NO140051B - PROCEDURE FOR THE PREPARATION OF ALUMINUM CHLORINE HYDROXIDE WITH A CONTROLLED AND REDUCED CHLORINE CONTENT - Google Patents
PROCEDURE FOR THE PREPARATION OF ALUMINUM CHLORINE HYDROXIDE WITH A CONTROLLED AND REDUCED CHLORINE CONTENT Download PDFInfo
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- NO140051B NO140051B NO755/73A NO75573A NO140051B NO 140051 B NO140051 B NO 140051B NO 755/73 A NO755/73 A NO 755/73A NO 75573 A NO75573 A NO 75573A NO 140051 B NO140051 B NO 140051B
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- Prior art keywords
- aluminum
- treatment
- electrolysis
- digestion
- chlorine
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- 239000000460 chlorine Substances 0.000 title claims description 14
- 229910052801 chlorine Inorganic materials 0.000 title claims description 12
- -1 ALUMINUM CHLORINE HYDROXIDE Chemical compound 0.000 title claims description 11
- 238000000034 method Methods 0.000 title claims description 10
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 title 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 25
- 238000005868 electrolysis reaction Methods 0.000 claims description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 17
- 230000029087 digestion Effects 0.000 claims description 16
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910001593 boehmite Inorganic materials 0.000 claims description 4
- 229910001648 diaspore Inorganic materials 0.000 claims description 4
- 229910001679 gibbsite Inorganic materials 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 4
- 229910001570 bauxite Inorganic materials 0.000 claims description 3
- 229910010293 ceramic material Inorganic materials 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 description 9
- 239000002245 particle Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- WWHZEXDIQCJXSV-UHFFFAOYSA-N aluminum;trihypochlorite Chemical compound [Al+3].Cl[O-].Cl[O-].Cl[O-] WWHZEXDIQCJXSV-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- CAYKLJBSARHIDI-UHFFFAOYSA-K trichloroalumane;hydrate Chemical class O.Cl[Al](Cl)Cl CAYKLJBSARHIDI-UHFFFAOYSA-K 0.000 description 4
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910001293 incoloy Inorganic materials 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- NHYCGSASNAIGLD-UHFFFAOYSA-N Chlorine monoxide Chemical class Cl[O] NHYCGSASNAIGLD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229910001680 bayerite Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910001902 chlorine oxide Inorganic materials 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension 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
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/22—Halogenating
- B01J37/24—Chlorinating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Plasma & Fusion (AREA)
- Toxicology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Electrolytic Production Of Metals (AREA)
Description
Foreliggende oppfinnelse vedrører en fremgangsmåte for fremstilling av aluminium-klorhydroksyd med styrt og redusert klorinnhold og med formel Al2 „(OH) x Cl y hvor forholdet mellom x og y som angitt i patent nr. 131.641 er fra 1 : 5 til 1,4: 1 og hvor et material som inneholder aluminiumoksyd eller hydratisert aluminiumoksyd, foretrukket valgt blant Bayer-aluminiumoksyd, gibbsitt, bauxitt, diaspor, hydrargilitt og bøhmitt, før en videre behandling underkastes en oppslutting med saltsyre ved temperaturer på fra 100 til 160°C ved 0,1-4" kg/cm2 slik at systemet holdes i flytende fase, idet oppsluttingen The present invention relates to a method for the production of aluminum chlorhydroxide with a controlled and reduced chlorine content and with the formula Al2 „(OH) x Cl y where the ratio between x and y as stated in patent no. 131,641 is from 1 : 5 to 1.4: 1 and where a material containing alumina or hydrated alumina, preferably selected from Bayer alumina, gibbsite, bauxite, diaspore, hydrargilite and boehmite, before further treatment is subjected to digestion with hydrochloric acid at temperatures of from 100 to 160°C at 0, 1-4" kg/cm2 so that the system is kept in liquid phase, as the absorption
gjennomføres i nærvær av en mengde aluminiumoksyd og/eller hydratiserte aluminiumoksyder som er fra 2,5 til 5 ganger så is carried out in the presence of an amount of alumina and/or hydrated aluminas which is from 2.5 to 5 times that
stor som den mengde som støkiometrisk trenges for å fremstille aluminium-trikloridet (AlCl^), og det særegne ved fremgangsmåten i henhold til oppfinnelsen er den modifikasjon at den videre behandling utgjøres av at produktet fra oppsluttingen underkastes en separasjonsbehandling under fjernelse av uomsatt material og deretter for å redusere klorinnholdet i forhold til hydroksydinnholdet i det aluminium-klorhydroksyd som er erholdt i form av en løsning fra oppsluttingen og separasjons-beliandlingen underkastes en elektrolysebehandling med påtrykt spenning fra 2 til 10 volt og med en strømtetthet på fra 20 as large as the amount that is stoichiometrically needed to produce the aluminum trichloride (AlCl^), and the distinctive feature of the method according to the invention is the modification that the further treatment consists of subjecting the product from the digestion to a separation treatment during the removal of unreacted material and then in order to reduce the chlorine content in relation to the hydroxide content in the aluminum chlorohydroxide obtained in the form of a solution from the absorption and separation process, it is subjected to an electrolysis treatment with applied voltage from 2 to 10 volts and with a current density of from 20
til 600 mA/cm 2 i en elektrolysecelle av diafragmatypen med diafragma av keramisk material og med elektroder av grafitt, idet både elektrolysebehandlingen, som foretas ved høy temperatur på fra 50 til 130°C, samt den ovennevnte separasjonsbehandling før elektrolysebehandlingen hindrer forstyrrelser av utfelt material ved elektrodene under elektrolysebehandlingen. to 600 mA/cm 2 in a diaphragm-type electrolysis cell with a diaphragm of ceramic material and with electrodes of graphite, as both the electrolysis treatment, which is carried out at a high temperature of from 50 to 130°C, as well as the above-mentioned separation treatment before the electrolysis treatment prevents disturbances of precipitated material at the electrodes during the electrolysis treatment.
Aluminium-klorhydroksyd er kjent som en nyttig katalysator Aluminum chlorohydroxide is known as a useful catalyst
for forskjellige prosesser. for different processes.
Ved således å gelere aluminium-klorhydroksyd med formel Al2(OH)5C1 oppnås kuleformet aluminiumoksyd som er en viktig katalysator for hydrokarbonraffinering og som basis for katalysator for forbrenning av forbrenningsgasser. Thus, by gelling aluminum chlorohydroxide with the formula Al2(OH)5C1, spherical alumina is obtained which is an important catalyst for hydrocarbon refining and as a basis for catalyst for combustion of combustion gases.
En vesentlig ulempe ved fremstillingen har hittil vært prisen på de fremstilte katalysatorer, hvorav prisen på utgangs-materialene for fremstilling av aluminium-klorhydroksydet har vært av vesentlig betydning. A significant disadvantage of the production has so far been the price of the catalysts produced, of which the price of the starting materials for the production of the aluminum chlorohydroxide has been of significant importance.
Den vanligste metode man hittil har anvendt for å fremstille aluminium-klorhydroksyd besto i å oppslutte aluminium-metall med saltsyre. The most common method used up to now to produce aluminum chlorhydroxide consisted of dissolving aluminum metal with hydrochloric acid.
Man har tidligere i patent nr. 131.641 foreslått en fremgangsmåte for fremstilling av aluminium-klorhydroksyd med det ønskede klorinnhold ved å gå ut fra et billig aluminiumholdig material i form av oksydet eller det vannholdige oksyd, særlig i form av Bayeritt, gibbsitt, bauxitt, hydrargilitt, diaspor eller bøhmitt. In patent no. 131,641, a method for the production of aluminum chlorhydroxide with the desired chlorine content has previously been proposed by starting from a cheap aluminum-containing material in the form of the oxide or the hydrous oxide, particularly in the form of bayerite, gibbsite, bauxite, hydrargilite , diaspore or boehmite.
Fremgangsmåten gikk ut på en forutgående oppslutting av utgangsmaterialet med saltsyre som frembringer et produkt med en ubestemt sammensetning og som vanlig inneholder en klormengde som er for høy for den påfølgende anvendelse. The method involved a prior digestion of the starting material with hydrochloric acid, which produces a product with an undetermined composition and which usually contains an amount of chlorine that is too high for the subsequent use.
Det produkt som ble oppnådd på den nevnte måte kunne underkastes nøytralisering med ammoniakk som muliggjorde frem— stilling av en forbindelse med en mer ønsket sammensetning. The product obtained in the aforementioned manner could be subjected to neutralization with ammonia, which enabled the production of a compound with a more desired composition.
Nøytraliseringen med ammoniakk medførte imidlertid etter-følgende operasjoner, hvorav særlig fjernelsen av ammonium-klorid ved krystallisering var av vesentlig betydning. However, the neutralization with ammonia entailed subsequent operations, of which the removal of ammonium chloride by crystallization was particularly important.
Oppfinnelsen gjelder en videreutvikling av den fremgangsmåte som er gjenstanden for patent nr. 131.641 hvor man da kan oppnå en mer ønsket sammensetning uten at man behøver å gjennom-føre kompliserte etterfølgende renseoperasjoner, idet den rense-operasjon som gjennomføres bare er en enkel fjernelse av en fast rest fra oppsluttingen med saltsyre, for eksempel i form av en enkel sentrifugering. Man foretar først en foreløpig oppslutting med saltsyre at et material som inneholder aluminiumoksyd eller vannholdig aluminiumoksyd, foretrukket Bayer-aluminiumoksyd, gibbsitt, diaspor, hydrargilitt eller bøhmitt, idet oppslutningen gjennomføres ved høy temperatur på fra 100 til 160°c og ved trykk som holder systemet i flytende fase. Produktet fra oppsluttingen underkastes en fraskilling av det uomsatte material, mens den del som er omsatt underkastes en elektrolyse. Det utvinnes derved hydrogen og klor som etter syntese til saltsyre på nytt kan anvendes og resirkuleres til oppsluttingssonen, og det ønskede aluminium-klorhydroksyd med et ønsket og redusert klorinnhold utvinnes. The invention relates to a further development of the method which is the subject of patent no. 131,641, where a more desired composition can then be achieved without having to carry out complicated subsequent cleaning operations, since the cleaning operation which is carried out is only a simple removal of a solid residue from the digestion with hydrochloric acid, for example in the form of a simple centrifugation. First, a preliminary digestion is carried out with hydrochloric acid that a material containing alumina or hydrous alumina, preferably Bayer alumina, gibbsite, diaspore, hydrarglite or boehmite, the digestion being carried out at a high temperature of from 100 to 160°c and at a pressure that maintains the system in liquid phase. The product from the digestion is subjected to a separation of the unreacted material, while the part that has been reacted is subjected to electrolysis. Hydrogen and chlorine are thereby recovered which, after synthesis into hydrochloric acid, can be used again and recycled to the absorption zone, and the desired aluminum chlorohydroxide with a desired and reduced chlorine content is recovered.
Utgangsmaterialet oppsluttes med saltsyre i vandig løsning for fremstilling av aluminium-klorhydroksyder med formel A^tOH^Cly hvori verdiene for x og y er fra 2,5 til 3,5 og 3,5 til 2,5, alt i avhengighet av oppsluttingsforholdene. Oppsluttingen med saltsyre gjennomføres ved temperaturer mellom 100 og 160°C og trykk på fra 0,1 til 4 kg/cm . Ved uforandret temperatur påvirkes oppsluttingshastigheten av partikkelstørrelsen for den anvendte aluminiumforbindelse. Det er særlig fordelaktig å anvende produkter med partikkelstørrelser på fra 500 til 1000Å. The starting material is digested with hydrochloric acid in aqueous solution to produce aluminum chloride hydroxides of the formula A^tOH^Cly in which the values for x and y are from 2.5 to 3.5 and 3.5 to 2.5, all depending on the digestion conditions. The digestion with hydrochloric acid is carried out at temperatures between 100 and 160°C and pressure of from 0.1 to 4 kg/cm. At unchanged temperature, the absorption rate is affected by the particle size of the aluminum compound used. It is particularly advantageous to use products with particle sizes of from 500 to 1000 Å.
Fra et økonomisk synspunkt er det imidlertid ikke lønnsomt å fremstille oksyder eller vannholdige oksyder med den nevnte lille partikkelstørrelse, og det er en fordel ved den foreliggende fremgangsmåte at man kan anvende materialer med partikkelstørrelser på fra noen få ^,um til noen hundre ^um. From an economic point of view, however, it is not profitable to produce oxides or hydrous oxides with the aforementioned small particle size, and it is an advantage of the present method that materials with particle sizes of from a few µm to a few hundred µm can be used.
Det aluminium-klorhydroksyd som oppnås ved den forutgående oppslutting med saltsyre, underkastes etter å være skilt fra uomsatt aluminiumoksyd, som kan resirkuleres til oppsluttings-reaktoren, for en elektrolyse hvorved det oppnås en forbindelse med en mer ønsket sammensetning. The aluminum chlorohydroxide obtained by the previous digestion with hydrochloric acid, after being separated from unreacted aluminum oxide, which can be recycled to the digestion reactor, is subjected to an electrolysis whereby a compound with a more desired composition is obtained.
Elektrolysen kan gjennomføres på forskjellige måter hvor det aluminium-klorhydroksyd som oppnås ved den forutgående -oppslutting føres inn i elektrolysecellen hvor hydrogen utvikles ved katoden og klor ved anoden. De to gasser kan isoleres separat og anvendes på nytt for syntese av HC1 som resirkuleres til reaktoren hvori aluminiumoksydet oppsluttes. The electrolysis can be carried out in different ways, where the aluminum chlorhydroxide obtained by the previous digestion is introduced into the electrolysis cell where hydrogen is developed at the cathode and chlorine at the anode. The two gases can be isolated separately and used again for the synthesis of HC1, which is recycled to the reactor in which the aluminum oxide is absorbed.
Elektrolysen gjennomføres ved spenning fra 2 til 10 volt og The electrolysis is carried out at a voltage from 2 to 10 volts and
med en strømtetthet på fra 20 til 600 mA/cm 2. with a current density of from 20 to 600 mA/cm 2.
Klorinnholdet i det oppnådde aluminium-klorhydroksyd avhenger The chlorine content of the aluminum chloride hydroxide obtained depends
av den strømstyrke som tilføres cellen og som utgjør fra 40 of the current supplied to the cell, which amounts to from 40
til 150 A.h/kg klor-hydroksydløsning, med et innhold av aluminium-klorhydroksyd (regnet som A^O^) på fra 15 til 20 vektprosent. to 150 A.h/kg chlorine hydroxide solution, with a content of aluminum chloride hydroxide (calculated as A^O^) of from 15 to 20 percent by weight.
Arbeidstemperaturen for cellen er fra 50 til 130°c. Anvendel-sen av høye temperaturer er meget viktig, særlig ved industriell gjennomføring med anvendelse av høye strømtettheter, idet man på denne måte unngås utfelling av aluminiumhydroksyd ved katoden, hvilket ellers ville øke katodepolariseringen og nødvendig- The working temperature for the cell is from 50 to 130°c. The use of high temperatures is very important, particularly in industrial implementation with the use of high current densities, as in this way precipitation of aluminum hydroxide at the cathode is avoided, which would otherwise increase the cathode polarization and necessary
gjøre tilførsel av høyere spenning med derav følgende økning i kostnadene. make supply of higher voltage with the consequent increase in costs.
Elektrolysen gjennomføres under anvendelse av et egnet diafragma, idet når man anvender en celle som ikke inneholder noe diafragma har elektrolytten overalt den samme kjemiske sammensetning og pH, og de gasser som utvikles kan blande seg og danne en eksplosiv blanding. Videre kan klor løses i elektrolytten og reagere med vann i samsvar med reaksjonen, The electrolysis is carried out using a suitable diaphragm, since when using a cell that does not contain a diaphragm, the electrolyte everywhere has the same chemical composition and pH, and the gases that are developed can mix and form an explosive mixture. Furthermore, chlorine can be dissolved in the electrolyte and react with water according to the reaction,
Den ovenstående reaksjon er mer sannsynlig ved høyere pH-verdier. På grunn av at pH kan variere under elektrolysen kan denne reaksjon bli meget viktig når man nærmer seg slutten av elektrolysen, og følgelig vil strømutbyttet synke og klorhydroksyd-sammensetningen endre, seg ved at det dannes kloroksyder av forskjellige typer. The above reaction is more likely at higher pH values. Due to the fact that the pH can vary during the electrolysis, this reaction can become very important when approaching the end of the electrolysis, and consequently the current yield will decrease and the chlorine hydroxide composition will change, with chlorine oxides of different types being formed.
Som elektrodematerial anvendes grafitt og diafragmaet utgjøres av et keramisk material. Graphite is used as electrode material and the diaphragm is made of a ceramic material.
Oppfinnelsen skal i det følgende forklares ved hjelp av følgende illustrerende og eksempelvise utførelseseksempel: In the following, the invention will be explained with the help of the following illustrative and exemplary embodiment example:
EKSEMPEL EXAMPLE
Det ble anvendt Bayer-aluminiumoksyd med partikkelstørrelse 40 - 70 ^um (a - Al2°3 3 H2°^ med følgende prosentvise sammensetning. Bayer alumina with a particle size of 40 - 70 µm (a - Al2°3 3 H2°^) with the following percentage composition was used.
Bayer-aluminiumoksydet ble oppsluttet med en vandig løsning The Bayer alumina was slurried with an aqueous solution
av saltsyre 37 % (d = 1,19). of hydrochloric acid 37% (d = 1.19).
Oppsluttingen ble gjennomført på følgende måte: The closing was carried out in the following way:
100 kg tørt hydratisert aluminiumoksyd ble blandet med 100 kg HCl i en reaktor av Pyrex-glass eller av emaljert stål, ved 100 kg of dry hydrated alumina was mixed with 100 kg of HCl in a Pyrex glass or enamelled steel reactor, at
en temperatur på fra 120 til 150°C, idet reaktoren befant seg under en inert gassatmosfære ved trykk mellom 0,8 og 1,5 kg/cm<2 >og som var underkastet kraftig mekanisk røring. a temperature of from 120 to 150°C, the reactor being under an inert gas atmosphere at a pressure between 0.8 and 1.5 kg/cm<2> and which was subjected to vigorous mechanical stirring.
Etter tre timers omsetning ble suspensjonen fortynnet med 25 liter destillert vann inneholdende 100 g HCl, tømt ut fra reaktoren og sentrifugert ved hjelp av en kurv-sentrifuge av "Incoloy"-825- After three hours of reaction, the suspension was diluted with 25 liters of distilled water containing 100 g of HCl, emptied from the reactor and centrifuged using a basket centrifuge of "Incoloy"-825-
står etter avkjøling til en temperatur på fra 50 til 85°C, stands after cooling to a temperature of from 50 to 85°C,
ved hjelp av en varmeveksler som også var fremstilt av den samme "Incoloy"-825-legering. using a heat exchanger that was also made from the same "Incoloy"-825 alloy.
Etter oppsluttingen var 50 % av det tørre utgangs-aluminiumoksyd (som bare inneholdt krystallisasjonsvannet) (ca. 50 kg) bragt i oppløsning, og resterende faststoff ble fjernet ved sentrifugering. After the digestion, 50% of the dry starting alumina (which only contained the water of crystallization) (approx. 50 kg) had been brought into solution, and the remaining solids were removed by centrifugation.
En kilo av løsningen av aluminium-klorhydroksydet som skrev One kilogram of the solution of the aluminum chloride hydroxide that wrote
seg fra oppsluttingen med HCl, og som var skilt fra det uomsatte aluminiumoksyd og som inneholdt 15 til 18 vektprosent Al203, med formel Al,, (OH) 2 ^ Cl^ ^, ble underkastet elektrolyse for å øke forholdet mellom OH og Cl. Elektrolysen ble gjennom-ført ved 80°C. from the digestion with HCl, and which was separated from the unreacted alumina and which contained 15 to 18 percent by weight Al 2 O 3 , of the formula Al,, (OH) 2 ^ Cl^ ^, was subjected to electrolysis to increase the ratio of OH to Cl. The electrolysis was carried out at 80°C.
Cellen var fremstilt av glass og hadde keramisk diafragma, og elektrodene beste av grafitt med en overflate på omtrent 80 The cell was made of glass and had a ceramic diaphragm, and the electrodes were made of graphite with a surface of about 80
2 2
til 100 cm . to 100 cm.
Det ble arbeidet ved en strømtetthet pa 300 mA/cm 2 med en spenning på 3,5 - 4 volt. Katodevæsken ble omrørt ved hjelp av en sirkulasjonspumpe. The work was done at a current density of 300 mA/cm 2 with a voltage of 3.5 - 4 volts. The cathode liquid was stirred using a circulation pump.
Under elektrolysen ble det tilført en strømmengde på 40 - 50 A.h, og etter omtrent 1 timer og 45 minutters elektrolyse ble det oppnådd et klorhydroksyd med formel A^ÉOH^Cl^ med et strøm-utbytte på 95 % regnet på klor-resten. During the electrolysis, a current amount of 40 - 50 A.h was supplied, and after approximately 1 hour and 45 minutes of electrolysis, a chlorine hydroxide with the formula A^ÉOH^Cl^ was obtained with a current yield of 95% calculated on the chlorine residue.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| IT21250/72A IT949754B (en) | 1972-03-01 | 1972-03-01 | PROCEDURE FOR THE PRODUCTION OF ALUMINUM CHLOROHYDROXIDES WITH CONTROLLED CHLORINE |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| NO140051B true NO140051B (en) | 1979-03-19 |
| NO140051C NO140051C (en) | 1979-06-27 |
Family
ID=11179031
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| NO755/73A NO140051C (en) | 1972-03-01 | 1973-02-26 | PROCEDURE FOR THE PREPARATION OF ALUMINUM CHLORINE HYDROXIDE WITH A CONTROLLED AND REDUCED CHLORINE CONTENT |
Country Status (27)
| Country | Link |
|---|---|
| JP (1) | JPS5341640B2 (en) |
| AR (1) | AR201099A1 (en) |
| AT (1) | AT330720B (en) |
| BE (1) | BE795921A (en) |
| BR (1) | BR7301578D0 (en) |
| CA (1) | CA1020903A (en) |
| CH (1) | CH578999A5 (en) |
| CS (1) | CS184322B2 (en) |
| DD (1) | DD102677A5 (en) |
| DE (1) | DE2310073A1 (en) |
| ES (1) | ES412314A1 (en) |
| FR (1) | FR2174118B1 (en) |
| GB (1) | GB1376885A (en) |
| IE (1) | IE39029B1 (en) |
| IN (1) | IN139216B (en) |
| IT (1) | IT949754B (en) |
| LU (1) | LU67118A1 (en) |
| NL (1) | NL7302917A (en) |
| NO (1) | NO140051C (en) |
| PL (1) | PL84526B1 (en) |
| RO (1) | RO63835A (en) |
| SE (1) | SE399868B (en) |
| SU (1) | SU660584A3 (en) |
| TR (1) | TR17276A (en) |
| YU (1) | YU36665B (en) |
| ZA (1) | ZA731240B (en) |
| ZM (1) | ZM3473A1 (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5560022A (en) * | 1978-10-26 | 1980-05-06 | Nikki Universal Co Ltd | Production of spherical alumina |
| JPS60134589A (en) * | 1983-12-22 | 1985-07-17 | Fuji Photo Film Co Ltd | Simultaneous system of line sequential chrominance signal |
| JPS60134588A (en) * | 1983-12-22 | 1985-07-17 | Fuji Photo Film Co Ltd | Simultaneous system of line sequential chrominance signal |
| JPS6199316A (en) * | 1984-10-19 | 1986-05-17 | Yukio Yoshizawa | Apparatus for planting terminal into transformer bobbin or the like |
| JPS61187489A (en) * | 1985-02-15 | 1986-08-21 | Canon Inc | Color signal processing device |
| WO2003053850A1 (en) * | 2001-12-21 | 2003-07-03 | Clariant Gmbh | Method for the production of highly pure basic aluminum halogenides |
| US8801909B2 (en) | 2006-01-06 | 2014-08-12 | Nextchem, Llc | Polymetal hydroxychloride processes and compositions: enhanced efficacy antiperspirant salt compositions |
| US7846318B2 (en) | 2006-01-06 | 2010-12-07 | Nextchem, Llc | Polyaluminum chloride and aluminum chlorohydrate, processes and compositions: high-basicity and ultra high-basicity products |
| EP2086675B1 (en) | 2006-11-13 | 2010-11-03 | Albemarle Netherlands B.V. | Process for the preparation of an fcc catalyst |
| CN103305862B (en) * | 2012-03-13 | 2015-09-16 | 温州大学 | High-basicity polymerize aluminum chloride and Al 13muriatic electrochemical production device and manufacture method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2392531A (en) * | 1937-05-15 | 1946-01-08 | Huehn Werner | Production of water-soluble basic aluminum compounds |
| GB655617A (en) * | 1947-10-30 | 1951-07-25 | Peter Spence & Sons Ltd | Production of aqueous solutions of aluminium chloride |
| US3113911A (en) * | 1960-09-06 | 1963-12-10 | Armour Pharma | Process of preparing aluminum chlorhydroxides and aluminum hydroxide |
-
1972
- 1972-03-01 RO RO197274039A patent/RO63835A/en unknown
- 1972-03-01 IT IT21250/72A patent/IT949754B/en active
-
1973
- 1973-02-21 ZA ZA731240A patent/ZA731240B/en unknown
- 1973-02-26 BE BE795921D patent/BE795921A/en not_active IP Right Cessation
- 1973-02-26 NO NO755/73A patent/NO140051C/en unknown
- 1973-02-26 ES ES412314A patent/ES412314A1/en not_active Expired
- 1973-02-26 AR AR246807A patent/AR201099A1/en active
- 1973-02-26 IE IE00291/73A patent/IE39029B1/en unknown
- 1973-02-26 CH CH278973A patent/CH578999A5/xx not_active IP Right Cessation
- 1973-02-27 TR TR17276A patent/TR17276A/en unknown
- 1973-02-27 GB GB964573A patent/GB1376885A/en not_active Expired
- 1973-02-28 IN IN446/CAL/73A patent/IN139216B/en unknown
- 1973-02-28 DE DE19732310073 patent/DE2310073A1/en active Pending
- 1973-02-28 FR FR7307011A patent/FR2174118B1/fr not_active Expired
- 1973-02-28 CA CA164,845A patent/CA1020903A/en not_active Expired
- 1973-02-28 SU SU731888666A patent/SU660584A3/en active
- 1973-02-28 YU YU0532/73A patent/YU36665B/en unknown
- 1973-02-28 DD DD169658A patent/DD102677A5/xx unknown
- 1973-02-28 CS CS7300001445A patent/CS184322B2/en unknown
- 1973-02-28 PL PL1973160966A patent/PL84526B1/pl unknown
- 1973-02-28 LU LU67118A patent/LU67118A1/xx unknown
- 1973-03-01 ZM ZM34/73*UA patent/ZM3473A1/en unknown
- 1973-03-01 BR BR731578A patent/BR7301578D0/en unknown
- 1973-03-01 AT AT182073A patent/AT330720B/en not_active IP Right Cessation
- 1973-03-01 JP JP2378673A patent/JPS5341640B2/ja not_active Expired
- 1973-03-01 SE SE7302922A patent/SE399868B/en unknown
- 1973-03-01 NL NL7302917A patent/NL7302917A/xx unknown
Also Published As
| Publication number | Publication date |
|---|---|
| NL7302917A (en) | 1973-09-04 |
| ZM3473A1 (en) | 1974-02-21 |
| LU67118A1 (en) | 1973-05-03 |
| JPS4930294A (en) | 1974-03-18 |
| BE795921A (en) | 1973-06-18 |
| BR7301578D0 (en) | 1974-05-16 |
| DD102677A5 (en) | 1973-12-20 |
| ES412314A1 (en) | 1976-05-01 |
| IE39029L (en) | 1973-09-01 |
| CS184322B2 (en) | 1978-08-31 |
| IN139216B (en) | 1976-05-22 |
| PL84526B1 (en) | 1976-04-30 |
| SE399868B (en) | 1978-03-06 |
| IE39029B1 (en) | 1978-07-19 |
| AT330720B (en) | 1976-07-12 |
| CH578999A5 (en) | 1976-08-31 |
| FR2174118B1 (en) | 1976-05-21 |
| IT949754B (en) | 1973-06-11 |
| ATA182073A (en) | 1975-10-15 |
| NO140051C (en) | 1979-06-27 |
| SU660584A3 (en) | 1979-04-30 |
| JPS5341640B2 (en) | 1978-11-06 |
| CA1020903A (en) | 1977-11-15 |
| AR201099A1 (en) | 1975-02-14 |
| RO63835A (en) | 1979-08-15 |
| FR2174118A1 (en) | 1973-10-12 |
| GB1376885A (en) | 1974-12-11 |
| YU36665B (en) | 1984-08-31 |
| TR17276A (en) | 1975-03-24 |
| ZA731240B (en) | 1973-11-28 |
| YU53273A (en) | 1981-11-13 |
| DE2310073A1 (en) | 1973-09-20 |
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