DE118073C - - Google Patents
Info
- Publication number
- DE118073C DE118073C DENDAT118073D DE118073DA DE118073C DE 118073 C DE118073 C DE 118073C DE NDAT118073 D DENDAT118073 D DE NDAT118073D DE 118073D A DE118073D A DE 118073DA DE 118073 C DE118073 C DE 118073C
- Authority
- DE
- Germany
- Prior art keywords
- boric acid
- borate
- crude
- chlorine
- chlorates
- 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
- 239000004327 boric acid Substances 0.000 claims description 19
- KGBXLFKZBHKPEV-UHFFFAOYSA-N Boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 18
- XTEGARKTQYYJKE-UHFFFAOYSA-M chlorate Chemical class [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 claims description 10
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 150000001642 boronic acid derivatives Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 150000001805 chlorine compounds Chemical class 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L Calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L MgCl2 Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 235000015450 Tilia cordata Nutrition 0.000 description 2
- 235000011941 Tilia x europaea Nutrition 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- 230000000875 corresponding Effects 0.000 description 2
- 239000004571 lime Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- VLCLHFYFMCKBRP-UHFFFAOYSA-N tricalcium;diborate Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]B([O-])[O-].[O-]B([O-])[O-] VLCLHFYFMCKBRP-UHFFFAOYSA-N 0.000 description 2
- NFMWFGXCDDYTEG-UHFFFAOYSA-N trimagnesium;diborate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]B([O-])[O-].[O-]B([O-])[O-] NFMWFGXCDDYTEG-UHFFFAOYSA-N 0.000 description 2
- YALMXYPQBUJUME-UHFFFAOYSA-L Calcium chlorate Chemical compound [Ca+2].[O-]Cl(=O)=O.[O-]Cl(=O)=O YALMXYPQBUJUME-UHFFFAOYSA-L 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N Silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229940077744 antacids containing magnesium compounds Drugs 0.000 description 1
- 125000005619 boric acid group Chemical group 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L cacl2 Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- NSDBGBPZNRLOBU-UHFFFAOYSA-L calcium;chlorate;chloride Chemical compound [Cl-].[Ca+2].[O-]Cl(=O)=O NSDBGBPZNRLOBU-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000001187 sodium carbonate Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/06—Boron halogen compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Description
KAISERLICHES PATENTAMT.IMPERIAL PATENT OFFICE.
Bei Herstellung von Borsäure nach irgend einem der bestehenden Verfahren tritt ein beträchtlicher Verlust an Borsäure auf, besonders wenn man es mit rohen Boraten zu thun hat, welche eine grofse Menge von Verunreinigungen, wie Sulfate und Chloride, enthalten.When boric acid is produced by any of the existing processes, there is a considerable incidence Loss of boric acid, especially when dealing with crude borates, which contain a great deal of impurities, such as sulfates and chlorides.
Vorliegende Erfindung bezweckt, diesen Verlust an Borsäure zu beseitigen und auch die Schwierigkeiten zu überwinden, welche die Verunreinigungen des Rohmaterials bereiten, ferner die Unkosten zu verringern, die durch die Anwendung starker Säuren entstehen, um die Borsäure in Freiheit zu setzen.The present invention aims to eliminate this boric acid loss, and also to To overcome difficulties caused by impurities in the raw material, also to reduce the expense of using strong acids to to set the boric acid free.
Um dies zu bewirken,: wendet man zur Abtrennung der Borsäure aus den Boraten Chlor an, wodurch man den weiteren Vortheil erzielt, dafs zugleich die in dem Rohborat an die Borsäure gebundenen Basen (Kalk u. s. w.) in Form von Chloraten gewonnen werden.To do this: one uses to separate the boric acid from the borates Chlorine, whereby the further advantage is obtained that at the same time that in the crude borate the boric acid-bound bases (lime etc.) can be obtained in the form of chlorates.
Die Ausführung des Verfahrens geschieht in folgender Weise:The procedure is carried out in the following way:
Das unreine Calcium- oder Magnesiumborat oder ein anderes Rohborat wird in feinem pulverförmigen Zustand in Wasser oder in einer von einer früheren Operation stammenden Mutterlauge zweckmäfsig in dem Verhältnifs von ungefähr 275 g auf 1 1 Wasser suspendirt. In diese Mischung wird Chlorgas eingeleitet, indem man sie in Bewegung hält. ■Wahrend der Behandlung mit Chlor wird die Temperatur der Mischung zweckmäfsig bei 60 bis 800C. gehalten. . · 'The impure calcium or magnesium borate, or some other crude borate, is suspended in a fine powdery state in water or in a mother liquor obtained from an earlier operation, expediently in the proportion of about 275 g to 1 liter of water. Chlorine gas is introduced into this mixture by keeping it moving. ■ During treatment with chlorine, the temperature of the mixture is maintained zweckmäfsig at 60 to 80 0 C.. . · '
Die Absorption des Chlorgases, welche hierbei sehr rasch erfolgt, bewirkt, dafs die ge-, bundene Borsäure völlig in Freiheit gesetzt wird, während die in dem Rohborat enthaltenen Basen, entsprechend dem absorbirten Chlor, Chloride und Chlorate bilden. Die auf diese Weise erhaltene Flüssigkeit wird nach Abtrennung irgend welcher unlöslicher Rückstände zweckmä'fsig auf ungefähr 1 5 bis 200 C. abgekühlt, wodurch der gröfste Theil der freien Borsäure auskrystallisirt.The absorption of the chlorine gas, which takes place very quickly, causes the bound boric acid to be completely set free, while the bases contained in the crude borate, corresponding to the absorbed chlorine, form chlorides and chlorates. The liquid thus obtained is cooled after separation of any insoluble residues zweckmä'fsig to about 1 5 to 20 0 C., auskrystallisirt whereby the greater part of free boric acid.
Die zurückbleibende Mutterlauge kann mit einer frischen Menge von Rohborat versetzt und nochmals mit Chlor behandelt werden, oder man kann die Mutterlauge mittels Eindampfens concentriren und die nach der mittels Abkühlung erfolgten Ausscheidung der rohen Borsäure rückständige Flüssigkeit auf Chlorate in gebräuchlicher Weise verarbeiten.The remaining mother liquor can be mixed with a fresh amount of raw borate and treated again with chlorine, or the mother liquor can be evaporated concentrate and after the cooling-off of the crude Process boric acid residual liquid on chlorates in the usual way.
Die in der beschriebenen Weise hergestellte , Borsäure ist durch Umkrystallisiren leicht zu reinigen und kann gewünschtenfalls auf Borax verarbeitet werden, indem man sie einfach mit , Aetznatronlösung oder Natriumcarbonatlösung in entsprechendem Verhältnifs gemäfs des Gehaltes an : vorhandener Borsäure behandelt. Dieses Alkali kann entweder in Form von Soda oder in Form von rohem Natrium-· bicarbonat angewendet werden, wie solche bei dem Ammoniaksoclaprocefs erhalten werden.The boric acid prepared in the manner described is easy to recrystallize clean and, if desired, can be processed on borax by simply using, Caustic soda solution or sodium carbonate solution in an appropriate proportion according to the content on: existing boric acid treated. This alkali can either be in the form of Soda or in the form of raw sodium bicarbonate can be used, as is the case with the ammonia claprocefs are obtained.
Das beschriebene Verfahren kann vortheilhaft in Verbindung mit einem elektrolytischenThe method described can advantageously be used in conjunction with an electrolytic
Verfahren ausgeführt werden, bei welchem sowohl Natron als auch Chlor erzeugt wird, in welchem Falle beide Producte, wie sie aus der elektrolytischen Zelle kommen, Verwendung finden können.Processes are carried out in which both sodium bicarbonate and chlorine are produced, in which case both products as they come from the electrolytic cell are used can find.
Wenn ein Kalkborat nach vorliegendem Verfahren behandelt wird, so kann die chemische Reaction durch folgende Gleichung veranschaulicht werden:If a lime borate is treated according to the present process, the chemical Reaction can be illustrated by the following equation:
3{Ca.2 B, O83H2O) + 6Cl2 + 9H2O =-- 12H3BO3 -f- 5CaQ2 -j- Ca(ClOJ2. 3 {approx. 2 B, O 83 H 2 O) + 6Cl 2 + 9 H 2 O = - 12H 3 BO 3 -f- 5CaQ 2 -j- Ca (ClOJ 2 .
Die gewonnene Lösung enthält demnach Borsäure, Calciumchlorid und Calciumchlorat. Wenn Magnesiumborat an Stelle von Calciumborat angewendet wird, so erhält man die entsprechenden Magnesiumverbindungen neben Borsäure u. s. w.The solution obtained therefore contains boric acid, calcium chloride and calcium chlorate. If magnesium borate is used instead of calcium borate, the corresponding results are obtained Magnesium compounds in addition to boric acid and so on.
Je stärker die Concentration der das Chlorid und Chlorat enthaltenen Lösung ist, desto vollständiger wird die Borsäure aus dieser auskrystallisiren. Die Borsäure kann auch durch Abkühlung der Lösung auf eine sehr niedrige Temperatur, z. B. —100C. ausgeschieden werden. Nach der in der beschriebenen Art erfolgten Trennung der Borsäure wird die zurückbleibende Lauge, welche Chloride und Chlorate enthält, in gewöhnlicher Weise zur Abscheidung der Chlorate behandelt. Im Falle dafs das angewendete Rohborat grofse Mengen von Verunreinigungen enthält, wie organische Substanzen, Chloride, Sulfate oder lösliche Kieselsäure, so beeinrlufst die Gegenwart aller oder einiger dieser Verbindungen keineswegs den Verlauf der Reaction oder die Abscheidung der Borsäure.The greater the concentration of the solution containing the chloride and chlorate, the more completely the boric acid will crystallize out of it. The boric acid can also be obtained by cooling the solution to a very low temperature, e.g. B. -10 0 C. to be excreted. After the boric acid has been separated in the manner described, the alkali which remains, which contains chlorides and chlorates, is treated in the usual way to separate the chlorates. In the event that the crude borate used contains large quantities of impurities, such as organic substances, chlorides, sulphates, or soluble silicic acid, the presence of all or some of these compounds in no way affects the course of the reaction or the deposition of boric acid.
Irgend welche organische Substanz· wird durch das Chlor zerstört,, während das' Sulfat in Calciumsulfat (vorausgesetzt, dafs Calciumsalze zugegen sind) übergeführt wird, welches nahezu in der heifsen Calcium- oder Magnesiumchloridlösung bezw. Chloratlösung unlöslich ist. Irgend welche in dem Rohborat enthaltenen Chloride bleiben naturgemäfs in der Mutterlauge gelöst. In dieser Hinsicht wird also das vorliegende Verfahren am wenigsten beeinflufst, wenn man mit sehr unreinen Rohboraten zu thun hat, welche so grofse Schwierigkeiten bei dem gebräuchlichen angewendeten ■ Verfahren hervorrufen.Any organic substance is destroyed by the chlorine, while the sulphate is converted into calcium sulphate (provided that calcium salts are present), which almost in the hot calcium or magnesium chloride solution respectively. Chlorate solution insoluble is. Any chlorides contained in the raw borate naturally remain in the Dissolved mother liquor. In this regard, then, the present method is the least influences, when one has to deal with very impure crude borates, which causes such great difficulties in the usual procedure used.
Claims (1)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE118073C true DE118073C (en) |
Family
ID=387297
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DENDAT118073D Active DE118073C (en) |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE118073C (en) |
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