DE165488C - - Google Patents
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- Publication number
- DE165488C DE165488C DENDAT165488D DE165488DA DE165488C DE 165488 C DE165488 C DE 165488C DE NDAT165488 D DENDAT165488 D DE NDAT165488D DE 165488D A DE165488D A DE 165488DA DE 165488 C DE165488 C DE 165488C
- Authority
- DE
- Germany
- Prior art keywords
- alumina
- hydroxide
- beryllium
- clay
- acid
- 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.)
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 26
- WPJWIROQQFWMMK-UHFFFAOYSA-L Beryllium hydroxide Chemical compound [Be+2].[OH-].[OH-] WPJWIROQQFWMMK-UHFFFAOYSA-L 0.000 claims description 24
- 229910001865 beryllium hydroxide Inorganic materials 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N AI2O3 Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 15
- 239000004927 clay Substances 0.000 claims description 15
- 229910052570 clay Inorganic materials 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 150000004679 hydroxides Chemical class 0.000 claims description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 13
- 239000003513 alkali Substances 0.000 claims description 12
- 229910052614 beryl Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003518 caustics Substances 0.000 claims description 10
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 5
- NCNCGGDMXMBVIA-UHFFFAOYSA-L Iron(II) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 235000014413 iron hydroxide Nutrition 0.000 claims description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910052790 beryllium Inorganic materials 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium(0) Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 235000015320 potassium carbonate Nutrition 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K Aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 229940072033 potash Drugs 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 5
- 238000000605 extraction Methods 0.000 claims 2
- 230000000996 additive Effects 0.000 claims 1
- 229910001767 beryllium mineral Inorganic materials 0.000 claims 1
- 230000005591 charge neutralization Effects 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 claims 1
- 230000000875 corresponding Effects 0.000 claims 1
- QUSNBJAOOMFDIB-UHFFFAOYSA-N ethyl amine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims 1
- 230000001264 neutralization Effects 0.000 claims 1
- 238000006386 neutralization reaction Methods 0.000 claims 1
- 230000002035 prolonged Effects 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 239000011780 sodium chloride Substances 0.000 claims 1
- 150000007513 acids Chemical class 0.000 description 4
- LTPBRCUWZOMYOC-UHFFFAOYSA-N BeO Chemical compound O=[Be] LTPBRCUWZOMYOC-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxyl anion Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- PRKQVKDSMLBJBJ-UHFFFAOYSA-N Ammonium carbonate Chemical compound N.N.OC(O)=O PRKQVKDSMLBJBJ-UHFFFAOYSA-N 0.000 description 1
- 241000216690 Gracula religiosa Species 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- -1 beryllium hydroxides Chemical class 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000001184 potassium carbonate Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 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
- C01F3/00—Compounds of beryllium
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Compounds Of Iron (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
Der Gegenstand der Erfindung ist ein Verfahren, Berylliumhydroxyd in fester Form durch Trocknen oder ausreichend langes Erhitzen so zu verändern, daß es seine Löslichkeit in verdünntem Alkali und dann weitergehend in Säuren fast ganz einbüßt. Zur Beschleunigung des Vorganges wird die Mitwirkung solcher Stoffe benutzt, welche das Hydroxyd entweder gar nicht oder nurThe subject of the invention is a method, beryllium hydroxide in solid form to change its solubility by drying or heating for a sufficient length of time almost completely forfeited in dilute alkali and then further in acids. To speed up the process, the With the help of such substances used, which the hydroxide either not at all or only
ίο in einem äußerst kleinen Betrage zu lösen vermögen.ίο to be solved in an extremely small amount capital.
In dieser Weise wirkt das Erhitzen in Wasser, Dampf oder anderen indifferenten Stoffen (z. B. wäßrigen Lösungen von Soda, Ammoniak) oder in so weit verdünnten wäßrigen Lösungen von Ätzalkalien, Pottasche oder dergl., daß das Berylliumhydroxyd nicht oder nur zu einem winzigen Anteile gelöst wird.In this way, heating acts in water, steam, or other indifferent ones Substances (z. B. aqueous solutions of soda, ammonia) or in so far diluted aqueous Solutions of caustic alkalis, potash or the like. That the beryllium hydroxide does not or is only dissolved to a tiny extent.
Diese neu gefundene Überführung kann vorteilhaft dazu benutzt werden, die Beryllerde von anderen Hydroxyden, besonders von den Hydroxyden der Tonerde und des Eisens zu trennen, indem das Gemenge des Berylliumhydroxyds und der anderen Hydroxyde in so weit verdünnten Lösungen von Ätzalkalien erhitzt wird, daß nur die Tonerde in Lösung geht, während Eisenhydroxyd und etwaige andere Hydroxyde später durch Säure entfernt werden.This newly found overpass can be used to advantage to the beryl alumina to be separated from other hydroxides, especially from the hydroxides of clay and iron, by adding the mixture of beryllium hydroxide and the other hydroxides are heated in solutions of caustic alkalis that are so dilute that only the alumina is in solution goes, while iron hydroxide and any other hydroxides are later removed by acid will.
Obwohl das Verhalten des Berylliumhydroxyds gegen Alkalien und Säuren seit der Entdeckung des Metalls durch V au qu el in oft untersucht worden ist, sind diejenigen Eigenschaften des Berylliumhydroxyds unbekannt geblieben, die der vorliegenden Erfindung zugrunde liegen und auch zur Trennung der Beryllerde von anderen Hydroxyden benutzt werden.Although the behavior of beryllium hydroxide towards alkalis and acids since The discovery of the metal by V au qu el in has often been investigated are those Properties of beryllium hydroxide remained unknown to those of the present invention and are also used to separate beryl alumina from other hydroxides.
Durch die Versuche von Graf Schaffgotsch und C. G,. Gmelin (Pogg. Ann. 50, 1840, S. 175 und 183) ist es bekannt geworden, nur in Ätzalkalien unlösliches Berylliumhydroxyd herzustellen, indem das in starker Kalilauge gelöste Hydroxyd nach dem Verdünnen durch Erhitzen gefällt wird.Through the experiments of Graf Schaffgotsch and C. G ,. Gmelin (Pogg. Ann. 50, 1840, pp. 175 and 183) it has become known only to produce beryllium hydroxide insoluble in caustic alkalis by adding the hydroxide dissolved in strong potassium hydroxide solution the dilution by heating is precipitated.
λ^οη diesem Vorschlage unterscheidet sich das vorliegende Verfahren dadurch, daß es von Berylliumhydroxyd in fester Form ausgeht und nicht wie im bekannten Falle von in Lösung befindlichem Berylliumhydroxyd; es hat vor diesem bekannten Verfahren den Vorzug, daß ein auch für Säure unlösliches Produkt entsteht.λ ^ οη this proposal is different the present process in that it starts from beryllium hydroxide in solid form and not as in the known case of beryllium hydroxide in solution; it has the advantage over this known process that one which is also insoluble for acid Product is created.
Der Erfindung liegen folgende Versuchsergebnisse zugrunde:The invention is based on the following test results:
1. Jede Form gefällten Berylliumhydroxyds geht durch Erhitzen mit einer kleinen, zur Lösung völlig unzureichenden Menge Ätzalkalis in eine in Säuren, sogar wenn diese konzentriert angewendet werden, schwer lösliche Form über.1. Any form of precipitated beryllium hydroxide can be heated with a small, to Solution completely insufficient amount of caustic alkali in one in acids, even if these be applied concentrated, difficult to dissolve form over.
2. Gleich schwer lösliche Formen entstehen auch, wenn man ein Gemenge von Beryllerde und Tonerde (bezw. auch noch anderen Hydroxyden) nur mit so viel Natron-2. Forms that are equally difficult to dissolve also arise when you mix a mixture of Beryl alumina and clay (or other hydroxides as well) only with so much soda
lauge (in geeigneter Konzentration) behandelt, als zur Lösung der Tonerde, aber nicht der Beryllerde erforderlich ist.lye (in a suitable concentration) treated as to dissolve the clay, but not the Beryl clay is required.
3. In Alkali fast unlösliche Formen der Beryllerde werden auch erreicht durch Behandeln des Berylliumhydroxyds bei gewöhnlicher und erhöhter Temperatur, durch Kochen mit reinem oder ammoniakalischem, sodaalkalischem oder auch indifferente Stoffe enthaltendem Wasser, was C. G. Gmelin (Pogg. Ann. 50, 1840, S. 175) ausdrücklich in Abrede gestellt hat.3. Forms of beryl alumina which are almost insoluble in alkali are also obtained by treatment of beryllium hydroxide at ordinary and elevated temperature, by boiling with pure or ammoniacal, soda-alkaline or water containing inert substances, which C. G. Gmelin (Pogg. Ann. 50, 1840, p. 175) has expressly denied.
So fand sich z. B. für die Löslichkeit eines Berylliumhydroxyds, das 8 Tage bei gewöhnlicher Temperatur getrocknet worden war:So found z. B. for the solubility of a beryllium hydroxide, which is 8 days normal temperature:
bei in n/2 m/iat in n / 2 m / i
20 bis 250C. 60 170
100° C. 80 29020 to 25 0 C. 60 170
100 ° C. 80 290
an Na OH at Na OH
570 mg pro Liter, 1020 -570 mg per liter, 1020 -
während für Tonerde, die über ι Jahr bei gewöhnlicher Temperatur gestanden hatte,while for clay that has been at normal temperature for more than ι year,
bei in n/z n/i 2 η Na OH at in n / zn / i 2 η Na OH
2Obis25°C. 9,26 g 11,39 g 14,4 g pro Liter, 1000C. 11,25 g 20,3 g 44,4 g -20 to 25 ° C. 9.26 g 11.39 g 14.4 g per liter, 100 0 C. 11.25 g 20.3 g 44.4 g -
gefunden wurden.were found.
Es fand sich ferner für die Löslichkeit von Berylliumhydroxyd, das während 5 Stunden in reinem Wasser bei ioo° C. erhitzt' worden war, daß 52 mg im Liter κ/2-Natronlauge löslich waren, während bei Verwendung von ammoniakalischem Wasser unter ähnlichen Bedingungen ganz gleichartige Werte erhalten wurden.It was also found for the solubility of beryllium hydroxide that for five hours heated in pure water at 100 ° C. That was 52 mg per liter of κ / 2 sodium hydroxide solution were soluble, while when ammoniacal water was used under similar conditions, they were quite similar Values were obtained.
Auf der anderen Seite wurde festgestellt, daß, wenn man Tonerde mit einer zur Lösung unzureichenden Menge κ/2-Natronlauge in der Hitze viele Stunden behandelt, der zurückbleibende Teil in einer neuen Menge Natronlauge fast ganz ebenso leicht gelöst werden kann, als wenn diese Behandlung nicht vorangegangen ist.On the other hand, it was found that when you use clay with a solution insufficient amount of κ / 2 sodium hydroxide solution treated in the heat for many hours, the remaining Part of it can be dissolved in a new amount of caustic soda almost as easily as if this treatment had not been preceded is.
Das Berylliumhydroxyd erleidet unter der Wirkung der Zeit eine Änderung, wobei aus der wohlbekannten, in verdünnten Alkalien, in Alkali- und Ammoniumkarbonat und Säuren leicht löslichen Form gealterte Formen entstehen, die in den angegebenen Lösungsmitteln unlöslich bezw. schwer löslich sind. Dieser Vorgang des Alterns vollzieht sich bei gewöhnlicher Temperatur, in der Siedehitze oder bei noch höherer Temperatur, die erhöhte Temperatur wirkt lediglich beschleunigend. Ebenfalls beschleunigend wirken manche gelöste Stoffe, insbesondere Ätzalkali. The beryllium hydroxide undergoes a change under the action of time, whereby off of the well-known forms, which are readily soluble in dilute alkalis, in alkali and ammonium carbonate and acids arise that are insoluble or in the specified solvents. are difficult to dissolve. This process of aging takes place at normal temperature, in the boiling point or at an even higher temperature, the increased temperature only has an accelerating effect. Some dissolved substances, in particular caustic alkali, also have an accelerating effect.
Tonerde und Eisenhydroxyd sowie manche andere Hydroxyde besitzen, wie Berthelot (Ann. chim. phys. [5], 4. Bd., S. 174) und Hantzsch (Zeitschrift f. anorg. Chem. 30, 1902, S. 338) bemerkt haben, ebenfalls die Eigenschaft zu altern, aber weder in dem Umfang noch unter den gleichen Verhältnissen wie das Berylliumhydroxyd.Have clay and iron hydroxide, as well as some other hydroxides, such as Berthelot (Ann. Chim. Phys. [5], 4th vol., P. 174) and Hantzsch (Zeitschrift f. Anorg. Chem. 30, 1902, p. 338) have also noticed the property of aging, but neither in that Extent still under the same proportions as the beryllium hydroxide.
Nachstehend sind die Löslichkeiten für frisch gefällte Berylliumhydroxyde bei Zimmertemperatur in Natronlauge verschiedener Konzentrationen angeführt, welche teils von Rubenbauer (Zeitschrift f. anorg. Chem. 30, 1902, S. 334) mitgeteilt werden, teils durch eigene Versuche ermittelt worden sind; es ist hieraus zu entnehmen, welche großen Unterschiede zwischen jungen und gealterten Hydroxydformen bestehen. .The following are the solubilities for freshly precipitated beryllium hydroxides at room temperature in sodium hydroxide solution of various concentrations, some of which were published by Rubenbauer (Zeitschrift f. anorg. Chem. 30, 1902, p. 334), some of which have been determined through our own experiments; it this shows the great differences between young and old Hydroxyd forms exist. .
Diese neu gefundenen Tatsachen lassen sich nun in folgender Weise benutzen.These newly found facts can now be used in the following way.
1. Man erhitzt ein Gemenge von Beryllium-, Aluminium- und Eisenhydroxyd mit so viel verdünnter, z. B. κ/2-Natronlauge, als notwendig ist, um die Tonerde in Lösung zu bringen. Wenn z. B. 13 g Be O als Berylliumhydroxyd, 17 g Al2 O3 als Aluminiumhydroxyd, 1 g Fe2O3 als Eisenhydroxyd gemengt vorliegen, so wird man 1,5 bis 1,6 1 κ/2-Natronlauge anwenden und damit 1 bis 2 Stunden erhitzen. Dabei gehen höchstens 0,1 g BeO in Form von Be(OH)2, d. h. 0,75 Prozent von der vorhandenen Beryllerde in Lösung, während die Tonerde vollständig entfernt wird. Die übrige Menge des Berylliumhydroxyds liegt nun in schwer löslicher Form vor und wird durch einfaches Auswaschen mit Säure, z. B. mit verdünnter warmer Salzsäure, von Eisen befreit.1. One heats a mixture of beryllium, aluminum and iron hydroxide with as much diluted, z. B. κ / 2 sodium hydroxide solution than is necessary to bring the clay into solution. If z. B. 13 g of Be O as beryllium hydroxide, 17 g of Al 2 O 3 as aluminum hydroxide, 1 g of Fe 2 O 3 as iron hydroxide are mixed, so you will use 1.5 to 1.6 1 κ / 2 sodium hydroxide solution and thus 1 to Heat for 2 hours. A maximum of 0.1 g of BeO in the form of Be (OH) 2 , ie 0.75 percent of the beryl alumina present, goes into solution, while the alumina is completely removed. The remaining amount of beryllium hydroxide is now in a poorly soluble form and is simply washed out with acid, e.g. B. with dilute warm hydrochloric acid, freed from iron.
2. Man erhitzt die gemengten Hydroxyde statt mit Alkali mit Wasser, Ammoniak enthaltendem Wasser, Soda oder Kaliumkarbonatlösung, mit oder ohne indifferente Zusätze. Dies kann z. B. in der Weise geschehen, daß man das unter 1. vorliegende Gemenge der Hydroxyde in feuchtem Zustande mit Wasser oder Wasserdampf von ioo° C. oder bei etwas höherer Temperatur etwa 5 Stunden lang behandelt. Das Berylliumhydroxyd be-2. The mixed hydroxides are heated with water containing ammonia instead of with alkali Water, soda or potassium carbonate solution, with or without indifferent additives. This can e.g. B. done in such a way that the mixture of hydroxides present under 1. in a moist state with water or water vapor at 100 ° C. or at a slightly higher temperature for about 5 hours long treated. The beryllium hydroxide
Claims (3)
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