WO1997021628A1 - Process for simultaneously preparing anhydrous aluminum chloride and zinc - Google Patents
Process for simultaneously preparing anhydrous aluminum chloride and zinc Download PDFInfo
- Publication number
- WO1997021628A1 WO1997021628A1 PCT/KR1996/000215 KR9600215W WO9721628A1 WO 1997021628 A1 WO1997021628 A1 WO 1997021628A1 KR 9600215 W KR9600215 W KR 9600215W WO 9721628 A1 WO9721628 A1 WO 9721628A1
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- WO
- WIPO (PCT)
- Prior art keywords
- aluminum
- zinc
- chloride
- aluminum chloride
- reactor
- Prior art date
Links
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 110
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 40
- 239000011701 zinc Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 33
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 84
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000011592 zinc chloride Substances 0.000 claims abstract description 43
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 42
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 22
- 239000002184 metal Substances 0.000 claims abstract description 22
- 238000007670 refining Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 239000008187 granular material Substances 0.000 claims abstract 4
- 238000007599 discharging Methods 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000010923 batch production Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910000611 Zinc aluminium Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910001297 Zn alloy Inorganic materials 0.000 description 2
- 229910001570 bauxite Inorganic materials 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 230000007096 poisonous effect Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 238000005727 Friedel-Crafts reaction Methods 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000011365 complex material Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004687 hexahydrates Chemical class 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- the present invention relates to a process for simultaneously preparing anhydrous aluminum chloride and zinc. More particularly, the present invention relates to a process for preparing anhydrous aluminum chloride which comprise mixing zinc chloride with aluminum metal at an equivalent ratio, and recovering the anhydrous aluminum chloride by cooling and condensing the vaporous aluminum chloride which is sublimated at a temperature of 183 ° C when to heat the said mixture; and simultaneously separating and recovering zinc, which is melted at a temperature of 420 ° C, by the difference of gravity.
- Anhydrous aluminum chloride has been used as a catalyst for cracking process of petroleum, Friedel-Craft Reaction, etc., and the hexa hydrate has been used for refining wool, an antiseptic for wood, an additive for dye, petroleum refining process, paper manufacturing, paint, pigments, printing ink, etc.; and zinc metal is used at a large amount for steel plating, pipe plating, die-casting, copper-alloy, etc.
- anhydrous aluminum chloride Conventionally, the various methods of production of anhydrous aluminum chloride have been known, and the methods thereof are classified generally as follows, for example, a method which reacting aluminum metal with chlorine at a high temperature; a method which reacting aluminum metal with hydrochloride gas at a high temperature; a method which reacting alumina or alumina-containing substance such as bauxite with carbon monoxide and chlorine or phosgene; a method thereof by reacting alumina or alumina- containing substance with chlorine under the present of carbon, etc.
- anhydrous aluminum chloride which comprises by reacting aluminum metal with chlorine or hydrochloride gas at a high temperature
- the said method comprises blowing chlorine gas into the melted aluminum and cooling the sublimated aluminum chloride to obtain it in a powder shape or massive state.
- it is necessary to melt alumina in the presence of a flux thereof around 960 °C or more, and subsequently subject to electrolysis it, thereby causing the method to be required much higher cost.
- Patent Publication No. 7640/1976 Japanese Patent Publication No. 27838/1975, Japanese Patent Publication No. 5526/1984, etc.).
- zinc metal has been conventionally prepared by dry preparation method and wet preparation method.
- the present inventors have undertaken earnest studies in order to solve the above problems in the prior art, and as a result, have found that aluminum chloride and zinc can be easily obtained by reacting zinc chloride with aluminum , which led to the completion ofthe invention.
- an object ofthe present invention is to provide a novel method of preparation of aluminum chloride and zinc simultaneously.
- Figure 1 is a front view of an apparatus for simultaneously preparing aluminum chloride and zinc in accordance with the present invention.
- Figure 2 is an enlarged front view of a shelf embedded with aluminum granules mounted inside the refining tower ofthe apparatus shown Figure 1.
- Figure 1 is a front view ofthe apparatus for simultaneously preparing aluminum chloride and zinc, which consists ofthe reactor 1. the multi-stage refining tower 6 and the rotating tube 9.
- the reactor is equipped with inlet 3 for introducing the molten zinc chloride, hopper 4 for introducing aluminum powder or aluminum particles, an agitator 2 And the bottom of the reactor 1 has the drain pipe 5 for draining the formed molten zinc metal
- the refining tower has the reticulated shape - shelves 7 embedded with aluminum granules 8
- the vaporous aluminum chloride and zinc chloride generated from the reactor 1 are contacted with aluminum granules on the shelves, thereby the unreacted mist zinc chloride from the reactor reacting with aluminum in this tower
- the obtained aluminum chloride containing a trace amount of zinc chloride from the refining tower is passed the rotating tube 9, wherein aluminum granules are embedded at an amount of about two third (2/3) ofthe volume of the rotating pipe
- Figure 2 is the shelves part 7 of Figure 1
- the present invention provides a method for producing aluminum chloride and zinc which comprises introducing molten anhydrous zinc chloride into the melt - bath (reactor) having an agitator 2, and adding, while agitating, aluminum powder or melted aluminum which is reacted with zinc chloride
- the molten aluminum or aluminum powder is added, while agitating , to a high purity zinc chloride in molten state in the reactor, maintaining the average temperature of 420 to 500 ° C , whereby aluminum chloride being sublimated at 183 °C or more, and then the sublimated aluminum chloride is subjected to be cooled and desublimated to produce aluminum chloride in power or flake shape (crystal or prismatic state).
- zinc metal is settled down on the bottom ofthe zinc chloride melt in the reactor by the difference of specific gravity and the resulted zinc metal is drained through drain pipe to a mold and then solidified to give a desired product.
- the high-value zinc metal and aluminum chloride can be obtained by reaction of zinc chloride and the molten aluminum metal, especially zinc metal is obtained at the rate of 3.6 times in weight with regard to an amount of aluminum metal being reacted. Accordingly, the present invention is a useful melt- metathesis reaction economically to obtain aluminum chloride and zinc metal
- the reaction is preferably carried out in the aforementioned temperature range. It is not proper to carry out the reaction more than 740 ° C , since zinc chloride is vaporized at the said temperature to contaminate the sublimated aluminum chloride, and also below 420 ° C which is fusing temperature of zinc, it is difficult to obtain zinc continuously.
- the reaction temperature is preferably 420 to 500 ° C , more preferably 450 to 480 °C .
- the purity of zinc metal and aluminum chloride depend on the purity ofthe raw material, zinc chloride and aluminum. Especially, when pure zinc chloride containing not more than 100 ppm of iron, nickel, cadmium, etc., or refined zinc chloride being eliminated the above metal components is used, the zinc is produced with high purity, i.e. 99% to 99.8% purity.
- the pure aluminum chloride being sublimated is subjected to be guided to a multi-stage contact refining tower 6, in which vaporized zinc chloride being accompanied, maintaining vapor temperature of 185 to 80 ° C , is mostly converted to zinc and aluminum chloride by contact with aluminum granules or particles, and then in the next step, vaporous aluminum chloride is passed through the rotating tube 9 being embedded with aluminum particles (5 to 10 mm thick) to react zinc chloride being present at a trace amount, thereby zinc chloride being eliminated as being converted to zinc metal, and then gaseous aluminum chloride with high purity is cooled to give as powder or prismatic shape
- the molten liquid consisted of 95% of zinc chloride, 2% of iron, 1% of lead and 2% of zinc oxide, and 26.4 g of aluminum powder were added, and then the reactor was heated at an average temperature of 480 ° C for 50 minutes to obtain 97.4 g of metal consisted of 98.5% of zinc metal, 1% of iron, and 0.5% lead.
- the vaporous zinc chloride being contaminated with vaporous aluminum chloride simultaneously is reacted with aluminum granules or particles and subsequently, zinc chloride is converted to zinc powder, which is settled down on the reactor, thereby pure aluminum chloride can be obtained.
- the refined zinc chloride being used leads to a production ofthe pure zinc metal. Since aluminum metal is easily become an alloy with zinc metal, it is preferable to feed aluminum power to become an equivalent amount to the molten zinc chloride, which is present as a little excess, in the reactor, in order to avoid formation of alloy. And such a product can be obtained without any further refining process
- a process for simultaneously preparing anhydrous aluminum chloride and zinc according to the present invention provides an industrially useful and economical one for obtaining the pure final product without further refining process
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention discloses a process for simultaneously preparing zinc metal and aluminum chloride, which comprises reacting melted zinc chloride with aluminum in powder, granule or molten liquid thereof shape at an elevated temperature in the reactor while agitating, contacting the generated vaporous aluminum chloride containing zinc chloride with aluminum in a refining tower embedded with aluminum granules, and desublimating the resulting gaseous aluminum chloride; and discharging zinc metal from the bottom of the reactor, and if necessary, the resulting produced aluminum chloride gas is additionally passed to the rotating pipe embedded with aluminum granule in order to obtain the high purity aluminum chloride.
Description
DESCRIPTION
PROCESS FOR SIMULTANEOUSLY PREPARING ANHYDROUS ALUMINUM
CHLORIDE AND ZINC
BACKGROUND OF THE INVENTION
FIELD OF THE INVENTION
The present invention relates to a process for simultaneously preparing anhydrous aluminum chloride and zinc. More particularly, the present invention relates to a process for preparing anhydrous aluminum chloride which comprise mixing zinc chloride with aluminum metal at an equivalent ratio, and recovering the anhydrous aluminum chloride by cooling and condensing the vaporous aluminum chloride which is sublimated at a temperature of 183°C when to heat the said mixture; and simultaneously separating and recovering zinc, which is melted at a temperature of 420°C, by the difference of gravity.
DESCRIPTION OF THE PRIOR ART
Anhydrous aluminum chloride has been used as a catalyst for cracking process of petroleum, Friedel-Craft Reaction, etc., and the hexa hydrate has been used for refining wool, an antiseptic for wood, an additive for dye, petroleum refining process, paper manufacturing, paint, pigments, printing ink, etc.; and zinc metal is used at a large amount for steel plating, pipe plating, die-casting, copper-alloy, etc.
Conventionally, the various methods of production of anhydrous aluminum chloride have been known, and the methods thereof are classified generally as follows, for example, a method which reacting aluminum metal with chlorine at a high temperature; a method which reacting aluminum metal with hydrochloride gas at a high temperature; a method which reacting alumina or alumina-containing substance such as bauxite with carbon monoxide and chlorine or phosgene; a method thereof by reacting alumina or alumina-
containing substance with chlorine under the present of carbon, etc.
Among the above methods, a method of production of anhydrous aluminum chloride, which comprises by reacting aluminum metal with chlorine or hydrochloride gas at a high temperature is generally employed in the industrial scale, and more specifically, the said method comprises blowing chlorine gas into the melted aluminum and cooling the sublimated aluminum chloride to obtain it in a powder shape or massive state. However, in order to obtain the raw aluminum metal, it is necessary to melt alumina in the presence of a flux thereof around 960 °C or more, and subsequently subject to electrolysis it, thereby causing the method to be required much higher cost. In order to remove the said defect, many methods have been proposed, for example, a process for preparing anhydrous aluminum chloride which comprises by reacting alumina with chlorinating agent in the salt- melted bath containing alkali metal or alkali earth metal halide at the presence of reducing agent such as carbon (Japanese Patent Publication No. 293/1989), a process therefor which comprises by reacting oxide of aluminum with chlorinated hydrocarbon without a catalyst at a high temperature (Japanese Patent Publication No. 54286/1988); a process therefor which comprises sintering the mixture of raw material composed of aluminum- containing fine particle, carbon-containing fine particle and binder, and chlorinating the resulted sintered mixture by utilizing gaseous oxygen-containing chlorine (Japanese Patent Publication No. 1655/1990); and also a process for enhancing the purity of obtained aluminum chloride (Japanese Patent Publication No. 38287/1978, Japanese
Patent Publication No. 7640/1976, Japanese Patent Publication No. 27838/1975, Japanese Patent Publication No. 5526/1984, etc.).
The above methods have drawbacks that uses the expensive raw material, or occurs simultaneously carbon monoxide and carbon dioxide gas in the course of preparing anhydrous aluminum chloride when reacting aluminum oxide (bauxite) with reducing agent, carbon at the high temperature, and these methods require the step of cooling the gaseous complex material and also step of refining aluminum chloride in order to obtain
high purity aluminum chloride.
And, zinc metal has been conventionally prepared by dry preparation method and wet preparation method.
Accordingly, development ofthe improved method of preparation of aluminum chloride with high purity and low cost, being as solved the above defects, has been desired.
The present inventors have undertaken earnest studies in order to solve the above problems in the prior art, and as a result, have found that aluminum chloride and zinc can be easily obtained by reacting zinc chloride with aluminum , which led to the completion ofthe invention.
SUMMARY OF THE INVENTION
Accordingly, an object ofthe present invention is to provide a novel method of preparation of aluminum chloride and zinc simultaneously.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 is a front view of an apparatus for simultaneously preparing aluminum chloride and zinc in accordance with the present invention.
Figure 2 is an enlarged front view of a shelf embedded with aluminum granules mounted inside the refining tower ofthe apparatus shown Figure 1.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In the detailed description of preferred embodiments, the same numerals will be utilized to designate the same parts in the respective views. Figure 1 is a front view ofthe apparatus for simultaneously preparing aluminum chloride and zinc, which consists ofthe reactor 1. the multi-stage refining tower 6 and the rotating tube 9.
The reactor is equipped with inlet 3 for introducing the molten zinc chloride, hopper 4 for introducing aluminum powder or aluminum particles, an agitator 2 And the bottom of the reactor 1 has the drain pipe 5 for draining the formed molten zinc metal
The refining tower has the reticulated shape - shelves 7 embedded with aluminum granules 8 The vaporous aluminum chloride and zinc chloride generated from the reactor 1 are contacted with aluminum granules on the shelves, thereby the unreacted mist zinc chloride from the reactor reacting with aluminum in this tower
The obtained aluminum chloride containing a trace amount of zinc chloride from the refining tower is passed the rotating tube 9, wherein aluminum granules are embedded at an amount of about two third (2/3) ofthe volume of the rotating pipe
Figure 2 is the shelves part 7 of Figure 1
The above apparatus are provided herein for purposes of illustration only and are not intended to be limiting the present invention
The present invention provides a method for producing aluminum chloride and zinc which comprises introducing molten anhydrous zinc chloride into the melt - bath (reactor) having an agitator 2, and adding, while agitating, aluminum powder or melted aluminum which is reacted with zinc chloride
The chemical formula ofthe present invention can be shown as follows.
3ZnCl2 + 2A1 → 3Zn + 2A1CU
To explain it more specifically, the molten aluminum or aluminum powder is added, while agitating , to a high purity zinc chloride in molten state in the reactor, maintaining the average temperature of 420 to 500 °C , whereby aluminum chloride being sublimated at 183 °C or more, and then the sublimated aluminum chloride is subjected to be cooled and desublimated to produce aluminum chloride in power or flake shape (crystal or prismatic
state).
And also, zinc metal is settled down on the bottom ofthe zinc chloride melt in the reactor by the difference of specific gravity and the resulted zinc metal is drained through drain pipe to a mold and then solidified to give a desired product.
According to the present invention, the high-value zinc metal and aluminum chloride can be obtained by reaction of zinc chloride and the molten aluminum metal, especially zinc metal is obtained at the rate of 3.6 times in weight with regard to an amount of aluminum metal being reacted. Accordingly, the present invention is a useful melt- metathesis reaction economically to obtain aluminum chloride and zinc metal
The reaction is preferably carried out in the aforementioned temperature range. It is not proper to carry out the reaction more than 740 °C , since zinc chloride is vaporized at the said temperature to contaminate the sublimated aluminum chloride, and also below 420 °C which is fusing temperature of zinc, it is difficult to obtain zinc continuously. In view of such property of the reaction material and resulting material, the reaction temperature is preferably 420 to 500 °C , more preferably 450 to 480 °C .
The purity of zinc metal and aluminum chloride depend on the purity ofthe raw material, zinc chloride and aluminum. Especially, when pure zinc chloride containing not more than 100 ppm of iron, nickel, cadmium, etc., or refined zinc chloride being eliminated the above metal components is used, the zinc is produced with high purity, i.e. 99% to 99.8% purity.
And, the pure aluminum chloride being sublimated is subjected to be guided to a multi-stage contact refining tower 6, in which vaporized zinc chloride being accompanied, maintaining vapor temperature of 185 to 80 °C , is mostly converted to zinc and aluminum chloride by contact with aluminum granules or particles, and then in the next step, vaporous aluminum chloride is passed through the rotating tube 9 being embedded
with aluminum particles (5 to 10 mm thick) to react zinc chloride being present at a trace amount, thereby zinc chloride being eliminated as being converted to zinc metal, and then gaseous aluminum chloride with high purity is cooled to give as powder or prismatic shape
It is possible to accomplish the present invention by the batch process, but it is very difficult to control the reaction rate of zinc chloride and aluminum of reactant by the batch process And therefore, it is preferable to carry out the present invention by a continuous process That is to say, molten zinc chloride and molten aluminum metal are continuous fed to the reactor during the process ofthe reaction, thereby the productivity of zinc being obtained more than 10 to 100 ton per day from one reactor(diameter 4 m, height 3 m) having a refining tower and the rotating pipe (diameter 1 2 m, length 2 m)
In the conventional methods, poisonous chlorine or hydrochloride gas has been used for obtaining aluminum chloride, but in the present invention, such poisonous gas is not used, and moreover zinc scrap, etc is reacted with hydrochloric acid to form the pure zinc chloride and the resulted zinc chloride is reacted with aluminum powder or molten aluminum which is obtained from aluminum metal or aluminum scrap, at a melt state to produce aluminum chloride and zinc metal with high purity Such a method is very economical, since the present process is proceeded to be completed at a relatively low temperature, compared to the conventional methods
EXAMPLES
More detail descriptions are explained by the following examples In the examples, "%" means % by weight
Example 1
To the Erlenmeyer flask having the condenser, 200 g of purified zinc chloride and
average temperature of 480 °C for 40 minutes to collect 130 g (yield: 99.65%) ofthe pure aluminum chloride at the condenser and also to obtain 92.16 g(96.07%) of zinc metal from the bottom ofthe flask. In this reaction, what the yield of zinc was 96.07% means the loss due to unreaction and un-progress ofthe reactant by the batch process.
Example 2
To the Erlenmeyer flask having the condenser, 210.5 g ofthe molten liquid consisted of 95% of zinc chloride, 2% of iron, 1% of lead and 2% of zinc oxide, and 26.4 g of aluminum powder were added, and then the reactor was heated at an average temperature of 480 °C for 50 minutes to obtain 97.4 g of metal consisted of 98.5% of zinc metal, 1% of iron, and 0.5% lead.
From the above, it is proved that impurities such as chlorides of iron, cadmium, lead, etc. in the molten liquid of zinc chloride are reduced simultaneously to form alloy of zinc, thereby such impurities causing to lower the purity of product. And therefore, it is necessary to purify the raw material, zinc chloride before being introduced to the reactor, in order to obtain the high pure product.
Example 3
To the Erlenmeyer flask having the condenser, 200 g of purified zinc chloride and 27.2 g of aluminum scrap (purity : 97%) which was obtained from aluminum can were added, and then the flask was heated at an average temperature of 480 °C for 40 minutes to complete the reaction, and as a result, 128.7 g of zinc metal being consisted of 97.5% Zn, 0.5% Fe, and 1% Si, and 93 g of aluminum chloride.
Example 4
To the Erlenmeyer flask of 500 mi, 200 g of zinc chloride and 26.4 g of aluminum powder were added, while heating 480 °C and as a result of analysis of vaporous
aluminum chloride being produced, about below 3% zinc chloride was contaminated therein. In order to eliminate zinc chloride in the vaporous aluminum chloride, the resulting vaporous aluminum chloride was passed through the pipe (diameter 30 mm, length lm) embedded with aluminum granules (diameter 5 to 10 mm) at an amount of two third(2/3) volume ofthe pipe, maintaining the average temperature of 380 °C, and then passed vaporous aluminum chloride was subjected to be cooled to give 130.44 g of crystal aluminum chloride. As a result of analysis of obtained aluminum chloride, the purity thereof was 99.1% and the contained zinc chloride therein was 0.02%.
Example 5
To the Erlenmeyer flask of 500 m , 200 g of zinc chloride and 40 g of aluminum powder were added, and the flask was heated until the reaction is completed to give zinc which is alloyed with a relatively large amount of aluminum. The resulted aluminum alloy was added to pure molten zinc chloride in order to react aluminum in the alloy continuously, thereby obtaining pure zinc (99.3%).
From this experiment, it is proved that when aluminum and zinc alloy are also reacted with zinc chloride at the sufficient reaction temperature, aluminum in the alloy is selectively reacted.
As apparent in the above examples, the vaporous zinc chloride being contaminated with vaporous aluminum chloride simultaneously is reacted with aluminum granules or particles and subsequently, zinc chloride is converted to zinc powder, which is settled down on the reactor, thereby pure aluminum chloride can be obtained.
And also, the refined zinc chloride being used leads to a production ofthe pure zinc metal. Since aluminum metal is easily become an alloy with zinc metal, it is preferable to feed aluminum power to become an equivalent amount to the molten zinc chloride, which is present as a little excess, in the reactor, in order to avoid formation of alloy. And such a
product can be obtained without any further refining process
INDUSTRIAL APPLICABILITY
A process for simultaneously preparing anhydrous aluminum chloride and zinc according to the present invention provides an industrially useful and economical one for obtaining the pure final product without further refining process
Claims
10
1 A process for simultaneously preparing zinc metal and aluminum chloride, which comprises reacting melted zinc chloride with aluminum in powder, granule or molten liquid thereof shape at an elevated temperature in the reactor while agitating, contacting the generated vaporous aluminum chloride containing zinc chloride with aluminum in a refining tower embedded with aluminum granules, and desublimating the resulted gaseous aluminum chloride, and discharging zinc metal from the bottom ofthe reactor
2 A process according to claim 1 , wherein the said elevated temperature is the range of 420 to 500 °C
3 A process according to claim 1, wherein the produced aluminum chloride gas is passed to the rotating pipe embedded with aluminum granule, and desublimated
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1019950048797A KR0161098B1 (en) | 1995-12-12 | 1995-12-12 | Simultaneous preparation of anhydrous aluminum chloride and zinc |
KR1995/48797 | 1995-12-12 |
Publications (1)
Publication Number | Publication Date |
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WO1997021628A1 true WO1997021628A1 (en) | 1997-06-19 |
Family
ID=19439323
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/KR1996/000215 WO1997021628A1 (en) | 1995-12-12 | 1996-11-25 | Process for simultaneously preparing anhydrous aluminum chloride and zinc |
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KR (1) | KR0161098B1 (en) |
WO (1) | WO1997021628A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106277036A (en) * | 2015-05-21 | 2017-01-04 | 华仁药业股份有限公司 | Anhydrous organic solvent method prepares the preparation method of zinc chloride |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20010087955A (en) * | 2000-03-09 | 2001-09-26 | 김수태 | Process for simultaneously preparing anhydrous aluminum chloride and iron powder |
KR101219184B1 (en) * | 2010-10-18 | 2013-01-07 | 한국기계연구원 | The method for preparation of Alumium Chloride and Alumium Chloride using the same |
KR101404762B1 (en) * | 2013-06-24 | 2014-06-12 | 김수태 | Process for preparing aluminum chloride and zinc in high purity at the same time |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1467268A1 (en) * | 1964-10-06 | 1969-03-13 | Imp Smelting Corp N S C | Process for producing aluminum chloride |
GB1185234A (en) * | 1967-10-13 | 1970-03-25 | Imp Smelting Corp Ltd | Production of High-Purity Aluminium Chloride |
FR2277038A1 (en) * | 1974-07-05 | 1976-01-30 | Esb Inc | Purified aluminium chloride - alkali chloride melt - for battery electrolytes, has improved coulombic yield |
FR2449059A1 (en) * | 1979-02-16 | 1980-09-12 | Alusuisse | PLANT FOR PRODUCING SOLID ALUMINUM CHLORIDE |
-
1995
- 1995-12-12 KR KR1019950048797A patent/KR0161098B1/en not_active IP Right Cessation
-
1996
- 1996-11-25 WO PCT/KR1996/000215 patent/WO1997021628A1/en active Application Filing
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1467268A1 (en) * | 1964-10-06 | 1969-03-13 | Imp Smelting Corp N S C | Process for producing aluminum chloride |
GB1185234A (en) * | 1967-10-13 | 1970-03-25 | Imp Smelting Corp Ltd | Production of High-Purity Aluminium Chloride |
FR2277038A1 (en) * | 1974-07-05 | 1976-01-30 | Esb Inc | Purified aluminium chloride - alkali chloride melt - for battery electrolytes, has improved coulombic yield |
FR2449059A1 (en) * | 1979-02-16 | 1980-09-12 | Alusuisse | PLANT FOR PRODUCING SOLID ALUMINUM CHLORIDE |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106277036A (en) * | 2015-05-21 | 2017-01-04 | 华仁药业股份有限公司 | Anhydrous organic solvent method prepares the preparation method of zinc chloride |
Also Published As
Publication number | Publication date |
---|---|
KR0161098B1 (en) | 1998-11-16 |
KR970042265A (en) | 1997-07-24 |
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