SK279011B6 - Method for conversion of ammonium sulphate to potassium sulphate - Google Patents
Method for conversion of ammonium sulphate to potassium sulphate Download PDFInfo
- Publication number
- SK279011B6 SK279011B6 SK449-95A SK44995A SK279011B6 SK 279011 B6 SK279011 B6 SK 279011B6 SK 44995 A SK44995 A SK 44995A SK 279011 B6 SK279011 B6 SK 279011B6
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- Slovakia
- Prior art keywords
- potassium
- water
- suspension
- sulphate
- ammonium
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- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims abstract description 17
- 235000011130 ammonium sulphate Nutrition 0.000 title claims abstract description 17
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 title claims abstract description 13
- 229910052939 potassium sulfate Inorganic materials 0.000 title claims abstract description 13
- 235000011151 potassium sulphates Nutrition 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 title abstract description 9
- 239000001166 ammonium sulphate Substances 0.000 title abstract description 5
- 239000001120 potassium sulphate Substances 0.000 title abstract description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 19
- 150000003839 salts Chemical class 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001103 potassium chloride Substances 0.000 claims abstract description 10
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 10
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 11
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000011591 potassium Substances 0.000 abstract description 3
- 229910052700 potassium Inorganic materials 0.000 abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract 1
- 150000003841 chloride salts Chemical class 0.000 abstract 1
- 210000003608 fece Anatomy 0.000 abstract 1
- 239000010871 livestock manure Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000618 nitrogen fertilizer Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- DHKHZGZAXCWQTA-UHFFFAOYSA-N [N].[K] Chemical compound [N].[K] DHKHZGZAXCWQTA-UHFFFAOYSA-N 0.000 description 1
- -1 ammonia cation Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910052815 sulfur oxide Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
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- Fertilizers (AREA)
Abstract
Description
Oblasť technikyTechnical field
Vynález sa týka spôsobu premeny síranu amónneho na síran draselný, pri ktorom sa zmiešavajú vodné roztoky síranu amónneho a chloridu draselného v mólovom pomere čistých solí 1 až 1,25 ku 2.The present invention relates to a process for the conversion of ammonium sulfate to potassium sulfate by mixing aqueous solutions of ammonium sulfate and potassium chloride in a molar ratio of pure salts of 1 to 1.25 to 2.
Doterajší stav technikyBACKGROUND OF THE INVENTION
Síran draselný je syntetická draselná soľ používaná najmä ako draselné hnojivo na pestovanie kvetov, zeleniny, ovocia, tabaku a iných rastlín neznášajúcich vysokú koncentráciu chloridov obsiahnutých v lacnejšom draselnom hnojive - chloride draselnom.Potassium sulphate is a synthetic potassium salt used mainly as a potassium fertilizer for the cultivation of flowers, vegetables, fruit, tobacco and other plants not tolerating the high concentration of chlorides contained in the cheaper potassium fertilizer - potassium chloride.
Dominantným spôsobom výroby síranu draselného je podvojný rozklad minerálu schonitu s chloridom draselným podľa reakcie:The dominant method of potassium sulfate production is the double decomposition of schonite mineral with potassium chloride according to the reaction:
Kaso4 . MgSO„ . 6H20 + 2KC1 —— 2K2SO4 + MgCl2 . 6H2OKaso 4 . MgSO '. 6 H 2 0 + 2KC1 - 2R 2 SO 4 + MgCl second 6H 2 O
Síran amónny je syntetické dusíkaté hnojivo. V súčasnosti sa vyrába spracovávaním jeho vodných roztokov odpadajúcich zo syntézy kaprolaktámu, metylmetakrylátu a amoniakálnej výpierky odplynov obsahujúcich oxidy síry.Ammonium sulfate is a synthetic nitrogen fertilizer. It is currently produced by treating its aqueous solutions resulting from the synthesis of caprolactam, methyl methacrylate and the ammonia scrubber containing sulfur oxides.
Veľký nárast uvádzaných výrob spojených s nutným sprievodným výrobkom síranom amónnym viedol k mimoriadnemu zvýšeniu produkcie síranu amónneho a spôsobil pokles jeho ceny pod úroveň hodnoty v ňom obsiahnutých surovín.The large increase in the reported production linked to the necessary by-product ammonium sulphate led to an extraordinary increase in the production of ammonium sulphate and caused its price to fall below the value of the raw materials contained therein.
Tento stav je príčinou hľadania postupov umožňujúcich efektívnejšie zužitkovanie síranu amónneho.This situation is the reason for the search for methods for more efficient utilization of ammonium sulfate.
Jednou z možností riešenia problému je v technickej literatúre už dávno opísaná premena síranu amónneho na síran draselný účinkom chloridu draselného, prebiehajúca podľa rovnice:One possible solution to the problem is the conversion of ammonium sulphate to potassium sulphate by the action of potassium chloride in the technical literature, according to the equation:
(NH4)25O4 + 2KC1 --->- K2SO4 + 2NH4C1(NH 4 ) 2 5O 4 + 2KCl ---> - K 2 SO 4 + 2NH 4 C1
Z tejto rekcie vychádza aj spôsob opísaný v CS AO č. 269030. Jeho nevýhodou je vyššia energetická náročnosť a nižšia výťažnosť.The reaction described in CS AO no. 269030. Its disadvantage is higher energy consumption and lower yield.
Cieľom vynálezu je vytvoriť postup umožňujúci dosahovanie vysokých výťažkov a dobrej kvality síranu draselného.It is an object of the present invention to provide a process for achieving high yields and good quality of potassium sulfate.
Podstata vynálezuSUMMARY OF THE INVENTION
Uvedenú úlohu rieši spôsob premeny síranu amónneho na síran draselný, pri ktorom sa zmiešavajú vodné roztoky síranu amónneho a chloridu draselného v mólovom pomere čistých solí 1 až 1,25 ku 2, ktorého podstata spočíva v tom, že sa odparením vody upraví jej mólový pomer proti súčtu molov vstupujúcich solí na 7,5 až 5,0 ku 1, horúca suspenzia sa ochladí na teplotu +45 až +20°C, prídavkom čpavku sa upraví jej pil na hodnotu 7,0 až 12,0, výhodne na hodnotu pH 10,0, a takáto suspenzia sa separuje za súčasného premývania oddeľovaného kryštálu vodou.The object of the present invention is to provide a process for converting ammonium sulfate to potassium sulfate by mixing aqueous solutions of ammonium sulfate and potassium chloride at a molar ratio of pure salts of 1 to 1.25 to 2 by adjusting the molar ratio of the the sum of moles of the incoming salts to 7.5 to 5.0 to 1, the hot suspension is cooled to +45 to + 20 ° C, the ammonia is adjusted to pH 7.0 to 12.0 by addition of ammonia, preferably pH 10 1.0, and such a suspension is separated by washing the separated crystal with water.
Výhodou premeny síranu amónneho na síran draselný podľa vynálezu je nízka energetická náročnosť procesu, nakoľko do premeny priamo vstupuje vodný roztok síranu amónneho.The advantage of the conversion of ammonium sulfate to potassium sulfate according to the invention is the low energy consumption of the process, as the aqueous ammonium sulfate solution directly enters the conversion.
Výhodou postupu je dosahovanie 86 až 93 percentnej výťažnosti síranu draselného na do premeny vstupujúci drahší chlorid draselný.The advantage of the process is to achieve 86 to 93 percent recovery of potassium sulfate per conversion of more expensive potassium chloride.
Ďalšou výhodou postupu je získavanie produktu s nízkym obsahom chloridov - na úrovni 0,3 až 1,0 % hmotn. a stopercentná rozpustnosť získanej soli.Another advantage of the process is to obtain a product with a low chloride content - at a level of 0.3 to 1.0% by weight. and 100% solubility of the salt obtained.
Charakteristickým znakom technického síranu draselného vyrobeného postupom podľa vynálezu je súčasná prítomnosť amoniakálneho dusíka s koncentráciou 0,6 až 3,0 % hmotn., čo ho čiastočne zaraďuje medzi dvojzložkové draselno-dusíkaté hnojivá.A characteristic feature of the technical potassium sulphate produced by the process of the invention is the simultaneous presence of ammoniacal nitrogen at a concentration of 0.6 to 3.0% by weight, which partially classifies it as a two-component potassium-nitrogen fertilizer.
Príklady uskutočnenia vynálezuDETAILED DESCRIPTION OF THE INVENTION
Príklad 1Example 1
400 g vodného roztoku síranu amónneho obsahujúceho 150,8 g rozpustnej soli bolo zmiešané so 450 g vodného roztoku chloridu draselného obsahujúceho 149,1 g rozpustnej soli.400 g of an aqueous ammonium sulfate solution containing 150.8 g of a soluble salt was mixed with 450 g of an aqueous potassium chloride solution containing 149.1 g of a soluble salt.
Zo vzniknutej suspenzie bolo za atmosférického tlaku odparené 13,4 g vody.13.4 g of water were evaporated from the resulting suspension under atmospheric pressure.
Horúca suspenzia s teplotou 108 °C bola za miešania ochladzovaná na vodnom kúpeli. Pri dosiahnutí teploty +60°C bol do suspenzie uvádzaný plynný čpavok. Suspenzia bola ochladená na teplotu +28°C a pH upravené na hodnotu 11.The hot suspension at 108 ° C was cooled in a water bath with stirring. Ammonia gas was suspended in the suspension at + 60 ° C. The suspension was cooled to + 28 ° C and adjusted to pH 11.
Takto upravená suspenzia bola separovaná vákuovou filtráciou. Kryštál bol premytý 30 g vody. Po vysušení bolo získané 161 g soli a 578 g materského lúhu. Výťažok kryštálu K2SO4 predstavoval 92,4 %.The suspension thus treated was separated by vacuum filtration. The crystal was washed with 30 g of water. After drying, 161 g of salt and 578 g of mother liquor were obtained. The yield of K 2 SO 4 crystal was 92.4%.
Príklad 2Example 2
Dávkovacím čerpadlom bolo do zmiešavača uvádzané 1807 kg/hod. vodného roztoku chloridu draselného obsahujúceho 594,2 kg čistej soli. Druhým dávkovacím čerpadlom bolo do toho istého zmiešavača privádzané 1379 kg/hod. vodného roztoku síranu amónneho obsahujúceho 579,3 kg čistej soli.1807 kg / h was fed into the mixer via a metering pump. aqueous potassium chloride solution containing 594.2 kg of pure salt. A second metering pump supplied 1379 kg / h to the same mixer. aqueous ammonium sulfate solution containing 579.3 kg of pure salt.
Zmes roztokov plynulé vstupovala do vákuovej odparky pracujúcej za absolútneho tlaku 40 kPa. Pri teplote cca 70°C bolo zo zmesi oddestilované 398,2 kg/hod. vody. Horúca suspenzia odtekala do kryštalizátora s nútenou cirkuláciou suspenzie cez chladič, v ktorom bola ochladzovaná na teplotu +33°C. Do ochladenej suspenzie bol privádzaný plynný čpavok v množstve 8 kg/hod., ktorého účinkom dochádzalo k úprave pH roztoku na hodnoty 9,5 až 10,5.The solution mixture was continuously fed to a vacuum evaporator operating at an absolute pressure of 40 kPa. At a temperature of about 70 ° C, 398.2 kg / h were distilled off from the mixture. water. The hot slurry flowed to a crystallizer with forced circulation of the slurry through a condenser where it was cooled to + 33 ° C. The cooled slurry was fed with ammonia gas at a rate of 8 kg / hr to adjust the pH of the solution to 9.5-10.5.
Suspenzia bola odvádzaná na odstredivku. Odstreďovaný kryštál bol premývaný 80 1 /hod. vody.The suspension was drained onto a centrifuge. The centrifuged crystal was washed with 80 L / h. water.
Hodinové množstvo vyrábaného síranu draselného po vysušení na obsah vody 0,4 % hmotn. predstavovalo 598 kg·The amount of potassium sulfate produced per hour after drying to a water content of 0.4% by weight. amounted to 598 kg ·
Analýzami bol vo vysušenom produkte zistený obsah chloridov 0,56 % hmotn., síranov 55,9 % hmotn. a amoniakového katiónu 3,.4 %, čo zodpovedá 49 % K2O a 2,7 %Analyzes revealed a chloride content of 0.56% by weight, a sulfate content of 55.9% by weight in the dried product. and an ammonia cation of 3.4%, which corresponds to 49% K 2 O and 2.7%
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SK449-95A SK279011B6 (en) | 1995-04-05 | 1995-04-05 | Method for conversion of ammonium sulphate to potassium sulphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SK449-95A SK279011B6 (en) | 1995-04-05 | 1995-04-05 | Method for conversion of ammonium sulphate to potassium sulphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| SK44995A3 SK44995A3 (en) | 1996-11-06 |
| SK279011B6 true SK279011B6 (en) | 1998-05-06 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SK449-95A SK279011B6 (en) | 1995-04-05 | 1995-04-05 | Method for conversion of ammonium sulphate to potassium sulphate |
Country Status (1)
| Country | Link |
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| SK (1) | SK279011B6 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000021887A1 (en) * | 1998-10-13 | 2000-04-20 | Airborne Industrial Minerals Inc. | Method of formulating alkali metal salts |
-
1995
- 1995-04-05 SK SK449-95A patent/SK279011B6/en unknown
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000021887A1 (en) * | 1998-10-13 | 2000-04-20 | Airborne Industrial Minerals Inc. | Method of formulating alkali metal salts |
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| Publication number | Publication date |
|---|---|
| SK44995A3 (en) | 1996-11-06 |
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