NO133363B - - Google Patents
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- NO133363B NO133363B NO724/72A NO72472A NO133363B NO 133363 B NO133363 B NO 133363B NO 724/72 A NO724/72 A NO 724/72A NO 72472 A NO72472 A NO 72472A NO 133363 B NO133363 B NO 133363B
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- Prior art keywords
- hydrogen fluoride
- fluoride
- alkali metal
- liquid
- metal fluoride
- Prior art date
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 43
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 19
- 229910001515 alkali metal fluoride Inorganic materials 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910001868 water Inorganic materials 0.000 claims description 9
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- 150000001491 aromatic compounds Chemical class 0.000 claims description 3
- 125000006267 biphenyl group Chemical group 0.000 claims description 3
- 235000010290 biphenyl Nutrition 0.000 claims description 2
- 239000004305 biphenyl Substances 0.000 claims description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002002 slurry Substances 0.000 description 6
- 239000010436 fluorite Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 description 3
- 239000008246 gaseous mixture Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- -1 phthalate esters Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- ZQPPMHVWECSIRJ-MDZDMXLPSA-N elaidic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(O)=O ZQPPMHVWECSIRJ-MDZDMXLPSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Gas Separation By Absorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Sorption Type Refrigeration Machines (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Hydrogen, Water And Hydrids (AREA)
Description
Foreliggende opfinnelse .vedrører en fremgangsmåte for-utvinning av hydrogenfluordi >fra;en gassblanding ,som,inneholder hydrogenfluorid og som eventuelt også inneholder vanndamp, og.. særlig for fremstilling av i alt vesentlig.tørt hydrogenfluorid fra vandige blandinger av denne type. .... I. et større antall av fremgangsmåter hvor .hydrogenf luor id _ fremstilles eller anvendes fåes hydrogenfluorid. i form av en for-tynnet gassblanding, eller hydrogenfluoridet er forurenset med vann. Adskillelsen av hydrogenfluorid fra vann er særlig vanskelig som. følge av det faktum at disse to komponenter danner en azeotrop blanding, og kan således ikke adskilles på en enkel måte veavanlig destillasjon. Det der derfor ønskelig å tilveiebringe en effektiv fremgangsmåte for utvinning av hydrogenfluorid, og særlig for utvinning av hydrogenfluoridet i en i alt vesentlig vannfri tilstand fra vandige blandiger. The present invention relates to a method for the extraction of hydrogen fluoride from a gas mixture which contains hydrogen fluoride and which optionally also contains water vapour, and in particular for the production of essentially dry hydrogen fluoride from aqueous mixtures of this type. .... I. a larger number of methods in which hydrogen fluoride is produced or used, hydrogen fluoride is obtained. in the form of a diluted gas mixture, or the hydrogen fluoride is contaminated with water. The separation of hydrogen fluoride from water is particularly difficult as. due to the fact that these two components form an azeotropic mixture, and thus cannot be separated in a simple way by ordinary distillation. It is therefore desirable to provide an efficient method for extracting hydrogen fluoride, and in particular for extracting the hydrogen fluoride in an essentially anhydrous state from aqueous mixtures.
Det er kjent at hydrogenfluorid.kan absorberes av fast natriumfluorid og kan derefter utvinnes fra dette ved opphetning, men denne fremgangsmåte medfører store vanskeligheter i praksis,. F.eks. medfører varmeoverføringsproblemer at apparatet er temmelig volumi-nøst, og.nedbrytning av det faste absorberingsmiddel (som:forårsakes av utvidelsen og< sammentrekning under prosessen) resulterer i at det bygges opp trykk i apparatet. It is known that hydrogen fluoride can be absorbed by solid sodium fluoride and can then be extracted from this by heating, but this method entails great difficulties in practice. E.g. causes heat transfer problems that the apparatus is rather bulky, and breakdown of the solid absorbent (caused by the expansion and contraction during the process) results in pressure building up in the apparatus.
Vi har nu funnet at disse ulemper kan unngåes ved å anvende det absorberende faste stoff i en inert væske. -I henhold til foreliggende oppfinnelse er det således til-veiebragt en fremgangsmåte for utvinning av hydrogenfluorid fra en gassblanding som inneholder hydrogenfluorid og som eventuelt også inneholder vanndamp,og fremgangsmåten karakteriseres ved. at nevnte gassblanding føres gjennom en suspensjon av et alkalimetallfluorid i en inert væske med et kokepunkt på minst 25o°c som holdes ved en temperatur under 180°C for å frigjøre hydrogenfluorid. We have now found that these disadvantages can be avoided by using the absorbent solid in an inert liquid. -According to the present invention, there is thus provided a method for extracting hydrogen fluoride from a gas mixture which contains hydrogen fluoride and which possibly also contains water vapour, and the method is characterized by that said gas mixture is passed through a suspension of an alkali metal fluoride in an inert liquid with a boiling point of at least 25o°C which is kept at a temperature below 180°C to release hydrogen fluoride.
Alkalimetallfluoridet er fortrinnsvis natriumfluorid, men andre alkalimetallfluorider eller blandinger herav kan om ønskes anvendes. The alkali metal fluoride is preferably sodium fluoride, but other alkali metal fluorides or mixtures thereof can be used if desired.
Alkalimetallfluoridet anvendes vanligvis i form av en suspensjon i den inerte væske, og kan suspenderes i væsken ved hjelp av hvilke som helst passende midler, f.eks. ved mekanisk omrøring, men en tilfredsstillende suspensjon kan oppnås i enkelte tilfelle ved å la den gassformige blanding strømme gjennom suspensjonen. Partikkelstørrelsen av alkalimetallfluoridet er ikke av kritisk betydning, og kan velges for å oppnå den ønskede suspensjonsgrad i det system som foreligger. The alkali metal fluoride is usually used in the form of a suspension in the inert liquid, and can be suspended in the liquid by any suitable means, e.g. by mechanical stirring, but a satisfactory suspension can be obtained in some cases by allowing the gaseous mixture to flow through the suspension. The particle size of the alkali metal fluoride is not of critical importance, and can be chosen to achieve the desired degree of suspension in the existing system.
Væsken kan være en hvilken som helst som er r alt vesentlig inert under bruksbetingelsene. Således må den ikke spaltes ved å komme i kontakt med hydrogenfluorid eller alkalimetallfluorideL eller reagere i noen vesentlig utstrekning med noen av disse stof-fer, og den skal videre ikke spaltes i nevneverdig grad ved bruks-temperaturen. Fortrinnsvis er væsken en som har et kokepunkt av i det minste 250°c, og hensiktsmessig er den en væske som er i alt vesentlig ikke blandbar med vann. Det er også ønskelig at væsken er en som kan oppløse hydrogenfluorid, selv om dette bare er i en begrenset utstrekning, og at den er en væske som ikke nevneverdig oppløser alkalimetallfluoridet. The liquid may be any that is substantially inert under the conditions of use. Thus, it must not be decomposed by coming into contact with hydrogen fluoride or alkali metal fluorideL or reacting to any significant extent with any of these substances, and it must also not be decomposed to an appreciable extent at the temperature of use. Preferably, the liquid is one which has a boiling point of at least 250°c, and suitably it is a liquid which is substantially immiscible with water. It is also desirable that the liquid is one that can dissolve hydrogen fluoride, even if this is only to a limited extent, and that it is a liquid that does not significantly dissolve the alkali metal fluoride.
Eksempler på passende væsker omfatter høytkokende aromatiske forbindelser, f.eks. difenyl, difenyleter og blandinger av disse, særlig den eutektiske blanding, og halogenerte aromatiske forbindelser, f.eks. klorert difenyl; estere, f.eks. ftalatestere, og særlig di-n-butylftalat; polyglykoler, f.eks. slike som har en molekylvekt av minst looo, f.eks. polypropylenglykol,' mineraloljer; lang-kjedede karboksylsyrer, f.eks. oljesyre! og blandinger av slike væsker. Examples of suitable liquids include high-boiling aromatic compounds, e.g. diphenyl, diphenyl ether and mixtures thereof, especially the eutectic mixture, and halogenated aromatic compounds, e.g. chlorinated diphenyl; esters, e.g. phthalate esters, and in particular di-n-butyl phthalate; polyglycols, e.g. such as have a molecular weight of at least looo, e.g. polypropylene glycol,' mineral oils; long-chain carboxylic acids, e.g. oleic acid! and mixtures of such liquids.
Konsentrasjonen av alkali-metallfluoridet i væsken er ikke av kritisk betydning og kan varieres over et vidt område, f.eks. mellom 1 og 5o vektprosent, fortrinnsvis mellom 15 og 25 vektprosent, av alkalimetallfluoridet i blandingen. The concentration of the alkali metal fluoride in the liquid is not of critical importance and can be varied over a wide range, e.g. between 1 and 50% by weight, preferably between 15 and 25% by weight, of the alkali metal fluoride in the mixture.
Absorbsjonen utføres generelt ved en temperatur i området The absorption is generally carried out at a temperature in the range
av 7o-18o°c, og fortrinnsvis i området llo - 13o°C. Den videre opphetning for å frigjøre hydrogenfluorid, utføres ved en temperatur over 18ooc, f.eks. i området 24o - 28o°C. of 7o-18o°c, and preferably in the range llo - 13o°C. The further heating to release hydrogen fluoride is carried out at a temperature above 18oC, e.g. in the range 24o - 28o°C.
Fremgangsmåten ifølge foreliggende oppfinnelse kan utføres for utvinning av hydrogenfluorid fra et vidt område av gassformige blandinger. Således kan den anvendes for å utvinne hydrogenfluorid fra blandinger i hvilke hydrogenfluoridinnholdet kan variere så meget som f.eks. fra 2 til 96 vektprosent, og den uønskede komponent i gassblandingen kan f.eks. være en eller flere av gassene nitrogen, oksygen, vanndamp, organiske damper, oksyder av karbon og andre sure gasser, f.eks. svoveldioksyd, hydrogensulfid, silisiumtetrafluorid og hydrogenklorid. De . uønskede komponenter i gassblandingen passerer videre i uab-sorbert tilstand, og følgelig skal temperaturen som anvendes for absorbsjonstrinnet Utvelges for å redusere til et minimum eller unngå kondensering av disse komponenter, f.eks. damp. Fremgangsmåten er særlig nyttig for utvinning av hydrogenfluorid fra blandinger som inneholder vann. The method according to the present invention can be carried out for the extraction of hydrogen fluoride from a wide range of gaseous mixtures. Thus, it can be used to extract hydrogen fluoride from mixtures in which the hydrogen fluoride content can vary as much as e.g. from 2 to 96 percent by weight, and the unwanted component in the gas mixture can e.g. be one or more of the gases nitrogen, oxygen, water vapour, organic vapours, oxides of carbon and other acidic gases, e.g. sulfur dioxide, hydrogen sulphide, silicon tetrafluoride and hydrogen chloride. They . unwanted components in the gas mixture pass on in an unabsorbed state, and consequently the temperature used for the absorption step must be selected to reduce to a minimum or avoid condensation of these components, e.g. steam. The method is particularly useful for extracting hydrogen fluoride from mixtures containing water.
Fremgangsmåten ifølge foreliggende oppfinnelse kan anvendes for utvinning av hydrogenfluorid fra rå reaksjonsdamper som fåes f.eks. ved pyrohydrolyse av flusspat (kalsiumfluorid). Da fremgangsmåten ifølge oppfinnelsen er meget effektiv for å adskille hydrogenfluorid fra et stort antall forskjellige gasser, er oppfinnelsen særlig anvendbar for å adskille hydrogenfluorid fra damper som fåes ved pyrohydrolyse av rått flusspat og/eller flusspat av lav kvalitet. The method according to the present invention can be used for the extraction of hydrogen fluoride from raw reaction vapors which are obtained, e.g. by pyrohydrolysis of fluorspar (calcium fluoride). As the method according to the invention is very effective for separating hydrogen fluoride from a large number of different gases, the invention is particularly applicable for separating hydrogen fluoride from vapors obtained by pyrohydrolysis of raw fluorspar and/or low-quality fluorspar.
Således kan hydrogenfluorid fåes ved pyrohydrolyse eller annen behandling av flusspat som varierer i kvalitet fra rå malm slik som denne utvinnes i bergverk, og som kan inneholde så lite som 2o vektprosent av kalsiumfluorid, og til konsentrerte malmer av lav kvalitet og til konsentrater av høy kvalitet som inneholder minst 97 vektprosent kalsiumfluorid. Thus, hydrogen fluoride can be obtained by pyrohydrolysis or other treatment of fluorspar, which varies in quality from raw ore such as is extracted in quarries, and which can contain as little as 20% by weight of calcium fluoride, and into low-quality concentrated ores and into high-quality concentrates which contains at least 97% calcium fluoride by weight.
Typiske forurensninger i flusspat omfatter kiselsyre, aluminiumoksyd, barytter og tungmetallkarbonater og sulfider. Typical contaminants in fluorspar include silicic acid, alumina, barytes and heavy metal carbonates and sulphides.
En av de vesentlig forurensende gasser fra hvilke hydrogenfluoridet skal fraskilles, kan således være svoveldioksyd som fåes f.eks. ved spaltning av barytter eller ved oksydasjon av sulfidene. One of the significantly polluting gases from which the hydrogen fluoride must be separated can thus be sulfur dioxide, which is obtained e.g. by cleavage of barytes or by oxidation of the sulphides.
Fremgangsmåten ifølge oppfinnelsen kan også anvendes for The method according to the invention can also be used for
å utvinne hydrogenfluorid som f åes ved pyrohydrolyse av heksa-fluorkiselsyre eller dens salter, f.eks. kalsiumfluorsilikat, hvilke salter eventuelt kan være blandet med et silikat, f.eks. kalsiumsilikat. Fremgangsmåten ifølge oppfinnelsen kan også anvendes for utvinning av hydrogenfluorid som fåes som et biprodukt ved andre kjemiske reaksjoner eller hvor det utvinnes ved re - aksjoner når det anvendes som et utgangsmateriale, f.eks. ved fluorering av klorerte hydrokarboner. Det kan også utvinnes fra vandig oppløsning, f.eks. de vandige kondensater som fåes fra hvilke som helst av de ovennevnte prosesser. Om ønskes kan den anvendes for å utvinne vannfritt hydrogenfluorid fra den vandige to extract hydrogen fluoride obtained by pyrohydrolysis of hexafluorosilicic acid or its salts, e.g. calcium fluorosilicate, which salts may optionally be mixed with a silicate, e.g. calcium silicate. The method according to the invention can also be used for the extraction of hydrogen fluoride which is obtained as a by-product in other chemical reactions or where it is extracted in reactions when it is used as a starting material, e.g. by fluorination of chlorinated hydrocarbons. It can also be recovered from aqueous solution, e.g. the aqueous condensates obtained from any of the above processes. If desired, it can be used to extract anhydrous hydrogen fluoride from the aqueous one
konstant kokende syre, som inneholder ca. 38% hydrogenfluorid. constant boiling acid, which contains approx. 38% hydrogen fluoride.
Det gassformige produkt som inneholder hydrogenfluorid som fåes som et resultat av det annet opphetningstrinn ved fremgangsmåten ifølge oppfinnelsen, skal behandles på vanlig måte for å utvinne hydrogenfluoridet fra det gassformige produkt. F.eks. The gaseous product containing hydrogen fluoride which is obtained as a result of the second heating step in the method according to the invention, must be treated in the usual way in order to recover the hydrogen fluoride from the gaseous product. E.g.
kan det avkjøles til en temperatur under 19,5°c for å kondensere hydrogenfluoridet, eller den gassformige strøm av hydrogenfluorid kan anvendes direkte for hvilken som helst annen ønsket kjemisk reaksjon uten mellomliggende isolering. it can be cooled to a temperature below 19.5°C to condense the hydrogen fluoride, or the gaseous stream of hydrogen fluoride can be used directly for any other desired chemical reaction without intermediate isolation.
Fremgangsmåten kan utføres chargevis eller på en kontinuerlig måte, men den er særlig nyttig for kontinuerlig drift. The method can be carried out batchwise or in a continuous manner, but it is particularly useful for continuous operation.
Tegningen viser skjematisk fremgangsmåten ifølge foreliggende oppfinnelse, tillempet for kontinuerlig drift. En gass-strøm som inneholder hydrogenfluorid går gjennom kanalen 3 inn i en reaktor 1 som inneholder en oppslemning av alkalimetallfluorid i en inert væske som holdes ved absorbsjonstemperaturen, f.eks. ved ca. 12o°c, og ikke absorberte gasser forlater reaktoren gjennom kanalen 4. Oppslemning av alkalimetallfluoridet som inneholder absorbert hydrogenfluorid, føres langs kanalen 5 til reaktoren 2, hvor det opphetes til frigjøringstemperaturen, f.eks. ca.26o°c. Tørt hydrogenfluorid frigjøres på denne måte og føres bort gjennom kanalen 6. Den gjenværende oppslemning føres derpå tilbake til reaktoren 1 gjennom kanalen 7 for å resirkulere i prosessen. The drawing schematically shows the method according to the present invention, applied for continuous operation. A gas stream containing hydrogen fluoride passes through channel 3 into a reactor 1 containing a slurry of alkali metal fluoride in an inert liquid which is maintained at the absorption temperature, e.g. at approx. 12o°c, and unabsorbed gases leave the reactor through channel 4. Slurry of the alkali metal fluoride containing absorbed hydrogen fluoride is passed along channel 5 to reactor 2, where it is heated to the release temperature, e.g. approx. 26o°c. Dry hydrogen fluoride is released in this way and is carried away through the channel 6. The remaining slurry is then returned to the reactor 1 through the channel 7 to be recycled in the process.
EKSEMPEL EXAMPLE
Gassformige blandinger av damp, hydrogenfluorid og nitrogen ble ført inn i en oppslemning inneholdende 55g natriumfluorid i 188g inert væske som holdes ved llo - 12o°C. Oppslemningen ble analysert for å bestemme hvor meget hydrogenfluorid var blitt absorbert. Gaseous mixtures of steam, hydrogen fluoride and nitrogen were introduced into a slurry containing 55 g of sodium fluoride in 188 g of inert liquid maintained at 110 - 120°C. The slurry was analyzed to determine how much hydrogen fluoride had been absorbed.
Oppslemningen ble derpå opphetet til 26o°c over en periode av 2 timer og vekten av det frigjorte hydrogenfluorid ble målt. The slurry was then heated to 26o°c over a period of 2 hours and the weight of the liberated hydrogen fluoride was measured.
Resultatene er vist i den følgende tabell: The results are shown in the following table:
Claims (6)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB626971 | 1971-03-08 |
Publications (2)
Publication Number | Publication Date |
---|---|
NO133363B true NO133363B (en) | 1976-01-12 |
NO133363C NO133363C (en) | 1976-04-21 |
Family
ID=9811456
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
NO724/72A NO133363C (en) | 1971-03-08 | 1972-03-07 |
Country Status (20)
Country | Link |
---|---|
JP (1) | JPS5229276B1 (en) |
AT (1) | AT325010B (en) |
AU (1) | AU463078B2 (en) |
BE (1) | BE780060A (en) |
BR (1) | BR7201280D0 (en) |
CA (1) | CA957132A (en) |
CS (1) | CS170181B2 (en) |
DD (1) | DD94807A5 (en) |
DE (1) | DE2209841B2 (en) |
ES (1) | ES400511A1 (en) |
FR (1) | FR2128712B1 (en) |
GB (1) | GB1332968A (en) |
IL (1) | IL38841A (en) |
IT (1) | IT959556B (en) |
NL (1) | NL151043B (en) |
NO (1) | NO133363C (en) |
SE (1) | SE379994B (en) |
SU (1) | SU459884A3 (en) |
TR (1) | TR19068A (en) |
ZA (1) | ZA721323B (en) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4491570A (en) * | 1984-05-03 | 1985-01-01 | Pennwalt Corporation | Removal of arsenic from hydrogen fluoride |
US4832935A (en) * | 1987-11-04 | 1989-05-23 | Gte Laboratories Incorporated | Method for dehydrating hydrogen fluoride |
GB9305148D0 (en) * | 1993-03-12 | 1993-04-28 | Ici Plc | Hydrogen fluoride recovery process |
US5800795A (en) * | 1993-03-12 | 1998-09-01 | Imperial Chemical Industries Plc | Hydrogen fluoride recovery process |
ES2155201T3 (en) * | 1995-10-10 | 2001-05-01 | Ici Plc | PROCEDURE FOR THE RECOVERY OF HYDROGEN FLUORIDE. |
GB9707176D0 (en) * | 1997-04-09 | 1997-05-28 | Ici Plc | Hydrogen fluoride recovery process |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB605472A (en) * | 1945-10-02 | 1948-07-23 | Standard Oil Co | Improvements relating to the recovery of fluorides |
DE938964C (en) * | 1953-11-08 | 1956-02-09 | Harpener Bergbau Ag | Process for the recovery of boron trifluoride and anhydrous hydrofluoric acid from aqueous solutions |
-
1972
- 1972-02-16 GB GB626971A patent/GB1332968A/en not_active Expired
- 1972-02-24 AU AU39316/72A patent/AU463078B2/en not_active Expired
- 1972-02-25 IL IL38841A patent/IL38841A/en unknown
- 1972-02-28 ZA ZA721323A patent/ZA721323B/en unknown
- 1972-03-01 NL NL727202681A patent/NL151043B/en unknown
- 1972-03-01 TR TR19068A patent/TR19068A/en unknown
- 1972-03-01 DE DE19722209841 patent/DE2209841B2/en active Granted
- 1972-03-01 BE BE780060A patent/BE780060A/en unknown
- 1972-03-06 BR BR1280/72*[A patent/BR7201280D0/en unknown
- 1972-03-07 ES ES400511A patent/ES400511A1/en not_active Expired
- 1972-03-07 IT IT21537/72A patent/IT959556B/en active
- 1972-03-07 SE SE7202891A patent/SE379994B/xx unknown
- 1972-03-07 DD DD161409A patent/DD94807A5/xx unknown
- 1972-03-07 SU SU1757268A patent/SU459884A3/en active
- 1972-03-07 CS CS1507A patent/CS170181B2/cs unknown
- 1972-03-07 FR FR7207921A patent/FR2128712B1/fr not_active Expired
- 1972-03-07 NO NO724/72A patent/NO133363C/no unknown
- 1972-03-08 JP JP47023250A patent/JPS5229276B1/ja active Pending
- 1972-03-08 CA CA136,720A patent/CA957132A/en not_active Expired
- 1972-03-08 AT AT194072A patent/AT325010B/en not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
ZA721323B (en) | 1973-10-31 |
SU459884A3 (en) | 1975-02-05 |
JPS5229276B1 (en) | 1977-08-01 |
TR19068A (en) | 1978-05-01 |
DE2209841B2 (en) | 1976-11-11 |
DE2209841A1 (en) | 1972-09-28 |
NL151043B (en) | 1976-10-15 |
BE780060A (en) | 1972-09-01 |
NO133363C (en) | 1976-04-21 |
IT959556B (en) | 1973-11-10 |
AU463078B2 (en) | 1975-06-25 |
GB1332968A (en) | 1973-10-10 |
ES400511A1 (en) | 1975-02-16 |
BR7201280D0 (en) | 1973-07-03 |
NL7202681A (en) | 1972-09-12 |
CA957132A (en) | 1974-11-05 |
FR2128712B1 (en) | 1977-01-14 |
DD94807A5 (en) | 1973-01-05 |
FR2128712A1 (en) | 1972-10-20 |
CS170181B2 (en) | 1976-08-27 |
AT325010B (en) | 1975-09-25 |
AU3931672A (en) | 1973-08-30 |
IL38841A (en) | 1974-12-31 |
IL38841A0 (en) | 1972-04-27 |
SE379994B (en) | 1975-10-27 |
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