CS197399B1 - Antimony chloridating deroasting from tetraedrite calcines - Google Patents
Antimony chloridating deroasting from tetraedrite calcines Download PDFInfo
- Publication number
- CS197399B1 CS197399B1 CS764474A CS764474A CS197399B1 CS 197399 B1 CS197399 B1 CS 197399B1 CS 764474 A CS764474 A CS 764474A CS 764474 A CS764474 A CS 764474A CS 197399 B1 CS197399 B1 CS 197399B1
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- CS
- Czechoslovakia
- Prior art keywords
- antimony
- tetraedrite
- mixture
- hydrochloric acid
- drying
- Prior art date
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- 229910052787 antimony Inorganic materials 0.000 title claims description 14
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000008188 pellet Substances 0.000 claims description 6
- 238000005453 pelletization Methods 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 3
- 239000011363 dried mixture Substances 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims 1
- 239000010949 copper Substances 0.000 description 6
- 238000010511 deprotection reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012188 paraffin wax Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- MUXFZBHBYYYLTH-UHFFFAOYSA-N Zaltoprofen Chemical group O=C1CC2=CC(C(C(O)=O)C)=CC=C2SC2=CC=CC=C21 MUXFZBHBYYYLTH-UHFFFAOYSA-N 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- -1 halide salts Chemical class 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 230000002140 halogenating effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- PDWVXNLUDMQFCH-UHFFFAOYSA-N oxoantimony;hydrochloride Chemical compound Cl.[Sb]=O PDWVXNLUDMQFCH-UHFFFAOYSA-N 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 229910052969 tetrahedrite Inorganic materials 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Description
Vynález sa týká ohloridačného odpraženia antimonu z tetraedritových výpražkov, ktoré sa za studená upravujú s kyselinou soTnou a po zreagovaní a vysušení sn odprnžujú na antimon Pri výrobě ortute z flotačných tetraedritových konoentrátov oxidnčným odprežením sa získává jú výpražky, ktoré možno pokladať za Cu-konoent.rát s měnlivým ohsnhora antimonu, Obsah antimonu sa pohybuje spravidla od 3 až 15 a překážka pri hutníokom spracovaní výpražkov na meS. Sir vypracované rózne postupy oddel’ovania antimonu od médi, ako‘ například chloridačné odpražovonie antimonu, ktoré spočívá v tom, že výpražky sa miešnjú so seltomi chloridov, napr. s NH^Cl a pražia sa pri 600 až 700 °C. Antimon, ktorý je tu přítomný zvřičša vo formě oxizlúóenín, 1’ahko prechádza na chlorid a prchá ako SbCl^BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to the chloridation deprotection of antimony from tetrahedronic esters which are cold treated with hydrochloric acid and, after reacting and drying, to degrade to antimony. The content of antimony is usually from 3 to 15 and an obstacle in the metallurgical processing of fryers into meS. Sir elaborated different methods of separating antimony from the medium, such as the antifungal chlorinating agents of the antimony, which consist in mixing the frying agents with seltium chloride, e.g. with NH 4 Cl and roasted at 600 to 700 ° C. Antimony, which is present here in the form of oxizluoroenines, is easily converted to chloride and fills like SbCl ^
Zistilo sa, že odpražovanie SbCl^ je možné prevádzať ekonomickojšie a pri nižšej teplote, napr. pri 300 °C a za súčasného skusovatenia prachových tetjraedritovýoh výpražkov, ak ohloridačný poohod antimonu vo výpražkooh prebehne v hmotě za studená účinkom koncentrovanéj kyseliny sďne j,ktorá přednostně rozpúšťo oxizlúčeni,ny antimonu, Reakcia je slabo exotermioká, takže upravené výpražky pri zachovaní pevnejkonzistoncie vyschnú za atmosférických podmienok a súčasne skusovatejú.It has been found that degassing of SbCl 2 can be carried out more economically and at a lower temperature, e.g. at 300 ° C, while concurrently biting the powdered tetrahedrates, if the halide oxidation of the antimony in the arsenic takes place in the cold mass under the effect of concentrated sulfuric acid j, which preferably dissolves the oxidation of antimony, the reaction is weakly exothermic atmospheric conditions and at the same time bite.
Nevýhody známého stavu techniky nemá spósob ohloridačného odpraženia antimonu z tetraedritovýoh výpražkov podl’a vynálezu, ktorého podstata spočívá v tom, že prachové tetraedritové výpražky, výhodné suché, sa raiešajú s koncentrovanou kyselinou sol’nou, výhodné 35 ^-nou, v množstve, ktoré je minimálně o 50 $ vKčšie, než zodpoveda stechiometricky obsahu antimonu vo výpražkoch, zmes sa ponechá reagovat’ vol’ne za otmosferickýeh podmienok a po samovďnom vysušení, alebo za použitia tepla, sa vysušená zmes odprožuje pri teplote 300 až 600 °C minimálně 30 minút.The disadvantages of the prior art do not have the method of the oxidative deposition of antimony from the tetrahedronic sticks according to the invention, which consists in that the powdered tetrahedron stents, preferably dry, are mixed with concentrated hydrochloric acid, preferably 35%, in an amount which is at least 50% higher than the stoichiometric antimony content of the scrubs, the mixture is allowed to react freely under atmospheric conditions and, after spontaneous drying or using heat, the dried mixture is fried at a temperature of 300 to 600 ° C for at least 30 minutes .
S výhodou sa pri zmiešavaní výpražkov s kyselinou solnou súčasne prevádza peletizá197 399Advantageously, pelletizing 197 399 is simultaneously carried out when mixing the calcines with hydrochloric acid
197 399 tizácia, alebo zmes peletu je až po predsušení, pričom velkost' poliet sn reguluje 3nlším prídavkom kyseliny soPnej. Pojivom sú tu vo vodě rozpustné soli, ktoré vznikli účinkom HCl. Pri obsahu antimánu vo výpražkooh pod 6 % je výhodné koncentrovanú kyselinu soPnú přidávat’ priamo do peletizačného zariadenia a vyrábat’ mikropeletky Pri vyššora obsahu antimonu je potřebné přidávat’ viao kyseliny, zmes je menej súdržná a pre peletizáoiu je vhodná až po predbežnom sušení, a to vol*ne, alebo za použitia teplého vzduohu Množstvo kyseliny soPnej sa přidává minimálně o 50 $ viac, než zodpovedá stechiometrioký obsahu antimónu vo výpražkooh. Doba pdsobenia kyseliny vo výpražkooh uloženýoh v»Pne vo formo pelňet pri teplote ovzdušia nad 15 °C je minimálně doň. Pre odpraženie Sb je výhodné používat' vysúšenú zmes, aby sa odstránili zbytky voPnej HCl, pretože tým sa podstatné zníži korózia kondenzáčného zariadenia odplynmi.197 399, or the pellet mixture is only after pre-drying, and the size of the pellets is controlled by the 3% addition of hydrochloric acid. The binder here is the water-soluble salts formed by HCl. If the antiman content is less than 6%, it is preferable to add concentrated salic acid directly to the pelletizer and to produce micropellets. freely, or using warm air. The amount of salt is added at least 50 $ more than the stoichiometric content of antimony in the arterial. The duration of acid exposure in the paraffin deposited in the form of pellets at an air temperature above 15 ° C is at least one. For evaporation of Sb, it is advantageous to use a dried mixture to remove residual aqueous HCl, since this will substantially reduce the corrosion of the condensation apparatus by the gases.
Podstata vynálezu spočívá v úpravě tetraedritových výpražkov s koncentrovanou kyselinou soPnou, ktorá v zmesi za studená před odpraženini vytvára SbCl^, teda nezávisle na podmienkach odpražovania.SUMMARY OF THE INVENTION The present invention is based on the treatment of tetrahedrite fumers with concentrated hydrochloric acid, which in the cold mixture before evaporation forms SbCl2, i.e. independently of the deprotection conditions.
Uvedeným postupom je možné prevádzať skusovanie praohových tetraedritových vvnrožkov, čo priaznivo ovplyvňuje úlet pri odsávaní odplynov Tekanie SbCl^ zaČína už pri 300 °C a je spravidla ukončené po 1 hodině praženia. Znižuje sa oelkove množstvo odplynov, pretože je vylúčené tekanie nezreagovaného ohloridačného činidla, ako to je pri použití solí ohloridov.By this procedure, it is possible to bite the threshold tetra-tetritic inlay, which favorably influences the flue gas exhaust as it starts at 300 ° C and is usually terminated after 1 hour of roasting. The total amount of offgasses is reduced because the flow of unreacted halogenating agent is avoided, as is the case with the use of halide salts.
Odpražovanie SbCl^ zo zmesi je možné prevádzať v rotačnej peci, tiež v etážovoj peci nezávisle na zložení peonej atmosféry.The deprotection of SbCl2 from the mixture can be carried out in a rotary kiln, also in a multi-stage furnace independently of the composition of the peon atmosphere.
Příklad 1Example 1
Suché prachové tetraedritové měděné výpražky s obsahom Cu 19,20 $ a Sb 5,76 % sa v peletizačnej mise zmiešali s koncentrovanou kyselinou soPnou /35 $-nou/ v množstve 25 1 na 100 kg výpražkov. Pelety sa poneohali vol’ne sušit’, pričom ich teplota samovoPne vystúpila na 55 °C. Po dvoch dňoch stánia pelety boli už vysušené.The dry powdered tetrahedron copper plumes containing Cu of 19.20 $ and Sb 5.76% were mixed with concentrated hydrochloric acid (35 $) in a pelletizing bowl in an amount of 25 L per 100 kg of the flakes. The pellets were allowed to dry freely and their temperature rose to 55 ° C. After two days of standing, the pellets were already dried.
Odpražovanie SbCl^ sa previedlo v etážovej peci s priaraym ohrevom pri teplote zmesi 300 až 550 °C po dobu 1 hodiny. Odplyny sa viedli oez teplú vápennú vodu, v ktorej sa zaohytil antimon ako SbOCl, resp. antimonitan vápenatý.The deprotection of SbCl2 was carried out in a multi-stage oven with direct heating at a temperature of 300-550 ° C for 1 hour. The off-gases were passed through hot lime water, in which antimony was captured as SbOCl, respectively. calcium antimonite.
Zloženie Výpražkov po odpražení Sb bolo: 21,8$ Cu a 0,56 $ Sb. Obsah Sb v zaohytenom kondenzáte bol 43 $.The composition of the Collections after detaching Sb was: 21.8 $ Cu and 0.56 $ Sb. The Sb content in the trapped condensate was 43 $.
Příklad 2Example 2
Suché prachové tetraedritové měděné výpražky s obsahom Cu 22,8 $ a Sb 10,5 $ sp zmiešali s HCl /35 $-nou/ v množstve 35 1 na 100 kg výpražkov Zmes sa ponechala reaeovať deň, a potom sa v teplom vzduohu dosušila. Pri vlhkosti ooa 8 $ sn zo zmesi připravili milcropelety v peletizačnej mise a po vysušení podrobili odpraženiu Sb v otáčívej peci pri teplote 450 až 500 °C po dobu 2 hodin. Odplyny sa spraoovali ako v příklade 1.Dry copper tetraedrite dusts containing Cu of 22.8 $ and Sb 10.5 $ sp were mixed with HCl (35 $) in an amount of 35 L per 100 kg of the blend. The mixture was allowed to react for a day and then dried in a warm air. At a humidity of about 8 ° C, the pelletizing pans were prepared from the mixture in a pelletizing dish and dried after drying in a rotary oven at 450-500 ° C for 2 hours. The gases were treated as in Example 1.
Zloženie výpražkov po odpražení Sb bolo: 26,3 $ Cu a 1,3θ $ Sb Obsah Sb v zaohytenom kondenzáte bol 58 $.The composition of the paraffin after removal of Sb was: 26.3 $ Cu and 1.3θ $ Sb The Sb content in the trapped condensate was 58 $.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS764474A CS197399B1 (en) | 1974-11-11 | 1974-11-11 | Antimony chloridating deroasting from tetraedrite calcines |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS764474A CS197399B1 (en) | 1974-11-11 | 1974-11-11 | Antimony chloridating deroasting from tetraedrite calcines |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS197399B1 true CS197399B1 (en) | 1980-05-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS764474A CS197399B1 (en) | 1974-11-11 | 1974-11-11 | Antimony chloridating deroasting from tetraedrite calcines |
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| Country | Link |
|---|---|
| CS (1) | CS197399B1 (en) |
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1974
- 1974-11-11 CS CS764474A patent/CS197399B1/en unknown
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