DE1592036A1 - Process for the production of potassium sulphate - Google Patents

Description

Our Hr ₉ 13 764

SINCAT Societei Industriale Catanese S-.p.A. Palermo / Italy

Process for the production of potassium sulphate

The present invention relates to a method for Hera division of potassium sulfate, especially using of cainite raw materials as raw materials

It is known that such raw material _p having a erhebliohen NAOL content j which belauft usually to 20-40 percent by $ *. | In order to avoid that the potassium sulphate or some other salts obtainable from the kainite are contaminated by those of the sodium, it is necessary to remove the larger part of the NaOl present in the kainite before or during its treatment.

So far, this has been done by flotation of the ground Kalnite, using suitable 3ammXerreagentlen _t whereby the NaOl Sun. Larger rope in the flotation waste "Bai so du £> © h dl® Flotation" contains ngertiolierte Kainit inlinmtr no oh © a $ 5 Öew _f ji KaOl *

solohe implementation de *? flotation iet-awar ^ © Qht kostspi «

lig, but inevitably continues to be exercised there other technically equivalent processes for the separation of NaCl have not yet become known.

From the Italian patent specification 672,661 a method for the recovery of potassium and magnesium salts using Kainit as the starting material is already known · MOQH This procedure treats the kainite at about 90 ⁰ C temperatures lying with brines, the composition of the a _n schliestjend taking place Extraction of langbainite favored; this langbainite is cooled to below 40 ° in the presence of its mother liquor? at the final concentration of the MgGIp of the brine and under the saturation conditions for potassium chloride and magnesium sulphate, either arise during cooling

1) Schoenit (or Leonit) and KCl or

2) ·· "" and MgSO..7 ίΙ _£ 0 or

3) KCl and MgSO ₄ .6 H ₃ O and / or, MgSO ₄ .7 H ₂ O

This process leads to optimal yields of potassium, since the brines, which are in equilibrium with the salt mixtures obtained by cooling, have a low potassium content, which is attributable to the high MgClp content of those brines and at the same time to the solubility of the NaCl in the Brine to a large extent. The amount of NaCl removed from the process cycle with salt waste liquors is correspondingly small, which is why the amount of NaOL added to the cycle together with the kainite is very low} otherwise the potassium and magnesium salts would be contaminated by those of the sodium. In practice, the "\ lnit" supplied to the circuit cannot contain more than 2 · 5 # NaCl, as long as the LangDeinite is converted into KCl and MgSO ₄ , 6 HpO and or «or MgSO ₄ * 7 H ₀ O, while in the case of conversion of Langbeinite in Sohbriit and KCl or Schoenite and MgSO ₄ , 7 H ^ O ₁ this kainite must no longer contain all b $> NaCl.

For a conversion of liWigbeinit in kcfi and MgSO _4, 6 H ^ O and / • the MGSC _4, 7HpO detnnaoh dns Flοtntionsverfahren only uniulÄnglloh fulfilled uolohee lung NaOH in the Lfcallen.ijohtn PatenteohrLft no. Preconditions for a Kainlt-nimbly " 672 t <b! bo-

009S12 / U2S SADOfflG.NAL

described processes with high potassium yields. Will however, according to this patent specification Langbeinit in Schoenit and KCl or Epsomit, then corresponds to that by the pre-flootion achievable optimal improvement of the kainite exactly the process conditions that an extremely careful flotation presuppose.

The same patent already describes an alternative process for the preflotation of kainite. Thereafter, the Langbainit obtained by Heissauslaugen the crude kainite by cold treatment may be in a mixture of KCl, HACL, MfcS0., 6H ₂ 0 and / or MgSO, .- 7H ₀ O are converted. The magnesium sulfate can

4 Cl s ι e ration
by ; or sieve off the chlorides, while the potassium chloride can be separated from the sodium chloride by flotation. Using this procedure, potassium chloride with an NaCl content of less than 5% by weight can be obtained.

However, the flotation carried out within the circuit proves to be quite expensive, partly because of the large amount of sodium chloride present; in fact, the weight ratio between KCl and NaCl is generally about 0.5 be milled ore fine, would than leaching for Hei ss required. Thus, the updated Kainiterz sodium chloride Mj-Idene prev even after a supply for a Heissauslau- Λ sufficient crushing the kainite a still substantial percentage of relatively large crystals Since the Korriverteilung dec üatriumchlorids during the various stages of processing virtually unchanged finds " the larger crystals are placed in the magnesium sulphate again. Therefore, the ore must be ground more effectively if the grain size of the sodium chloride is actually reduced.

The aim of ürf J n <\ r.ai, i ^ t (lM.fi _(i. · Ο in Vcrf.-ihrcn for making ven y iiliui-K3Uli "f.'t .'J ₁ J · J .. "jnit with rjiihr luilif-r Kalium-Ausbeiito, whereby 1 ', Mi ₁ - ^ i i oh from i: iii.il .'my <ici /; becomes ungeii, so oh no Vorv; fMnung a

SAD ORIGINAL 0098A2 / 1 A29

-4- 1592Ö36

serer Kaliumchloridquellu'i ,,

Furthermore, aluminum sulfai from raw kainite is said to have gained infiltration without enrichment of the ore ?! the greater part of the :. liatriumciilcriie liao '. 'jiiieni very economical, choosing the working cycle easily feasible, uiechani.schen separation methods are a _u sgeschieden.

These and other objectives are achieved by dt s present method, this method of producing Kaliunisul.rt a _u s Rohkainit COVERED st steps?:

(1) Leaching of the ground raw material at over 90 ⁰ G with

P Epsomit circulating brine from stage 3 rait subsequent extraction a Langbeinite pulp consisting of a solid phase which contains langbeinite and sodium chloride, and a langbeinite brine;

Classification

(2) the Langbeinit pulp with excretion of the largest Part of sodium chloride;

(3) Subsequent cooling of the Langbeinit pulp to 35 to 20 ⁰ G in the presence of a Schoenite brine from stage 6 with the formation of a solid phase "a mixture of KCl ₁ ΝειΟΙ, MgSO. _Β 6H ₂ O and / or MgSO..7H ₂ O and an epsomite brine;

(4) Separation of the magnesium sulfate from the chlorides by classification

^ or sieving with partial rejection and partial- wise return of the epsomite brine in stage 1, whereby the Magnesium sulphate is partly fed back into stage 6 and is partially removed from the cycle;

(5) Separation of the potassium chloride from the sodium chloride by dc5s Flotation; ·

(6) At 20 to 35 ° C conversion of part of the Potassium chloride from stage 5 with part of the magnesium sulfate from stage 4 in the presence of a sulphate brine from stage 7 to the extraction of oohoenite (or leonite) a Schoenitsole which is returned to stage 3;

(7) ^ ei 20 bit! 40 G IJmse U-iUiif ·, · des bchoenits with the remaining sodium chloride from the stage [^ in the presence of

009842 / U29 BADORSGiNAL

Water with the production of ivaliumaul <'ut uivi sulfntsole, which is returned to stage 6,

With the present decay, the sodium chloride is not only discharged from the cycle with the drained Üpaomite brine, but also by means of two work processes carried out in two different stages, namely by ^u afr Lan ^ beinit sludge from the hot treatment and

by flotation of the KCl from cold working, because it was found the.; Langbeinite obtained by hot leaching present in the form of small crystals, which after a single

Klaasierungs
After a few minutes, allow the largest part of the iiatrium criloride to separate out easily.

In this way about 70 Isis 30 ^v / o dea of the sodium chloride contained in the kangbeinito sludge can be removed. In the meantime, the small liquid chloride crystals remain in the Langbeinite flame and are therefore to be found in the mixture of the salts obtained by cold treatment, because during the cold

It X £ ls s χ θ run β * "

or sieving process, these crystals pass through together with potassium chloride and a small amount of magnesium sulphate. By means of ari.-jchliesüeride flotation, the potassium chloride is separated from the remaining sodium chloride and magnesium sulphate, which are discharged from the circuit. Thus, according to the invention, a very high potassium sulphate yield is obtained, dl =; based on the ratio between the K ^ O leaving the Kreialauf as KpöO, to the K ^ O introduced into the Kreialauf alo Kainit, and the generally between 84 and 85 "fa" This yield is clearly above the W _a rt, the claimed "the most common process for producing potassium sulfate from kainite _f nämlioh the method of double decomposition and conversion with annohliegaender double implementation, achievable 1st. by double decomposition , .da · dl · Conversion of Kainit into Schoenit and anaohliesaend nozzles Umin KgSO >. includes and that no ® K01 «supply of ausaen

requ-erlioh miiGht »© raiolt raa" a potassium-off booty τοη 60 $ jp .bere-ßhne-t due ü® &
Erelslauf as Ii ₀ BO _n i? 0rl®ßi.®ni, © ßl IC «ü

BATH ORIGINAL

1592Ü38

Kainit ZugG carried out K "0 .. The conversion and application process, η ch dem. Cainite. converted into Schoenit and then the Schoenit is reacted twice with KGl introduced into the circuit, results in a potassium yield of usually JO. . to $ 75, calculated based on the ratio between the circulatory system ais K _? SO. leaving. K _o ü to the dm Kreisla _u f supplied as kainite and KCl Κ-, Ο '

According to the invention, only a small amount of potassium (about 11% by weight) is lost by lowering a rope of the epaomite brine, and the potassium is lost through the solid phases withdrawn from the circuit (waste from hot or raw or hot water) Seven A and by cold flotation) are very limited. Of the three possible treatments of the Langbeinite pulp from hot processing, the conversion into Schoenite and KG1, the conversion into Schoerit and HgSO..7H ₉ O and the conversion into KG1 and. ' HgSO., 6HpO and / or MgSO., 7H ₂ O ₉ leads to the procedure chosen according to the invention, ie the conversion of Langbein into KGl and MgSu ₄ .6H ₂ O and / or MgSO ₄ , 7H ₃ O,: uir. Formation a mother liquor with an increased MgClp content and a low potassium content, so that this process is most advantageous with regard to the potassium yield,

The magnesium chloride content (52 to 65 mol per ΊϋϋΟ mol of water) of the brines, which are in equilibrium with a solid phase consisting of KGl and MgSO..6H ₂ O and / or MgSO ,, 7H ₂ O, ubars * » actually fceigt the already high switching ( "45'bis 52 mol per 1000 mol of water) is of the brine, the solid phase in equilibrium with eLuvr _n us Schoenlt and KGL or Schienit and MgSO _4, 7H O _3.

All of the potassium chloride from the cold treatment of the Langbeinits and a part of M _a gneoiumaulfates from the same 13ohandlungflstufe be umgenetzt ansohlLesaend i "Awei separate stages under Zwißchenbildung of schoenite zu.Kaliumsulfat. Thus, it is erfindungsgemäaa möglioh, Kaliumnulfab leidiglich from kainite herzuotelltn * ie without _e-in; doubles Umio ^ w'isQhen -KGl and Schoonit KOl iiua - a 'äöösereii .Qualle' must be unguided ■■■ "^ -""-'■■■■■ · ■'. = - · ■■. = ■ ■■. ,

BLq varüohledenen stages of eH'induugagemiiuo ^ n föi'i'ahreiui

BATH ORIGINAL

009842 / 142®

-7- 159203Θ

below based on the attached schematic illustration described in detail. In this figure, the solid lines denote the solid phases and the dashed lines denote the Brines.

First stage: leaching of kainite

Per Iio-hkairiit is crushed into pieces, their dimensions between 1 and 10 mm, preferably between 5 and 8 mm. The reduced ore 11 is introduced into the leaching stage 1 together with part 12 of the epsomite brine 17-18 from stage 3.

Leaching takes place at over 90.1 ^° C., preferably at about 100 ^° C.

Second stage: ^K i * üil £ ^U ctis Langbeinits

The Langbeinite pulp 13 from stage 1, consisting of Langbeinite, Sodium chloride and Langbeinitsole is in sTuie 2 introduced. Thereby the solid substances that are due to their Dimensions of a sieve with a mesh size of 0.246 "to 0.4ΐ7 mm, preferably 0.295 to 0.417 mm are not more happen, severed. The 'turnip 14, which is the largest Contains part of the atrium chloride is eliminated from the circulation.

DU »Sh-15 contains the rest of the long-legged accessories, namely 'Lang.beinit, the Uatriumchlorid-Peinteile and'die Langbeinitsole ·

Third stage: conversion of langbeinite into potassium chloride and Epsornit,

The. | Iäü | Ä £ SlS Langbeinlt-Turbidity 15 is combined with the SchoenitBole 16 combined and cooled in stage 3 to 35 to 20 C «Preferably · this cooling takes place step by step in order to achieve the most favorable To create floors for thermal insulation.

On fj-ic-fe V / (, ii.; E one obtains a üomji.eh from KCl, NaCl and MgSO _4. F>] { _? Ü and / or MgSO ^ .VligO. The 'l' temperature of the lower (ir en «β of the mentioned range, namely 20 ° C," so nei./;t

BATH ORIGINAL

- 8 »" · ■■ ".- 1592038

the magnesium sulphate dasu " to precipitate in IOrra by Epsön &t" but if the temperature is near the upper limit, there is a tendency to form MgSO, "6 HgO. If you prefer ^{to work at 20 0} G, the magnesium sulfate precipitates as epsomite

Fourth stage t sieving or cold drainage

The turnip 17 from level 3 is practiced in level 4 or £ e- “Usually sieving is done with a sieve with a clear one

Mesh size from 0.246 to 0.589 mm, but preferably from 0.417 to 0.589 mm *

The above separation 20 of MgSO, _e 6H ₂ O and / or MgSO ^, 7H ₂ O is divided into two parts. The first rope 21 is separated from the circuit, the second rope 22 is introduced into the stage -6 will. secreted yon the Ipsomitsole 18 which WiM divided '-Seils in srwoi ₀ l> he first cable 12 is in the ckge stuf © 1 I ¹ Ii: handle ₉ of the aweito i'eil 19 ^m, optionally after Weiterbeiiaaüliing swee s & ©© yimmag the fact contained potassium - drained »¥ orsugsvi @ is © will be $ 35 to $ 40 am? Ipso- with brine discarded « .""■ - ■■" -. ■

Should Stiafei Sllötation that

Bas Gern! See 23-S- ^ g Kaliiamchlorid "and Matriiaachloraä Mira in the flotation stage 9 entered." As llotatlonsmittol wa? A ; _{,;; u vors}

™ wise aliphatisclie iaaiae veei-jaMoto Di © liaup'tsuell "from Ivatri ehlorid existing flotatlosis waste 24 i ^? @ rclen

SeohstQ Stuf ο s Herst sllimg voa Seaoeait {oaQ & r Sjeosilt)

he

Am Seil äee flootiertexi JCSl 25 wis? D susasMen mit. des Ipsoiiiite (sdea? MgSO _-1 Jο6H _o 0) lsi the Sciiooiiit- (or production stage © 6 QiageiQl-tw '«© - -

As Sol © is in Choe ^ e 8i; ufe © iae sulphate as Ie 26-üiis $ gv öiirCv airigeiulii-to-Up iiksetsmiijg sirii soiisa IiGl usjd Epsomite QSXQl ^ hl · :: Giner ii'empepivfcni? swisölioa CO'ujici 35 ^ 0 ₀ - Toi '^ u ^ svjolusi bei et ".;: ¹ 2Q ^u Go üüü n-ci? liOOMdotüSr ily ^ ötsi« ^ eüifalloütie «^ dut'lv ₍ rr ■ l? o = -

BATH ORIGINAL

-. ! 309041/1428 -

Stuf® -t ZMBQkB ^; 'double ^ r. I ^ BetjBtüig 'is supplied »and from © iiser SG & oenitsole 1§> the bodice in stage 3 ssurtieiegel

Seventh level * double cut

The presence of iron, the water 28 Semisoh 27 from schoenite and possibly KOL with the zurUafcgeblieoenen KCl at between 20 and 40 ⁰ of, iroraugsweise at about 30 ⁰ C

Instead of the potassium chloride from stage 5 being partly fed into stage 6 and partly into stage 7, one passes - as the message shows - the 6eaamtißenge in the

& © in * $ ®.oh . The double liinsetajing you get potassium mlfet 2§ tmä Bulfatsole to, which is led to stage 6 afttefc

the one in the Terseliledeiiön work stages Solen bo-ara ^ ilieroxi -am lEösmen ^ - daaa you the for ^ e-Stuftvoptiaal © ' Show contraction, can raan iioö // ^ efeaXi * -äeap- ^ in - ^ © dt- level / atezutrtgende. Sole. By Busatz in such a way that the saline content is

* D «, there are no rascals φ # ^ iia 4awerjtidt Auf-. Terfitfi3 * # n8to®diRgu »geii Äinsichtlioh

e'inströenden ß

Joltn. irote .Ve- ^ iKdβirong 4 ^ j. Ugly ä @ a eitttitttfföideia-Sr «e # on optimal» keep values «

4 «iV.iieBj | beliii't ₁ r -« «B« - Sieben / * SyklontoelJftBälimg or Ätntr fie-ir «Äy. sti elM-öfeaÄ00ta gutfii l3? getoi «ö« E _r insofar as diee © i in -föisigttitoj? ^ ela · angiwettilet wtrdtn «

% to further I.

BATH ORIGINAL

1592038

Example 1 .

, des- Bfcirijfcargaar Jbai, .1 Op ₁ ⁰ C,

100 g Kainitarss consisting of 67.15 g kainite and 32.85 g NaCl, mrden to a maximum of 6 mm or smaller than large pieces crushed and © ine hour at 100 ⁰ C with 87.30 g circulation brine from the "Step 3 treated" 40.43 g of Iiangbeinite, 29.91 g of NaCl _5, 2.01 g of unconverted kainite and 114.95 g of \

2I ₁₁₁ KIa ₁ Sai _i ermag; _iiiiiii der _{iii i} 1janjgi3sini1; ~ 1! rfit> _i e _ii at _m IQO ⁰ Q '

187 * 30 ' S laagfeeiäit turbidity from level 1 become in one

Kl & aeiere? feeltssidelt & A suitable regulation this »class lmföt iiss excretion of the feilchen with one size. ε1§ / § ₀ 4Ί? ssb., & * 1u der 3? eilehen, which pass a clear sieve- »masehenweit®? © a 0.42 ®® aioht- kQnne'n- · 'Hach 2entri-. _: - fuss. and Waeetaen srlilel't man, - '. 25 * 94 g Klaasierungsabfalle, · ■ passed ms ' 2 ^ 01 g kainite. and "23 ₁ 93 g KaCl. As a fine part ge ^; waam -mm 161 _s | i ^; g Langbainit ^ f rufe® s -4 ¹ CI» 43 g Langbsinit »5.98 € - ^:

161.36 g SaEgbelnit-dÜrübedtr under 2) were given with simultaneous Sue at ζ of "* 76.98 g of mother liquor of the stuf" δ cooled and 5.61 g of water at 2O ⁰ C. It is exceeded

. the '' roaltanä mixture was allowed for four hours at 2O ⁰ C himself "

It was # »22 - ₉ .16. g KGl, 69.49 g MgSo ₄ . 7HgO, 12.42 g NaCl and 139 # 88 g Eps ©! Ttit-Muttt liquor obtained. The potassium content of this mother liquor was 1.89 (5% w. Oil, the sodium content 0, | o #.

4-5) Screening and ff latation at 20 ⁰ C

- Aue one du ^ sh tint lioMe iiebmasohen size of 0.589 mm sitrt® Srttbe of the previous hondan level (243.95 g) was the for the Epsofais to boil, which after Stntrifugitren and Wasohi »- an S®» large 55 # 59 g resulted in *

ufttt! iit #! t "c $$ !! @ Sick Tung consisted of 22, ¹ S g KUX, 12.42 g KECI, S MgSO ^^ LGQ and 138f88'g Sol *. 87 _s 3O g brine were in the

ORIGINAL

1592038-

Step; 1 tückgefüiirt, wMlirenä der Hest (52.58 g) from the circulation discharged * i

flotation - the sifting below, 26.20 g were obtained

■ .Konzentrat (21.50 g-Köl and. 4 * 70 g Nagl) and 22.28 g of waste (15s90 S MgSO ^ ₉ TH ₉ O, _7? 72 g HaOl and 0.66 g £ oil) _# waste 33ie were drained «» ■ '■■.'"" ■

6) Production-vonSchoenit- "at 2G ⁰ O '»

During 1.5 hours, at a temperature of 2O ⁰ O, 26p20 g of Sylvit-Konaentra * and 39.94 g of MgSO ^ 7HgO from the overhead sifting with 55 $ 13 g of sulphate mother liquor from the stage

■ implemented »; Do. "Centrifugation and washing gave 44.34 g | solids; (29 »26 g Solioeait usd 15.08 g IaOl) tmd 76-, 98 g- '

1CÖX was in dis level 7 »the Sol © In the level. 3

■ initiated

At "efaer" Tesperatiii? - iron SO ^V G iDeaandslts mmi 44 ₃ 34 g. solids outside ^: € er Stuf © 6 ös? ei "Stiindes -laag with 3; ϊ ₃ 43 g ^ a ^ r.es ¹ !, Hach Sentrifugierea eriiislt 'maa 22 ₀ 59 g feudales SgiO ^ .- {ga ^ iohts »= · -Massige / Ziasaiiasasetsuag3 It 40 ₃ 21f ^ l MgI O ^ SS ^ I GIs ..O ₅ 96 Pj

re ... vmr4e in Me Stuf © 6 süokssffairöo "

laugh ä ⁵ roclcnc3n Isgea SI ₅ S? § % S0 _£ with an IS ^ O- «Qiialt voa -: 50p04. ^ ο · «α - = / δ Toro. -Bes? © hurries .aui ^ iiid. "des ^ esMlt / ilgsGe tgii doa

■ -Circle in 1? Orni vox »S _n SO„ t ^ sL ^ aü QmXo ^ 'K ₁ J) around the rope / I "ro is- ·" ■■■ - ■ - ■ ■ ■. . "& .- ^ i- ■ ή

Run as XaiKit sufliö3S © «u © Ei IC ₉ O ₅ oet-i; g dig WOi ^ ositaiiisbouts

2.

/ _c '"β

nl 3Z ₀ m s ϊϊ

Π 1.

O Q t ß 4 "? / 1 O S

^ßAD

treated from level 3. 39 »95 g of iangbeinit, 2.01 g were obtained unconverted ICainit, 30.33 g NaCl and 115.01 g Langbeinitsole * , "

2) Classification of the! »Angbeinit-Schläiame at 100 ° €

187 _t 30 g of Langbeinit fruits from stage 1 are treated in a classifier. A suitable regulation of this classifier allows the separation of particles larger than - 0 _t 295 mm. After centrifugation and washing, 27.79 g (2 .01 g bainite and -25.78 g WaOl) classification waste, while 159.51 g Jiangbeinite pulp was made up of 159.51 g Langbeinite pulp from 39.95 g liÄngtoelnit, 4.55 g NaCl and 115.01 g Langbeinite brine won.

3) cooling and decomposition Jer Ijangbeinit-frübe at 20 ⁰ C

159.51 g langbeinite the composition shown under 2) were gleiehgeltigeiB! Susatz> g at 78.05 schoenite-Multer- 'liquor of stage 6 and from 5> 48 g of water at 20 ⁰ C cooled. The obtained fruit was left to stand at 20 ° for four hours.

Bs were 22,311X01 ^ 10,59g HaOl _t 69.92 "β _MgSO4, THgO and 140.21 g Epsomite-Miitterlaugs gewoiwen" Ber potassium content of 'feetrug 1, B? "Tew" $ - ^_r: the Hatrittiagehalt i, 07 -fC. "

Using a sieve with a larger mesh size of 0.417 mm, the Irtibe name of the previous stage (243.04 g) was sieved, as above "msht ^ tinar" 4 the largest part of the Bpsomits'-eliminated. -der-naoh 'Zan'trlügi «rm ^; and an amount of $ 48, $ 4 sold »·

The lowest; SichtttÄg -bsstati4; am «■."22> 31 β-KOl * 10.59 g NaCl ₉ 20 _r 98 g MgSO ₄₄ ? Ugß wi & 140t-tΐ-f.-Bpssomit ^ lltttttriAttgA, 87.30- &. The mother liquor Nurden: -in- di · 'Scales ^1; rtißteg * ftöirs _f - wiflirond-di "remaining 5.2." 91- $: - dem- & re ^

By flotation - the "oait © ren -;. Siei! ItTa» e.received meö- 26 »69- ~ g

^; _? 97 "g NaCl) and 2? 2Ο, 9β g" IgSO ₄ «7 Ha

Let Q ■ i

Manufacture of Schoenit at 2Q ⁰ C

At 20 °, 26.69 g of Sylvit Concentrate and 40.26 g of KgSCL were added. H ₂ O from the overhead sighting with 55.6? g SuIfatliirfeterlauge from step 7 for 1.5 hours. After centrifuging and washing, 29.41 g of sehoenite, 15.16 g of mineral oil, and g of the sehoenite Hutterlauge were obtained.

and, KOl were added in stage 6, the brine in stage 3

In © tar feasferatur of 30 ⁰ C to benandelte 44 * 57 g of solid Stoffel 'from the St ^ fe ß three hours "it 33 _r 61 g of water. üAfter conductive fifuge »erieit 22.32 g of feuciites KgSO ^ (weight

moderate ^ usauanensetssrnngi K 40.47 $ l Ägs 0.8? i »\ Oil 0.90 fi \ "

4-'JSf H ₂ O? 5.82} and $ 5fc # 7 g of sulphate mother liquor * was returned to stage 6.

dry lageit 21 ^ 86 g KgSO ^ with a KgO content of 50> 22 0e ** si. Calculated on the basis of the ratio of the circulation channels K ₂ SO ₄ verlassendem K ₂ O to the circuit supplied as kainite K ₂ O, was the so Gesamtauabeute f 84.84.

of the time limit is called 1OO ⁰ O

100 g of Kiinfttrif consisting of 71.70 g of kainite and 28 _f 30 g of NaCl, were crushed to a maximum or smaller than 6 mm pieces and were treated with 87> 30 g of residual brine from stage 3 at 100%. This gave 42.50 g langbeinite, 2> f $ $ üicht converted © »Ksinlt, 25" 77 g KSCL and f? _R 6 8 $ g

21 .: MiMpM $ mm ^ d # r Xaggfeiinlt ^ Sohlimm »b» i TOO ⁰ O

f % mt0§ixu% ^ SvWtm & m of level 1 will be treated »in tintm classifiers. Mn * appropriate regulation theeaee

#rlapfet ari "e ^ tteeohlfnung dtr f eiloh ·" with a height of "O _f 4t7 m, Nftoh Zeistrifugieriii and fieche" er \ "®" fa, 77 g {% _f n β kainite and 20.62 g NaOl ) Klaeeierung-

BAD 0R! G5NAL

~ ^H ~ 1592038

As a gBenTiegeHde sighting, 16.4 »33 g long-legged beets were obtained 42.50 g Langbeinit, 5 # 15 g 'NaCl and 116.88 g Langbeinit brine obtained,

5) Cooling and decomposition of the Langteinit ~ M.be at 2Ö ° Q

164 »g of 53-Langheinit irübe the stated under 2) were cooperation ^ setaung with simultaneous addition of 87.60 g Schoenit- mother liquor from the stuf β 5 and cooled by 5 ₁ 92 g water at 20 ⁰ C," Man conditioned © the Bread obtained four hours at 2O ⁰ C /

There were 24 * 93 & 11 * K ql _t 58 g NaCl, 77.04 g MgSO ^ .THgO and 144 _f: 5Q g epsomite mother liquor gewoBnen "The potassium content diesex mother liquor was 1 91 _e ^ ew '- ^ ,. the sodium gelialt 1,11 ^ *

4-5) Sieving and flotation

Was repeated using a screen with a clear mm Masehenweite of 0.589 <UEE SchlMnmie from the preceding stage (258> 05g) sieved · As obtnliegende sighting of the largest! Ceil of Epsomits was excreted which gave 61.63 S after centrifugation and washing *

The one below; Sifting consisted of 24 _ft 95 g KCil _t 1t> 58 g 15.1 g MgSO. and t44 _t 5O g Efsoiait ^ slutter liquor; "8ty3Q g liquor were returned to stage 1, while the remainder g) was discharged from the circuit"

By flotation of the belowi; Sifting to obtain _29; 93 g. Sylvit concentrate (24 »45 g KHl and 5» 5 © g Iaßl> and 2f * 99 g incidents (0 ^ 50 g: KGa _t 6.08 gHassl and t5 »4t g waste were drained»

6) H _e3 ? Position of Schoenit at

While t, 5 Stuiid <in were at a '! Outrage of 30 Q 29.93 8 Sylvi-NKonKöÄtrst xmä 45 _t 3? gMgS © ^ »TB ₂ O from the lying Siohttmg with 59p-9Ö g- SuIfat-Mutterlause ftüe-dea? Stuf © umgeaetsst "W, to3te ^ iitrifugiereii and Waecheii you yehielt 31 _t 28 g

QQ9842 / U29

Schoenit * 16 * 39 g KGi and 87.60 g Sühaaiit mother liquor · Schoenit μηά.ΚαΙ - were introduced into stage 7, the brine into stage 3 «;

7) Double insertion "at 30 ^Q ö

At a temperature of 30 ° C., 47.67 g of pesticides from level 6 were treated for three hours with 36.34 g of water. After centrifugation, 24.04 kg of moisture were obtained. (weight composition Kf 40.66 $$ MgJ 0.76 $ | Olί 1 * 03 $> \ SO »; 51.62? 6} .; ~ Brfi _: f0i $ l & Ψ) and 59 _f 98 g sulphate mother liquor« The latter was carried out in äti® level β jDücfc *. ;

23 g 35 g of K ₉ SO, with a K O content of A, were found

- ^ forward «\

due to the fact that the cycle is called K; "SO, read a © next KoO zn d © a the cycle as Kainit flows into the cycle as Kainit-jadem..K ₉ O ^ feetrmg-die ßesamtausfeeute thus 85» 25 ^ ·

BATH ORIGINAL

Claims (1)

P A T E NTANSPR f C H B ί 1. Process for the production of potassium sulfate from raw kainite, characterized in that one a) the comminuted raw ore at a temperature of about 9O ⁰ C by means of a epsomite brine from step 3 to obtain a slurry of a solid-langbeinite, long leg t! and sodium chloride-containing phase and a Langteinitsöle leaching. b) the angbeinite pulp with separation of most of the sodium chloride •, ¹ ' c) the kangbeinit- ^ beet then in the presence of a Schoenitsole from stage 6 while obtaining a solid ■ phase from a mixture of KCl, NaCl and MgSO..6H ₃ O and / or MgSO., 7HpO and an epsomite brine cools down ^{to 20 to 35 0 C,} Classification d) the magnesium sulphate by sieving or from the chlorides separates, with the epsomite brine partially drained and partially recycled to stage 1 and the magnesium sulfate to the. rope in level 6 and partly out of the cycle is deducted, e) the potassium chloride by flotation from the satriuric chloride separates, * f) at a temperature of 20 to 35 ⁰ C and in the presence of sulfate brine from stage 7-part of the potassium chloride from stage 5 with part of the magnesium sulphate from stage 4 with the production of Schoenit (or Leonit) and one in stage 3 rüokzuführendeii ^L ajngbeinitsql © converts and the resulting Sohooniibdi a temperature between 20 and 40 ⁰ C in the presence of water with the remaining potassium chloride from the ^ stage. | with the recovery of potassium sulphate and a sulphate oil to be fed back into stage 6. ; '-; y ■ . .'- 2, method, according to Ansp.ruoh I _1, thereby gekenhBelehnet _# that the kainite ore is comminuted to pieces with abraessungen below 5 to 8 mm. . : 3 · The method according to claim 2, characterized in that at gs iangbeinits the solids, the dimensions of which are so large that they have a sieve with a clear mesh size from 0.295 - 0.417 mm not flour? happen from the one to be treated Material to be separated »" 4 * Terfahren according to claim 1 to 3 # characterized in that the separation of the MgSO ^ * 6HgO and / or MgS0. * 7Hg0 from KCl and Jiaßl is carried out using sieve devices with clear mesh sizes of 0.417 ~ 0.589 n " ¹¹ . For SINCAT Söcietä Industriale Catanese S.p.A. Lawyer BATH ORIGINAL »■■ ti- - .. ft Blank page