DE5061C - Process for the preparation of pure potassium carbonate and potassium hydrocyte - Google Patents
Process for the preparation of pure potassium carbonate and potassium hydrocyteInfo
- Publication number
- DE5061C DE5061C DENDAT5061D DE5061DA DE5061C DE 5061 C DE5061 C DE 5061C DE NDAT5061 D DENDAT5061 D DE NDAT5061D DE 5061D A DE5061D A DE 5061DA DE 5061 C DE5061 C DE 5061C
- Authority
- DE
- Germany
- Prior art keywords
- potassium
- potash
- chlorine
- carbonate
- soda
- 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
Links
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 title claims description 38
- 239000001184 potassium carbonate Substances 0.000 title claims description 11
- 229910000027 potassium carbonate Inorganic materials 0.000 title claims description 11
- 238000002360 preparation method Methods 0.000 title claims description 4
- 238000000034 method Methods 0.000 title description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 title description 2
- 239000011591 potassium Substances 0.000 title description 2
- 229910052700 potassium Inorganic materials 0.000 title description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 57
- 235000015320 potassium carbonate Nutrition 0.000 claims description 25
- 229940072033 potash Drugs 0.000 claims description 16
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 13
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- 239000012452 mother liquor Substances 0.000 claims description 5
- 239000001187 sodium carbonate Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 4
- 150000003841 chloride salts Chemical class 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000005712 crystallization Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxyl anion Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 239000003518 caustics Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 description 9
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate dianion Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- -1 potassium chlorine Chemical compound 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 150000003464 sulfur compounds Chemical class 0.000 description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N Potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L Potassium sulfate Chemical group [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- DPLVEEXVKBWGHE-UHFFFAOYSA-N Potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 235000013379 molasses Nutrition 0.000 description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 description 2
- 239000001120 potassium sulphate Substances 0.000 description 2
- 235000011151 potassium sulphates Nutrition 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000016068 Berberis vulgaris Nutrition 0.000 description 1
- 241000335053 Beta vulgaris Species 0.000 description 1
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N iron-sulfur Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000003112 potassium compounds Chemical class 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- 239000004323 potassium nitrate Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
- C01D1/30—Purification; Separation by crystallisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Paper (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Description
1877.1877.
Klasse 76.Class 76.
EMIL MEYER in CÖPENICK.
Verfahren zur Darstellung von reinem Kaliumcarbonat und Kaliumhydroxyd,EMIL MEYER in CÖPENICK.
Process for the preparation of pure potassium carbonate and potassium hydroxide,
Patentirt im Deutschen Reiche vom 19. October 1877 ab.Patented in the German Empire on October 19, 1877.
Die Leiclitlöslichkeit des Carbonats und des Hydroxyds von Kalium erschwert deren technisch ausführbare Trennung von anderen leicht löslichen Salzen. Während die Abscheidung von Kaliumsulfat verhältnifsmäfsig leicht möglich ist, bietet die vollständige Entfernung des Natriumcarbonats und des Chlorkaliums gröfsere Schwierigkeiten. The solubility of the carbonate and the hydroxide of potassium makes them technically difficult feasible separation from other easily soluble salts. During the deposition of Potassium sulphate is relatively easily possible, but the complete removal of the sodium carbonate offers and potassium chlorine greater difficulties.
i. Trennung der Soda.
Es ist zwar bekannt, dafs beim Eindampfen einer Lösung von Soda und Potasche das
erstere Alkali zunächst und in gröfserer Menge ausfällt, jedoch hat bisher die auf diesem Wege
durch Calciniren der Mutterlauge hergestellte Potasche noch immer einen Gehalt von 3
bis 4pCt. Soda. Die Abscheidung des Natriumcarbonats
gelingt jedoch vollständig, wenn die Lösung des Kaliumcarbonats bis zum Volumengewicht
von 1,6 verdampft wird. Dann, jedoch erst bei dieser Concentration, fällt alle
Soda vollständig aus; die in der Hitze davon getrennte Lösung von Potasche erstarrt beim
Erkalten zu einer Krystallmasse, dem Hydrat des Kaliumcarbonats (K1 CO3 -f- 2 H2 O), und
giebt nachher beim Eindampfen und Calciniren ein natriumfreies Carbonat. Letzteres ist, falls
Chlorverbindungen in der Lösung enthalten waren, nicht frei davon, sondern enthält noch
bis zu 2 pCt. Chlorkalium.i. Separation of the soda.
It is known that when a solution of soda and potash is evaporated, the first alkali precipitates out in greater quantities, but the potash produced in this way by calcining the mother liquor still has a content of 3 to 4 pCt. Soda. However, the separation of the sodium carbonate is complete if the solution of the potassium carbonate is evaporated to a volume weight of 1.6. Then, but only at this concentration, all the soda falls out completely; The solution of Potasche, separated from it in the heat, solidifies on cooling to a crystalline mass, the hydrate of potassium carbonate (K 1 CO 3 -f- 2 H 2 O), and afterwards gives a sodium-free carbonate on evaporation and calcination. If the solution contained chlorine compounds, the latter is not free of it, but still contains up to 2 pCt. Potassium chloride.
Die Abscheidung des Natriumcarbonats gelingt nur dann vollständig, wenn aufser Chloriden und Carbonaten keine anderen Verbindungen vorhanden sind. Bei Gegenwart von Schwefelkalium, Hyposulfit oder Aetzkali wird nicht alle Soda durch die Concentration auf 1,6 Volum-Gewicht ausgefällt. Das Verfahren eignet sich namentlich zur Reinigung der aus den Rübenmelassen gewonnenen Potasche, bei deren Herstellung die vollständige Abscheidung der Soda bisher nicht ausgeführt wurde. Für diesen Zweck ist es jedoch erforderlich, vorher die Schwefelverbindungen der Melassenkohle dadurch zu entfernen, dafs sie mittelst Calcinirens in Sulfat übergeführt werden. Nachdem dies geschehen und aus der wiedergelösten Potasche. das schwerlösliche Sulfat abgeschieden ist, gelingt es, eine vollständig natriumfreie Potasche zu gewinnen, wie sie für Herstellung der Naturkorn-Schmierseifen erforderlich ist, und von der selben Güte, wie sie bisher nach dem Leblanc-Procefs nur aus einem ganz natriumfreien Chlorkalium gewonnen wurde.The separation of the sodium carbonate only succeeds completely if in addition to chlorides and carbonates no other compounds are present. In the presence of potassium sulphide, Hyposulfite or caustic potash is not all soda by concentrating to 1.6 volume weight failed. The process is particularly suitable for cleaning the potash obtained from the beet molasses Manufacture the complete separation of the soda has not been carried out so far. For this Purpose it is however necessary beforehand the sulfur compounds of the molasses charcoal thereby to be removed, so that they are converted into sulphate by means of calcination. After this happen and from the redissolved potash. the sparingly soluble sulfate is deposited, succeeds it is to win a completely sodium-free potash, as it is required for the production of natural grain soft soaps, and of the the same quality as it was previously made from a completely sodium-free potassium chloride based on the Leblanc Procefs was won.
Diese nach letzterem Verfahren hergestellte sehr reine Potasche ist jedoch selten ganz chlorfrei, weil das durch Behandlung von Chlorkalium mit Schwefelsäure im technischen Grofsbetriebe hergestellte Kaliumsulfat stets geringe Mengen Chlor enthält, das sich nacher in der Potasche wiederum vorfindet. Im Handel ist deshalb natriumfreie, selten aber chlorfreie Potasche anzutreffen.This very pure potash produced by the latter process is seldom completely chlorine-free, however, because this is achieved by treating potassium chlorine with sulfuric acid in large-scale technical operations Potassium sulphate produced always contains small amounts of chlorine, which is later in the potash again finds. Sodium-free, but rarely chlorine-free, potash is therefore on the market to be found.
2. Trennung des Chlorkaliums.2. Separation of the potassium chlorine.
Ich bewirke die Herstellung eines chlorfreien und gleichzeitig natriumfreien Kaliumcarbonats dadurch, dafs ich die Schwerlöslichkeit desselben in Aetzkalilösung für die technische Reinigung benutze. s I produce a chlorine-free and at the same time sodium-free potassium carbonate by using its poor solubility in caustic potash solution for technical cleaning. s
Die beim Leblanc-Procefs entstehenden Potaschelaugen enthalten eine grofse Menge Kaliumhydroxyd und man hat nur nöthig, die aus den Schmelzen entstehenden Laugen zur Dichtigkeit von 1,47 bis 1,56 Volum-Gewicht einzudampfen und in geklärtem Zustande abkühlen zu lassen. Es krystallisirt dann reines Kaliumcarbonat von der Formel K1 CO3, 2 H1 O in grofsen Krystallen aus. Die Krystalle sind leicht von der Mutterlauge zu befreien und lassen nach dem Auflösen in Wasser die etwa mechanisch beigemengten Unreinigkeiten von Schwefeleisen etc. ungelöst. Die Lösung giebt beim Calciniren eine Potasche, die nur 0,1 bis 0,2 pCt. Chlorkalium enthält und ganz frei von Natrium ist. Durch Wiederholung dieses Vorganges bezw. durch Auskrystallisiren aus einer reineren Aetzkalilösung ist die Herstellung eines vollkommen reinen Kaliumcarbonats möglich.The potash eyes produced in the Leblanc process contain a large amount of potassium hydroxide, and it is only necessary to evaporate the alkalis produced from the melts to a density of 1.47 to 1.56 volume weight and to allow them to cool in a clarified state. Pure potassium carbonate then crystallizes out of the formula K 1 CO 3 , 2 H 1 O in large crystals. The crystals can easily be freed from the mother liquor and, after dissolving in water, leave the impurities of iron sulphide, etc., mechanically mixed in, undissolved. When calcined, the solution gives a potash which is only 0.1 to 0.2 pct. Contains potassium chlorine and is completely free of sodium. By repeating this process respectively. by crystallizing out a purer caustic potash solution, the production of a completely pure potassium carbonate is possible.
3. Herstellung von Kaliumhydroxyd.3. Manufacture of potassium hydroxide.
Wenn die rohen, Aetzkali enthaltenden Laugen, die übrig bleiben, nachdem die gröfsten Mengen Carbonat auf eben beschriebenem Wege auskrystallisirt sind, bis zur Stärke von 1,5 oder 1,54 Volum-Gewicht eingedampft werden, so fällt fast alles Carbonat in der Siedhitze aus. Aus der übrig bleibenden Lauge von Aetzkali und Schwefelkalium krystallisirt beim Erkalten die Verbindung KOH, H1 O, und zwar in grofsen blättrigen Krystallen. von bedeutenderIf the crude alkalis containing caustic potash, which remain after the greatest amounts of carbonate have crystallized out in the manner just described, are evaporated to a strength of 1.5 or 1.54 volume weight, almost all the carbonate precipitates in the boiling point . From the remaining lye of caustic potash and potassium sulphide, the compound KOH, H 1 O, crystallizes on cooling, in large, leafy crystals. of significant
Reinheit, wenn] man, nach dem Erkalten auf 40 bis 6p° C. die noch nicht erstarrte Flüssigkeit von den Krystallen trennt. Die Chlor- und Schwefelverbindungen bleiben in der Mutterlauge, welche ein Aetzkali mit weniger Wasser enthält, als die Krystalle, und welche nachher weiter auf ein unreines Aetzkali oder auf Potasche verarbeitet wird, während die zurückbleibenden Krystalle durch Erwärmen zum Schmelzen gebracht werden und flüssig in die zum Versandt bestimmten Gefäfse gelangen, um darin zu erstarren. Falls eine noch gröfsere Reinheit dieser Krystalle erfordert wird, kann durch nochmaliges Schmelzen derselben eine zweite Krystallisation in gleicher Weise vorgenommen werden. Ein etwaiger Natriumgehalt bleibt ebenfalls jedesmal in der Mutterlauge. Für den praktischen Betrieb ist es vortheilhaft, vor der Eindampfung der Aetzkalilauge die in der Lösung enthaltenen Schwefelverbindungen durch Chlorkalk, Kalisalpeter, Lufteinblasung oder dergl. zu zerstören, weil dann die Krystalle sich leichter rein und weifs herstellen lassen.Purity, if] you, after cooling down 40 to 6p ° C. separates the not yet solidified liquid from the crystals. The chlorine and sulfur compounds remain in the mother liquor, which a caustic potash with less Contains water as the crystals, and which afterwards further to an impure caustic potash or is processed on potash, while the remaining crystals by heating to Melting are brought and liquid get into the vessels intended for dispatch to to freeze in it. If an even greater purity of these crystals is required, then a second crystallization carried out in the same way by melting them again will. Any sodium content also remains in the mother liquor every time. For practical operation it is advantageous to use the in sulfur compounds contained in the solution by means of chlorinated lime, potassium nitrate, air injection or the like, because then the crystals can be more easily produced pure and white.
Wenn aus der bekannten Schwerlöslichkeit der Soda in heifsen Potaschelösungen leicht geschlossen werden kann, dafs bei weiterer Concentration der letzteren die vollständige Abscheidung der Soda möglich sei, so ist doch bisher dies Verfahren noch nicht angewendet worden. Andererseits ist die Thatsache, dafs Kaliumcarbonat und Hydroxyd in Aetzkali haltenden Laugen schwer löslich ist, nicht bekannt gewesen und zur Reindarstellung dieser Kaliumverbindungen noch nicht benutzt worden.If from the well-known poor solubility of soda in hot potash solutions easy it can be concluded that with further concentration of the latter the complete Separation of the soda is possible, this method has not yet been used been. On the other hand, the fact is that potassium carbonate and hydroxide hold in caustic potash Alkali is sparingly soluble, was not known and for the pure preparation of these potassium compounds has not yet been used.
Claims (3)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE5061C true DE5061C (en) |
Family
ID=283645
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT5061D Active DE5061C (en) | Process for the preparation of pure potassium carbonate and potassium hydrocyte |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE5061C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1053493B (en) * | 1956-11-07 | 1959-03-26 | Hoechst Ag | Process for the production of sulfonyl urethanes with a blood sugar lowering effect |
| DE1058504B (en) * | 1956-11-07 | 1959-06-04 | Hoechst Ag | Process for the preparation of N-cyclohexylmethylene sulfonyl urethanes |
| DE1075587B (en) * | 1960-02-18 | Farbwerke Hoechst Aktiengesellschaft vormals Meister Lucius & Bruning Frankfurt/M | Process for the preparation of sulfonyl urethanes |
-
0
- DE DENDAT5061D patent/DE5061C/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1075587B (en) * | 1960-02-18 | Farbwerke Hoechst Aktiengesellschaft vormals Meister Lucius & Bruning Frankfurt/M | Process for the preparation of sulfonyl urethanes | |
| DE1053493B (en) * | 1956-11-07 | 1959-03-26 | Hoechst Ag | Process for the production of sulfonyl urethanes with a blood sugar lowering effect |
| DE1058504B (en) * | 1956-11-07 | 1959-06-04 | Hoechst Ag | Process for the preparation of N-cyclohexylmethylene sulfonyl urethanes |
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