CN104386652B - Sulfur hexafluoride recovery processing technique - Google Patents

Sulfur hexafluoride recovery processing technique Download PDF

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CN104386652B
CN104386652B CN201410637349.6A CN201410637349A CN104386652B CN 104386652 B CN104386652 B CN 104386652B CN 201410637349 A CN201410637349 A CN 201410637349A CN 104386652 B CN104386652 B CN 104386652B
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content
fluoride
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sulfur hexafluoride
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CN104386652A (en
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刘静涛
李小明
曹勇
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/45Compounds containing sulfur and halogen, with or without oxygen
    • C01B17/4507Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only
    • C01B17/4515Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only containing sulfur and fluorine only
    • C01B17/453Sulfur hexafluoride
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00Purification or separation of specific gases
    • C01B2210/0001Separation or purification processing
    • C01B2210/0003Chemical processing

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

The invention discloses sulfur hexafluoride recovery processing technique, this process technique by adding thermal cracking, multi-stage water wash, multistage alkali cleaning, pressure-variable adsorption, rectification step form, the sulfur hexafluoride obtained by the application recovery processing technique, its purity is more than 99.999%, industrial gas sulfur hexafluoride GB/T12022 2014 standard and Electronic Gases sulfur hexafluoride GB/T18867 xxxx (paper for approval) standard are reached, improve the quality of sulfur hexafluoride in existing recycling technology, extend its application performance in electronics industry.

Description

Sulfur hexafluoride recovery processing technique
Technical field
The present invention relates to gas recovery processing technique, be specifically related to the recovery processing technique of sulfur hexafluoride gas.
Background technology
In power industry, sulfur hexafluoride (SF6) gas is with its high insulation resistance, high arc extinguishing ability and highly thermally conductive Property, be widely used in insulation and the arc extinguishing of electric equipment, the performance of its brilliance achieve electric device economization and The low-maintenance of operation.
But existing current sulphur hexafluoride gas purity is not enough, and also can be difficult to avoid that in the running of electrical equipment Ground produces other impurity, and these gaseous impurities have hazardness to operation equipment, as in the presence of water vapor, and SF6 Catabolite generation hydrolysis, hinders SF6Being combined of catabolite, reduces SF6Medium recovery strength, Thus reduce the insulation characterisitic of equipment;SF6Catabolite can with steam, oxygen, metal vapors and arc-chutes its The biochemical reaction of pyrolytic produce of its material, the fluorination sulfurous acid of generation and Fluohydric acid. have severe toxicity, can corrode electricity Pole and insulant;Many carbon fluoride (C in gas2F6、C3F8) under high voltages, it is possible to create simple substance carbon, Form equipment surface carbon distribution, insulating properties are worked the mischief;It is right that fluorination sulfonyl in gas can cause after entering air Human body and the harm of environment.
Common practice is to be periodically detected operation sulfur hexafluoride gas, changes and is unsatisfactory for electric equipment operation The sulfur hexafluoride of safety condition runs gas, will recycle in used sulfur hexafluoride gas, but existing The recycling ability of the recovery and processing system of sulfur hexafluoride is the least, the sulfur hexafluoride gas matter after on-the-spot recycling Amount does not reaches GB/T12022-2014 standard, and Practical Performance is poor.
Summary of the invention
In view of this, this application provides sulfur hexafluoride recovery processing technique, the sulfur hexafluoride quality after recycling Industrial gas sulfur hexafluoride GB/T12022-2014 standard and Electronic Gases sulfur hexafluoride can be reached GB/T18867-xxxx (paper for approval) standard, sulfur hexafluoride purity reaches 99.999%, and its practicality is greatly improved.
For solving above technical problem, the technical scheme that the present invention provides is the recovery processing technique of sulfur hexafluoride, by Following steps form:
(1) add thermal cracking: sulfur hexafluoride waste gas is passed through pyrolysis oven, be warming up to 200 450 DEG C at ambient pressure and carry out Cracking, obtains mixed gas A;This step is for by the S in waste gas2F10、S2OF10It is cracked into SF6、SOF4、SF4, Wherein SF6For the purpose of product, SOF4、SF4Available washing alkali cleaning removes;
(2) washing: carry out multi-stage water wash by after mixed gas A pass-out, control the ladder of fluoride in cleaning mixture at different levels Secondary content, obtains mixed gas B;HF in waste gas can be removed by this step, and subfluoride is converted into fluorine sulfur Oxygen compound;
(3) alkali cleaning: carry out multistage alkali cleaning by after mixed gas B pass-out, controls the echelon concentration of alkali liquor at different levels, fluorine The content of compound, obtains mixed gas C;Fluorine oxygen sulfur compound in upper step can be removed by this step;
By above step, the composition of mixed gas C obtained and content it is: SF6> 95%, moisture content: 1%, N2+O2: 3%, other: 1%;
(4) pressure-variable adsorption:
A, mixed gas C is pressurized to 0.25 0.30Mpa, carries out multistage silica gel adsorption, multistage three at normal temperatures Al 2 O absorption, multistage fluorine adsorbent;After this step, composition and the content of mixed gas is: SF6 > 96%, moisture content: < 30ppm, N2+O2: 3%, other: < 1%;
B, a step gained mixed gas is pressurized to 1.2 1.9Mpa, carries out multistage aluminium sesquioxide at normal temperatures Absorption, multistage fluorine adsorbent, multistage 13X molecular sieve adsorption, obtain mixed gas D;
(5) rectification: by mixed gas D at 1.2 1.9Mpa pressure, be condensed into gas-liquid at a temperature of-45-30 DEG C After mixture, being passed through light point of tower, described light point of tower tower pressure is 1.2 1.9Mpa, and tower top temperature is-55-50 DEG C, Bottom temperature is 18 25 DEG C;To gently divide tower tower bottoms to be passed through Chong Fenta mutually, described heavy point of tower tower pressure is 0.8 1.2 Mpa, tower top temperature is-23-12 DEG C, and bottom temperature is-4 5 DEG C;Tower tower reactor gas phase will be heavily divided to be passed through dealkylation tower, Described dealkylation tower tower pressure is 0.6 0.9Mpa, and tower top temperature is-28-18 DEG C, and bottom temperature is-25-15 DEG C, Described dealkylation tower tower reactor derives liquid phase and is the sulfur hexafluoride processed, and the purity of described sulfur hexafluoride is more than 99.999%.
Wherein, light point of column overhead derives consisting of of gas: SF6< 20%, N2+O2+CF4> 80%, tower reactor is led Go out consisting of of liquid: SF6> 99.9%, N2+O2+CF4< 10ppm, C2F6Deng heavy component < 500ppm;
Wherein, heavily point column overhead derives consisting of of gas: SF6> 99.998%, C2F6< 50ppm, tower reactor is led Go out SF in liquid6< 60%;
Wherein, dealkylation tower tower top derives consisting of of gas: SF6< 99.95%, C2F6< 500ppm, tower reactor is led Go out liquid by being filled into steel cylinder after metering, consisting of: SF6> 99.999%, other component: < 10ppm.
Preferably, described water-washing step is made up of 5 grades of washings, controls the echelon content of fluoride in cleaning mixture and is: One-level content of fluoride: 25% 50%, two grades of content of fluoride: 10% 25%, three grades of content of fluoride: 5% 10%, level Four content of fluoride: 1% 5%, Pyatyi content of fluoride: 0% 1%.
Preferably, described caustic scrubbing step is made up of 7 grades of alkali cleanings, controls the echelon concentration of alkali liquor at different levels and fluoride Content is: one-level concentration of lye: 15% 40%, one-level content of fluoride: 0 1%;Two grades of concentration of lye: 12% 15%, two grades of content of fluoride: 0 1%;Three grades of concentration of lye: 8% 12%, three grades of fluorides contain Amount: 0 1%;Level Four concentration of lye: 5% 8%, level Four content of fluoride: 0 1%;Pyatyi concentration of lye: 5% 8%, Pyatyi content of fluoride: 0 1%;Six grades of concentration of lye: 3% 5%, six grades of content of fluoride: 0 1%;Seven grades of concentration of lye: 1% 3%, seven grades of content of fluoride: 0 1%.
Preferably, in described caustic scrubbing step, alkali liquor is the aqueous solution of potassium hydroxide.
Preferably, in a step of described pressure-variable adsorption, silica gel adsorption is divided into 1 section or 2 sections absorption, three oxidations two Aluminum is adsorbed as 1 section of absorption, and fluorine adsorbent is 1 section of absorption.
Preferably, in the b step of described pressure-variable adsorption, aluminium sesquioxide is adsorbed as 1 section or 2 sections absorption, and fluorine is inhaled Attached dose is adsorbed as 1 section of absorption, and 13X molecular sieve adsorption is 1 section or 2 sections absorption.
Preferably, in described rectification step, light Fen Ta, Chong Fenta, the overhead condenser coolant of dealkylation tower are alcohols, Tower reactor reboiler heating agent is the hydrate of alcohols.
Being more highly preferred to, in described rectification step, light Fen Ta, Chong Fenta, the overhead condenser coolant of dealkylation tower are one Unit's alcohol, tower reactor reboiler heating agent is the hydrate of monohydric alcohol.
Preferably, described step can also wash, alkali cleaning, add thermal cracking, alkali cleaning, pressure-variable adsorption, rectification suitable Sequence is carried out successively.
Compared with prior art, its detailed description is as follows for the application: the sulfur hexafluoride recycling work that the application provides Skill, by cracking, multi-stage water wash, multistage alkali cleaning, pressure-variable adsorption, the step of rectification, it is possible to make to finally obtain The purity of sulfur hexafluoride product reaches more than 99.999%, and gas reaches industrial gas sulfur hexafluoride GB/T12022- 2014 standards and Electronic Gases sulfur hexafluoride GB/T18867-xxxx (paper for approval) standard, add its Electrical equipment and the application in electronics industry, solve the problem that in existing recycling technology, sulfur hexafluoride purity is inadequate.
Detailed description of the invention
In order to make those skilled in the art be more fully understood that technical scheme, below in conjunction with specific embodiment The present invention is described in further detail.
Embodiment one
The recovery processing technique of sulfur hexafluoride, comprises the steps of:
(1) add thermal cracking: sulfur hexafluoride waste gas is passed through pyrolysis oven, be warming up to 200 450 DEG C at ambient pressure and carry out Cracking, obtains mixed gas A;
(2) washing: will carry out 5 grades of washings after mixed gas A pass-out, controls the echelon of fluoride in cleaning mixture and contains Amount is: one-level content of fluoride: 25% 50%, two grades of content of fluoride: 10% 25%, and three grades of fluorides contain Amount: 5% 10%, level Four content of fluoride: 1% 5%, Pyatyi content of fluoride: 0% 1%, obtain mixing Gas B;
(3) alkali cleaning: 7 grades of alkali cleanings will be carried out after mixed gas B pass-out, alkali liquor uses the aqueous solution of potassium hydroxide, The content of the echelon concentration and fluoride that control alkali liquor at different levels is: one-level concentration of lye: 15% 40%, one-level fluorine U content: 0 1%;Two grades of concentration of lye: 12% 15%, two grades of content of fluoride: 0 1%;Three grades of alkali Liquid concentration: 8% 12%, three grades of content of fluoride: 0 1%;Level Four concentration of lye: 5% 8%, level Four fluorine U content: 0 1%;Pyatyi concentration of lye: 5% 8%, Pyatyi content of fluoride: 0 1%;Six grades of alkali liquor Concentration: 3% 5%, six grades of content of fluoride: 0 1%;Seven grades of concentration of lye: 1% 3%, seven grades of fluorides Content: 0 1%;
By above step, the composition of mixed gas C obtained and content it is: SF6> 95%, moisture content: 1%, N2+O2: 3%, other: 1%;
(4) pressure-variable adsorption:
A, mixed gas C is pressurized to 0.25 0.30Mpa, carry out at normal temperatures 2 sections of silica gel adsorptions, 1 section three Al 2 O absorption, 1 section of fluorine adsorbent;After this step, composition and the content of mixed gas is: SF6 > 96%, moisture content: < 30ppm, N2+O2: 3%, other: < 1%;
B, a step gained mixed gas is pressurized to 1.2 1.9Mpa, carries out multistage aluminium sesquioxide at normal temperatures Absorption, multistage fluorine adsorbent, multistage 13X molecular sieve adsorption, obtain mixed gas D;Mix after this step Close the composition of gas D and content is: SF6> 97%, moisture content: < 20ppm, N2+O2: < 3%, other: < 500ppm。
(5) rectification: by mixed gas D at 1.2 1.9Mpa pressure, be condensed into gas-liquid at a temperature of-45-30 DEG C After mixture, being passed through light point of tower, a light point tower tower pressure is 1.2 1.9Mpa, and tower top temperature is-55-50 DEG C, tower reactor Temperature is 18 25 DEG C, and light point of column overhead derives consisting of of gas: SF6< 20%, N2+O2+CF4> 80%, Tower reactor derives consisting of of liquid: SF6> 99.9%, N2+O2+CF4< 10ppm, C2F6Deng heavy component < 500ppm; To gently divide tower tower bottoms to be passed through Chong Fenta mutually, heavily dividing tower tower pressure is 0.8 1.2Mpa, and tower top temperature is-23-12 DEG C, Bottom temperature is-4 5 DEG C, and heavily point column overhead derives consisting of of gas: SF6> 99.998%, C2F6< 50ppm, Tower reactor derives SF in liquid6< 60%;To heavily divide tower tower reactor gas phase to be passed through dealkylation tower, dealkylation tower tower pressure is 0.6 0.9Mpa, tower top temperature is-28-18 DEG C, and bottom temperature is-25-15 DEG C, and dealkylation tower tower top derives the group of gas Become: SF6< 99.95%, C2F6< 500ppm, tower reactor derivation liquid is by being filled into steel cylinder after metering, and it forms For: SF6> 99.999%, other component: < 10ppm, this dealkylation tower tower reactor derivation liquid phase is and has recycled The sulfur hexafluoride product become.
Sulfur hexafluoride product recycling completed carries out composition and content detection, testing result and industrial gas Sulfur hexafluoride GB/T12022-2014 standard and Electronic Gases sulfur hexafluoride GB/T18867-xxxx (declaration Original text) contrast of standard is as follows:
Table 1 embodiment one testing result and the contrast table of GB/T12022-2014
As known from Table 1, the sulfur hexafluoride product obtained by the sulfur hexafluoride recovery processing technique of the application, its purity More than 99.999%, it is much better than in GB/T12022-2014 the sulfur hexafluoride purity rubric of regulation, and other are every Index has also reached this national standard, adds its application in electrical industry, solves existing recycling The problem that in technology, sulfur hexafluoride purity is inadequate.
Table 2 embodiment one testing result and the contrast table of GB/T18867-XXXX
As known from Table 2, the sulfur hexafluoride product obtained by the sulfur hexafluoride recovery processing technique of the application, its purity More than 99.999%, and other indices also reach Electronic Gases sulfur hexafluoride GB/T18867- XXXX standard, improves application performance, has expanded range of application and the market space.
Below it is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred implementation is not construed as Limitation of the present invention, protection scope of the present invention should be as the criterion with claim limited range.For this skill For the those of ordinary skill in art field, without departing from the spirit and scope of the present invention, it is also possible to make some changing Entering and retouch, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (7)

1. sulfur hexafluoride recovery processing technique, it is characterised in that: described process technique comprises the steps of:
(1) add thermal cracking: sulfur hexafluoride waste gas is passed through pyrolysis oven, be warming up to 200 450 DEG C at ambient pressure and crack, obtain mixed gas A;
(2) washing: carry out multi-stage water wash by after mixed gas A pass-out, control the echelon content of fluoride in cleaning mixture at different levels, obtain mixed gas B;
(3) alkali cleaning: carry out multistage alkali cleaning by after mixed gas B pass-out, controls the echelon concentration of alkali liquor at different levels, the content of fluoride, obtains mixed gas C;
(4) pressure-variable adsorption:
A, mixed gas C is pressurized to 0.25 0.30MPa, carries out multistage silica gel adsorption, the absorption of multistage aluminium sesquioxide, multistage fluorine adsorbent at normal temperatures;
B, a step gained mixed gas is pressurized to 1.2 1.9MPa, carries out multistage aluminium sesquioxide absorption, multistage fluorine adsorbent, multistage 13X molecular sieve adsorption at normal temperatures, obtain mixed gas D;
(5) rectification: by mixed gas D at 1.2 1.9MPa pressure, be condensed into gas-liquid mixture at a temperature of-45-30 DEG C after, be passed through light point of tower, described light point of tower tower pressure is 1.2 1.9MPa, and tower top temperature is-55-50 DEG C, and bottom temperature is 18 25 DEG C;To gently divide tower tower bottoms to be passed through Chong Fenta mutually, described heavy point of tower tower pressure is 0.8 1.2MPa, and tower top temperature is-23-12 DEG C, and bottom temperature is-4 5 DEG C;It is passed through dealkylation tower by heavily dividing tower tower reactor gas phase, described dealkylation tower tower pressure is 0.6 0.9MPa, and tower top temperature is-28-18 DEG C, and bottom temperature is-25-15 DEG C, described dealkylation tower tower reactor derives liquid phase and is the sulfur hexafluoride processed, and the purity of described sulfur hexafluoride is more than 99.999%;
Described water-washing step is made up of 5 grades of washings, controlling the echelon content of fluoride in cleaning mixture is: one-level content of fluoride: 25% 50%, two grades of content of fluoride: 10% 25%, three grades of content of fluoride: 5% 10%, level Four content of fluoride: 1% 5%, Pyatyi content of fluoride: 0% 1%;
Described caustic scrubbing step is made up of 7 grades of alkali cleanings, and the content of the echelon concentration and fluoride that control alkali liquor at different levels is: one-level concentration of lye: 15% 40%, one-level content of fluoride: 0 1%;Two grades of concentration of lye: 12% 15%, two grades of content of fluoride: 0 1%;Three grades of concentration of lye: 8% 12%, three grades of content of fluoride: 0 1%;Level Four concentration of lye: 5% 8%, level Four content of fluoride: 0 1%;Pyatyi concentration of lye: 5% 8%, Pyatyi content of fluoride: 0 1%;Six grades of concentration of lye: 3% 5%, six grades of content of fluoride: 0 1%;Seven grades of concentration of lye: 1% 3%, seven grades of content of fluoride: 0 1%.
Process technique the most according to claim 1, it is characterised in that: in described caustic scrubbing step, alkali liquor is the aqueous solution of potassium hydroxide.
Process technique the most according to claim 1, it is characterised in that: in a step of described pressure-variable adsorption, silica gel adsorption 2 sections absorption.
Process technique the most according to claim 1, it is characterised in that: in the b step of described pressure-variable adsorption, aluminium sesquioxide is adsorbed as 2 sections of absorption, and 13X molecular sieve adsorption is 2 sections of absorption.
Process technique the most according to claim 1, it is characterised in that: in described rectification step, light Fen Ta, Chong Fenta, the overhead condenser coolant of dealkylation tower are alcohols, and tower reactor reboiler heating agent is the hydrate of alcohols.
Process technique the most according to claim 1, it is characterised in that: in described rectification step, light Fen Ta, Chong Fenta, the overhead condenser coolant of dealkylation tower are monohydric alcohol, and tower reactor reboiler heating agent is the hydrate of monohydric alcohol.
Process technique the most according to claim 1, it is characterised in that: described step replace with washing, alkali cleaning, add thermal cracking, alkali cleaning, pressure-variable adsorption, the order of rectification are carried out successively.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111470479A (en) * 2020-04-29 2020-07-31 福建德尔科技有限公司 Purification method of crude sulfur hexafluoride
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
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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CN102923673A (en) * 2012-11-21 2013-02-13 四川众力氟业有限责任公司 Purification technology for sulfur hexafluoride
CN103754834A (en) * 2013-12-17 2014-04-30 福建省邵武市永晶化工有限公司 Rectification device and rectification process used for electronic grade sulfur hexafluoride production
CN104108685A (en) * 2014-07-24 2014-10-22 四川众力氟业有限责任公司 Recovery processing and reusing technology of sulfur hexafluoride for power grid

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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
CN102923673A (en) * 2012-11-21 2013-02-13 四川众力氟业有限责任公司 Purification technology for sulfur hexafluoride
CN103754834A (en) * 2013-12-17 2014-04-30 福建省邵武市永晶化工有限公司 Rectification device and rectification process used for electronic grade sulfur hexafluoride production
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