CS209103B1 - Method of regeneration of waste sulphur - Google Patents
Method of regeneration of waste sulphur Download PDFInfo
- Publication number
- CS209103B1 CS209103B1 CS907979A CS907979A CS209103B1 CS 209103 B1 CS209103 B1 CS 209103B1 CS 907979 A CS907979 A CS 907979A CS 907979 A CS907979 A CS 907979A CS 209103 B1 CS209103 B1 CS 209103B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- sulfur
- contaminated
- waste
- regeneration
- separated
- Prior art date
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims description 28
- 239000002699 waste material Substances 0.000 title claims description 9
- 238000000034 method Methods 0.000 title claims description 6
- 239000005864 Sulphur Substances 0.000 title 1
- 230000008929 regeneration Effects 0.000 title 1
- 238000011069 regeneration method Methods 0.000 title 1
- 229910052717 sulfur Inorganic materials 0.000 claims description 25
- 239000011593 sulfur Substances 0.000 claims description 25
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 229910052785 arsenic Inorganic materials 0.000 claims description 4
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 3
- 230000008014 freezing Effects 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 150000003463 sulfur Chemical class 0.000 description 8
- 238000000605 extraction Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 3
- 229910052683 pyrite Inorganic materials 0.000 description 3
- 239000011028 pyrite Substances 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 150000004992 toluidines Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Processing Of Solid Wastes (AREA)
Description
(54) Spósob regeneráoie odpadovej -síry(54) Waste sulfur recovery method
1,1
Vynález sa týká spósobu regeneráoie odpadovej síry znečistenej bitumenickými látkami, arzénom a anorganickými nečistotami. Kyselina sírová sa do nedávná vyrábala pražením pyritu v etážových peoiach, oxidáciou vzniklého oxitu siřičitého na osid sírový a sorbciou oxidu sírového v kyselině sírovej. Súčasne sa vyrába kyselina sírová spalováním elementárnej síry. Nakolko síra je znečistěná organickými a aňorganickými látkami rafinuje sa přetavením. Nečistoty sa po usadení oddelia. Odpadá znečistěná síra, ktorá obsahuje 60 - 70 % čistej síry, ostávajúce podiely tvoří oxid křemičitý a ostatně nečistoty, ktoré bežne obsahuje síra. Odpad sa drvil a spracoval spolu, s pyritom v etážových peciaoh. Vzhíadom k tomu, že sa od výroby kyseliny sírovej z pyritu upúšťa, vyváža sa odpadná síra na skládku, čo je nehospodárne a vzhíadom na povahu odpadu je skladovanie odpadu síry nepřípustné.The present invention relates to a process for the recovery of waste sulfur contaminated with bituminous substances, arsenic and inorganic impurities. Recently, sulfuric acid has been produced by roasting pyrite in deck pens, by oxidizing the resulting sulfur oxide to sulfur trioxide, and by absorbing sulfur trioxide in sulfuric acid. At the same time, sulfuric acid is produced by burning elemental sulfur. Since sulfur is contaminated with organic and inorganic substances, it is refined by remelting. The impurities are separated after settling. Contaminated sulfur, which contains 60-70% pure sulfur, is eliminated, the remainder being silicon dioxide and impurities normally contained in sulfur. The waste was crushed and treated together, with pyrite in deck ovens. Since the production of sulfuric acid from pyrite is abandoned, waste sulfur is exported to landfill, which is uneconomical and due to the nature of the waste storage of sulfur waste is unacceptable.
Uvedené nedostatky sú odstránené spósobom regeneráoie odpadovej síry podía vynálezu, ktorého podstata spočívá v tom, že sa znečistěná rozdrvená síra rozpúšťa za miešania v organiokom rozpúátadle zo skupiny zahrňujúoej benzén a jeho homology, potom sa reakčná zmes zahřeje na teplotu 115 až 120 °0 s výhodou 120 °0, a vzniklá emulzia sa ochladí na teplotu 2 aŽ 5 °C pod teplotu tuhnutia síry a síra sa oddělí.These drawbacks are overcome by the method of recovering waste sulfur according to the invention, which consists in dissolving the contaminated crushed sulfur in an organic solvent selected from the group consisting of benzene and its homologues, then heating the reaction mixture to a temperature of 115 to 120 ° C. 120 ° 0, and the resulting emulsion is cooled to 2 to 5 ° C below the freezing point of sulfur and the sulfur is separated.
Výhodou spósobu podlá vynálezu je, že získaná síra je velkej čistoty a pretože sa vyzráža, z roztoku, získá sa jemná síra o velkosti zrna do priemeru 0,25 mm.An advantage of the process according to the invention is that the sulfur obtained is of high purity and, since it precipitates out of solution, fine sulfur of grain size up to a diameter of 0.25 mm is obtained.
209 103209 103
Dokonalým zmiešaním sa sira v rozpúšťadla emulguje, čo je možné uskutočniť diskontinuálne v jednom alebo viaoerýoh stupňoch. Po oohladení síra vykrystalizuje a po zastavení miešadla sa usadí na dne reaktoru v podobě jemných krystalických podieloch. Oohladenie postupné znižujeme tak, aby bola tesne pod tuhnutím síry, čo je výhodné z hladiska tepelnej bilanoie, nakolko ešte horúoe roZpúšťadlo sa použije na 3alšiu rafináoiu znečistenej síry. V priebehu miešania dochádza k extrakci! organických bitumenických látok obsiahnutých v znečistenej sire do rozpúšťadla, napr. xylénu. V případe, že sa použije xylén je možné zo síry oddělit extrakoiou aj arzén, ktorý pósobí ako katalytický jed na vanádiový katalyzátor.By thoroughly mixing the sulfur in the solvent is emulsified, which can be carried out discontinuously in one or more stages. Upon cooling, the sulfur crystallized out and upon stirring of the stirrer settle to the bottom of the reactor in the form of fine crystalline fractions. Gradually, the reduction is reduced to just below the solidification of the sulfur, which is advantageous from the point of view of thermal bilanoea, since the still hot solvent is used for further refining the contaminated sulfur. Extraction takes place during stirring! organic bitumen substances contained in the contaminated sulfur into a solvent, e.g. xylene. When xylene is used, arsenic may also be separated from the sulfur by extrac- tion, which acts as a catalytic poison to the vanadium catalyst.
Rafináciu znečistenej síry je možné uskutočniť kontinuálně, čo je najma výhodné použiť v případe velmi znečistenej síry, Rafináoia znečistenej síry sa uskutočňuje protiprúdnou extrakoiou roztavenéj síry organickým rozpúšťadlom v extrakčnej koloně pri teplote nad bodom topenia síry. Emulzia síry a rozpúšťadla, ktorá vychádza z extrakčného zariadeňia sa ochladí, pričom sa.vylúči zrnitá síra, ktorá sa oddělí odstředěním. Z Salšíoh organiokýoh rozpúšťadiel je možné použiť na rafináciu znečistenej síry chlórbenzén, cyklohexanón a toluidin.The refining of the contaminated sulfur may be carried out continuously, which is particularly advantageous in the case of highly contaminated sulfur. The contaminated sulfur refining is carried out by countercurrent extraction of molten sulfur with an organic solvent in an extraction column at a temperature above the melting point of sulfur. The sulfur-solvent emulsion emanating from the extraction apparatus is cooled, precipitating granular sulfur which is separated by centrifugation. Of the other organic organic solvents, chlorobenzene, cyclohexanone and toluidine can be used to refine contaminated sulfur.
Příklad 1Example 1
120 hmotn. dielov rozdrvenej znečistenej síry obsahujúcej 4,14 % popola a 0,0001 hmotnostného diela arzénu sa roztaví pri teplote 120 °C a filtruje oez sklennú vatu do reaktora, v ktorom sa nachádza 240'hmotn. dielov xylénu. Zmes sa za miešania vyhřeje na 120 °C a po vzniku emulzie sa bez prerušenia mieša, ochladí až na teplotu okolo 20 °C, potom sa odstaví miešadlo a vypadlý prášok síry sa odfiltruje, zbaví sa rozpúšťadla premytím metanolem alebo etanolom. Získá sa 110 hmotn. dielov síry o velkosti zrna do priemeru 0,25 mm.,120 wt. parts of crushed contaminated sulfur containing 4.14% ash and 0.0001 parts by weight of arsenic are melted at 120 ° C and filtered through a glass wool into a reactor containing 240 wt. parts of xylene. The mixture is heated to 120 ° C with stirring and after formation of the emulsion it is stirred without interruption, cooled down to about 20 ° C, then the stirrer is removed and the precipitated sulfur powder is filtered off, freed from solvent by washing with methanol or ethanol. 110 wt. parts of sulfur of a grain size up to a diameter of 0,25 mm,
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS907979A CS209103B1 (en) | 1979-12-20 | 1979-12-20 | Method of regeneration of waste sulphur |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS907979A CS209103B1 (en) | 1979-12-20 | 1979-12-20 | Method of regeneration of waste sulphur |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS209103B1 true CS209103B1 (en) | 1981-10-30 |
Family
ID=5442095
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS907979A CS209103B1 (en) | 1979-12-20 | 1979-12-20 | Method of regeneration of waste sulphur |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS209103B1 (en) |
-
1979
- 1979-12-20 CS CS907979A patent/CS209103B1/en unknown
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