KR20170027068A - Apparatus and method for separation and recovery of hexafluorosulfide gas - Google Patents

Apparatus and method for separation and recovery of hexafluorosulfide gas Download PDF

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KR20170027068A
KR20170027068A KR1020150123512A KR20150123512A KR20170027068A KR 20170027068 A KR20170027068 A KR 20170027068A KR 1020150123512 A KR1020150123512 A KR 1020150123512A KR 20150123512 A KR20150123512 A KR 20150123512A KR 20170027068 A KR20170027068 A KR 20170027068A
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sulfur hexafluoride
hexafluoride gas
gas
hydrate
recovering
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KR1020150123512A
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Korean (ko)
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안치규
한건우
이만수
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재단법인 포항산업과학연구원
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Priority to KR1020150123512A priority Critical patent/KR20170027068A/en
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    • 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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • 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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/68—Halogens or halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/11—Noble gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • 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
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/30—Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
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  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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Abstract

The method for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention includes the steps of recovering waste sulfur hexafluoride gas; Pressurizing and cooling the recovered waste sulfur hexafluoride gas; Adding an alkaline solution to the pressurized and cooled sulfur hexafluoride gas stream to form a hydrate and a salt of sulfur hexafluoride gas and to remove the impurity gas; And dissociating the hydrate of the sulfur hexafluoride gas, and removing water to recover the hexafluorosulfur gas.

Description

[0001] APPARATUS AND METHOD FOR SEPARATION AND RECOVERY OF HEXAFLUOROSULFIDE GAS [0002]

And an apparatus and a method for separating and recovering sulfur hexafluoride gas.

Sulfur hexafluoride gas (SF 6) is colorless at room temperature to the highly stable inert gas chemically, odorless, harmless, has high dielectric strength of a material with a non-flammable, have a characteristic degradation is not easy, and etching of the semiconductor manufacturing process (etching ), Cover gas of magnesium refining process, and insulated gas of a gas insulated switchgear (GIS: Gas Insulated Switchgear).

The global warming index of SF 6 is about 23,900 times higher than that of CO 2. Therefore , there is a high demand for SF 6 separation and recovery technology in terms of greenhouse gas reduction.

On the other hand, in the case of a heavy SF 6 for heavy electric power, it is known that the SF 6 is re-injected and refined in the SF 6 production process, but only a small fraction of the generated SF 6 is separated and recovered through this method. But also it proposed a method for processing the waste by pyrolysis SF 6, SF 6, because the lung is to occur at a high concentration, there is a limit to the variety of problems such as equipment corrosion due to decomposition products.

An apparatus and a method for separating and recovering sulfur hexafluoride gas are provided. More particularly, the present invention provides an apparatus and method for separating and recovering sulfur hexafluoride gas using the hydrate formation principle.

The method for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention includes the steps of recovering waste sulfur hexafluoride gas; Pressurizing and cooling the recovered waste sulfur hexafluoride gas; Adding an alkaline solution to the pressurized and cooled sulfur hexafluoride gas stream to form a hydrate and a salt of sulfur hexafluoride gas and to remove the impurity gas; And dissociating the hydrate of the sulfur hexafluoride gas, and removing water to recover the hexafluorosulfur gas.

In recovering the waste SF6 gas, waste SF6 gas is HF 10 to 10,000 ppmv, SO 2 10 to 1,000ppmv, N 2 0.1 to 5% by volume, SOF 2 to 10 5,000ppmv, SOF 4 10 to 1,000 ppmv, 0.1 to 5 vol% O 2 , and SF 6 as the remainder.

The step of pressurizing and cooling the recovered pulverized sulfur hexafluoride gas can pressurize and cool the recovered pulverized sulfur hexafluoride gas at a pressure of 1 to 15 bar and a temperature of 0 to 10 ° C.

In the step of forming the hydrate and the salt of sulfur hexafluoride gas and removing the impurity gas, the impurity gas may include HF, SO 2 , SOF 2, SOF 4 , N 2 and O 2 .

The step of forming the hydrate and the salt of sulfur hexafluoride gas and removing the impurity gas may include adding 210 to 250 parts by weight of the alkali solution to 100 parts by weight of the pressurized and cooled sulfur hexafluoride gas.

The alkali solution may contain at least one alkali component selected from NaOH, Ca (OH) 2 , CaO and MgO.

And 0.1 to 10% by weight of an alkali component with respect to 100% by weight of the alkali solution.

The alkali solution may further comprise an anionic surfactant, tetrahydrofuran or ammonium salt.

The anionic surfactant may be sodium dodecylsulfate or linear alkyl benzene sulfonate.

The ammonium salt may be tetrabutylammonium bromide.

The anionic surfactant, tetrahydrofuran or ammonium salt may be added in an amount of 0.001 to 5% by weight based on 100% by weight of the total alkali solution.

The hydrate of sulfur hexafluoride gas can be dissolved at a temperature of 15 to 50 캜.

And pressurizing the recovered sulfur hexafluoride gas to charge the heavy fuel cell.

The salt can be filtered out from the liquid in which the hexafluorosulfur gas is dissociated, and the alkali component can be supplemented and reused for the hydrate of the sulfur hexafluoride gas.

The apparatus for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention includes: a recovery unit for recovering waste sulfur hexafluoride gas; A first reactor connected to the recovery section and pressurizing or cooling the recovered waste sulfur hexafluoride gas to form a hydrate of sulfur hexafluoride gas together with the alkali solution contained therein; And a second reactor connected to the first reactor for receiving the hydrate of the sulfur hexafluoride gas and decompressing or raising the temperature to dissociate and separate the hexafluorosulfur gas.

The alkali solution may contain at least one alkali component selected from NaOH, Ca (OH) 2 , CaO and MgO.

And 0.1 to 10% by weight of the alkali component with respect to 100% by weight of the alkali solution.

The first reactor can be maintained at a pressure of from 1 to 15 bar and a temperature of from 0 to 10 < 0 > C.

The first reactor is composed of the upper part and the lower part, the upper part collects and discharges the residual gas including N 2 and O 2 , and the lower part collects the hydrated gas and can move to the second reactor.

The second reactor can be maintained at a temperature of 15 to 50 < 0 > C.

The upper part of the second reactor can be used for removing water by installing silica gel, molecular sieve or zeolite.

The liquid in which the hexafluorosulfur gas is dissociated is collected in the lower part of the second reactor, the salt is filtered in the collected liquid, and the alkaline component can be replenished and put back into the first reactor.

The sulfur hexafluoride gas generated in the heavy electric power can be selectively recovered and concentrated and reused in the heavy electric power, so that the amount of sulfur hexafluoride gas generated in the heavy electric power can be reduced.

It can contribute to greenhouse gas reduction by recovering sulfur hexafluoride gas, which has a high global warming index.

1 is a schematic flowchart of a method for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention.
2 is a schematic block diagram of an apparatus for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention.
3 is a graph showing the temperature and pressure of Example 1 and Comparative Example 1 over time.
4 is a graph showing the temperature and pressure of Example 2 and Comparative Example 2 over time.

The terms first, second and third, etc. are used to describe various portions, components, regions, layers and / or sections, but are not limited thereto. These terms are only used to distinguish any moiety, element, region, layer or section from another moiety, moiety, region, layer or section. Thus, a first portion, component, region, layer or section described below may be referred to as a second portion, component, region, layer or section without departing from the scope of the present invention.

The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the invention. The singular forms as used herein include plural forms as long as the phrases do not expressly express the opposite meaning thereto. Means that a particular feature, region, integer, step, operation, element and / or component is specified and that the presence or absence of other features, regions, integers, steps, operations, elements, and / It does not exclude addition.

Unless otherwise defined, all terms including technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Commonly used predefined terms are further interpreted as having a meaning consistent with the relevant technical literature and the present disclosure, and are not to be construed as ideal or very formal meanings unless defined otherwise.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily carry out the present invention. The present invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.

1 schematically shows a flowchart of a method for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention. The flowchart of the method for separating and recovering sulfur hexafluoride gas of FIG. 1 is for illustrating the present invention only, and the present invention is not limited thereto. Therefore, the method of separating and recovering sulfur hexafluoride gas can be variously modified.

As shown in FIG. 1, the method for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention includes: (S10) recovering waste sulfur hexafluoride gas; A step (S20) of pressurizing and cooling the recovered waste sulfur hexafluoride gas; Adding an alkaline solution to the pressurized and cooled sulfur hexafluoride gas stream to form a hydrate and a salt of sulfur hexafluoride gas and removing the impurity gas (S30); And dissociating the hydrate of sulfur hexafluoride gas and removing water to recover sulfur hexafluoride gas (S40). In addition, the separation and recovery method of sulfur hexafluoride gas may further include other steps as required.

First, in step S10, the waste sulfur hexafluoride gas is recovered. At this time, the sulfur hexafluorosulfur gas can be the sulfur hexafluoride gas generated in the heavy electric power. More specifically, it can be a sulfur hexafluoride gas generated from a gas circuit breaker or a gas isolator.

The SF 6 used in the heavy electric field is decomposed by arc discharge or the like under a high voltage to generate acid gases such as HF, SO 2 , SOF 2 and SOF 4 . In addition, N 2 , O 2 may exist due to external air inflow while recovering the sulfur hexafluoride gas from the heavy electric machine. Specifically lung SF6 gas is HF 10 to 10,000 ppmv, SO 2 10 to 1,000ppmv, SOF 2 10 to 5,000ppmv, SOF 4 10 to 1,000ppmv, N 2 0.1 to 5 vol%, O 2 0.1 to 5% by volume and an SF 6 glass parts. In one embodiment of the present invention, impurity gases such as HF, SO 2 , SOF 2, SOF 4, N 2 and O 2 are removed from the waste sulfur hexafluoride gas and pure SF 6 is recovered.

Next, in step S20, the recovered waste sulfur hexafluoride gas is pressurized and cooled. By pressurizing and cooling the recovered sulfur hexafluoride gas, only sulfur hexafluoride gas forms hydrate in step S30. At this time, the pressure may be 1 to 15 bar, and the temperature may be 0 to 10 ° C. In the above-mentioned range, the hydrate of sulfur hexafluoride gas is appropriately formed.

Next, in step S30, an alkaline solution is added to the pressurized and cooled sulfur hexafluoride sulfur gas to form a hydrate and a salt of sulfur hexafluoride gas, and the impurity gas is removed. The impurity gas means a gas such as an acid gas, N 2 and O 2 . Here, the acid gas means a gas such as HF, SO 2 , SOF 2, SOF 4, and the like.

Conventionally, the pretreatment process for the acid gas is complicated and it is difficult to remove the inflow air (N 2 , O 2 ) during the recovery process. Therefore, the waste sulfur hexafluoride gas generated in the heavy electricity can not be re-injected into the production process of sulfur hexafluoride gas Sulfur hexafluoride was discarded or released into the atmosphere.

However, according to the embodiment of the present invention, it is possible to simply remove the impurity gas in addition to SF 6 .

The amount of the alkali solution to be added may be 210 to 250 parts by weight based on 100 parts by weight of pressurized and cooled sulfur hexafluoride gas. If the amount of the alkali solution is too small, a problem may arise that the sulfur hexafluoride gas can not be entirely hydrated. If the amount of the alkali solution is too large, the amount of the alkali solution that needs to be raised in temperature in order to recover SF 6 increases, and the energy consumption may increase. Therefore, the addition amount of the alkali solution can be adjusted within the range described above.

The alkali solution is a solution containing an alkali component and water, which is added to remove acidic gas contained in the sulfur hexafluorosulfur gas and to form a hydrate of sulfur hexafluoride gas.

In the alkali solution, the alkali component reacts with the acid gas contained in the sulfur hexafluoride gas to form a salt. The salt is dissolved in the liquid phase, or remains in a solid state, and is not gasified again, but remains as a salt even if the temperature is raised in step S40 to be described later. If the sulfur hexafluoride gas is hydrated using water without using an alkali solution, the acidic gas physically dissolved in water is discharged again in the form of gas in the step S40 to be described later, and the dissociated sulfur hexafluoride gas And then mixed again.

As the alkali component, any substance capable of reacting with an acidic gas to form a salt can be used without limitation. Concretely, at least one alkali component selected from NaOH, Ca (OH) 2 , CaO and MgO can be used.

And 0.1 to 10% by weight of an alkali component with respect to 100% by weight of the alkali solution. When the alkali component is contained in an excessively small amount, the acid gas contained in the sulfur hexafluoride gas gas may partially remain unreacted and the problem may remain. If the alkali component is contained too much, the generation rate of the hydrate may be slowed or the induction time of the initial hydrate may be prolonged. Therefore, the amount of the alkali component can be controlled within the above-mentioned range.

An additive may be included in the added alkali solution to help hydrate the sulfur hexafluoride gas. The additive may be an anionic surfactant, tetrahydrofuran or ammonium salt. More specifically, the anionic surfactant may be sodium dodecyl sulfate (SDS) or linear alkyl benzene sulfonate (LABS). As the ammonium salt, tetrabutylammonium bromide (tetra- n-butyl ammonium bromide).

The anionic surfactant, tetrahydrofuran or ammonium salt may be added in an amount of 0.001 to 5% by weight based on 100% by weight of the alkali solution. If the addition amount is too small, the effect of improving the hydrate formation rate may be insignificant. If the addition amount is too large, it may interfere with hydrate formation or may not be as effective as the amount of the added additive. Therefore, the addition amount can be adjusted within the above-mentioned range.

Some of the separated sulfur hexafluorosulfur gas hydrate may be put into step S30 again and used for further recovery of sulfur hexafluoride by injection into the hydrate formation reactor.

Next, in step S40, the hydrate of sulfur hexafluoride gas is dissociated, and moisture is removed to recover the hexafluorosulfur gas. The hydrate of sulfur hexafluoride gas can be easily dissociated by controlling the temperature. Specifically, the temperature can be raised to 15 to 50 DEG C to dissociate the hydrate of sulfur hexafluoride gas. If the temperature is too low, the dissociation rate is slow and the dissociation amount may not be sufficient. If the temperature is too high, the moisture contained in the SF 6 may be too high to increase the load at the stage of removing moisture. Also, if the temperature is too high, N 2 , O 2, etc. physically dissolved in water may be converted to gas and mixed with SF 6 . Therefore, the temperature can be controlled within the above-mentioned range.

When the hydrate of the sulfur hexafluoride gas dissociates into the sulfur hexafluoride gas and the liquid containing the salt, the sulfur hexafluoride gas and the amount of the saturated water vapor are present in the upper part of the reactor. At this time, water can be adsorbed and removed by using silica gel, molecular sieve or zeolite to remove moisture, and pure sulfur hexafluoride gas can be recovered.

On the other hand, the liquid in which the hexafluorosulfur gas is dissociated is collected and returned to the step S30, and can be used for forming the hydrate of the sulfur hexafluoride gas in the step S30. At this time, the salt present in the liquid can be separated by filtration, and the alkali component can be supplemented.

The recovered sulfur hexafluoride gas can be pressurized and charged in the heavy electricity. At this time, the pressure may be 2 to 5 bar. The pressurized sulfur hexafluoride gas may also be used to purge the hydrate reactor in step S40 described above to remove impurity gases.

2 schematically shows a configuration of an apparatus for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention. The arrangement of the apparatus for separating and recovering sulfur hexafluoride gas of FIG. 2 is merely for illustrating the present invention, and the present invention is not limited thereto. Therefore, the apparatus for separating and recovering sulfur hexafluoride gas can be modified in various ways.

2, the apparatus for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention includes a recovery unit 10 for recovering waste sulfur hexafluoride gas, a recovery unit 10 connected to the recovery unit, A first reactor (20) which pressurizes or cools sulfur fluoride gas to form a hydrate of sulfur hexafluoride gas together with an alkali solution contained therein, a first reactor (20) connected to the first reactor, and a formed hydrate of sulfur hexafluoride gas , And a second reactor (30) for decompressing or raising the temperature to dissociate and separate the hexafluorosulfur gas. In addition, the apparatus for separating and recovering sulfur hexafluoride gas may further include other structures as needed.

First, the recovery unit 10 recovers waste sulfur hexafluoride gas. At this time, the waste sulfur hexafluoride gas can recover the waste sulfur hexafluoride gas generated in the heavy electric power. More specifically, it is possible to recover the sulfur hexafluoride gas generated in the gas circuit breaker or the gas isolator. As the recovery unit, recovery suction or the like can be used.

The SF 6 used in the heavy electric field is decomposed by arc discharge or the like under a high voltage to generate acid gases such as HF, SO 2 , SOF 2 and SOF 4 . In addition, N 2 , O 2 may exist due to external air inflow while recovering the sulfur hexafluoride gas from the heavy electric machine. Specifically lung SF6 gas is HF 10 to 10,000 ppmv, SO 2 10 to 1,000ppmv, SOF 2 10 to 5,000ppmv, SOF 4 10 to 1,000ppmv, N 2 0.1 to 5 vol%, O 2 0.1 to 5% by volume and an SF 6 glass parts. In one embodiment of the present invention, impurity gases such as HF, SO 2 , SOF 2, SOF 4, N 2 and O 2 are removed from the waste sulfur hexafluoride gas and pure SF 6 is recovered.

Next, the first reactor 20 is connected to the recovery section 10, and pressurizes or cools the recovered pulverized sulfur hexafluoride gas to form a hydrate of sulfur hexafluoride gas together with the alkali solution contained therein. At this time, the pressure may be 1 to 15 bar, and the temperature may be 0 to 10 ° C. In the above-mentioned range, the hydrate of sulfur hexafluoride gas is appropriately formed.

Conventionally, the pretreatment process for the acid gas is complicated and it is difficult to remove the inflow air (N 2 , O 2 ) during the recovery process, so that the sulfur hexafluoride gas generated in the heavy electric power can not be re-injected into the production process of sulfur hexafluoride gas Sulfur hexafluoride was discarded or released into the atmosphere.

The apparatus for separating and recovering sulfur hexafluoride gas according to an embodiment of the present invention can remove impurity gas with a simple structure.

In the first reactor 20, a hydrate of sulfur hexafluoride gas is formed and the impurity gas is removed. The impurity gas means a gas such as an acid gas, N 2 and O 2 . The acid gas means HF, SO 2 , SOF 2, SOF 4 , and the like.

The amount of the alkali solution present in the first reactor 20 may be 210 to 250 parts by weight based on 100 parts by weight of the pressurized, cooled, purged sulfur hexafluoride gas. If the amount of the alkali solution is too small, a problem may arise that the sulfur hexafluoride gas can not be entirely hydrated. If the amount of the alkali solution is too large, the amount of the alkali solution that needs to be raised in temperature in order to recover SF 6 increases, and the energy consumption may increase. Therefore, the amount of the alkali solution can be controlled within the above-mentioned range.

In the alkali solution, the alkali component reacts with the acid gas contained in the sulfur hexafluoride gas to form a salt. Even if the temperature is raised in the second reactor 30 described later as a dissolved ion state or solid state in the liquid phase, it is not gasified again but remains as a salt. If the sulfur hexafluoride gas is hydrated using water without using an alkali solution, the acidic gas dissolved in the water is again discharged in the form of gas in the second reactor 30, which will be described later, and dissociated sulfur hexafluoride gas And the like.

As the alkali component, any substance capable of reacting with an acidic gas to form a salt can be used without limitation. Concretely, at least one alkali component selected from NaOH, Ca (OH) 2 , CaO and MgO can be used.

And 0.1 to 10% by weight of an alkali component with respect to 100% by weight of the alkali solution. When the alkali component is contained in an excessively small amount, the acid gas contained in the sulfur hexafluoride gas gas may partially remain unreacted and the problem may remain. If the alkali component is contained too much, the generation rate of the hydrate may be slowed or the induction time of the initial hydrate may be prolonged. Therefore, the amount of the alkali component can be controlled within the above-mentioned range.

The alkaline solution may contain an additive to aid hydrate formation of the sulfur hexafluoride gas. The additive may be an anionic surfactant, tetrahydrofuran or ammonium salt. More specifically, the anionic surfactant may be sodium dodecyl sulphate (SDS) or linear alkyl benzene sulphonate (LABS). The ammonium salt may be tetra-n-butyl ammonium bromide.

The anionic surfactant, tetrahydrofuran or ammonium salt may be added in an amount of 0.001 to 5% by weight based on 100% by weight of the alkali solution. If the addition amount is too small, the effect of improving the hydrate formation rate may be insignificant. If the addition amount is too large, it may interfere with hydrate formation or may not be as effective as the amount of the added additive. Therefore, the addition amount can be adjusted within the above-mentioned range.

Some of the separated hexafluorosulfur gas hydrate may be reintroduced into the first reactor 20 and used for further recovery of sulfur hexafluoride.

The first reactor 20 is divided into an upper portion and a lower portion. The upper portion collects impurity gas that has not been hydrated and discharges through the outlet, and the lower portion moves the hydrated liquid to the second reactor 30.

Next, the second reactor 30 is connected to the first reactor 20, dissociates the hydrate of sulfur hexafluoride gas formed in the first reactor 20, removes moisture, and recovers the sulfur hexafluoride gas . In the second reactor (30), the temperature of the reactor can be adjusted to easily dissociate. Specifically, the temperature can be raised to 15 to 50 DEG C to dissociate the hydrate of sulfur hexafluoride gas. If the temperature falls outside the above range, dissociation is not smooth, so that the temperature can be controlled within the above-mentioned range.

If the temperature is too low, the dissociation rate is slow and the dissociation amount may not be sufficient. When the temperature is too high, the load may be increased in the step of removing much moisture from the gaseous phase contained in the SF 6 . Also, if the temperature is too high, N 2 , O 2, etc. physically dissolved in water may be converted to gas and mixed with SF 6 . Therefore, the temperature can be controlled within the above-mentioned range.

When the hydrate of the sulfur hexafluoride gas dissociates into sulfur hexafluoride gas and water, moisture of hexafluorosulfur gas and water as much as the amount of saturated water vapor is present in the upper portion of the second reactor 30. At this time, water can be adsorbed and removed by using silica gel, molecular sieve or zeolite to remove moisture, and pure sulfur hexafluoride gas can be recovered. Specifically, a silica gel, a molecular sieve or a zeolite may be provided on the top of the water removing unit 50.

In the lower portion of the second reactor (30), a liquid containing a salt dissociated with sulfur hexafluoride gas is collected. The collected liquid may again be introduced into the first reactor 20 and used to form the hydrate of sulfur hexafluoride gas in the first reactor 20. The salt existing in the liquid may be filtered through the filtration unit 40 and may be introduced into the first reactor 20 after the alkali component is replenished.

The recovered sulfur hexafluoride gas can be pressurized through the pressurizing portion to be charged in the heavy electricity. At this time, the pressure may be 2 to 5 bar. The pressurized sulfur hexafluoride gas may also be used to purge the first reactor 20 to remove the impurity gas.

Hereinafter, preferred embodiments and comparative examples of the present invention will be described. However, the following examples are only a preferred embodiment of the present invention, and the present invention is not limited to the following examples.

Example 1

For recovery of sulfur hexafluoride gas using hydrate, 0.3 mL of SDBS (sodium dodecylbenzenesulfonate) and 170 mL of an aqueous solution containing 1 wt% of NaOH were charged into a sealed 300 mL reactor, and 99.8% sulfur hexafluoride gas Lt; / RTI >

The initial operation was carried out while gradually lowering the temperature at 15 ° C and 17.5 bar. The hydrate formation reactor formed hydrate as the pressure dropped to about 1 bar at 1 ° C. When the temperature was raised to 15 ° C without regulating the pressure to regenerate the formed hydrate, the hydrate formed disappeared and the initial temperature pressure of 15 ° C was recovered to the level of 17.5 bar. That is, almost all of the sulfur hexafluoride trapped on the hydrate phase could be recovered.

Comparative Example 1

Comparative Example 1 was carried out in the same manner as in Example 1, but no aqueous solution was added. As the temperature was lowered, the pressure was lowered to 1 캜 and decreased to 12.2 bar, but the hydrate was not formed. When the temperature was raised to 15 ° C, the initial temperature was restored to 15.5 ° C, 17.5 bar.

FIG. 3 shows the temperature and pressure of Example 1 and Comparative Example 1 over time.

Example 2

In order to recover sulfur hexafluoride gas using hydrate, 0.3 mL of SDBS (sodium dodecylbenzenesulfonate) and 170 mL of an aqueous solution containing 2 wt% of NaOH were charged into a sealed 300 mL reactor, and 99.8% sulfur hexafluoride gas Lt; / RTI >

The initial operation was carried out while gradually lowering the temperature at 15 ° C and 17.5 bar. The hydrate formation reactor formed hydrate as the pressure dropped to about 1 bar at 1 ° C. When the temperature was raised to 15 ° C without regulating the pressure to regenerate the formed hydrate, the hydrate formed disappeared and the initial temperature pressure of 15 ° C was recovered to the level of 17.5 bar. That is, almost all of the sulfur hexafluoride trapped on the hydrate phase could be recovered.

Comparative Example 2

Comparative Example 2 was carried out in the same manner as in Example 2, but no aqueous solution was added. As the temperature was lowered, the pressure was lowered to 1 캜 and decreased to 12.2 bar, but the hydrate was not formed. When the temperature was raised to 15 ° C, the initial temperature was restored to 15.5 ° C, 17.5 bar.

FIG. 4 shows the temperature and pressure of Example 2 and Comparative Example 2 over time.

It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims. As will be understood by those skilled in the art. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.

10: recovery section 20: first reactor
30: second reactor 40: filtration device

Claims (22)

Recovering waste sulfur hexafluoride gas;
Pressurizing and cooling the recovered waste sulfur hexafluoride gas;
Adding an alkaline solution to the pressurized and cooled sulfur hexafluoride gas stream to form a hydrate and a salt of sulfur hexafluoride gas and to remove the impurity gas; And
Dissociating the hydrate of sulfur hexafluoride gas and removing water to recover the hexafluorosulfur gas;
And separating and recovering the sulfur hexafluoride gas. The method according to claim 1,
In the step of recovering the waste sulfur hexafluoride gas,
10 to 10,000 ppmv of HF, 10 to 1,000 ppmv of SO 2 , 0.1 to 5% by volume of N 2 , 10 to 5,000 ppmv of SOF 2 , 10 to 1,000 ppmv of SOF 4 , 0.1 to 5% by volume of O 2 , parts of separation and recovery method of SF6 gas containing SF 6. The method according to claim 1,
The step of pressurizing and cooling the recovered waste sulfur hexafluoride gas
And separating and recovering the sulfur hexafluoride gas to pressurize and recover the recovered waste sulfur hexafluoride gas at a pressure of 1 to 15 bar and a temperature of 0 to 10 ° C. The method according to claim 1,
In the step of forming the hydrate and the salt of sulfur hexafluoride gas and removing the impurity gas,
Wherein the impurity gas is HF, SO 2 , SOF 2, SOF 4 , N 2, and O 2 . The method according to claim 1,
The step of forming a hydrate and a salt of sulfur hexafluoride gas and removing the impurity gas
And adding 210 to 250 parts by weight of an alkaline solution to 100 parts by weight of the pressurized and cooled sulfur hexafluoride gas. The method according to claim 1,
Wherein the alkali solution comprises at least one alkaline component selected from the group consisting of NaOH, Ca (OH) 2 , CaO and MgO. The method according to claim 6,
A method for separating and recovering sulfur hexafluoride gas containing 0.1 to 10% by weight of the alkali component with respect to 100% by weight of the alkali solution. The method according to claim 1,
Wherein the alkali solution further comprises an anionic surfactant, a tetrahydrofuran or an ammonium salt. 9. The method of claim 8,
Wherein said anionic surfactant is sodium dodecylsulfate or linear alkylbenzene sulfonate. 9. The method of claim 8,
Wherein said ammonium salt is tetrabutylammonium bromide. 9. The method of claim 8,
Wherein the anionic surfactant, tetrahydrofuran or ammonium salt is added in an amount of 0.001 to 5% by weight based on 100% by weight of the alkali solution. The method according to claim 1,
And separating and recovering the sulfur hexafluoride gas dissociating the hydrate of the sulfur hexafluoride gas at a temperature of 15 to 50 캜. The method according to claim 1,
Further comprising the step of pressurizing the recovered sulfur hexafluoride gas to charge the heavy fuel cell. The method according to claim 1,
A method for separating and recovering sulfur hexafluoride gas which is used for filtration of a salt in a liquid in which sulfur hexafluoride gas is dissolved and for reusing the alkaline component to the hydrate of sulfur hexafluoride gas. A recovery unit for recovering waste sulfur hexafluoride gas;
A first reactor connected to the recovery unit, for pressurizing or cooling the recovered pulverized sulfur hexafluoride gas to form a hydrate of sulfur hexafluoride gas together with the alkali solution contained therein; And
A second reactor connected to the first reactor for receiving the hydrate of the sulfur hexafluoride gas and decompressing or raising the temperature to dissociate and separate the hexafluorosulfur gas;
And separating and recovering the sulfur hexafluoride gas. 16. The method of claim 15,
Wherein the alkali solution comprises at least one alkaline component selected from the group consisting of NaOH, Ca (OH) 2 , CaO and MgO. 16. The method of claim 15,
And 0.1 to 10% by weight of the alkali component with respect to 100% by weight of the alkali solution. 16. The method of claim 15,
Wherein the first reactor is maintained at a pressure of 1 to 15 bar and a temperature of 0 to 10 < 0 > C. 16. The method of claim 15,
The first reactor is composed of an upper part and a lower part, and the upper part collects and discharges the residual gas including N 2 and O 2 , and the lower part collects the hydrated liquid and transfers the liquid to the second reactor A device for separating and recovering sulfur fluoride gas. 16. The method of claim 15,
And the second reactor is maintained at a temperature of 15 to 50 ° C. 16. The method of claim 15,
And an upper portion of the second reactor is provided with a silica gel, a molecular sieve or zeolite. 16. The method of claim 15,
And a separator for separating and recovering the sulfur hexafluoride gas, which is supplied to the first reactor and replenishes the alkaline component, for filtering the salt in the collected liquid, .
KR1020150123512A 2015-09-01 2015-09-01 Apparatus and method for separation and recovery of hexafluorosulfide gas KR20170027068A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
KR20190079971A (en) * 2017-12-28 2019-07-08 한국전력공사 Hexafluorosulfide recovery system for electrical installation and hexafluorosulfide recovery method using the same
KR20200024036A (en) 2018-08-27 2020-03-06 한국전력공사 A sf6 refinement system and method including hybrid reactors utilizing gas hydrate formation
CN114397224A (en) * 2021-12-09 2022-04-26 河南省日立信股份有限公司 Sulfur hexafluoride gas recovery rate measuring device and measuring method

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20190079971A (en) * 2017-12-28 2019-07-08 한국전력공사 Hexafluorosulfide recovery system for electrical installation and hexafluorosulfide recovery method using the same
KR20200024036A (en) 2018-08-27 2020-03-06 한국전력공사 A sf6 refinement system and method including hybrid reactors utilizing gas hydrate formation
CN114397224A (en) * 2021-12-09 2022-04-26 河南省日立信股份有限公司 Sulfur hexafluoride gas recovery rate measuring device and measuring method
CN114397224B (en) * 2021-12-09 2024-05-14 河南省日立信股份有限公司 Sulfur hexafluoride gas recovery rate measuring device and measuring method

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