683 A CN 112978683A
- Authority
- CN
- China
- Prior art keywords
- pressure adsorption
- adsorption tower
- pressure
- low
- tower
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/45—Compounds containing sulfur and halogen, with or without oxygen
- C01B17/4507—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only
- C01B17/4515—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only containing sulfur and fluorine only
- C01B17/453—Sulfur hexafluoride
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/104—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/106—Silica or silicates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/116—Molecular sieves other than zeolites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/40—Further details for adsorption processes and devices
- B01D2259/406—Further details for adsorption processes and devices using more than four beds
- B01D2259/4068—Further details for adsorption processes and devices using more than four beds using more than ten beds
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
Abstract
The invention provides an electronic grade sulfur hexafluoride adsorption device which comprises a low-pressure adsorption unit and a high-pressure adsorption unit, wherein the low-pressure adsorption unit and the high-pressure adsorption unit are communicated in series; the low-pressure adsorption unit comprises a first low-pressure adsorption tower and a second low-pressure adsorption tower which are sequentially communicated in series, wherein the first low-pressure adsorption tower contains a silica gel adsorbent, and the second low-pressure adsorption tower contains an aluminum gel adsorbent; the high-pressure adsorption unit comprises a first high-pressure adsorption tower, a second high-pressure adsorption tower, a third high-pressure adsorption tower, a fourth high-pressure adsorption tower and a fifth high-pressure adsorption tower, wherein the first high-pressure adsorption tower contains an alumina gel adsorbent, the second high-pressure adsorption tower contains a 5A molecular sieve adsorbent, the third high-pressure adsorption tower contains a 13X molecular sieve adsorbent, the fourth high-pressure adsorption tower contains a CUCL molecular sieve adsorbent, and the fifth high-pressure adsorption tower contains an F-03 molecular sieve adsorbent. The device has high adsorption efficiency.
Description
Technical Field
The invention relates to an electronic grade sulfur hexafluoride adsorption device and application, and belongs to the technical field of sulfur hexafluoride preparation.
Background
The sulfur hexafluoride is an inert gas, is colorless and odorless, is slightly soluble in water, has stable chemical properties, good electrical insulation performance and excellent arc extinguishing performance, and is widely applied to the fields of electric power, electronics, electrical industry, laser, medical treatment, meteorology, physical research and the like. The common preparation method of sulfur hexafluoride products is to prepare the sulfur hexafluoride products by reacting fluorine gas with sulfur, and the most main impurity in the preparation process is low fluoride. Subfluorides are by-products of the reaction of fluorine and sulfur, often referred to as subfluorides of sulfur, and mainly comprise two main classes: one being a fluorosulfur compound, e.g. SF2、SF4、S2F2、S2F10Etc.; di is a fluorooxysulfide compound, e.g. SOF2、SOF4、SO2F2And the like. The purity of sulfur hexafluoride used in the electronic industry is up to 99.9%. Therefore, measures are required to remove the low fluoride in the sulfur hexafluoride raw gas.
The reaction by-product, namely low fluoride, can be partially removed by water washing and alkali washing, but trace low fluoride in the crude gas is difficult to remove by a purification method of water washing and alkali washing alone, and the low fluoride still needs to be further removed by adopting an adsorption mode. In the existing adsorption mode, due to the fact that the types of adsorbents selected for adsorption are various, the adsorbents are often unreasonable in configuration or unreasonable in selective adsorption and purification sequence, so that the adsorption efficiency is low, the adsorption capacity is weak, the effect of removing low fluoride is poor, and the high-purity requirement used in the electronic industry is difficult to meet.
Disclosure of Invention
The invention provides an electronic grade sulfur hexafluoride adsorption device and application thereof, which can effectively solve the problems.
The invention is realized by the following steps:
an electronic grade sulfur hexafluoride adsorption device comprises a low-pressure adsorption unit (1) and a high-pressure adsorption unit (2), wherein the low-pressure adsorption unit (1) and the high-pressure adsorption unit (2) are communicated in series, and a high-pressure compressor (3) is communicated between the low-pressure adsorption unit (1) and the high-pressure adsorption unit (2); the low-pressure adsorption unit (1) comprises a first low-pressure adsorption tower (11) and a second low-pressure adsorption tower (12) which are sequentially communicated in series, wherein the first low-pressure adsorption tower (11) contains a silica gel adsorbent, and the second low-pressure adsorption tower (12) contains an alumina gel adsorbent; the high-pressure adsorption unit (2) comprises a first high-pressure adsorption tower (21), a second high-pressure adsorption tower (22), a third high-pressure adsorption tower (23), a fourth high-pressure adsorption tower (24) and a fifth high-pressure adsorption tower (25), wherein the first high-pressure adsorption tower (21) contains an alumina gel adsorbent, the second high-pressure adsorption tower (22) contains a 5A molecular sieve adsorbent, the third high-pressure adsorption tower (23) contains a 13X molecular sieve adsorbent, the fourth high-pressure adsorption tower (24) contains a CUCL molecular sieve adsorbent, the fifth high-pressure adsorption tower (25) contains a F-03 molecular sieve adsorbent, and the communication sequence of the high-pressure adsorption unit (2) is as follows: the first high-pressure adsorption tower (21), the second high-pressure adsorption tower (22), the third high-pressure adsorption tower (23), the fourth high-pressure adsorption tower (24) and the fifth high-pressure adsorption tower (25) are sequentially communicated in series, or the first high-pressure adsorption tower (21), the second high-pressure adsorption tower (22), the fourth high-pressure adsorption tower (24), the third high-pressure adsorption tower (23) and the fifth high-pressure adsorption tower (25) are sequentially communicated in series; the number of stages of the fourth high-pressure adsorption tower (24) is 3-5, and the number of stages of the fifth high-pressure adsorption tower (25) is 8-10.
As a further improvement, the number of stages of the first low-pressure adsorption tower (11) is 3-5; the number of stages of the second low-pressure adsorption tower (12) is 3-5.
As a further improvement, a first bypass branch pipe (13) is communicated between an inlet and an outlet of any stage of the first low-pressure adsorption tower (11), and a first valve (14) is arranged on the inlet of the first low-pressure adsorption tower (11) of the stage and the first bypass branch pipe (13); and a second bypass branch pipe (15) is communicated between an inlet and an outlet of any stage of the second low-pressure adsorption tower (12), and a second valve (16) is arranged on the inlet of the second low-pressure adsorption tower (12) and the second bypass branch pipe (15).
As a further improvement, the number of stages of the second high-pressure adsorption column (22) is 2 or 3.
As a further improvement, the number of stages of the third high-pressure adsorption column (23) is 2 or 3.
As a further improvement, the number of stages of the fourth high-pressure adsorption column (25) is 9.
As a further improvement, a third bypass branch pipe (26) is communicated between an inlet and an outlet of any stage of the fourth high-pressure adsorption tower (24), and a third valve (27) is arranged on the inlet of the fourth high-pressure adsorption tower (24) and the third bypass branch pipe (26); and a fourth bypass branch pipe (28) is communicated between an inlet and an outlet of any stage of the fifth high-pressure adsorption tower (25), and fourth valves (29) are arranged on the inlet of the fifth high-pressure adsorption tower (25) and the fourth bypass branch pipe (28).
The method for applying the electronic grade sulfur hexafluoride adsorption device comprises the steps of introducing prepared sulfur hexafluoride crude gas into the low-pressure adsorption unit (1) for adsorption, blowing air by the high-pressure compressor (3), then introducing the air into the high-pressure adsorption unit (2) for further adsorption, and finally introducing the air into the rectifying tower (4) for rectification to obtain high-purity sulfur hexafluoride.
As a further improvement, the blast of the blast is alternately low-pressure blast and high-pressure blast, the low-pressure blast is 0.12-0.13MPa blast for 10-15min, and the high-pressure blast is 0.15-0.20MPa blast for 5-10 min.
As a further improvement, the flow speed of the sulfur hexafluoride coarse gas is 0.1-0.5m3/S。
The invention has the beneficial effects that:
the electronic grade sulfur hexafluoride adsorption device is used for adsorption treatment of sulfur hexafluoride, has high adsorption efficiency on low fluoride, and the purity of sulfur hexafluoride in the treated sulfur hexafluoride gas is 99.9995% through detection, thereby meeting the use requirements of the electronic industry.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate 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 structural diagram of an electronic grade sulfur hexafluoride adsorption device provided in an embodiment of the present invention.
Reference numerals:
a low-pressure adsorption unit 1, a first low-pressure adsorption tower 11, a second low-pressure adsorption tower 12, a first bypass branch pipe 13, a first valve 14, a second bypass branch pipe 15, and a second valve 16;
the high-pressure adsorption unit 2, a first high-pressure adsorption tower 21, a second high-pressure adsorption tower 22, a third high-pressure adsorption tower 23, a fourth high-pressure adsorption tower 24, a fifth high-pressure adsorption tower 25, a third bypass branch pipe 26, a third valve 27, a fourth bypass branch pipe 28 and a fourth valve 29;
a high-pressure compressor 3;
a rectifying column 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Example 1
Referring to fig. 1, the embodiment provides an electronic grade sulfur hexafluoride adsorption device, which includes a low pressure adsorption unit 1 and a high pressure adsorption unit 2, where the low pressure adsorption unit 1 and the high pressure adsorption unit 2 are connected in series and communicated, and a high pressure compressor 3 is communicated between the low pressure adsorption unit 1 and the high pressure adsorption unit 2. The low-pressure adsorption unit 1 comprises a first low-pressure adsorption tower 11 and a second low-pressure adsorption tower 12 which are sequentially communicated in series, wherein the first low-pressure adsorption tower 11 contains a silica gel adsorbent, and the second low-pressure adsorption tower 12 contains an alumina gel adsorbent. The high-pressure adsorption unit 2 comprises a first high-pressure adsorption tower 21, a second high-pressure adsorption tower 22, a third high-pressure adsorption tower 23, a fourth high-pressure adsorption tower 24 and a fifth high-pressure adsorption tower 25, wherein the first high-pressure adsorption tower 21 contains an alumina gel adsorbent, the second high-pressure adsorption tower 22 contains a 5A molecular sieve adsorbent, the third high-pressure adsorption tower 23 contains a 13X molecular sieve adsorbent, the fourth high-pressure adsorption tower 24 contains a CUCL molecular sieve adsorbent, and the fifth high-pressure adsorption tower 25 contains an F-03 molecular sieve adsorbent. The communication sequence of the high-pressure adsorption unit 2 is as follows: the first high-pressure adsorption tower 21, the second high-pressure adsorption tower 22, the third high-pressure adsorption tower 23, the fourth high-pressure adsorption tower 24 and the fifth high-pressure adsorption tower 25 are sequentially communicated in series, or the first high-pressure adsorption tower 21, the second high-pressure adsorption tower 22, the fourth high-pressure adsorption tower 24, the third high-pressure adsorption tower 23 and the fifth high-pressure adsorption tower 25 are sequentially communicated in series.
The working principle of the electronic grade sulfur hexafluoride adsorption device is as follows:
introducing sulfur hexafluoride coarse gas into an electronic grade sulfur hexafluoride adsorption device, and sequentially entering a 4-grade first low-pressure adsorption tower 11 and a 4-grade second low-pressure adsorption tower 12; then, the air is blown by the high-pressure compressor 3 to enter a first high-pressure adsorption tower 21, a second high-pressure adsorption tower 22, a third high-pressure adsorption tower 23, a fourth high-pressure adsorption tower 24 and a fifth high-pressure adsorption tower 25, or the first high-pressure adsorption tower 21, the second high-pressure adsorption tower 22, the fourth high-pressure adsorption tower 24, the third high-pressure adsorption tower 23 and the fifth high-pressure adsorption tower 25; finally, the mixture enters a rectifying tower 4 for rectification.
When the relative humidity of the sulfur hexafluoride is high, the moisture adsorption capacity of molecular sieve adsorbents such as 5A, 13X, CUCL and F-03 is not different from that of silica gel adsorbents and aluminum gel adsorbents, and when the relative humidity of the sulfur hexafluoride is low, the moisture adsorption capacity of the molecular sieve adsorbents such as 5A, 13X, CUCL and F-03 is much higher than that of the silica gel adsorbents and the aluminum gel adsorbents; the adsorption capacity of the molecular sieve adsorbent is far greater than that of the silica gel alumina adsorbent in the aspect of low fluoride adsorption capacity, but after a large amount of moisture is adsorbed by one molecular sieve adsorbent, the capacity of adsorbing low-sulfur fluoride is greatly reduced. In this embodiment, the sulfur hexafluoride coarse gas has a high humidity, and is subjected to a silica gel adsorbent in the first low-pressure adsorption tower 11 to remove most of the moisture, and then is further dried by an alumina gel adsorbent in the second low-pressure adsorption tower 12, and is blown by the high-pressure compressor 3 to enter the high-pressure adsorption unit 2. In the high-pressure adsorption unit 2, under the high-pressure condition, moisture is further removed through a first-stage alumina gel adsorbent, and trace water is removed through two stages of 5A molecular sieves, so that the follow-up 13X, CUCL and F-03 molecular sieve adsorbents have strong adsorption capacity on low fluoride; two-stage 13X molecular sieve adsorbent for CO removal2Two-stage CUCL molecular sieve adsorbent for removing CO and adsorbing CO2The adsorption of CO is not interfered mutually, and the sequence can be interchanged; then passing through 9-grade F-03 molecular sieve adsorbent to obtain sulfur fluoride compound, such as SF2、SF4、S2F2、S2F10Etc. and fluorooxysulfur compounds, e.g. SOF2、SOF4、SO2F2And adsorbing, and finally, rectifying in a rectifying tower. 13X molecular sieve adsorbent to CO2The adsorption capacity of the zeolite is high; the adsorption capacity of the CUCL molecular sieve adsorbent to the COI is stronger than that of other molecular sieve adsorbents; the F-03 molecular sieve adsorbent has the strongest adsorption capacity to low fluoride, but can be subjected to CO and CO2The adsorption capacity of the adsorbent is reduced. Meanwhile, silica gel and alumina gel adsorbent, 5A, 13X, CUCL and F-03 molecular sieve adsorbent pairLittle adsorption of sulfur hexafluoride itself. Therefore, the adsorption sequence of the molecular sieve is arranged in such a way that the low fluoride adsorption efficiency can be improved to the maximum extent, and the purity of the sulfur hexafluoride is improved.
As a further improvement, the number of stages of the first low-pressure adsorption tower 11 is 3-5, and the first low-pressure adsorption towers 11 of multiple stages are communicated in series. The number of stages of the second low-pressure adsorption tower 12 is 3-5, and the second low-pressure adsorption towers 12 are communicated in series. The silica gel adsorbent in the multistage first low-pressure adsorption tower 11 and the alumina gel adsorbent in the multistage second low-pressure adsorption tower 12 fully absorb moisture in the sulfur hexafluoride coarse gas, so that the moisture is prevented from influencing the subsequent 13X, CUCL and the F-03 molecular sieve adsorbent to have stronger adsorption capacity on low fluoride. If the number of stages is less than 3, it is difficult to sufficiently absorb moisture, and the more the number of stages is, the more sufficient the moisture is to be absorbed, the more favorable the subsequent molecular sieve absorbent is to absorb low fluoride, and in view of cost, both the first low pressure adsorption tower 11 and the second low pressure adsorption tower 12 are preferably 4 stages in this embodiment.
As a further modification, the number of stages of the second high-pressure adsorption column 22 is 2 or 3. The multistage second high-pressure adsorption columns 22 are connected in series in this embodiment. The 5A molecular sieve in the second high-pressure adsorption tower 22 further adsorbs trace water under high-pressure conditions, so that insufficient moisture adsorption under low-pressure conditions is avoided. If the number of stages is less than 2, it is difficult to sufficiently absorb moisture, and if the number of stages is more, moisture is more sufficiently absorbed, which is more advantageous for the subsequent molecular sieve absorbent to absorb low fluoride, and in view of cost, the number of stages is preferably 2 in the present embodiment.
As a further modification, the number of stages of the third high-pressure adsorption column 23 is 2 or 3. The multistage third high-pressure adsorption columns 23 are connected in series. The CUCL molecular sieve in the third high-pressure adsorption tower 23 has good adsorption capacity for low fluoride and also has good adsorption effect for CO. The inventor finds that the removal of CO in the sulfur hexafluoride crude gas by the CUCL molecular sieve can avoid the interference of CO on the adsorption capacity of the F-03 molecular sieve adsorbent to the low fluoride, and improves the adsorption capacity of the F-03 molecular sieve to the low fluoride. If the number of stages is less than 2, it will be difficult to sufficiently absorb CO, and the more the number of stages is, the more sufficient the absorption of CO is, the more advantageous the subsequent molecular sieve absorbent is to absorb low fluoride, and in view of cost, the number of stages is preferably 2 in this embodiment.
As a further improvement, the fourth high-pressure adsorption tower 24 has the stage number of 3-5; the multistage fourth high-pressure adsorption columns 24 are connected in series. The 13X molecular sieve in the fourth high-pressure adsorption tower 24 not only has good absorption capacity for low fluoride, but also has good absorption capacity for CO2Also has good adsorption capacity. The inventor finds that the CO in the sulfur hexafluoride crude gas is removed by the 13X molecular sieve in advance2Can avoid CO2The interference to the adsorption capacity of the F-03 molecular sieve adsorbent to the low fluoride improves the adsorption capacity of the F-03 molecular sieve to the low fluoride. If the number of stages is less than 3, it will be difficult to sufficiently absorb CO2The more the number of stages, for CO2The more sufficient the absorption of (b) is, the more favorable the subsequent molecular sieve absorbent is for low fluoride absorption, and in view of cost, the grade 4 is preferred in this embodiment.
The number of stages of the fourth high-pressure adsorption tower 25 is 8-10, the F-03 molecular sieve adsorbent in the fourth high-pressure adsorption tower 25 has strong adsorption capacity on low fluoride, and the multistage fourth high-pressure adsorption towers 25 are communicated in series, so that the low fluoride can be fully absorbed. The end of the treatment process of the F-03 molecular sieve adsorbent arrangement can be used for removing water, CO and CO in the front2Under the condition (2), the absorption capacity of the F-03 molecular sieve to low fluoride is exerted to the maximum extent. In the present embodiment, 9 stages are preferable.
As a further modification, a first bypass branch pipe 13 is connected between an inlet and an outlet of any one of the stages of the first low pressure adsorption tower 11, and a first valve 14 is provided in each of the inlet of the first low pressure adsorption tower 11 and the first bypass branch pipe 13. When the sulfur hexafluoride coarse gas is relatively dry, the first valve 14 on the first bypass branch pipe 13 can be opened, the first valve 14 at the inlet of the first low-pressure adsorption tower 11 is closed, and the sulfur hexafluoride coarse gas passes through the first bypass branch pipe 13, so that the first low-pressure adsorption tower 11 in one stage can be reduced, and the cost is reduced on the premise of ensuring the low fluoride adsorption efficiency.
A second bypass branch pipe 15 is communicated between an inlet and an outlet of any stage of the second low-pressure adsorption tower 12, and a second valve 16 is arranged on the inlet of the second low-pressure adsorption tower 12 of the stage and the second bypass branch pipe 15. In a similar way, the cost is reduced on the premise of ensuring the low fluoride adsorption efficiency.
A third bypass branch pipe 26 is communicated between an inlet and an outlet of any one stage of the fourth high-pressure adsorption tower 24, and a third valve 27 is arranged on both the inlet of the fourth high-pressure adsorption tower 24 and the third bypass branch pipe 26. A fourth bypass branch pipe 28 is communicated between an inlet and an outlet of any stage of the fifth high-pressure adsorption tower 25, and a fourth valve 29 is arranged on the inlet of the fifth high-pressure adsorption tower 25 and the fourth bypass branch pipe 28. In a similar way, the cost is reduced on the premise of ensuring the low fluoride adsorption efficiency.
Example 2
The method for applying the electronic grade sulfur hexafluoride adsorption device comprises the steps of introducing prepared sulfur hexafluoride crude gas into the low-pressure adsorption unit 1 for adsorption, blowing air by the high-pressure compressor 3, then introducing the air into the high-pressure adsorption unit 2 for further adsorption, and finally introducing the air into the rectifying tower 4 for rectification to obtain high-purity sulfur hexafluoride.
The blowing and blowing of the air blowing are alternately performed by low-pressure air blowing and high-pressure air blowing, the low-pressure air blowing is 0.12-0.13MPa for 10-15min, and the high-pressure air blowing is 0.15-0.20MPa for 5-10 min. The inventor finds that the low-pressure blast and the high-pressure blast are alternately carried out, so that the fact that the retention time of impurities of each molecular sieve adsorbent is long and the molecular sieve adsorbent is fully adsorbed when the molecular sieve adsorbent is at low pressure is ensured, gas is quickly blown to the next adsorbent when the molecular sieve adsorbent is at high pressure, the next adsorbent is convenient to adsorb, and the overall adsorption efficiency is greatly improved.
The flow velocity of the sulfur hexafluoride coarse gas is 0.1-0.5m3and/S. This flow rate is very critical. The multistage adsorbents can influence each other, especially the adsorption effect of the previous stage and the adsorption effect of the next stage, and the various adsorbents can exert synergistic effect to maximize the adsorption effect. The flow velocity can influence the adsorption effect of different adsorbents at each stage, and the flow velocity is matched with the adsorption capacity of multiple adsorbents in a multi-stage adsorption tower to ensure that various adsorbents perform synergistic adsorptionThe best adsorption effect is achieved.
The content of sulfur hexafluoride in sulfur hexafluoride gas is determined by gas chromatography.
The toxicity of sulfur hexafluoride gas was determined by the following method:
simulating the oxygen and nitrogen contents in air to prepare 79X 10-2(V/V) Sulfur hexafluoride gas and 21X 10-2(V/V) test gas of oxygen. Continuously infecting the mice with the toxin for 24h, observing for 72h, and checking whether the mice have toxic symptoms.
Experimental procedures
Female mice weighing about 20g were purchased from 15-20 mice and housed in cages. Before the test, observation should be carried out for 3 to 5 days to confirm the health of the white mouse.
Opening the sulfur hexafluoride sample gas cylinder and the oxygen gas cylinder, adjusting to the required proportion, wherein the gas flow per minute is not less than 1/8 of the volume of the contamination cylinder. After the flow rate was stabilized, 5 mice were placed in a contamination jar, and drinking water and food were supplied for 24 hours. The results were recorded hourly, in the case of mice.
The mice were then returned to their cages for further observation for 72h and recorded.
And (4) judging and processing a result:
if the white mouse has no abnormal performance, the batch of the product is determined to be non-toxic.
The white mouse has abnormal manifestations, such as low head without eating, crazy jumping and death. Another 10 experiments were newly performed. If the test result shows no abnormal performance, the product is qualified, and if the test result shows abnormal performance, the product is disqualified, and the mice with abnormal performance are subjected to careful autopsy so as to further confirm the reason of the abnormal performance.
Through detection, the content of sulfur hexafluoride in the sulfur hexafluoride gas sample is 99.9995%, which is far higher than the requirement of the electronic industry. The toxicity test result is non-toxic. The toxicity result is non-toxic, and further verifies that the sulfur hexafluoride gas does not contain low fluorine compounds.
Comparative example 1
The blast pressure of the blast is 0.15-0.20MPa, and low-pressure blast and high-pressure blast are not alternately carried out. The other operations were the same as in example 2. The sulfur hexafluoride gas sample is detected to have the sulfur hexafluoride content of 94.69%.
Comparative example 2
The operation was otherwise the same as in example 2 without the third high-pressure absorption column. The sulfur hexafluoride gas sample is detected to have the sulfur hexafluoride content of 92.54 percent.
Comparative example 3
The flow velocity of the sulfur hexafluoride coarse gas is 0.8m3(S) the other operations were the same as in example 2. Through detection, the content of sulfur hexafluoride in the sulfur hexafluoride gas sample is 88.45%.
Comparative example 4
The flow velocity of the sulfur hexafluoride coarse gas is 0.06m3(S) the other operations were the same as in example 2. Through detection, the content of the sulfur hexafluoride in the sulfur hexafluoride gas sample is 91.62%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The electronic grade sulfur hexafluoride adsorption device is characterized by comprising a low-pressure adsorption unit (1) and a high-pressure adsorption unit (2), wherein the low-pressure adsorption unit (1) and the high-pressure adsorption unit (2) are communicated in series, and a high-pressure compressor (3) is communicated between the low-pressure adsorption unit (1) and the high-pressure adsorption unit (2); the low-pressure adsorption unit (1) comprises a first low-pressure adsorption tower (11) and a second low-pressure adsorption tower (12) which are sequentially communicated in series, wherein the first low-pressure adsorption tower (11) contains a silica gel adsorbent, and the second low-pressure adsorption tower (12) contains an alumina gel adsorbent; the high-pressure adsorption unit (2) comprises a first high-pressure adsorption tower (21), a second high-pressure adsorption tower (22), a third high-pressure adsorption tower (23), a fourth high-pressure adsorption tower (24) and a fifth high-pressure adsorption tower (25), wherein the first high-pressure adsorption tower (21) contains an alumina gel adsorbent, the second high-pressure adsorption tower (22) contains a 5A molecular sieve adsorbent, the third high-pressure adsorption tower (23) contains a 13X molecular sieve adsorbent, the fourth high-pressure adsorption tower (24) contains a CUCL molecular sieve adsorbent, and the fifth high-pressure adsorption tower (25) contains an F-03 molecular sieve adsorbent; the communication sequence of the high-pressure adsorption units (2) is as follows: the first high-pressure adsorption tower (21), the second high-pressure adsorption tower (22), the third high-pressure adsorption tower (23), the fourth high-pressure adsorption tower (24) and the fifth high-pressure adsorption tower (25) are sequentially communicated in series, or the first high-pressure adsorption tower (21), the second high-pressure adsorption tower (22), the fourth high-pressure adsorption tower (24), the third high-pressure adsorption tower (23) and the fifth high-pressure adsorption tower (25) are sequentially communicated in series; the number of stages of the fourth high-pressure adsorption tower (24) is 3-5, and the number of stages of the fifth high-pressure adsorption tower (25) is 8-10.
2. An electronic grade sulphur hexafluoride adsorption unit as claimed in claim 1 wherein the first low pressure adsorption column (11) is in the order of 3 to 5; the number of stages of the second low-pressure adsorption tower (12) is 3-5.
3. An electronic grade sulphur hexafluoride adsorption unit as claimed in claim 2 wherein a first bypass branch (13) is connected between the inlet and the outlet of any one of the first low pressure adsorption columns (11), and a first valve (14) is provided in each of the inlet and the first bypass branch (13) of the first low pressure adsorption column (11); and a second bypass branch pipe (15) is communicated between an inlet and an outlet of any stage of the second low-pressure adsorption tower (12), and a second valve (16) is arranged on the inlet of the second low-pressure adsorption tower (12) and the second bypass branch pipe (15).
4. An electronic grade sulphur hexafluoride adsorption unit as claimed in claim 1 wherein the second high pressure adsorption column (22) is in the order of 2 or 3.
5. An electronic grade sulphur hexafluoride adsorption unit as claimed in claim 1 wherein the third high pressure adsorption column (23) is in the order of 2 or 3.
6. An electronic grade sulphur hexafluoride adsorption unit as claimed in claim 1 wherein the fifth high pressure adsorption column (25) is in the order of 9.
7. The electronic grade sulphur hexafluoride adsorption device of claim 1 wherein a third bypass branch (26) is connected between the inlet and the outlet of any one of the fourth high pressure adsorption columns (24), and a third valve (27) is provided in each of the inlet of the fourth high pressure adsorption column (24) and the third bypass branch (26); and a fourth bypass branch pipe (28) is communicated between an inlet and an outlet of any stage of the fifth high-pressure adsorption tower (25), and fourth valves (29) are arranged on the inlet of the fifth high-pressure adsorption tower (25) and the fourth bypass branch pipe (28).
8. A method using the electronic grade sulfur hexafluoride adsorption device of claims 1 to 7, wherein the prepared crude sulfur hexafluoride gas is introduced into the low-pressure adsorption unit (1) for adsorption, is blown by the high-pressure compressor (3) and then enters the high-pressure adsorption unit (2) for further adsorption, and finally enters the rectifying tower (4) for rectification, so that high-purity sulfur hexafluoride is obtained.
9. The method according to claim 8, characterized in that the blasting of the blast is performed alternately with low pressure blasting of 0.12-0.13MPa for 10-15min and with high pressure blasting of 0.15-0.20MPa for 5-10 min.
10. The method as claimed in claim 8, wherein the sulfur hexafluoride gas is introduced at a flow rate of 0.1-0.5m3/S。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110173728.4A CN112978683A (en) | 2021-02-06 | 2021-02-06 | Electronic-grade sulfur hexafluoride adsorption device and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110173728.4A CN112978683A (en) | 2021-02-06 | 2021-02-06 | Electronic-grade sulfur hexafluoride adsorption device and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112978683A true CN112978683A (en) | 2021-06-18 |
Family
ID=76347741
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110173728.4A Pending CN112978683A (en) | 2021-02-06 | 2021-02-06 | Electronic-grade sulfur hexafluoride adsorption device and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112978683A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114873568A (en) * | 2022-04-11 | 2022-08-09 | 福建德尔科技股份有限公司 | Electronic grade SF 6 Rectification pretreatment system |
| CN114890388A (en) * | 2022-04-11 | 2022-08-12 | 福建德尔科技股份有限公司 | Electronic-grade sulfur hexafluoride pretreatment system and control method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002114504A (en) * | 2000-10-02 | 2002-04-16 | Toshiba Corp | Device and method for recovering sf6 gas |
| KR100584687B1 (en) * | 2005-11-10 | 2006-05-29 | 주식회사 아토 | Purification method of sf6 |
| CN202212084U (en) * | 2011-07-27 | 2012-05-09 | 安徽省电力科学研究院 | Purification treatment system for sulfur hexafluoride gas decomposition product |
| CN202569897U (en) * | 2012-05-03 | 2012-12-05 | 广州市恒力安全检测技术有限公司 | Sulfur hexafluoride gas purification device |
| CN111470478A (en) * | 2020-04-29 | 2020-07-31 | 福建德尔科技有限公司 | High-purity sulfur hexafluoride and preparation method thereof |
-
2021
- 2021-02-06 CN CN202110173728.4A patent/CN112978683A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002114504A (en) * | 2000-10-02 | 2002-04-16 | Toshiba Corp | Device and method for recovering sf6 gas |
| KR100584687B1 (en) * | 2005-11-10 | 2006-05-29 | 주식회사 아토 | Purification method of sf6 |
| CN202212084U (en) * | 2011-07-27 | 2012-05-09 | 安徽省电力科学研究院 | Purification treatment system for sulfur hexafluoride gas decomposition product |
| CN202569897U (en) * | 2012-05-03 | 2012-12-05 | 广州市恒力安全检测技术有限公司 | Sulfur hexafluoride gas purification device |
| CN111470478A (en) * | 2020-04-29 | 2020-07-31 | 福建德尔科技有限公司 | High-purity sulfur hexafluoride and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 陈敏: "六氟化硫气体吸附提纯技术与吸附剂选择研究", 《广州化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114873568A (en) * | 2022-04-11 | 2022-08-09 | 福建德尔科技股份有限公司 | Electronic grade SF 6 Rectification pretreatment system |
| CN114890388A (en) * | 2022-04-11 | 2022-08-12 | 福建德尔科技股份有限公司 | Electronic-grade sulfur hexafluoride pretreatment system and control method thereof |
| CN114890388B (en) * | 2022-04-11 | 2022-12-20 | 福建德尔科技股份有限公司 | Electronic-grade sulfur hexafluoride pretreatment system and control method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112978683A (en) | Electronic-grade sulfur hexafluoride adsorption device and application | |
| US20100024647A1 (en) | Method and Device for Separating Methane and Carbon Dioxide from Biogas | |
| EP1334758A1 (en) | Gas separating and purifying method and its apparatus | |
| CN1137418A (en) | Removal of carbon dioxide from gas streams | |
| AU2017234497A1 (en) | Method and device for recovering carbon dioxide | |
| CN103920365A (en) | Method for recycling nitrogen gas and sulfur dioxide from calcining iron pyrite burner gas through variable-voltage variable-frequency adsorption | |
| CN108100994A (en) | A kind of hydrogen recycling purification system and its control method | |
| CN214437760U (en) | Electronic grade sulfur hexafluoride adsorption device | |
| CN104108685B (en) | The recycling reutilization technology of electrical network sulfur hexafluoride | |
| EP1281430A2 (en) | Purification of gases | |
| CN202212084U (en) | Purification treatment system for sulfur hexafluoride gas decomposition product | |
| KR100856912B1 (en) | Purifying nitrogen supply apparatus | |
| CN110040692B (en) | Method and device for preparing high-purity sulfur dioxide gas | |
| CN115869729A (en) | SF6 purification device and method for full-automatic impurity gas detection | |
| CN214937122U (en) | Purification system of electron-level purity acetylene | |
| CN105502317A (en) | Device for recycling and purifying nitrous oxide | |
| CN105727686B (en) | A kind of method for adsorbing purification sulfur hexafluoride | |
| CN211521583U (en) | Nitrogen-hydrogen gas recovery device of open-type continuous annealing furnace | |
| CN113772673A (en) | Process system and method for recovering and purifying carbon dioxide from lime kiln tail gas | |
| TWM626483U (en) | Vacuum pressure swing adsorption system for separation of carbon dioxide | |
| CN106731497B (en) | Decarbonizing and extracting N from nitric acid industrial tail gas 2 O purification device and process method | |
| CN207943869U (en) | A kind of hydrogen recovery and purification system | |
| CN112850668A (en) | Chlorine-containing tail gas helium purification system | |
| CN202912696U (en) | Pressure swing adsorption type air separation nitrogen making equipment for keeping grain fresh | |
| CN205815181U (en) | A kind of organic solvent refining plant |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: No. 6, Gongye Road, Jiaoyang industrial concentration zone, Jiaoyang Town, Shanghang County, Longyan City, Fujian Province, 364204 Applicant after: Fujian del Technology Co.,Ltd. Address before: No. 6, Gongye Road, Jiaoyang industrial concentration zone, Jiaoyang Town, Shanghang County, Longyan City, Fujian Province, 364000 Applicant before: FUJIAN DEER TECHNOLOGY CO.,LTD. |