CS221002B1 - Method of making the water solutions of nitrates and/or magnesium chlorides - Google Patents
Method of making the water solutions of nitrates and/or magnesium chlorides Download PDFInfo
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- CS221002B1 CS221002B1 CS667781A CS667781A CS221002B1 CS 221002 B1 CS221002 B1 CS 221002B1 CS 667781 A CS667781 A CS 667781A CS 667781 A CS667781 A CS 667781A CS 221002 B1 CS221002 B1 CS 221002B1
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- Czechoslovakia
- Prior art keywords
- magnesium
- calcium
- carbon dioxide
- reaction mixture
- nitrate
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- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical class [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 title claims description 19
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 235000011147 magnesium chloride Nutrition 0.000 title claims description 12
- 150000002823 nitrates Chemical class 0.000 title claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 48
- 239000011777 magnesium Substances 0.000 claims description 43
- 239000011575 calcium Substances 0.000 claims description 32
- 229910052749 magnesium Inorganic materials 0.000 claims description 26
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 25
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 18
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 claims description 17
- 239000001569 carbon dioxide Substances 0.000 claims description 17
- 239000011541 reaction mixture Substances 0.000 claims description 17
- 239000000395 magnesium oxide Substances 0.000 claims description 15
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 15
- 235000012245 magnesium oxide Nutrition 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 229910052791 calcium Inorganic materials 0.000 claims description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 10
- 239000003337 fertilizer Substances 0.000 claims description 10
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 9
- 229910002651 NO3 Inorganic materials 0.000 claims description 8
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000001110 calcium chloride Substances 0.000 claims description 8
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 8
- 235000011148 calcium chloride Nutrition 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 7
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 6
- 239000000347 magnesium hydroxide Substances 0.000 claims description 6
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 6
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000012736 aqueous medium Substances 0.000 claims description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 2
- 229940091250 magnesium supplement Drugs 0.000 claims 3
- 229960000869 magnesium oxide Drugs 0.000 claims 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 16
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 11
- 235000010216 calcium carbonate Nutrition 0.000 description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 5
- 235000019341 magnesium sulphate Nutrition 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000001095 magnesium carbonate Substances 0.000 description 4
- 235000014380 magnesium carbonate Nutrition 0.000 description 4
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 4
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001863 plant nutrition Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- ICSSIKVYVJQJND-UHFFFAOYSA-N calcium nitrate tetrahydrate Chemical compound O.O.O.O.[Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ICSSIKVYVJQJND-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000009533 lab test Methods 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- ZHJGWYRLJUCMRT-UHFFFAOYSA-N 5-[6-[(4-methylpiperazin-1-yl)methyl]benzimidazol-1-yl]-3-[1-[2-(trifluoromethyl)phenyl]ethoxy]thiophene-2-carboxamide Chemical compound C=1C=CC=C(C(F)(F)F)C=1C(C)OC(=C(S1)C(N)=O)C=C1N(C1=C2)C=NC1=CC=C2CN1CCN(C)CC1 ZHJGWYRLJUCMRT-UHFFFAOYSA-N 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005842 biochemical reaction Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000000102 chelatometric titration Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000009109 curative therapy Methods 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 239000000040 green colorant Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003898 horticulture Methods 0.000 description 1
- 229910052928 kieserite Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- OJXVUEMVNWMNCR-UHFFFAOYSA-L magnesium;potassium;sulfate Chemical compound [Mg+2].[K+].[O-]S([O-])(=O)=O OJXVUEMVNWMNCR-UHFFFAOYSA-L 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000011785 micronutrient Substances 0.000 description 1
- 235000013369 micronutrients Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- -1 sulphate anion Chemical class 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/38—Magnesium nitrates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Description
-Vynález, sa týká.sposobu výroby vodných roztokov dusičnanov a/alebo chloridov horečnatých z horečnatých surovin obsahujúcich uhličitanový, alebo hydrogenuhličitanový anión, kysličník, alebo hydroxid horečnatý, ktorého podstata spočívá v tom, že horečnatá surovina obsuhujúca uhličitanový a/alebo hydrogenuhličitanový anión, a/alebo kysličník a/alebo hydroxid horečnatý sa vo vodnom prostředí podrobí chemickej reakcii s dusičnanom a/alebo chloridom vápenatým, a to bez, alebo v přítomnosti kysličníka uhličitého a/alebo kyseliny uhličitej a/alebo v přítomnosti niektorej z jej vo vodě rozpustných solí, pričom volný kysličník uhličitý a připadne tiež kysličník uhličitý odpovedajúci konverzii hydrogenuhličitanov na normálně uhličitany sa připadne z reakčnej zmesi v ďalšom stupni výrobného procesu odstráni a reakciou vzniknutý dusičnan a/ /alebo chlorid horečnatý sa z reakčnej zmesi připadne ďalej oddělí vo formě vodného roztoku, alebo reakčná zmes sa spracuje na suspenzné hnojivo obsahujúce hořčík a vápník.
Vynález sa týká spósobu výroby vodných roztokov dusičnanov a/alebo chloridov horečnatých z horečnatých surovin obsahujúcich uhličitanový alebo hydrouhličitanový anion, kysličník alebo hydroxid horečnatý.
Hořčík patří medzi nevyhnutné zložky rastlinné] výživy a je podstatnou zložkou rastlinného zeleného farbiva chlorofylu.
Vplýva na premiesťovanie živin, predovšetkým fosforu zo starých listov a stoniek do rastúcich rastlín. Zjistil sa tiež priaznivý vplyv horčíka na priebeh oxido-redukčných procesov v rastlinách. Je aktivátorom biochemických reakcí vedúcich k tvorbě glycidov a procesov spojených s premenou fosforu v rastlinách. Potvrdilo sa tiež, že pri nedostatku horčíka sa hromadia v listoch rastlín monosacharidy.
Nateraz medzi najpoužívanejšie priemyselné hnojivá obsahujúce hořčík patria například Thomasova múčka (7 % MgO); Kamex (asi 3,5 % MgO viazaného vo formě MgSOá); Emgekali (asi 5 % vo formě MgSOd) kieserit (technický MgSCh); dolomitické vápence s obsahom asi 20 % MgCb; magnezitový úlet z kalcinačných pecí, obsahujúci asi 65 % MgO a špeclálne listové hnojivá, ktoré sa v súčasnosti pripravyjú do výroby a ktoré obsahujú hořčík viazaný na síranový anión.
Hořčík patří medzi tie rastlinné živiny, ktoré sú rastliny schopné velmi dobře sorbovať aj fcez listy. Ako uvádza JÚRGENS, G. [Der Erwerbs — Gártner č. 17 (26), apríl 1972]; WITTWER, S. H. („Foliar Application of Fertilizer“ — Department of Horticulture, Michigan State University, East Lansing, Michigah, USA) a HUDSKÁ, G. [Agrochemie 16 (5), 144 (1976)] doba polovičnej sorbcie horčíka listovou plochou je asi 2 až 5 hodin, kým například pre sorbciu vápnika, zinku a mangánu sa uvádza doba 1 až 2 dni a 50%-ná sorbcia draslíka po jeho foliarnej aplikácii sa dosahuje až počas ,10 až 24 dni.
Z uvedených dóvodoch sa v zahraničí a v posledných rokoch i u nás vyvíja viacero špeciálnych priemyselných hnojív obsahujúcich popři ostatných základných, sekundárných a mikroživinách tiež hořčík, určený predovšetkým pre mimokoreňovú výživu rastlín.
Popři sírane horečnatom, resp. sírane horečnato-draselnom sa ako vhodný zdroj horčíka uvádza tiež dusičnan horečnatý, najmá v zmesiach s močovinou a základným dusíkatým roztokom [Agrochémia 16, 12, 344-348 (1976)]. Ukázalo sa, že MgSCU a Mg(NO3)2
MgCCb + Ca(NO3)2 ----MgCO3 + CaCk ----MgCCb + CO2 + H2O ---MgO + 2CO2 + H2O ----Mg(OH + 2CO2 ----Mg(HCO3)2 + Ca(NO3)2 ----Mg(HCO3)2 + CaCl2 ---MgO + 2CO2 + Ca(NO3)2 + H2O--MgO + 2CO + CaCl2 + H2O ---Ca(HCO3)2 —---► sú vhodnými zdrojmi horčíka pre preventivné ale i kuratívne ošetrovanie pofnohospodárskych kuitúr.
Základem doposial' používaných spůsobov výroby Mg(N£>3)2 je rozklad — tzv. vylúhovanie horečnatej suroviny (obvykle kalcinovaného magnezitu) kyselinou dusičnou za vzniku tzv. hnedej suspenzie, filtráciou ktorej sa v ďalšej časti výrobného procesu získá čistý roztok dusičnanu horečnatého a vápenatého. NAJMR, S. uvádza („Výroba MgO nitrátovým zposobom s využitím vedlejších produktov a odpadlých látok“, Košice 1974), že proces vylúhovania možno viesf tak, aby filtrát pozostával prevažne z Mg(NO3)2 s malým obsahom Ca(NO3)2, pričom ich koncentrácia v roztoku je asi 40 percent [Mg(NO3)2 4- CaíNOáJz], obsah Fe sa pohybuje okolo 2.10_4% sa vyskytuje len v stopách.
Teraz sa zistilo, že vodné roztoky dusičnanov a/alebo chloridov horečnatých možno z horečnatých surovin připravit spósobom podfa vynálezu, ktorého podstata spočívá v tom, že horečnatá surovina obsahujúca uhličitanový a/alebo hydrogenúhllčitanový anión a/alebo kysličník a/alebó hydroxid horečnatý sa vo vodnom prostředí podrobí chemické j reakcii s dusičnanom a/aiebo chlorídom vápenatým, a to bez alebo v přítomnosti kysličníka uhličitého a/alebo kyseliny uhličitej a/alebo v přítomnosti niektorej z jej vo vodě rozpustných solí.
Volný kysličník uhličitý a připadne tiež kysličník uhličitý odpovedajúci konverzii hydrogenuhličitanov na normálně uhličitany sa připadne z reakčnej zmesi v ďalšom stupni v záujme prehlbeniá konverzie odstráni. Nejjednoduchšie možno kysličník uhličitý z reakčnej zmesi odstráníf jej zahratim a/alebo prevzdušnením. Podvojným rozkladom vzniknutý dusičnan a/alebo chlorid horečnatý vo formě vodného roztoku sa z reakčnej zmesi připadne v ďalšej fáze výrobného procesu odstráni, s výhodou sedimentáciou, filtráciou alebo odstředěním. V případe výroby horečnato-vápenatého suspenzního hnojivá možno reakčnú zmes bez separácie špracovať na produkt uvedeného typu stabilizáciou tuhého podielu obsahujúceho uhličitan vápenatý vzniknutý reakciou.
Ako už z uvedeného vyplývá, pri značnom zjednodušení možno spósob výroby dusičnanu a/alebo chloridu horečnatého podfa vynálezu znázornit týmito chemickými rovnicami:
Mg(NG3)'2 -I- CaCO3 (1)
MgCl2 + CaCO3 (2)
Mg(HCO3)2 (3)
Mg(HCO3)2 (4)
Mg(HCO3)2 (5)
Mg(NO3(2 + Ca(HCO3)2 (6)
MgCl2 + Ca(HCOrf)>2 (7)
Mg(NO3)2 + Ca(HCO3)2 (8)
MgClz + Ca(HCO3)2 (9)
CaCO3 + CO2 + H2O (10)
Priebeh reakcii v smere zlava doprava je podmienený značnými rozdielmi v rozpustnosti jednotlivých zložiek, pričom najmenšiu rozpustnost v študovanom systéme vykazujú CaCO3 a Ca(HCO3)2 [rozpustnosti CaCO3, Ca(HCO3j2 a Mg(HO3j2 vo vodě sú pri 25 °C 3 . ΙΟ“3 o/o caCOs; 0,43% Ca(HCO3)2 a 13,0% Mg(HCO3)2 pri 18 °C],
V porovnaní s dnes používanými výrobnými postupmi má spósob podl'a vynálezu celý rad výhod, z ktorých možno uviesť, že příprava Mg(NO3)2, resp. MgCh týmto spósobom sa uskutočňuje bez nárokov na spotřebu minerálnych kyselin HNO3 resp. HClj, ako horečnatá surovina možu byť použité v hojnom množstve v přírodě sa vyskytujíce minerály (magnezit, dolomit).
Vhodným zdrojom Ca(NO3]2 a CaClž možu byť rózne sekundárné produkty anorganických technologií, ktorých významnou súčasťou sú uvedené typy vápenatých solí (napr. tetrahydrát dusičnanu vápenatého vznikajúci ako vedlejší produkt pri výrobě granulovaného NPK-hnojiva vymrazovacou technológiou, alebo koncentrovaný vodný roztok CaCh odpadajúci pri výrobě extrakčnej H3PO4 procesom „IMI“ — po rozklade fosfátu kyselinou chlorovodíkovou a pod.J.
Zdrojom kysličníka uhličitého možu byť odplyny z viacerých procesov anorganickej alebo organickej chemickej technologie (výpierky CO2 v súvislosti s přípravou syntéznej zmesi pri výrobě amoniaku, dekarbonizačné procesy, procesy kvasnej chémie a pod.), alebo tiež plynné produkty rozmanitých spalovacích procesov a podobné. Procesom podfa vynálezu sa zhodnocujú pre výživu rastlín obe reakčné zložky, keďže popři vodorozpustnej horečnatej soli tvoriacej hlavný reakčný produkt je úplné zhodnotitefná tiež druhá zložka reakcie — CaCO3 resp. Ca(HCO3). Vzhíadom na koloidný charakter v reakčnej sústave tvoriacich sa uhličitanov vápenatých, vyznačujú sa tieto vysokou neutralizačnou schopnosťou, čo móže byť s výhodou využité pri zásobnom melioračnom hnojení pódy vápenatou zložkou. Vychádzajúc z koloidného charakteru tuhých čiastočiek obsiahnutých v rovnovážnej sústave, uhličitany vápenaté, ktoré tvoria ich podstatu, možu byť s výhodou použité na přípravu stabilných vápenatých suspenzných hnojív.
Za určitých okolností, najma pre hnojenie pódy horčíkom. pri súčasnej potrebe vápenia, možno reakčnú zmes použiť po úpravě jej fyzikálno-mechanických vlastností (stabilizácii dispergovaných tuhých častíc) a připadne i po úpravě jej chemického zloženia, priamo ako účinné suspenzné horečnato-vápenaté hnojivo. Výrobný proces v zmysle vynálezu je mimoriadne jednoduchý, nekladie vysoké nároky na strojno-technologické zariadenie ani z Wadiska vývoja špeciálnych zariadení ani atypického riešenia jednotlivých aparátov. Vyvinutý proces neuvažuje s používáním látok hořlavých, žieravých ani toxických, nekladie mimoriadne požiadavky na obsluhu a možno ho kontinualizovať.
Ďalej uvádzané příklady objasňujú, avšak neobmedzujú predmet vynálezu.
Prieklad 1 až 5
Spósob výroby vodného roztoku dusičnanu horečnatého reakciou kysličníka horečnatého s dusičnanom vápenatým v přítomnosti kysličníka uhličitého a vody podfa vynálezu v zmysle ideovej reakčnej schémy:
I. MgO + 2CO2 + Ca(NO3)2 + H2O —> —> Mg(NO3)2 + Ca(HCO3)2 resp.
t
II. Ca(HCO3)2---> CaCO3 + CO2 + H2O sme experimentálně ověřovali v sérii orientačných laboratórnych pokusov.
Počas urobených piatich pokusov sme pracovali s rovnakými návažkami týchto základných reakčných zložiek:
.v. /? ΐ!’; (
8,2 g kysličníka horečnatého (chemicky čistý)
47,8 g kryštalického dusičnanu vápenatého [Ca(NO3]2.4H2O] a
59,1 g prevarenej destilóvanej vody (laboratórnej teplotýj.
V 1. a 2. pokuse sme pri teplote miestnosti reakčnú zmes — suspenziu připravená zhomogenizovaním vyššie uvedených zložiek sýtili po dobu 50 minút za miešania
17,8 g plynného kysličníka uhličitého, připraveného sublimácion tuhého kysličníka uhličitého.
Počas 3. a 4 pokusu sme sýtenie suspenzie kysličníkom uhličitým, vzhíadom na zvýšené množstvo použitého tuhého resp. plynného CO2, predížili na 60 resp. 71 minút. V piatom pokuse sme pracovali s navážkou
35,6 g tuhého CO2, pričom suspenziu připravenu zmiešaním 59,1 gramu vody, 47,8 gramu Ca-(NO3)2.4H2O a 8,2 gramu MgO sme sýtili kysličníkom uhličitým za miešania po dobu 80 minút. Po uplynutí uvedenej doby (po ukončení sýtenia kysličníkom uhličitým) sme v případe pokusov 1 a 3 reakčnú zmes ihned' rozdělili filtráciou cez sklenenú filtračnú fritu „S-4“, u pokusov 2, 4 a 5 sme tak urobili až po hodinovom povarení reakčnej zmesi na vodnom kúpeli (95 až 100 °Cj.
Vážením sme stanovili množstvá získaných filtrátov a vlhkých filtračných koláčov pre jednotlivé pokusy a vo filtráte sme chelatometrickými titráciami stanovili obsah horčíka a vápnika. Získané výsledky sú súhrnne uvedené v tabufke 1.
210 0 2
Tabulka 1
Hmotnostně množstvá zložiek Příklad získaných separáciou reakčnej zmesi resp. (g)
Obsah sledovaných zložiek vo filtráte
Příklad 6 až 9
Spósob výroby chloridu horečnatého vo formě jeho vodného roztoku reakciou kysličníka horečnatého s chloridom vápenatým v přítomností kysličníka a vody, podfa vynálezu, v zmysle ideovej reakčnej schémy:
I. MgO + 2CO2 + CaCl2 + H2O —---—-——► MgCl2 + Ca(HCO3)2 resp.
t
II. Ca(HCO3]2 ----> CaCO3 + CO2 + H2O sme experimentálně ověřovali v sérii nasledujúcich laboratórnych pokusov.
Vo všetkých pokusoch tejto série (příklady 6 až 9) sme pracovali s rovnakými navážkami týchto základných reakčných zložiek:
12,7 g kysličník horečnatý (chemicky čistý)
35,0 g bezvodý chlorid vápenatý
75,7 g prevarená destilovaná voda (labor. teploty).
V príkladoch 6 a 7 sme reakčnú zmes— — suspenziu pripravenú zhomogenízovaním vyššie uvedených zložiek sýtili prí teplote miestnosti po dobu 60 minút 41,6 g plynného kysličníka uhličitého, získaného odpařením tuhého CO2. Počas pokusov 8 a 9 sa postupovalo obdobným spósobpm pričpm reakčnú zmes sme po dobu 75 resp. 80 minút sýtili 55,5 g plynného CO2.
Po ukončení sýtenia reakčnej zmesi kysličníkom uhličitým sme u pokusov 6 a .8 reakčnú zmes ihned rozdělili filtrácipu cez sklenenú fritu „S-4“ a v případe pokusov 7 a 9 sme tak urobili až po 1 hodinovotn ppvarení reakčnej zmesi na vodnom kúpeli.
Vážením sme stanovili množstvá získaných filťrátov ako aj vlhkých koláčov a v čirých filtrátech sme chelatometricky stanovili obsah horčíka a vápnika.
Dosiahnuté výsledky sú zhrnuté v tabui'ke 2.
Tabulka 2
Příklad Hmotnostně množstva zložiek resp. získaných separáciou reakčnej zmesi Obsah sledovaných zložiek pokus (g)
číslo filtračný koláčThe invention relates to a process for the production of aqueous solutions of nitrates and / or magnesium chlorides from magnesium raw materials containing a carbonate or bicarbonate anion, an oxide or magnesium hydroxide, characterized in that the magnesium feedstock containing carbonate and / or bicarbonate anion, / or the oxygen and / or magnesium hydroxide is chemically reacted with nitrate and / or calcium chloride in the aqueous medium, without or in the presence of carbon dioxide and / or carbonic acid and / or in the presence of one of its water-soluble salts, wherein the free carbon dioxide and optionally also the carbon dioxide corresponding to the conversion of the bicarbonate to the normal carbonate is removed from the reaction mixture at a further stage in the production process and the nitrate and / or magnesium chloride formed therefrom is further separated from the reaction mixture in in the form of an aqueous solution, or the reaction mixture is worked up into a suspension fertilizer containing magnesium and calcium.
The invention relates to a process for the manufacture of aqueous solutions of nitrates and / or magnesium chlorides from magnesium raw materials containing a carbonate or bicarbonate anion, oxide or magnesium hydroxide.
Magnesium is one of the essential ingredients of plant nutrition and is an essential component of the plant green colorant chlorophyll.
It affects the transfer of nutrients, especially phosphorus from old leaves and stems into growing plants. The beneficial effect of magnesium on the course of oxidation reduction processes in plants was also found. It is an activator of biochemical reactions leading to the formation of carbohydrates and processes associated with phosphorus conversion in plants. It has also been confirmed that in the absence of magnesium, monosaccharides accumulate in plant leaves.
To date, the most commonly used fertilizers containing magnesium include, for example, Thomas meal (7% MgO); Camex (about 3.5% MgO bound as MgSO4); Emgekali (about 5% in the form of MgSO4) kieserite (technical MgSO4); dolomitic limestones containing about 20% MgCl2; magnesite drift from calcining furnaces, containing about 65% MgO and special foliar fertilizers that are currently being prepared for production and which contain magnesium bound to the sulphate anion.
Magnesium is one of the plant nutrients that plants are able to absorb sorbent leaves very well. As stated by JURGENS, G. (Der Erwerbs - Gártner No. 17 (26), April 1972); WITTWER, SH ("Foliar Application of Fertilizer" - Department of Horticulture, Michigan State University, East Lansing, Michigah, USA) and HUDSKÁ, G. [Agrochemistry 16 (5), 144 (1976)] about 2 to 5 hours, while for example, for the sorption of calcium, zinc and manganese, a period of 1 to 2 days is reported, and 50% sorption of potassium after its foliar application is only achieved for 10 to 24 days.
For these reasons, a number of special industrial fertilizers have been developed abroad and in the last few years also in our country containing magnesium along with other basic, secondary and micronutrients, intended especially for extra-root plant nutrition.
In addition to magnesium sulphate, respectively. magnesium potassium sulphate also mentions magnesium nitrate as a suitable source of magnesium, in particular in mixtures with urea and a nitrogenous basic solution [Agrochemistry 16, 12, 344-348 (1976)]. MgSO4 and Mg (NO3) 2 were shown
MgCCb + Ca (NO3) 2 and MgCO3 + CaCl ---- ---- MgCCb + CO2 + H2O --- MgO + 2CO 2 + H 2 O ---- Mg (OH + 2CO2 ---- Mg (HCO3) 2 + Ca (NO3) 2 ---- Mg (HCO3) 2 + CaCl2 --- MgO + 2CO2 + Ca (NO3) 2 + H2O - MgO + 2CO + CaCl2 + H2O --- Ca (HCO3) 2 —- --► are suitable sources of magnesium for preventive and curative treatment of agricultural cultivars.
The methods of Mg (N? 3) 2 production hitherto used are based on decomposition - the so-called leaching of the magnesium raw material (usually calcined magnesite) with nitric acid to form a so-called brown slurry, by filtration to obtain a pure magnesium nitrate solution. calcium. NAJMR, S. states ("Production of MgO by a nitrate process using by-products and waste products", Košice 1974) that the leaching process can be conducted so that the filtrate consists predominantly of Mg (NO 3) 2 with a low Ca (NO 3) 2 content, whereas their concentration in the solution is about 40 percent [Mg (NO 3) 2 4 - Ca 2 NO 2] 2, the Fe content is about 2.10 -4 % occurs only in traces.
It has now been found that aqueous solutions of nitrates and / or magnesium chlorides can be prepared from magnesium raw materials by the method of the invention, characterized in that the magnesium feedstock containing a carbonate and / or hydrogen carbonate anion and / or oxygen and / or magnesium hydroxide is aqueous. it is subjected to a chemical reaction with nitrate and / or calcium chloride, in the presence or absence of carbon dioxide and / or carbonic acid and / or one of its water-soluble salts.
Free carbon dioxide and optionally carbon dioxide corresponding to the conversion of bicarbonates to normal carbonates are removed from the reaction mixture in the next step in order to deepen the conversion. Most simply, the carbon dioxide can be removed from the reaction mixture by heating and / or aerating. The nitrate and / or magnesium chloride formed by the decomposition in the form of an aqueous solution is removed from the reaction mixture in a further stage of the production process, preferably by sedimentation, filtration or centrifugation. In the case of the production of magnesium-calcium suspension fertilizer, the reaction mixture can be worked up without separation into a product of the above type by stabilizing the solids containing the calcium carbonate formed by the reaction.
As is clear from the foregoing, the process for producing the nitrate and / or magnesium chloride of the present invention can be illustrated by the following chemical equations:
Mg (NG3) '2-I-CaCO3 (1)
MgCl 2 + CaCO 3 (2)
Mg (HCO 3) 2 (3)
Mg (HCO 3) 2 (4)
Mg (HCO 3) 2 (5)
Mg (NO 3 (2 + Ca (HCO 3 ) 2) (6)
MgCl 2 + Ca (HCOrf)> 2 (6)
Mg (NO 3) 2 + Ca (HCO 3) 2 (8)
MgCl 2 + Ca (HCO 3) 2 (9)
CaCO3 + CO2 + H2O
The progress of the reaction in the direction from left to right is conditional substantial difference in the solubility of the individual components, with the smallest solubility studied, the system exhibit CaCO3 and Ca (HCO3) 2 [solubility of CaCO3, Ca (HCO3j2 and Mg (HO 3 j2 water being at 25 ° C for 3 . ΙΟ "3 o / o CaCO 0.43% Ca (HCO 3) 2 and 13.0% Mg (HCO3) 2 at 18 ° C]
Compared with the production methods used today, the process according to the invention has a number of advantages, from which it can be stated that the preparation of Mg (NO3) 2, respectively. MgCl in this way is carried out without the requirement of consumption of mineral acids HNO3 resp. HCl, as a magnesium raw material, can be used in abundance of naturally occurring minerals (magnesite, dolomite).
Suitable sources of Ca (NO3) 2 and CaCl2 may be various secondary products of inorganic technologies, of which the aforementioned types of calcium salts (e.g. calcium nitrate tetrahydrate formed as a byproduct in the production of granular NPK fertilizer by freeze technology) or concentrated aqueous CaCl3 in the production of extraction H3PO4 by the "IMI" process - after decomposition of phosphate with hydrochloric acid and the like J.
The source of carbon dioxide can be degasses from several processes of inorganic or organic chemical technology (CO2 scrubbing in connection with the preparation of the synthesis mixture in ammonia production, decarbonisation processes, fermentation chemistry processes, etc.) or also gaseous products of various combustion processes and the like. In the process according to the invention, both reactants are evaluated for plant nutrition, since, in addition to the water-soluble magnesium salt constituting the main reaction product, the second reaction component - CaCO3 resp. Ca (HCO 3 ). Due to the colloidal nature of the calcium carbonate-forming reaction system, they are characterized by a high neutralization capacity, which can be advantageously used in the stock fertilization of the soil by the calcium component. Starting from the colloidal nature of the solid particles contained in the equilibrium system, the calcium carbonates constituting them can advantageously be used for the preparation of stable calcium suspension fertilizers.
In certain circumstances, especially for fertilizing the soil with magnesium. With the simultaneous need for liming, the reaction mixture can be used as an effective suspension magnesium-calcium fertilizer after adjusting its physico-mechanical properties (stabilization of the dispersed solid particles) and, optionally, after adjusting its chemical composition. The manufacturing process according to the invention is extremely simple, does not impose high demands on the machine-technology equipment either from the Wadiska development of special equipment or atypical solution of individual devices. The developed process does not consider the use of flammable, corrosive or toxic substances, does not impose any special requirements on operation and can be continualised.
The following examples illustrate but do not limit the invention.
Example 1 to 5
Process for producing an aqueous magnesium nitrate solution by reacting magnesium oxide with calcium nitrate in the presence of carbon dioxide and water according to the invention according to the ideological reaction scheme:
I. MgO + 2CO2 + Ca (NO3) 2 + H2O ->-> Mg (NO 3 ) 2 + Ca (HCO 3 ) 2 resp.
t
II. Ca (HCO3) 2 ---> CaCO3 + CO 2 + H2O was experimentally verified in a series of indicative laboratory experiments.
During the five experiments we worked with the same weights of the following basic reactants:
.in. /? ΐ! '; (
8.2 g of magnesium oxide (chemically pure)
47.8 g of crystalline calcium nitrate [Ca (NO3) 2.4H2O] a
59.1 g of boiled distilled water (room temperature).
In the first and second experiments at room temperature, the reaction mixture - suspension prepared by homogenizing the above-mentioned components was saturated with stirring for 50 minutes
17.8 g of carbon dioxide gas, prepared by sublimation of solid carbon dioxide.
During the 3 rd and 4 th trials, we were saturated with carbon dioxide, due to the increased amount of solids used, respectively. CO2, increased to 60 resp. 71 minutes. In the fifth experiment, we worked with the load
35.6 g of solid CO2, the suspension prepared by mixing 59.1 grams of water, 47.8 grams of Ca- (NO3) 2.4H2O and 8.2 grams of MgO, was saturated with carbon dioxide under stirring for 80 minutes. At the end of this time (after the carbonation), in the case of experiments 1 and 3, the reaction mixture was immediately separated by filtration through a glass filter frit "S-4", in experiments 2, 4 and 5 we did so after one hour of boiling. in a water bath (95-100 ° C).
We determined the amounts of filtrates and wet filter cakes obtained for each experiment by weighing, and we determined the magnesium and calcium contents in the filtrate by chelatometric titrations. The results obtained are summarized in Table 1.
210 0 2
Table 1
Mass quantities of ingredients (G)
Content of monitored components in the filtrate
Examples 6 to 9
Process for producing magnesium chloride in the form of an aqueous solution thereof by reacting magnesium oxide with calcium chloride in the presence of oxide and water according to the invention according to the ideological reaction scheme:
I. MgO + 2CO2 + CaCl2 + H2O —---—-—— ► MgCl2 + Ca (HCO3) 2 resp.
t
II. Ca (HCO3) 2 ----> CaCO3 + CO2 + H2O was experimentally verified in a series of laboratory experiments.
In all experiments of this series (Examples 6 to 9) we worked with the same weights of the following basic reactants:
12.7 g magnesium oxide (chemically pure)
35.0 g anhydrous calcium chloride
75.7 g boiled distilled water (room temperature).
In Examples 6 and 7, the reaction slurry prepared by homogenizing the above constituents was saturated at room temperature for 60 minutes with 41.6 g of carbon dioxide gas obtained by evaporating solid CO 2. Experiments 8 and 9 were followed in a similar manner, with a reaction time of 75 and 75, respectively. 80 minutes saturated with 55.5 g of CO2 gas.
After the carbonation of the reaction mixture was complete, in experiments 6 and 8, the reaction mixture was immediately distributed through the "S-4" sintered glass frit and in the case of experiments 7 and 9, this was done only after 1 hour of shaping the reaction mixture on a water bath.
We determined the amounts of the filtrates and wet cakes obtained by weighing, and the clear filtrates were chelatometrically determined for magnesium and calcium.
The results obtained are summarized in Table 2.
Table 2
Example The mass of the components respectively. obtained by separation of reaction mixture Content of monitored components experiment (g)
filter cake numberClaims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS667781A CS221002B1 (en) | 1981-09-10 | 1981-09-10 | Method of making the water solutions of nitrates and/or magnesium chlorides |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS667781A CS221002B1 (en) | 1981-09-10 | 1981-09-10 | Method of making the water solutions of nitrates and/or magnesium chlorides |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS221002B1 true CS221002B1 (en) | 1983-04-29 |
Family
ID=5414382
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS667781A CS221002B1 (en) | 1981-09-10 | 1981-09-10 | Method of making the water solutions of nitrates and/or magnesium chlorides |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS221002B1 (en) |
-
1981
- 1981-09-10 CS CS667781A patent/CS221002B1/en unknown
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