DK172381B1 - Process for condensation of aluminum chloride - Google Patents
Process for condensation of aluminum chloride Download PDFInfo
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- DK172381B1 DK172381B1 DK036388A DK36388A DK172381B1 DK 172381 B1 DK172381 B1 DK 172381B1 DK 036388 A DK036388 A DK 036388A DK 36388 A DK36388 A DK 36388A DK 172381 B1 DK172381 B1 DK 172381B1
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- aluminum chloride
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- condensation
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D7/00—Sublimation
- B01D7/02—Crystallisation directly from the vapour phase
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- 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
- C01F7/58—Preparation of anhydrous aluminium chloride
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- 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
- C01F7/62—Purification
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
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Abstract
Description
i DK 172381 B1in DK 172381 B1
Den foreliggende opfindelse angår en fremgangsmåde til kondensation af vandfrit aluminiumchlorid.The present invention relates to a process for condensing anhydrous aluminum chloride.
Aluminiumchlorid anvendes hyppigt som katalysator inden 5 for den organiske kemi og ligeledes i kosmetikindustrien. Aluminiumchloridet opnås under forløbet af fabrikationen deraf i gasformig fase eventuelt blandet med andre produkter, og man isolerer det ved at kondensere det på en kold væg ved omgivelsernes temperatur. Man opnår på denne 10 måde en skorpe aluminiumchlorid, som man løsner fra væggen ved hjælp af mekaniske midler, såsom vibrationer eller slag. Den kolde væg er simpelthen den indre væg af en stålbeholder udsat for den omgivende luft.Aluminum chloride is frequently used as a catalyst in organic chemistry and also in the cosmetics industry. The aluminum chloride is obtained during the course of its manufacture in the gaseous phase, possibly mixed with other products, and it is isolated by condensing it on a cold wall at ambient temperature. In this way, a crust of aluminum chloride is obtained, which is released from the wall by mechanical means such as vibration or impact. The cold wall is simply the inner wall of a steel container exposed to the surrounding air.
15 Skorperne af aluminiumchlorid formales for at opnå et produkt, hvori stykkerne af forskellige former er mindre end 5 cm i deres største dimension. Formalingen frembringer støv, det er nødvendigt at sigte aluminiumchloridet og at recirkulerer de fine produkter. I japanske patent-20 ansøgningsskrifter nr. 34988/70 og 34989/70 dateret 23. april 1970 og i japansk patentansøgningsskrift nr. 42243/70 dateret 18. maj 1970 omtales en fremgangsmåde til at isolere aluminiumchlorid i gasformig fase, hvilken fremgangsmåde består i at lade gassen passerer hen 25 over en væg, der holdes ved 80 °C eller ved 85 °C, hvorpå man, når aluminiumchloridet har dannet krystaller, genopvarmer denne væg til 220 °C for at løsne aluminiumchloridet, som man indvinder. Disse krystaller har ofte under dannelsen deraf og under deres vækst en tendens til at 30 klæbe sammen indbyrdes og til at danne en skorpe, som det er nødvendigt at formale og at sigte.The aluminum chloride crusts are ground to obtain a product in which the pieces of various shapes are less than 5 cm in their largest dimension. The milling produces dust, it is necessary to screen the aluminum chloride and to recycle the fine products. Japanese Patent Application Serial Nos. 34988/70 and 34989/70 dated April 23, 1970 and Japanese Patent Application Serial No. 42243/70 dated May 18, 1970 disclose a process for isolating gaseous aluminum chloride, which method comprises allow the gas to pass over a wall maintained at 80 ° C or 85 ° C, then, once the aluminum chloride has formed crystals, this wall is reheated to 220 ° C to release the recovered aluminum chloride. These crystals often, during their formation and during their growth, tend to adhere to one another and to form a crust which is necessary to grind and to aim.
I disse patentansøgningsskrifter beskriver man kondensationen af aluminiumchlorid på plane vægge under særlige 35 temperaturbetingelser; eller på den indre væg af en cylinder udstyret i sin base med en skrabende klinge til DK 172381 B1 2 opsamling af aluminiumchloridet og til udtagning af dette. Ved alle disse fremgangsmåder udvindes aluminiumchloridet i form af agglomerater eller af plader, som det er vanskeligt at udtage fra den beholder, hvori de er blevet 5 fremstillet. Dersom man ikke anvender mekaniske anordninger for at reducere størrelsen af disse agglomerater, risikerer man at tilstoppe udgangen fra beholderen. Ved alle disse fremgangsmåder underkastes apparaturet yderligere termiske cycliske forhold, som fremkalder udmattelses-10 spændinger, der fører til brud.These patent applications describe the condensation of aluminum chloride on flat walls under special temperature conditions; or on the inner wall of a cylinder equipped in its base with a scraping blade for collecting the aluminum chloride and for removing it. In all these processes, the aluminum chloride is recovered in the form of agglomerates or plates which are difficult to remove from the container in which they have been produced. If mechanical devices are not used to reduce the size of these agglomerates, there is a risk of clogging the outlet of the container. In all these methods, the apparatus is subjected to additional thermal cyclic conditions which produce fatigue stresses leading to rupture.
I Inorg. Nucl. Chem. Lett. 1979, 6(4), 399-401 omtales udvindingen af aluminiumchlorid ved kondensation af gasfasen af en blanding af NaCl og A1C13 på et koldt enkelt-15 rør (kold finger). Røret overføres derpå til en anden beholder, hvor man frembringer løsnelse af aluminiumchloridet ved at tilslutte en elektrisk varmespiral indeholdt i røret. I GB patentskrift nr. 1 410 800 er beskrevet et apparatur til at kondensere et produkt i fast form på et 20 bundt afkølede rør. Efter kondensationen smeltes kondensatet helt ved opvarmning leveret af en spiral rullet udenom apparaturet.In Inorg. Nucl. Chem. Lett. 1979, 6 (4), 399-401 discloses the recovery of aluminum chloride by condensing the gas phase of a mixture of NaCl and A1C13 on a cold single-tube (cold finger). The tube is then transferred to another container, whereby the aluminum chloride is released by connecting an electrical coil contained within the tube. GB patent specification 1,410,800 discloses an apparatus for condensing a solid product on a 20 bundle of cooled tubes. After the condensation, the condensate is completely melted by heating supplied by a coil rolled around the apparatus.
Man har nu fundet en fremgangsmåde, som gør det muligt at 25 fremstille aluminiumchlorid, som ikke optræder i form af plader, hvorved der anvendes et apparatur, der er meget mindre følsomt over for de termiske påvirkninger end apparaturerne ifølge den kendte teknik.A method has now been found which makes it possible to produce aluminum chloride which does not appear in the form of plates, using an apparatus which is much less sensitive to the thermal stresses than the apparatus of the prior art.
30 Denne fremgangsmåde er særegen ved, at (a) aluminiumchloridet alene eller indeholdt i en gasfor-mig strøm kondenseres til fast fase på ydersiden af i hovedsagen vertikale rør lukket ved deres nedre ende og 35 fastgjort til en rørplade ved deres øvre ende.This method is peculiar in that (a) the aluminum chloride alone or contained in a gaseous stream is condensed to solid phase on the outside of substantially vertical tubes closed at their lower end and attached to a tube plate at their upper end.
DK 172381 B1 3 (b) rørenes temperatur holdes mellem 40 og 60 °C under kondensationen, og (c) rørene derpå genopvarmes, for at aluminiumchloridet 5 løsnes.(B) the temperature of the tubes is kept between 40 and 60 ° C during the condensation, and (c) the tubes are then reheated to release the aluminum chloride 5.
Denne fremgangsmåde kan anvendes på alle gasarter indeholdende aluminiumchlorid, især på sådanne, der opnås under forløbet af fremstilling deraf. Man opnår under for-10 løbet af fremstillingen af aluminiumchlorid i et af trinene i de anvendte fremgangsmåder aluminiumchloridet i form af en gasart, der enten er ren eller en blanding af andre gasarter, som kan være inerte gasarter, såsom nitrogen eller luft, eller restgasarter fra reaktionen så-15 som carbondioxid, carbonmonoxid, chlor og chlorerede produkter. Dette kan være et trin i en fremgangsmåde til fremstilling af aluminiumchlorid eller et trin i en fremgangsmåde i løbet af hvilken man fremstiller aluminiumchlorid med henblik på at fremstille aluminium.This process can be applied to all gases containing aluminum chloride, especially to those obtained during the course of their preparation. During the course of the preparation of aluminum chloride in one of the steps of the processes employed, the aluminum chloride is obtained in the form of a gas species which is either pure or a mixture of other gases which may be inert gases such as nitrogen or air or residual gases. from the reaction such as carbon dioxide, carbon monoxide, chlorine and chlorinated products. This can be a step in a process for producing aluminum chloride or a step in a process during which aluminum chloride is prepared to produce aluminum.
20 På figuren er vist et eksempel på en anordning til iværksættelse af fremgangsmåden ifølge opfindelsen. Man fast-svej ser vertikale rør (2), der er lukket i den nederste del, ved deres øvre del på en rørplade (4), idet de pla-25 ceres i en beholder (1), der i sin nedre del er lukket med en ventil (3). Man indfører ved (10) gassen indeholdende aluminiumchloridet, og man af gasser gennem røret (11) de ikke-kondenserbare bestanddele. Ved (12) indfører man et flydende medium til varmeoverførsel, som fordeles 30 gennem rørene (5) ned i hvert rør (2) og derpå fjernes gennem røret (13).20 The figure shows an example of a device for initiating the method according to the invention. Vertical pipes (2) closed in the lower part are fixedly welded at their upper part to a pipe plate (4), being placed in a container (1) closed in its lower part. with a valve (3). The (10) gas containing the aluminum chloride is introduced and the non-condensable constituents of gases through the tube (11) are introduced. At (12), a liquid heat transfer medium is introduced which is distributed through the tubes (5) into each tube (2) and then removed through the tube (13).
Gassen indeholdende aluminiumchloridet bringes i kontakt med ydervæggen af de i overvejende grad vertikale rør.The gas containing the aluminum chloride is brought into contact with the outer wall of the predominantly vertical pipes.
35 Disse rør holdes ved en temperatur mellem 40 og 60 °C, således at aluminiumchloridet krystalliserer, hvorpå man DK 172381 B1 4 genopvarmer disse rør f.eks. ved cirkulation af et varme-overførende flydende medium for at sublimere alumini-umchloridet i kontakt med røret, aluminiumchloridet løsner sig og man kan opsamle det ved tyngdekraftens hjælp.These tubes are kept at a temperature between 40 and 60 ° C so that the aluminum chloride crystallizes, whereupon these tubes are reheated e.g. By circulating a heat-transferring liquid medium to sublimate the aluminum chloride in contact with the tube, the aluminum chloride dissolves and it can be collected by gravity.
55
De i hovedsagen vertikale rør kan have vilkårlige dimensioner; men man foretrækker, at forholdet mellem deres længde og deres ydre diameter er mellem 1 og 100, med fordel mellem 2 og 50. Disse rør kan være af ethvert ma-10 teriale forudsat, at det er resistent overfor alumini-umchlorid; man anvender fortrinsvis almindeligt stål, rustfrit stål eller en nikkelbaseret legering. Man foretrækker ligeledes, at disse rørs ydre overflade er glat.The substantially vertical tubes may have any dimensions; but it is preferred that the ratio of their length to their outer diameter be between 1 and 100, preferably between 2 and 50. These tubes may be of any material provided it is resistant to aluminum chloride; preferably ordinary steel, stainless steel or a nickel-based alloy is used. It is also preferred that the outer surface of these tubes be smooth.
Man foretrækker at disse rør er placeret i en beholder.It is preferred that these tubes be placed in a container.
15 Man holder fortrinsvis den indre side af væggene af denne beholder ved en tilstrækkelig høj temperatur til at undgå, at aluminiumchloridet aflejre sig derpå. Den beholder kan være forsynet i sin nedre del med et lukkeorgan, såsom en ventil. Man kan også anvende rør af konisk form, 20 hvori det største tværsnit befinder sig i den øvre del, der vender imod rørpladen.Preferably, the inner side of the walls of this container is maintained at a sufficiently high temperature to prevent the aluminum chloride from depositing thereon. That container may be provided at its lower end with a closure means such as a valve. Tapered tubes may also be used, the largest cross-section of which is in the upper portion facing the tube plate.
Når gasarten indeholdende aluminiumchloridet er indført i denne beholder, aflejrer aluminiumchloridet sig på røre-25 ne, og de ikke-kondenserbare bestanddele afgasses fortrinsvis gennem en åbning, der er forskellig fra indføringsåbningen for gasarterne indeholdende aluminiumchloridet .When the gas containing the aluminum chloride is introduced into this container, the aluminum chloride deposits on the tubes, and the non-condensable components are preferably degassed through an opening different from the introductory opening for the gases containing the aluminum chloride.
30 Temperaturen på væggen af rørene holdes mellem 40 og 60 °C ved hjælp af et varmeoverførende flydende medium. Man kan anvende ethvert varmeoverførende flydende medium såsom en gasart, en organisk forbindelse, varmt vand og lavtryksdamp.The temperature of the wall of the pipes is maintained between 40 and 60 ° C by means of a heat transfer liquid medium. Any heat-transferring liquid medium such as a gas species, an organic compound, hot water and low pressure steam can be used.
35 DK 172381 B1 5 Når man anvender et rør af metal er temperaturen af det flydende medium meget tæt ved væggens temperatur. Det er så tilstrækkeligt for at regulere væggens temperatur, at man regulerer temperaturen af det varmeoverførende fly-5 dende medium. Det foretrækkes, at væggens temperatur holdes konstant under kondensationen af aluminiumchloridet.35 DK 172381 B1 5 When using a metal tube, the temperature of the liquid medium is very close to the temperature of the wall. It is sufficient to control the temperature of the wall that the temperature of the heat transferring liquid medium is controlled. It is preferred that the temperature of the wall is kept constant during the condensation of the aluminum chloride.
Under disse betingelser kondenseres aluminiumchloridet i form af granuler, som i hovedsagen har form af en kegle.Under these conditions, the aluminum chloride is condensed in the form of granules which are essentially in the form of a cone.
10 Keglens højde er mellem 0,5 og 5 cm, og forholdet mellem højden og diameteren ved keglens basis er mellem 1 og 10. Keglens spids vender mod den kolde væg. Keglerne rører hinanden ved deres basis og er i almindelighed hverken indbyrdes sammenklæbede eller agglomererede.10 The height of the cone is between 0.5 and 5 cm, and the ratio of the height to the diameter at the base of the cone is between 1 and 10. The tip of the cone faces the cold wall. The cones touch each other at their base and are generally neither intertwined nor agglomerated.
1515
Trykket af den gas, som indeholder aluminiumchloridet, er uden særlig betydning, hvilket også gælder trykket i beholderen. Denne gas har næsten altid atmosfæretrykket eller tryk tæt derved, og man gennemfører kondensationen af 20 aluminiumchloridet ved dette tryk. Såsnart aluminiumchloridet befinder sig i kontakt med den kolde væg, kondenseres det. For at udvinde det faste aluminiumchlorid hæver man temperaturen af væggen, der tidligere var kold, således at aluminiumchloridet smelter eller sublimerer, hvil-25 ket fremkalder løsnelse af det faste stof ved tyngdekraftens hjælp. Man opnår en overgang til flydende tilstand eller en sublimering i afhængighed af, om trykket er større eller mindre end trykket ved tripelpunktet (2,3 atm absolut tryk). Man foretrækker at det faste stof løs-30 ner sig under indvirkning af sublimering. Det er tilstrækkeligt blot at opvarme væggen i et kort øjeblik for at fremkalde løsnelse af det faste stof. Man opvarmer hyppigst til mellem 200 og 250 °C.The pressure of the gas containing the aluminum chloride is of no particular importance, as is the pressure in the container. This gas almost always has atmospheric pressure or pressure close to it, and the condensation of the aluminum chloride is carried out at this pressure. As soon as the aluminum chloride is in contact with the cold wall, it condenses. To recover the solid aluminum chloride, raise the temperature of the wall, which was previously cold, so that the aluminum chloride melts or sublimates, which causes dissolution of the solid by gravity. A transition to liquid state or sublimation is achieved depending on whether the pressure is greater or less than the pressure at the triple point (2.3 atm absolute pressure). It is preferred that the solid dissolve under the effect of sublimation. It is sufficient merely to heat the wall for a short moment to induce the dissolution of the solid. It is most frequently heated to between 200 and 250 ° C.
35 Til at opvarme væggen kan man anvende et varmeoverførende flydende medium, som man opvarmer til tilstrækkelig høj DK 172381 B1 6 temperatur, til at væggen er tilstrækkelig varm til at smelte eller sublimere aluminiumchloridet. Man kan anvende det samme varmeoverførende flydende medium som det, der bringer væggen til mellem 40 og 60 °C; man kan lige-5 ledes have et reservoir af varmt medium og et reservoir af koldt medium, idet disse to flydende medier kan være identiske eller forskellige, og man lader dem cirkulere alternerende imod væggen.35 To heat the wall, one can use a heat-transferring liquid medium which is heated to a sufficiently high temperature for the wall to be sufficiently warm to melt or sublimate the aluminum chloride. One can use the same heat transfer liquid medium as that which brings the wall to between 40 and 60 ° C; one can also have a hot medium reservoir and a cold medium reservoir, these two liquid media being identical or different, and allowing them to circulate alternately against the wall.
10 Medens man genopvarmer væggen for at løsne aluminiumchloridet, kan man standse indføringen af gasser indeholdende aluminiumchloridet ind i beholderen for at undgå tab af produkt. Det foretrækkes at opvarme væggen hurtigt, således at man ikke skal opvarme hele det faste materiale.10 While reheating the wall to loosen the aluminum chloride, the introduction of gases containing the aluminum chloride into the container can be stopped to avoid loss of product. It is preferred to heat the wall quickly, so as not to heat the entire solid material.
1515
Under opvarmningen, som fremkalder løsneisen af aluminiumchloridet fra væggen, kan der sublimeres en lille mængde aluminiumchlorid; det er således interessant, at dette aluminiumchlorid vil kunne aflejre sig på en kold væg, 20 f.eks. i en anden beholder forbundet med den forudgående.During the heating, which causes the release of the aluminum chloride from the wall, a small amount of aluminum chloride can be sublimated; It is thus interesting that this aluminum chloride will be able to deposit on a cold wall, e.g. in another container associated with the preceding one.
Det er bekvemt, dersom man skal behandle en kontinuerlig gasformig strøm indeholdende aluminiumchlorid, at tilvejebringe mindst to beholdere, hvor den ene har en kold væg, og den anden er under opvarmning for at løsne alumi-25 niumchloridet; og man ombytter derpå beholdernes funktioner. Man kunne ligeledes have et vilkårligt antal beholdere. En fordel knyttet til anvendelsen af rør ifølge den foreliggende opfindelse, der er fastgjort ved en enkelt af deres ender til en rørplade, består i, at de ikke un-30 derkastes forskellige udvidelser under de cycliske termiske påvirkninger.It is convenient, if one is to treat a continuous gaseous stream containing aluminum chloride, to provide at least two containers, one having a cold wall and the other being heated to release the aluminum chloride; and then the functions of the containers are exchanged. You could also have any number of containers. An advantage associated with the use of pipes of the present invention, attached at a single of their ends to a pipe plate, is that they are not subjected to various extensions under the cyclic thermal stresses.
Det efterfølgende eksempel belyser opfindelsen nærmere.The following example illustrates the invention in more detail.
35 EKSEMPEL: 7 DK 172381 B1EXAMPLE: 7 DK 172381 B1
Man anvender et apparatur som vist på figuren og med følgende dimensioner: diameter af rørpladen (4): 750 mm otte rør (2) placeret regelmæssigt i et kvadratisk mønster med siden 210 mm og således, at man har - to rør af stål med yderdiameter 88,9 og tykkelse 3,2 mm - to rør af Inconel 600 med yderdiameter 88,9 og tykkelse 3,05 mm - to rør af Monel 400 med yderdiameter 88,9 og tykkelse 3,05 mm “ to rør af Uranus B6 med yderdiameter 88,9 og tykkelse 4 mm den nyttige længde af rørene er 700 mm, de andre dele af anordningen er udført af stål, den cylindriske del og den koniske del af beholderen (1) holdes ved 200 °C, ventilen (3) er en ventil med direkte passage og med diameteren 200 mm.An apparatus is used as shown in the figure and with the following dimensions: diameter of the pipe plate (4): 750 mm eight pipes (2) placed regularly in a square pattern with the side 210 mm and so that it has - two pipes of steel with outer diameter 88.9 and thickness 3.2 mm - two tubes of Inconel 600 with outer diameter 88.9 and thickness 3.05 mm - two tubes of Monel 400 with outer diameter 88.9 and thickness 3.05 mm “two tubes of Uranus B6 with outer diameter 88.9 and thickness 4 mm the useful length of the tubes is 700 mm, the other parts of the device are made of steel, the cylindrical part and the conical part of the container (1) are held at 200 ° C, the valve (3) is a valve with direct passage and with a diameter of 200 mm.
5 Man indfører aluminiumchloridet gennem røret (10) med en hastighed på 30 kg/time i 6 timer. Temperaturen af væggen af rørene (2) holdes på 55 °C ved cirkulation af varrae-overførende flydende medium. Temperaturen af det varme-overførende flydende medium er 50 °C målt ved røret (13).5 Insert the aluminum chloride through the tube (10) at a rate of 30 kg / h for 6 hours. The temperature of the wall of the tubes (2) is maintained at 55 ° C by circulation of varrae transferring liquid medium. The temperature of the heat-transferring liquid medium is 50 ° C as measured by the tube (13).
Efter 6 timers forløb modificerer man cirkulationen for at lade det varmeoverførende medium på 260 °C passere og bringe væggen op på 190 °C så hurtigt som muligt, i løbet 10 DK 172381 B1 8 af ca. 1 minut. Efter ca. 1 minut løsner aluminiumchlori-det sig, og det udvindes i en beholder placeret under den isolerede afsublimeringsbeholder gennem en ventil med direkte passage og med diameteren 0 = 200.After 6 hours, the circulation is modified to allow the heat transfer medium of 260 ° C to pass and bring the wall up to 190 ° C as quickly as possible, in the course of approx. 1 minute. After approx. For 1 minute, the aluminum chlorine dissolves and it is recovered in a container placed under the insulated sublimation vessel through a direct passage valve with a diameter of 0 = 200.
55
Man opnår 180 kg aluminiumchlorid i form af kegler med en længde på 30-35 mm og med en diameter i den yderste ende mellem 8 og 12 mm.180 kg of aluminum chloride is obtained in the form of cones with a length of 30-35 mm and with a diameter at the outer end between 8 and 12 mm.
10 Løsneisen er total efter ca. 2 minutters forløb, og man bringer det varmeoverførende flydende medium tilbage til 50 °C, hvorved det er klar til den efterfølgende cyclus.10 The loose ice is total after approx. 2 minutes and the heat transferring liquid medium is brought back to 50 ° C, ready for the subsequent cycle.
Claims (1)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8700938A FR2609977B1 (en) | 1987-01-27 | 1987-01-27 | PROCESS OF CONDENSATION OF ALUMINUM CHLORIDE |
| FR8700938 | 1987-01-27 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DK36388D0 DK36388D0 (en) | 1988-01-26 |
| DK36388A DK36388A (en) | 1988-07-28 |
| DK172381B1 true DK172381B1 (en) | 1998-05-04 |
Family
ID=9347311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DK036388A DK172381B1 (en) | 1987-01-27 | 1988-01-26 | Process for condensation of aluminum chloride |
Country Status (12)
| Country | Link |
|---|---|
| EP (1) | EP0278805B1 (en) |
| JP (1) | JPH0710725B2 (en) |
| AT (1) | ATE80131T1 (en) |
| CA (1) | CA1339826C (en) |
| DE (1) | DE3874163T2 (en) |
| DK (1) | DK172381B1 (en) |
| ES (1) | ES2034281T3 (en) |
| FR (1) | FR2609977B1 (en) |
| GR (1) | GR3006386T3 (en) |
| IE (1) | IE63079B1 (en) |
| IN (1) | IN170684B (en) |
| PT (1) | PT86633B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010131522A (en) * | 2008-12-04 | 2010-06-17 | Mitsubishi Rayon Co Ltd | Crystallizer and method of removing crystal |
| JP6274636B2 (en) * | 2012-06-29 | 2018-02-07 | 三菱ケミカル株式会社 | Crystallization method |
| CN107456776B (en) * | 2017-08-03 | 2020-02-11 | 山东飞扬化工有限公司 | Device and method for purifying dimethyl carbonate |
| CN115518408B (en) * | 2022-11-08 | 2024-04-26 | 山东坤宝新材料集团股份有限公司 | Scraper catcher and method for anhydrous aluminum trichloride production |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2852517A (en) * | 1955-11-07 | 1958-09-16 | Dow Chemical Co | Separating method |
| US3842163A (en) * | 1971-09-07 | 1974-10-15 | Aluminum Co Of America | Production of aluminum chloride |
| NL7117037A (en) * | 1971-12-13 | 1973-06-15 | ||
| SU1018910A1 (en) * | 1981-06-22 | 1983-05-23 | Предприятие П/Я В-2287 | Method for producing aliminium chloride |
-
1987
- 1987-01-27 FR FR8700938A patent/FR2609977B1/en not_active Expired - Lifetime
-
1988
- 1988-01-14 AT AT88400075T patent/ATE80131T1/en not_active IP Right Cessation
- 1988-01-14 ES ES198888400075T patent/ES2034281T3/en not_active Expired - Lifetime
- 1988-01-14 DE DE8888400075T patent/DE3874163T2/en not_active Expired - Fee Related
- 1988-01-14 EP EP88400075A patent/EP0278805B1/en not_active Expired - Lifetime
- 1988-01-25 JP JP63014362A patent/JPH0710725B2/en not_active Expired - Fee Related
- 1988-01-26 DK DK036388A patent/DK172381B1/en not_active IP Right Cessation
- 1988-01-26 IE IE19688A patent/IE63079B1/en not_active IP Right Cessation
- 1988-01-26 CA CA000557376A patent/CA1339826C/en not_active Expired - Fee Related
- 1988-01-27 IN IN53/MAS/88A patent/IN170684B/en unknown
- 1988-01-27 PT PT86633A patent/PT86633B/en unknown
-
1992
- 1992-11-30 GR GR920402759T patent/GR3006386T3/el unknown
Also Published As
| Publication number | Publication date |
|---|---|
| FR2609977A1 (en) | 1988-07-29 |
| JPS63185813A (en) | 1988-08-01 |
| PT86633B (en) | 1991-12-31 |
| CA1339826C (en) | 1998-04-21 |
| EP0278805A1 (en) | 1988-08-17 |
| JPH0710725B2 (en) | 1995-02-08 |
| IE880196L (en) | 1988-07-27 |
| FR2609977B1 (en) | 1991-06-07 |
| DK36388D0 (en) | 1988-01-26 |
| DE3874163T2 (en) | 1993-04-08 |
| DK36388A (en) | 1988-07-28 |
| EP0278805B1 (en) | 1992-09-02 |
| ES2034281T3 (en) | 1993-04-01 |
| IE63079B1 (en) | 1995-03-22 |
| ATE80131T1 (en) | 1992-09-15 |
| DE3874163D1 (en) | 1992-10-08 |
| IN170684B (en) | 1992-05-02 |
| GR3006386T3 (en) | 1993-06-21 |
| PT86633A (en) | 1988-02-01 |
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