CN103848402B - Sulfur hexafluoride preparation method - Google Patents
Sulfur hexafluoride preparation method Download PDFInfo
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- CN103848402B CN103848402B CN201210497190.3A CN201210497190A CN103848402B CN 103848402 B CN103848402 B CN 103848402B CN 201210497190 A CN201210497190 A CN 201210497190A CN 103848402 B CN103848402 B CN 103848402B
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Abstract
The invention discloses a kind of sulfur hexafluoride preparation method, comprise the following steps: make fluorine gas and gaseous state sulfur reaction generate thick sulfur hexafluoride gas, thick sulfur hexafluoride gas carried out pyrolysis, washs, dewater, deacidify and rectification process, obtain sulfur hexafluoride product, product is detected, relevant treatment is carried out until obtain qualified product to the underproof sulfur hexafluoride product of detection, isolated for rectification process tail gas is reclaimed.The fluorine gas that the inventive method adopts electrolytic process to prepare and high-quality sulphur react as raw material, and the thick sulfur hexafluoride gas impurity of generation is few, saves purification procedures, decreases energy consumption; Does is the sulfur hexafluoride indices of preparation better than standard GB/T/T? 18867-2002 " For The Electronic Gases sulfur hexafluoride "; Tail gas is reclaimed, decreases pollution, add output; The unacceptable product of different situations is controlled.
Description
Technical field
The invention belongs to chemical production field, particularly relate to a kind of lithium sulphur preparing process.
Background technology
Sulfur hexafluoride at normal temperatures and pressures for colourless, odorless, nontoxic, non-corrosiveness, do not fire, inexplosive gas, molecular weight 146.06, density 6.139g/L, is about 5 times of air.Its chemical composition stability, be one of best gaseous substance of known chemical stability, its inertia is similar to nitrogen.It has fabulous thermostability, though under pure state more than 500 DEG C high temperature also do not decompose.Sulfur hexafluoride has remarkable electrical insulating property and arc quenching characteristic, and under normal pressure, its insulating power is more than 2.5 times of air, and its arc extinguishing ability is equivalent to 100 times of air under the same terms.In addition, under identical condition and compensator or trimmer pressure, SF
6corona voltage be 2 times of gas.
Because sulfur hexafluoride has the remarkable chemical property such as electrical insulating property, arc quenching characteristic, it is widely used in the aspects such as the isolating switch of electric installation, combiner, transformer, large container cable, thunder arrester, x ray machine, ion accelerator, tracer analysis and nonferrous smelting.Sulfur hexafluoride also can be used as to produce the fluorine source of mixing fluorine glass in optical fiber preparation, manufacturing the doping agent being used as sealing coat in low-loss high-quality single-mode fiber, also can be used as oozing of nitrogen excimer laser and adding gas.High-purity sulfur hexafluoride in the semiconductor manufacturing industry, also can be used as plasma etchant.
At present, lithium magister of sulfur generally adopts fluorine gas and sulfur reaction, and the thick sulfur hexafluoride gas that reaction generates obtains the product meeting demand of industrial production by continuous purifying.As CN201110215105.5, the method for purifying produced by a kind of sulfur hexafluoride, comprises the unit such as Reactive Synthesis, pyrolysis, alkali cleaning, absorption, rectifying, gasification and impurity recycling process.First fluorine gas and molten sulfur Reactive Synthesis sulfur hexafluoride crude product; Then through pyrolysis tower, pyrolytic decomposition S
2f
10, S
2f
10o; Acid and hydrolyzable impurity is removed through washing tower; Enter adsorption dry tower, remove moisture and the low fluorine sulphur compound of part; Two-stage compression rectification tower is utilized to remove light constituent impurity CF
4, THC, O
2, N
2and heavy seeds, finally obtain the product that sulfur hexafluoride content is at least 99.8%; Two-stage rectification bottom product vaporization after through 500 ~ 600 DEG C of thermal treaters or directly turn back to fluorine gas filling tube together with fluorine gas as raw material enter synthesis reactor participate in reaction.This technique exists following not enough: it is more that the raw material selected contains impurity, and the thick sulfur hexafluoride of generation needs two stage rectification, and operation is many, consumes energy; Two-stage rectification tower bottom product turns back to fluorine gas filling tube and participate in reaction as raw material together with fluorine gas after overflash, can make again the purity drop of the sulfur hexafluoride product next produced, add the difficulty of purification; The sulfur hexafluoride product purity obtained after two stage rectification is not high; The treatment process of tail gas and substandard product is not provided.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of sulfur hexafluoride preparation method, object reduces purification process, and preparation high-quality sulfur hexafluoride product, reclaims sulfur hexafluoride in tail gas, fast the qualified sulfur hexafluoride product of preparation.
In order to achieve the above object, the invention provides a kind of sulfur hexafluoride preparation method, be made up of following steps:
1) fluorine gas and gaseous state sulfur reaction is made to generate thick sulfur hexafluoride gas;
2) thick sulfur hexafluoride gas is carried out pyrolysis processing, removing is wherein containing S
2f
10and S
2f
10the toxic gas of O;
3) the thick sulfur hexafluoride gas after pyrolysis is carried out carrying out washing treatment, removing hydrolyzable impurity and acidic impurities;
4) the thick sulfur hexafluoride gas after carrying out washing treatment carried out except water treatment, except acid treatment and rectification process, obtain sulfur hexafluoride product, product sampling is detected, if detect qualified, then product is entered product storage tank; If detect defective, then carry out relevant treatment, to obtain qualified product.
5) isolated for rectification process tail gas is recycled, reclaim sulfur hexafluoride wherein.
Fluorine gas described in step 1) be by with potassium bifluoride melting salt for electrolytic solution, take anhydrous hydrogen fluoride as raw material, carry out middle warm therapy electrolysis produce.
The weight ratio of fluorine gas described in step 1) and gaseous state sulphur is 1.03-1.06:1, is preferably 1.05:1.
The temperature of reaction of reacting described in step 1) is 150 ~ 180 DEG C, and reaction pressure is-50 ~-100Pa.
Step 2) described in pyrolysis processing be carry out in pyrolysis tower, the temperature of pyrolysis tower is 380 ~ 420 DEG C, and pressure is-150 ~-200Pa.
Carrying out washing treatment described in step 3) is divided into washing process and alkali cleaning process, and wherein, washing process is carried out in water wash column, and water wash column temperature is 30 ~ 35 DEG C, and pressure is-200 ~-250Pa; Alkali cleaning process is carried out in soda-wash tower, and soda-wash tower temperature is 50 ~ 60 DEG C, and pressure is-250 ~-300Pa.
The water treatment that removes described in step 4) is divided into two portions: condensation dewaters and low pressure adsorbent dewaters, wherein, described low pressure adsorbent dewaters and to carry out in low pressure adsorbent tower, the pressure of low pressure adsorbent tower is-250 ~-300Pa, low pressure adsorbent tower selects silica gel as sorbent material, silica gel is by heating rear regeneration, and silica regeneration temperature is 120 DEG C.
Described in step 4) except acid treatment be carry out in High Pressure Absorption tower, the pressure of High Pressure Absorption tower is 1.8 ~ 2.0MPa, High Pressure Absorption tower adopt gac be sorbent material, gac is by heating rear regeneration, and regeneration of activated carbon temperature is 150 DEG C.
Rectification process described in step 4) is carried out in rectifying tower, and the temperature of tower bottom of rectifying tower is 15 ~ 17 DEG C, and the temperature of rectifying tower overhead condenser is-30 ~-35 DEG C, and Rectification column pressure is 1.8 ~ 2.0MPa.
Relevant treatment described in step 4) comprises one of following:
A) if the CF of product detected
4exceed standard with air, then underproof sulfur hexafluoride again rectifying is removed;
B) if detect, the hydrolyzable fluorochemical of product and acidity exceed standard, then underproof sulfur hexafluoride is relaundered removal;
C) if the S of product detected
2f
10o exceeds standard, then removed by underproof sulfur hexafluoride again pyrolysis.
As the sulphur of reaction raw materials and fluorine gas quality-controlling parameters as shown in Table 1 and Table 2.
Table 1 sulphur quality-controlling parameters
| Sequence number | Index name | Index (massfraction %) |
| 1 | Sulphur | ≥99.9 |
| 2 | Ash content | ≤0.05 |
| 3 | Organism | ≤0.05 |
Table 2 fluorine gas quality-controlling parameters
| Sequence number | Project | Index (volume fraction %) |
| 1 | Fluorine gas | ≥99.0 |
| 2 | Tetrafluoro-methane | ≤0.05 |
| 3 | Air (O 2+N 2) | ≤0.05 |
| 4 | Hydrogen fluoride | ≤0.5 |
Beneficial effect:
1. the present invention's fluorine gas of adopting electrolytic process to prepare and high-quality sulphur react as raw material, and the thick sulfur hexafluoride gas impurity of generation is few, save purification process, decrease energy consumption.
2. in the sulfur hexafluoride product prepared of the present invention, sulfur hexafluoride content is more than 99.99%, and indices is better than standard GB/T/T18867-2002 " For The Electronic Gases sulfur hexafluoride ".[GB/T18867-2002] standard of sulfur hexafluoride is in table 3.
Below table 3 For The Electronic Gases sulfur hexafluoride [GB/T18867-2002] technical indicator and specification requirement are taken passages:
| Project name | Index |
| Sulfur hexafluoride (SF 6) volume fraction/10 -2≥ | 99.99 |
| Volume fraction/10 of air -6≤ | 50.0 |
| Tetrafluoro-methane (CF 4) volume fraction/10 -6≤ | 15.0 |
| Humidity (H 2O) volume fraction/10 -6≤ | 8.0 |
| Volume fraction/10 of acidity (in HF) -6≤ | 1.0 |
| Volume fraction/10 of hydrolyzable fluorochemical (in HF) -6≤ | 1.0 |
| Other impurity (CO 2、C 2F 6、C 3F 8、SO 2F 2、S 2OF 2、S 2OF 10) volume fraction/10 -6≤ | 15.0 |
| Volume fraction/10 of impurity summation -6≤ | 100 |
3. the inventive method is prepared in sulfur hexafluoride process, reclaims, decreases pollution, add output to the sulfur hexafluoride in tail gas.
4. the inventive method is prepared in sulfur hexafluoride process, controls the sulfur hexafluoride unacceptable product of different situations.
Accompanying drawing explanation
Fig. 1 is preparation flow figure of the present invention.
Embodiment
Below in conjunction with accompanying drawing 1 and embodiment, the present invention is described in detail.
Embodiment 1
1) react
Fluorine gas and gaseous state sulphur are reacted in the reactor, produce thick sulfur hexafluoride gas, wherein, described fluorine gas be by with potassium bifluoride melting salt for electrolytic solution, take anhydrous hydrogen fluoride as raw material, carry out middle warm therapy electrolysis and produce, the weight ratio of described fluorine gas and gaseous state sulphur is 1.05:1, described temperature of reaction is 150 DEG C, and reaction pressure is-100Pa.
2) pyrolysis
The thick sulfur hexafluoride gas generated is passed into pyrolysis tower, and pyrolysis is removed containing S
2f
10, S
2f
10the toxic gas of O.Wherein, described pyrolysis tower temperature is 380 DEG C, and pressure is-150Pa.
3) wash
Thick sulfur hexafluoride gas after pyrolysis is passed into water wash column, the impurity that wherein can be hydrolyzed is hydrolyzed, thicker sulfur hexafluoride gas is passed into soda-wash tower afterwards, remove the acidic impurities in thick sulfur hexafluoride gas.Wherein, the temperature of described water wash column is 30 DEG C, and pressure is-200Pa; The KOH solution that massfraction is 15% is housed in described soda-wash tower, and soda-wash tower temperature is 50 DEG C, and pressure is-250Pa.
4) dewater, deacidify, rectifying
Thick sulfur hexafluoride gas after alkali cleaning is extracted out by molding machine, passes into condensation water eliminator, removing portion of water, then pass into low pressure adsorbent tower removing residual moisture.Wherein, described low pressure adsorbent tower is built with silica gel absorber, and silica gel absorber regenerates by the mode of heating, and regeneration temperature is 120 DEG C, and low pressure adsorbent pressure tower is-250Pa.
The thick sulfur hexafluoride gas of the remaining moisture of removing is extracted out with molding machine again, passes into High Pressure Absorption tower after pressurization, remove remaining acidic impurities.Wherein, described High Pressure Absorption tower is built with acticarbon, and acticarbon regenerates by the mode of heating, and regeneration temperature is 150 DEG C, and High Pressure Absorption pressure tower is 1.8MPa.
By High Pressure Absorption tower thick sulfur hexafluoride gas out, pass into rectifying tower and carry out rectification process, obtain sulfur hexafluoride product at tower bottom of rectifying tower.Wherein, described tower bottom of rectifying tower temperature is 15 DEG C, and overhead condensation actuator temperature is-30 DEG C, and pressure is 1.8MPa.
5) Product checking and filling
According to the detection method in GB/T18867-2002 " electronic-grade industrial gasses sulfur hexafluoride ", detect the sulfur hexafluoride that tower bottom of rectifying tower flows out, detected result shows that product is qualified, and product is entered product storage tank, carries out finished product and fills.The design parameter of the sulfur hexafluoride product of preparation is in table 4.
6) vent gas treatment
Rectifying tower is ejected the noncondensable gas come and pass into tail gas gathering device, after tail gas collecting, reclaim sulfur hexafluoride gas wherein, sulfur hexafluoride gas yield is 0.8 ton/month.
Embodiment 2
1) react
Fluorine gas and gaseous state sulphur are reacted in the reactor, generates thick sulfur hexafluoride gas.Wherein, described fluorine gas be by with potassium bifluoride melting salt for electrolytic solution, take anhydrous hydrogen fluoride as raw material, carry out middle warm therapy electrolysis produce, the weight ratio of described fluorine gas and gaseous state sulphur is 1.03:1, and described temperature of reaction is 180 DEG C, and reaction pressure is-50Pa.
2) pyrolysis
The thick sulfur hexafluoride gas generated is passed into pyrolysis tower, removes containing S
2f
10, S
2f
10the toxic gas of O.Wherein, described pyrolysis tower temperature is 420 DEG C, and pressure is-200Pa.
3) wash
By the thick sulfur hexafluoride gas after pyrolysis by water wash column, the impurity that wherein can be hydrolyzed is hydrolyzed, passes into soda-wash tower afterwards, the acidic impurities in thick sulfur hexafluoride gas is removed in neutralization.Wherein, the temperature of described water wash column is 31 DEG C, and pressure is-250Pa; The KOH solution that massfraction is 19% is housed in described soda-wash tower, and soda-wash tower temperature is 60 DEG C, and pressure is-300Pa.
4) dewater, deacidify, rectifying
Thick sulfur hexafluoride gas after alkali cleaning is extracted out by molding machine, passes into condensation water eliminator, removing portion of water, then pass into low pressure adsorbent tower, remove remaining moisture.Wherein, described low pressure adsorbent tower is built with silica gel absorber, and silica gel absorber regenerates by the mode of heating, and regeneration temperature is 120 DEG C, and low pressure adsorbent pressure tower is-260Pa.
The thick sulfur hexafluoride gas of removing residual moisture is extracted out with molding machine again, passes into High Pressure Absorption tower after pressurization, remove remaining acidic impurities.Wherein, described High Pressure Absorption tower is built with acticarbon, and acticarbon section is regenerated by the mode of heating, and regeneration temperature is 150 DEG C, and High Pressure Absorption pressure tower is 1.9MPa.
By High Pressure Absorption tower thick sulfur hexafluoride gas out, pass into rectifying tower and carry out rectifying, obtain sulfur hexafluoride product at tower bottom of rectifying tower.Wherein, described tower bottom of rectifying tower temperature is 17 DEG C, and overhead condensation actuator temperature is-35 DEG C, and pressure is 1.9Mpa.
5) Product checking and filling
According to the detection method in GB/T18867-2002 " electronic-grade industrial gasses sulfur hexafluoride ", detect the sulfur hexafluoride that tower bottom of rectifying tower flows out, detected result shows CF
4exceed standard, underproof sulfur hexafluoride is led back to rectifying tower, again after rectifying, again detect, product is qualified, and sulfur hexafluoride product is entered product storage tank, carries out finished product and fills.The design parameter of the sulfur hexafluoride product of preparation is in table 4.
6) vent gas treatment
Rectifying tower is ejected the noncondensable gas come and pass into tail gas gathering device, after tail gas collecting, reclaim sulfur hexafluoride gas wherein, sulfur hexafluoride gas yield is 0.9 ton/month.
Embodiment 3
1) react
Fluorine gas and gaseous state sulphur are reacted in the reactor, produces thick sulfur hexafluoride gas.Wherein, described fluorine gas be by with potassium bifluoride melting salt for electrolytic solution, take anhydrous hydrogen fluoride as raw material, carry out middle warm therapy electrolysis produce, the weight ratio of described fluorine gas and gaseous state sulphur is 1.04:1, and described temperature of reaction is 160 DEG C, and reaction pressure is-60Pa.
2) pyrolysis
The thick sulfur hexafluoride gas generated is passed into pyrolysis tower, removes containing S
2f
10, S
2f
10the toxic gas of O.Wherein, described pyrolysis tower temperature is 390 DEG C, and pressure is-160Pa.
3) wash
Thick sulfur hexafluoride gas after pyrolysis is passed into water wash column, and the impurity of enable hydrolysis is hydrolyzed, and passes into soda-wash tower afterwards, and the acidic impurities in thick sulfur hexafluoride gas is removed in neutralization.Wherein, the temperature of described water wash column is 32 DEG C, and pressure is-210Pa; The KOH solution that massfraction is 16% is housed in described soda-wash tower, and described soda-wash tower temperature is 55 DEG C, and pressure is-260Pa.
4) dewater, deacidify, rectifying
Thick sulfur hexafluoride gas after alkali cleaning is extracted out by molding machine, passes into condensation water eliminator, removing portion of water, then pass into low pressure adsorbent tower, remove remaining moisture.Wherein, described low pressure adsorbent tower is built with silica gel absorber, and silica gel absorber section is regenerated by the mode of heating, and regeneration temperature is 120 DEG C, and low pressure adsorbent pressure tower is-270Pa.
Low pressure adsorbent tower thick sulfur hexafluoride gas is out extracted out with molding machine again, passes into High Pressure Absorption tower after pressurization, remove remaining acidic impurities.Wherein, described High Pressure Absorption tower is built with acticarbon, and acticarbon regenerates by the mode of heating, and regeneration temperature is 150 DEG C, and High Pressure Absorption pressure tower is 1.8MPa.
By High Pressure Absorption tower thick sulfur hexafluoride gas out, pass into rectifying tower and carry out rectifying, obtain sulfur hexafluoride product at tower bottom of rectifying tower.Wherein said tower bottom of rectifying tower temperature is 16 DEG C, and overhead condensation actuator temperature is-32 DEG C, and pressure is 1.8Mpa.
5) Product checking and filling
According to the detection method in GB/T18867-2002 " electronic-grade industrial gasses sulfur hexafluoride ", the sulfur hexafluoride that tower bottom of rectifying tower flows out is detected, detected result shows that air exceeds standard, underproof sulfur hexafluoride is led back to rectifying tower, again after rectifying, again detect, product is qualified, product is entered product storage tank, carries out finished product and fill.The design parameter of the sulfur hexafluoride product of preparation is in table 4.
6) vent gas treatment
Rectifying tower is ejected the noncondensable gas come and pass into tail gas gathering device, after tail gas collecting, the sulfur hexafluoride gas of recovery is 0.85 ton/month.
Embodiment 4
1) react
Fluorine gas and gaseous state sulphur are reacted in the reactor, generates thick sulfur hexafluoride gas.Wherein said fluorine gas be by with potassium bifluoride melting salt for electrolytic solution, take anhydrous hydrogen fluoride as raw material, carry out middle warm therapy electrolysis produce, the weight ratio of described fluorine gas and gaseous state sulphur is 1.05:1, and described temperature of reaction is 170 DEG C, and reaction pressure is-70Pa.
2) pyrolysis
The thick sulfur hexafluoride gas generated is passed into pyrolysis tower, removes containing S
2f
10, S
2f
10the toxic gas of O.Wherein, described pyrolysis tower temperature is 400 DEG C, and pressure is-170Pa.
3) wash
Thick sulfur hexafluoride gas after pyrolysis is passed into water wash column, and the impurity of enable hydrolysis is hydrolyzed, and passes into soda-wash tower afterwards, and the acidic impurities in thick sulfur hexafluoride gas is removed in neutralization.Wherein, the temperature of described water wash column is 33 DEG C, and pressure is-220Pa; Described soda-wash tower temperature is 60 DEG C, and pressure is-270Pa, and the KOH solution that massfraction is 15% is housed in soda-wash tower.
4) dewater, deacidify, rectification process
Thick sulfur hexafluoride gas after alkali cleaning is extracted out by molding machine, passes into condensation water eliminator, removing portion of water, then pass into low pressure adsorbent tower, remove remaining moisture.Wherein, described low pressure adsorbent tower is built with silica gel absorber, and silica gel absorber regenerates by the mode of heating, and regeneration temperature is 120 DEG C, and low pressure adsorbent pressure tower is-280Pa.
Low pressure adsorbent tower thick sulfur hexafluoride gas is out extracted out with molding machine again, passes into High Pressure Absorption tower after pressurization, remove remaining acidic impurities.Wherein, described High Pressure Absorption tower is built with acticarbon, and acticarbon regenerates by the mode of heating, and regeneration temperature is 150 DEG C, and High Pressure Absorption pressure tower is 2.0Mpa.
By High Pressure Absorption tower thick sulfur hexafluoride gas out, pass into rectifying tower and carry out rectifying, obtain sulfur hexafluoride product at tower bottom of rectifying tower.Wherein, described tower bottom of rectifying tower temperature is 15 DEG C, and overhead condensation actuator temperature is-33 DEG C, and pressure is 2.0Mpa.
5) Product checking and filling
According to the detection method in GB/T18867-2002 " electronic-grade industrial gasses sulfur hexafluoride ", the sulfur hexafluoride product that tower bottom of rectifying tower flows out is detected, result shows, hydrolyzable fluorochemical exceeds standard, and underproof sulfur hexafluoride is led back to water wash column, after relaundering, again detect, product is qualified, and sulfur hexafluoride product is entered product storage tank, carries out finished product and fills.The design parameter of the sulfur hexafluoride product of preparation is in table 4.
6) vent gas treatment
Rectifying tower is ejected the gas come and pass into tail gas gathering device, after tail gas collecting, the sulfur hexafluoride gas of recovery is 1.0 tons/month.
Embodiment 5
1) react
Fluorine gas and gaseous state sulphur are reacted in the reactor, generates thick sulfur hexafluoride gas.Wherein, described fluorine gas be by with potassium bifluoride melting salt for electrolytic solution, take anhydrous hydrogen fluoride as raw material, carry out middle warm therapy electrolysis produce, the weight ratio of described fluorine gas and gaseous state sulphur is 1.06:1, and described temperature of reaction is 180 DEG C, and reaction pressure is-80Pa.
2) pyrolysis
The thick sulfur hexafluoride gas generated is passed into pyrolysis tower, removes containing S
2f
10, S
2f
10the toxic gas of O.Wherein, described pyrolysis tower temperature is 410 DEG C, and pressure is-180Pa.
3) wash
Thick sulfur hexafluoride gas after pyrolysis is passed into water wash column, and the impurity of enable hydrolysis is hydrolyzed, and passes into soda-wash tower afterwards, and the acidic impurities in thick sulfur hexafluoride gas is removed in neutralization.Wherein, the temperature of described hydrolysis tower is 34 DEG C, and pressure is-230Pa, and the KOH solution that massfraction is 15% is housed in described soda-wash tower, and soda-wash tower temperature is 50 DEG C, and pressure is-280Pa.
4) dewater, deacidify, rectifying
Thick sulfur hexafluoride gas after alkali cleaning is extracted out by molding machine, passes into condensation water eliminator, removing portion of water, then enter low pressure adsorbent tower, remove remaining moisture.Wherein, described low pressure adsorbent tower is built with silica gel absorber, and silica gel absorber regenerates by the mode of heating, and regeneration temperature is 120 DEG C, and low pressure adsorbent pressure tower is-290Pa.
Low pressure adsorbent tower thick sulfur hexafluoride gas is out extracted out with molding machine again, passes into High Pressure Absorption tower after pressurization, remove remaining acidic impurities.Wherein, described High Pressure Absorption tower is built with acticarbon, and acticarbon regenerates by the mode of heating, and regeneration temperature is 150 DEG C, and High Pressure Absorption pressure tower is 1.8MPa.
By High Pressure Absorption tower thick sulfur hexafluoride gas out, pass into rectifying tower and carry out rectifying, obtain sulfur hexafluoride product at tower bottom of rectifying tower.Wherein, described tower bottom of rectifying tower temperature is 15 DEG C, and overhead condensation actuator temperature is-34 DEG C, and pressure is 1.8Mpa.
5) Product checking and filling
According to the detection method in GB/T18867-2002 " electronic-grade industrial gasses sulfur hexafluoride ", the sulfur hexafluoride that tower bottom of rectifying tower flows out is detected, result shows that acidity exceeds standard, underproof sulfur hexafluoride is led back to soda-wash tower, again after alkali cleaning, again detect, product is qualified, sulfur hexafluoride product is entered product storage tank, carries out finished product and fill.The design parameter of the sulfur hexafluoride product of preparation is in table 4.
6) vent gas treatment
Rectifying tower is ejected the gas come and pass into tail gas gathering device, after tail gas collecting, the sulfur hexafluoride gas of recovery is 1.0 tons/month.
Embodiment 6
1) react
Fluorine gas and gaseous state sulphur are reacted in the reactor, generates thick sulfur hexafluoride gas.Wherein, described fluorine gas be by with potassium bifluoride melting salt for electrolytic solution, take anhydrous hydrogen fluoride as raw material, carry out middle warm therapy electrolysis produce, the weight ratio of described fluorine gas and gaseous state sulphur is 1.05:1, and described temperature of reaction is 160 DEG C, and reaction pressure is-90Pa.
2) pyrolysis
The thick sulfur hexafluoride gas generated is passed into pyrolysis tower, removes containing S
2f
10, S
2f
10the toxic gas of O.Wherein, described pyrolysis tower temperature is 420 DEG C, and pressure is-190Pa.
3) wash
Thick sulfur hexafluoride gas after pyrolysis is passed into water wash column, and the impurity of enable hydrolysis is hydrolyzed, and passes into soda-wash tower afterwards, and the acidic impurities in thick sulfur hexafluoride gas is removed in neutralization.Wherein, the temperature of described water wash column is 35 DEG C, and pressure is-240Pa; The KOH solution that massfraction is 20% is housed in described soda-wash tower, and soda-wash tower temperature is 55 DEG C, and pressure is-290Pa.
4) dewater, deacidify, rectification process
Thick sulfur hexafluoride gas after alkali cleaning is extracted out by molding machine, passes into condensation water eliminator, removing portion of water, then pass into low pressure adsorbent tower, remove remaining moisture.Wherein, described low pressure adsorbent tower is built with silica gel absorber, and silica gel absorber regenerates by the mode of heating, and regeneration temperature is 120 DEG C, and low pressure adsorbent pressure tower is-300Pa.
Low pressure adsorbent tower thick sulfur hexafluoride gas is out extracted out with molding machine again, passes into High Pressure Absorption tower after pressurization, remove remaining acidic impurities.Wherein, described High Pressure Absorption tower is built with acticarbon, and acticarbon regenerates by the mode of heating, and regeneration temperature is 150 DEG C, and High Pressure Absorption pressure tower is 1.8MPa.
By High Pressure Absorption tower thick sulfur hexafluoride gas out, pass into rectifying tower and carry out rectifying, obtain sulfur hexafluoride product at tower bottom of rectifying tower.Wherein, described tower bottom of rectifying tower temperature is 15 DEG C, and overhead condensation actuator temperature is-35 DEG C, and pressure is 1.8Mpa.
5) Product checking and filling
According to the detection method in GB/T18867-2002 " electronic-grade industrial gasses sulfur hexafluoride ", detect the sulfur hexafluoride that tower bottom of rectifying tower flows out, result shows S
2oF
10exceed standard, lead back to pyrolysis tower to by underproof sulfur hexafluoride, again after pyrolysis, again detect, product is qualified, and product is entered product storage tank, carries out finished product and fills.The design parameter of the sulfur hexafluoride product of preparation is in table 4.
6) vent gas treatment
Rectifying tower is ejected the gas come and pass into tail gas gathering device, after tail gas collecting, the sulfur hexafluoride gas of recovery is 0.95 ton/month.
The design parameter of sulfur hexafluoride product prepared by table 4: embodiment 1-6
As can be seen from Table 4, in sulfur hexafluoride product prepared by the present invention, sulfur hexafluoride (SF
6) volume fraction/10
-2>=99.992, volume fraction/10 of air
-6≤ 48, tetrafluoro-methane (CF
4) volume fraction/10
-6≤ 14, humidity (H
2o) volume fraction/10
-6≤ 7.1; Volume fraction/10 of acidity (in HF)
-6≤ 0.9; Volume fraction/10 of hydrolyzable fluorochemical (in HF)
-6≤ 0.9; Other impurity (CO
2, C
2f
6, C
3f
8, SO
2f
2, S
2oF
2, S
2oF
10) volume fraction/10
-6≤ 14, sulfur hexafluoride indices prepared by the present invention is all better than standard GB/T/T18867-2002 " For The Electronic Gases sulfur hexafluoride ".
Above content is the further description done the present invention in conjunction with optimal technical scheme, can not assert that the concrete enforcement of invention is only limitted to these explanations.Concerning general technical staff of the technical field of the invention, under the prerequisite not departing from design of the present invention, simple deduction and replacement can also be made, all should be considered as protection scope of the present invention.
Claims (7)
1. a sulfur hexafluoride preparation method, is characterized in that, comprises the following steps:
1) fluorine gas and gaseous state sulfur reaction is made to generate thick sulfur hexafluoride gas;
2) thick sulfur hexafluoride gas is carried out pyrolysis processing, removing is wherein containing S
2f
10and S
2f
10the toxic gas of O;
3) the thick sulfur hexafluoride gas after pyrolysis is carried out carrying out washing treatment, removing hydrolyzable impurity and acidic impurities;
4) the thick sulfur hexafluoride gas after washing carried out except water treatment, except acid treatment and rectification process, obtain sulfur hexafluoride product, product sampling is detected, if detect qualified, then product is entered product storage tank; If detect defective, then carry out relevant treatment, to obtain qualified product;
5) isolated for rectification process tail gas is recycled, reclaim sulfur hexafluoride wherein;
Wherein, described carrying out washing treatment is divided into washing process and alkali cleaning process, and wherein, described washing process is carried out in water wash column, and water wash column temperature is 30 ~ 35 DEG C, and pressure is-200 ~-250Pa; Described alkali cleaning process is carried out in soda-wash tower, and soda-wash tower temperature is 50 ~ 60 DEG C, and pressure is-250 ~-300Pa;
Wherein, the described water treatment that removes is divided into two portions: condensation dewaters and low pressure adsorbent dewaters, wherein, described low pressure adsorbent dewaters and to carry out in low pressure adsorbent tower, the pressure of low pressure adsorbent tower is-250 ~-300Pa, and low pressure adsorbent tower selects silica gel as sorbent material, and silica gel is by heating rear regeneration;
Wherein, described except acid treatment be carry out in High Pressure Absorption tower, the pressure of High Pressure Absorption tower is 1.8 ~ 2.0MPa, and High Pressure Absorption tower adopts gac to be sorbent material, and gac is by heating rear regeneration.
2. the method for claim 1, is characterized in that, step 1) described in fluorine gas be by with potassium bifluoride melting salt for electrolytic solution, take anhydrous hydrogen fluoride as raw material, carry out middle warm therapy electrolysis produce.
3. the method for claim 1, is characterized in that, step 1) described in the weight ratio of fluorine gas and gaseous state sulphur be 1.03-1.06:1.
4. the method for claim 1, is characterized in that, step 1) described in reaction temperature of reaction be 150 ~ 180 DEG C, reaction pressure is-50 ~-100Pa.
5. the method for claim 1, is characterized in that, step 2) described in pyrolysis processing be carry out in pyrolysis tower, the temperature of pyrolysis tower is 380 ~ 420 DEG C, and pressure is-150 ~-200Pa.
6. the method for claim 1, it is characterized in that, step 4) described in rectification process be carry out in rectifying tower, the temperature of tower bottom of rectifying tower is 15 ~ 17 DEG C, the temperature of rectifying tower overhead condenser is-30 ~-35 DEG C, and Rectification column pressure is 1.8 ~ 2.0MPa.
7. the method for claim 1, is characterized in that, step 4) described in relevant treatment comprise one of following:
A) if the CF of product detected
4exceed standard with air, then underproof sulfur hexafluoride again rectifying is removed;
B) if detect, the hydrolyzable fluorochemical of product and acidity exceed standard, then underproof sulfur hexafluoride is relaundered removal;
C) if the S of product detected
2f
10o exceeds standard, then removed by underproof sulfur hexafluoride again pyrolysis.
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| CN111470478B (en) * | 2020-04-29 | 2021-07-23 | 福建德尔科技有限公司 | High-purity sulfur hexafluoride and preparation method thereof |
| CN111470479A (en) * | 2020-04-29 | 2020-07-31 | 福建德尔科技有限公司 | Purification method of crude sulfur hexafluoride |
| CN113307232A (en) * | 2021-05-20 | 2021-08-27 | 洛阳森蓝化工材料科技有限公司 | Preparation and separation method of sulfur hexafluoride and sulfur tetrafluoride mixed gas |
| CN114873568B (en) * | 2022-04-11 | 2022-11-11 | 福建德尔科技股份有限公司 | Electronic grade SF 6 Rectification pretreatment system |
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| CN102328913A (en) * | 2011-07-29 | 2012-01-25 | 天津市泰亨气体有限公司 | Method for producing and purifying sulfur hexafluoride |
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