DE82460C - - Google Patents
Info
- Publication number
- DE82460C DE82460C DENDAT82460D DE82460DA DE82460C DE 82460 C DE82460 C DE 82460C DE NDAT82460 D DENDAT82460 D DE NDAT82460D DE 82460D A DE82460D A DE 82460DA DE 82460 C DE82460 C DE 82460C
- Authority
- DE
- Germany
- Prior art keywords
- phosphoric acid
- phosphate
- lime
- calcium
- alkali
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 10
- 235000015450 Tilia cordata Nutrition 0.000 claims description 10
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 10
- 239000004571 lime Substances 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 235000021317 phosphate Nutrition 0.000 claims description 7
- QORWJWZARLRLPR-UHFFFAOYSA-H Tricalcium phosphate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 6
- 239000001506 calcium phosphate Substances 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011593 sulfur Substances 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- JGIATAMCQXIDNZ-UHFFFAOYSA-N Calcium sulfide Chemical compound [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 claims description 2
- FAYYUXPSKDFLEC-UHFFFAOYSA-L calcium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [Ca+2].[O-]S([O-])(=O)=S FAYYUXPSKDFLEC-UHFFFAOYSA-L 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims 2
- 229940078499 tricalcium phosphate Drugs 0.000 claims 2
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims 2
- 235000019731 tricalcium phosphate Nutrition 0.000 claims 2
- 238000004140 cleaning Methods 0.000 claims 1
- 238000010309 melting process Methods 0.000 claims 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims 1
- 159000000000 sodium salts Chemical class 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K [O-]P([O-])([O-])=O Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 6
- 239000010452 phosphate Substances 0.000 description 6
- AGVJBLHVMNHENQ-UHFFFAOYSA-N Calcium sulfide Chemical compound [S-2].[Ca+2] AGVJBLHVMNHENQ-UHFFFAOYSA-N 0.000 description 4
- 229910000318 alkali metal phosphate Inorganic materials 0.000 description 4
- 229910000389 calcium phosphate Inorganic materials 0.000 description 4
- 235000011010 calcium phosphates Nutrition 0.000 description 4
- 229940055700 calcium sulfide Drugs 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate dianion Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K Tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L na2so4 Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N Sodium sulfide Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- MBMLMWLHJBBADN-UHFFFAOYSA-N iron-sulfur Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 description 2
- 150000004763 sulfides Chemical class 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N AI2O3 Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000004135 Bone phosphate Substances 0.000 description 1
- 229960003563 Calcium Carbonate Drugs 0.000 description 1
- JUNWLZAGQLJVLR-UHFFFAOYSA-J Calcium pyrophosphate Chemical compound [Ca+2].[Ca+2].[O-]P([O-])(=O)OP([O-])([O-])=O JUNWLZAGQLJVLR-UHFFFAOYSA-J 0.000 description 1
- RXBWSDCVQBUVEC-UHFFFAOYSA-K P(=O)([O-])([O-])[O-].[O-2].[Fe+5] Chemical class P(=O)([O-])([O-])[O-].[O-2].[Fe+5] RXBWSDCVQBUVEC-UHFFFAOYSA-K 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L Potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- DPLVEEXVKBWGHE-UHFFFAOYSA-N Potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 1
- 229910052936 alkali metal sulfate Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium monoxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000005712 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- WMWXXXSCZVGQAR-UHFFFAOYSA-N dialuminum;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3] WMWXXXSCZVGQAR-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011872 intimate mixture Substances 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical group [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910000160 potassium phosphate Inorganic materials 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000001187 sodium carbonate Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000019798 tripotassium phosphate Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B11/00—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
- C05B11/04—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMT.^PATENT OFFICE. ^
Um phosphorsaure Alkalien aus dreibasisch phosphorsaurem Kalk oder einem Rohmaterial, welches solchen enthält, zu gewinnen, erhitzt man diese Körper in fein vertheiltem Zustande mit Lösungen von Schwefelalkalien, wobei sich das Kalkphosphat mit dem Alkalisulfid derartig umsetzt, dafs phosphorsaures Alkali in Lösung geht.To obtain phosphoric acid alkalis from tribasic phosphoric acid lime or a raw material, to obtain whatever contains such, these bodies are heated in a finely divided state with solutions of alkaline sulfur, the lime phosphate with the alkali sulfide in such a way converts that phosphoric acid alkali goes into solution.
Zum Gelingen des Verfahrens ist es nothwendig, dafs der phosphorsaure Kalk als Tricaiciumphosphat, nicht etwa, wie in der Thomasschlacke, als vierbasisch phosphorsaurer Kalk zur Anwendung kommt; sodann mufs die benutzte Lösung mehr Schwefelalkali enthalten, als zur Zersetzung des phosphorsauren Kalkes erfordert wird. Die Ausbeute erhöht sich überdies beträchtlich, wenn man die Erhitzung unter Druck bei ca. 1500 C. vornimmt. For the process to be successful it is necessary that the phosphoric acid lime be used as tricaicium phosphate, not, as in the Thomas slag, as tetrabasic phosphoric acid lime; then the solution used must contain more alkaline sulfur than is required for the decomposition of the phosphoric acid lime. The yield is increased, moreover, considerably when the heating is carried out under pressure at about 150 0 C..
Man kann das Verfahren auch dahin abändern, dafs man das Kalkphosphat mit Kohle und einem Ueberschufs von Alkalisulfat zusammenschmilzt, um die Schmelze dann entweder in der Siedehitze oder unter Druck bei 1500C. zu behandeln. Hierzu mufs man die Menge des zur Verwendung gelangenden Alkalisulfates gröfser bemessen, als es die Ueberführung des gesammten Calciumphosphats und des möglicherweise auch vorhandenen Calciumcarbonats in Calciumsulfid erfordern würde. Es bilden sich dann hauptsächlich Schwefelalkalien nebst wenig Alkaliphosphat und -carbonat; aber beim Behandeln der Schmelze mit kaltem Wasser tritt alsbald eine ergiebige Umsetzung zu Alkaliphosphat ein,One can also modify then, that melting together the phosphate of lime with carbon and an excess Schufs of alkali sulfate to treat the melt then either at the boiling temperature or under pressure at 150 0 C. the process. For this purpose, the amount of alkali metal sulfate used must be larger than would be required to convert all of the calcium phosphate and any calcium carbonate that may also be present into calcium sulfide. Mainly alkaline sulfur and a little alkali phosphate and carbonate are then formed; but when the melt is treated with cold water, a productive conversion to alkali metal phosphate takes place immediately,
die beim Erhitzen auf 1 oo° bezw. 1500 C. fast vollständig wird.which when heated to 1 oo ° respectively. 150 0 C. almost completely.
Das beschriebene Verfahren unterscheidet sich wesentlich von den früheren Versuchen, den phosphorsauren Kalk durch Schmelzen mit Natriumsulfat und Kohle aufzuschliefsen, wobei man entweder auf eine Ausbeute an Alkaliphosphat gänzlich verzichtete oder diese Ausbeute durch nachträgliche Einwirkung von Kohlensäure zu erzielen strebte. Nach dem neuen Verfahren wird durch das Zusammenschmelzen von Tricaiciumphosphat mit überschüssigen Mengen von Natriumsulfat und Kohle die Bildung einer reichlichen Menge von Natriumsulfid und eine innige Mischung dieses Körpers mit dem Calciumphosphat bezweckt, wonach dann erst durch Behandlung des erhaltenen Gemisches mit Wasser die Umsetzung zu Natriumphosphat und Calciumsulfid von Statten geht.The procedure described differs significantly from previous attempts, the To dissolve phosphoric acid lime by melting with sodium sulfate and charcoal, whereby either a yield of alkali metal phosphate was dispensed with entirely or this yield sought to achieve by subsequent exposure to carbonic acid. According to the new process, by melting together of tricaicium phosphate with excess amounts of sodium sulfate and charcoal the formation of an abundant amount of Sodium sulphide and an intimate mixture of this body with calcium phosphate are intended, after which the reaction is only then carried out by treating the mixture obtained with water to sodium phosphate and calcium sulfide.
In der letzteren Reaction, nämlich der Umwandlung von Tricaiciumphosphat in Alkalipliosphat durch Kochen mit überschüssiger Alkalisulfidlösung, liegt die Eigenart des neuen Verfahrens. Dasselbe war auch dadurch noch nicht gegeben, dafs man versucht hatte, Thonerde- und Eisenoxydphosphate durch Schwefelnatrium umzusetzen (engl. Pat. Nr. 2069 vom Jahre 1876). Denn Thonerde- und Eisenoxydverbindungen bilden mit Schwefelalkalien vollkommen unlösliche Körper (nämlich Aluminiumoxydhydrat bezw. Schwefeleisen), die durch Alkaliphosphatlösungen unter keinen Umständen verändert werden; dals aber Kalkverbindungen durch Behandlung mit Lösungen von über-In the latter reaction, viz. The conversion of tricium phosphate into alkali metal phosphate by boiling with excess alkali sulfide solution, lies the peculiarity of the new Procedure. The same was not yet the case because attempts had been made to and to convert iron oxide phosphates with sodium sulphide (English Pat. No. 2069 of Year 1876). Because alumina and iron oxide compounds form perfectly with alkaline sulfur insoluble bodies (namely aluminum oxide hydrate or sulfur iron), which under no circumstances are affected by alkali metal phosphate solutions to be changed; then, however, lime compounds by treatment with solutions of over-
schüssigem Schwefelalkali zersetzt werden, war nach den bisherigen Erfahrungen nicht vorauszusehen, ebensowenig dals das hierbei gebildete Calciumsulfid durch Einwirkung von Alkaliphosphatlösungen nicht wiederum in Calciumphosphat zurückverwandelt wird.are decomposed by excess sulfuric alkali, could not be foreseen based on previous experience, just as little as the calcium sulfide formed by the action of Alkali phosphate solutions are not converted back into calcium phosphate.
Aus den erhaltenen Laugen kann man das Natriumphosphat durch Eindampfen und Auskrystallisiren bald chemisch rein erhalten; das rückständige Schwefelnatnum wird wieder eingedickt und von neuem benutzt oder durch Einblasen von Kohlensäure in Natriumcarbonat übergeführt.The sodium phosphate can be obtained from the alkaline solutions obtained by evaporation and crystallization soon obtained chemically pure; the remaining sulfurous atnum is thickened again and used again or converted into sodium carbonate by blowing in carbonic acid.
Das Kaliumphosphat, welches nicht krystallisirbar ist, wird von dem beigemengten Schwefelkaiium befreit, indem man den letzteren Körper entweder durch Phosphorsäurelösung zersetzt oder in Sulfat bezw. Carbonat überführt und diese Salze dann auskrystallisiren läfst. Das gewonnene Erzeugnifs ist dann natürlich nicht vollkommen frei von Kaliumsulfat bezw. -carbonat. The potassium phosphate, which cannot be crystallized, is obtained from the admixed potassium sulphide liberated by decomposing the latter body either by phosphoric acid solution or in sulfate respectively. Carbonate and these salts are then allowed to crystallize out. That Obtained product is then of course not completely free from potassium sulfate or. carbonate.
Der beim Auslaugen der Schmelze verbleibende Rückstand besteht wesentlich noch aus Kohle, Schwefelcalcium (nebst etwas Schwefeleisen, möglicherweise auch kohlensaurem Kalk und Aetzkalk), sowie aus geringen Mengen unzersetzten phosphorsauren Kalkes. Um letzteren nutzbar zu machen, führt man das Calciumsulfid durch Oxvdation an der Luft in Calciumhyposulfit über, laugt dasselbe mit Wasser aus und setzt es dann mit Natriumsulfat um. Das nach dem Auslaugen zurückbleibende Gemenge von Calciumphosphat, Kohle und Gyps dient entweder als Düngemittel oder zur Darstellung von Phosphorsäure.The residue that remains when the melt is leached out still exists from coal, calcium sulphide (along with some iron sulphide, possibly also carbonic acid Lime and caustic lime), as well as from small amounts of undecomposed phosphoric acid lime. In order to make the latter usable, the calcium sulfide is carried out by oxidation on the Air in calcium hyposulfite, leaches the same with water and then sets it with sodium sulfate around. The mixture of calcium phosphate, coal and gypsum that remains after leaching is used either as fertilizer or for the preparation of phosphoric acid.
Claims (4)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE82460C true DE82460C (en) |
Family
ID=354866
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT82460D Active DE82460C (en) |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE82460C (en) |
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0
- DE DENDAT82460D patent/DE82460C/de active Active
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