WO2006107020A1 - 高純度無水塩化アルミニウム及びその製造方法 - Google Patents
高純度無水塩化アルミニウム及びその製造方法 Download PDFInfo
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- WO2006107020A1 WO2006107020A1 PCT/JP2006/307048 JP2006307048W WO2006107020A1 WO 2006107020 A1 WO2006107020 A1 WO 2006107020A1 JP 2006307048 W JP2006307048 W JP 2006307048W WO 2006107020 A1 WO2006107020 A1 WO 2006107020A1
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- aluminum
- anhydrous
- salt
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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
-
- 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
- This invention is a highly pure anhydrous aluminum chloride which is made of industrially produced crude anhydrous salty aluminum and has an extremely low purity by reducing impurity components (impurity metals) as much as possible. -Um and its manufacturing method. Background art
- Anhydrous aluminum salt is generally used as a Lewis acid catalyst for petroleum refining and many organic synthesis.
- ALE Electro Layer Epitaxial
- EL electroluminescence
- This anhydrous salted aluminum is industrially manufactured by blowing chlorine gas into a molten metal aluminum and solidifying the vaporized salted aluminum vapor generated by reaction in a condenser. .
- Anhydrous salted aluminum produced industrially in this way is derived from, for example, metallic aluminum used as a raw material or equipment used as a manufacturing apparatus, such as salty ferric iron (FeCl ) And other metal chlorine compounds are inevitably mixed in as impurities, and the product turns yellow
- Japanese Patent Laid-Open No. 9-301,714 discloses the temperature of the molten metal aluminum in the reactor.
- a method for producing high-purity anhydrous salty-aluminum by introducing purified chlorine gas with a carbon dioxide content reduced as much as possible into the molten metal aluminum while maintaining the predetermined range is described. .
- Japanese Patent Application Laid-Open No. 2002-12993 discloses that a mixed molten salt bath containing 72.8 wt% of aluminum chloride and 7% by weight of aluminum chloride is used to form metallic aluminum and sodium chloride. It has been proposed to produce anhydrous salt and aluminum by electrochemical reaction with chlorine gas.
- Japanese Patent Laid-Open No. 6-1,607 discloses that a mixed molten salt layer composed of salty aluminum and salty sodium is formed on the surface of a molten metal aluminum so that the metal aluminum and chlorine gas are mixed. It has been proposed that anhydrous aluminum chloride vapor produced by the reaction is brought into contact with the mixed molten salt layer and washed to produce high-purity anhydrous salt-aluminum.
- the temperature of the molten metal aluminum requires a reaction temperature of 660 ° C or higher, and a mixed molten salt layer is formed on the surface of the molten metal.
- JP-A-6-263,438 discloses a high-purity anhydrous salt-aluminum having a low temperature of 120 ° C using a mixed molten salt bath of salt-aluminum and onium salt salt. A method of manufacturing is proposed.
- Japanese Patent Application Laid-Open No. 55-158,121 discloses titanium tetrachloride (TiCl), tetrasalt silicate (SiCl), ferric chloride (FeCl), etc. by fractional distillation using a distillation column.
- Metal chlorinated compounds TiCl, tetrasalt silicate (SiCl), ferric chloride (FeCl), etc. by fractional distillation using a distillation column.
- the composition must be 90% by weight or more of aluminum chloride and the liquid temperature must be 191 ° C or more.
- this state cannot be realized in an open system, and the purification apparatus is limited to a closed system. Therefore, this method is industrially adopted because it is difficult in the laboratory but difficult to mass-produce. Is not appropriate.
- Patent Document 1 Japanese Patent Laid-Open No. 9-301,417
- Patent Document 2 JP 2002-12993 A
- Patent Document 3 Japanese Patent Laid-Open No. 6-1,607
- Patent Document 4 JP-A-6-263,438
- Patent Document 5 Japanese Patent Laid-Open No. 55-158, 121
- Non-Patent Document 1 Agne Technology Center Co., Ltd. Issued on August 10, 1993 "Mixed Salts' Fundamentals of Thermal Technology” pp. 268-269
- the present inventor has sought to produce highly pure anhydrous aluminum chloride having an extremely high purity by separating and removing impurity components (impurity metals) mixed in anhydrous salt and aluminum as much as possible.
- impurity metals impurity metals
- a mixed molten salt bath of aluminum chloride and sodium chloride Is used to control the generation conditions of anhydrous aluminum chloride vapor and the condensation conditions of the generated anhydrous aluminum chloride vapor, thereby producing gallium (Ga) derived from the aluminum raw material used in industrial production of anhydrous aluminum chloride.
- the purity of the anhydrous salt ⁇ ⁇ aluminum obtained by refining the content of the main impurity components excluding to 1 ppm or less and subtracting the total of the impurity components to 99.99 wt% or more easily industrially, if necessary 99. 9 It was found that the content could be 99 wt% or more, and the present invention was completed.
- gallium (Ga) belongs to the same group of elements of the periodic table as aluminum (A1), and is an amphoteric metal that is soluble in both acid and alkali like aluminum, and its chemical property is aluminum.
- this gallium can enter the same lattice as aluminum, so it is judged that there is no influence as an impurity in most applications. In the present invention, it was decided that it would be sufficient to maintain the purity of anhydrous salt-aluminum without determining the individual allowable content.
- the object of the present invention is to provide the main impurity components (impurity metals) derived from aluminum raw materials used in the production of industrial anhydrous salt and aluminum, namely sodium (Na), potassium (K). , Lithium (Li), magnesium (Mg), silicon (Si), calcium (Ca), beryllium (Be), titanium (Ti), vanadium (V), chromium (Cr), scandium (Sc), manganese (Mn ), Iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), zinc (Zn), gallium (Ga) and germanium (Ge)
- the content of major impurity components excluding gallium (Ga) is less than lppm, and the purity of anhydrous aluminum chloride obtained by subtracting the total of impurity components is 99.99% by weight
- An object of the present invention is to provide a high-purity anhydrous salt-aluminum as described above.
- Another object of the present invention is anhydrous salt-aluminum in which main impurity components derived from an aluminum raw material used in the production of industrial anhydrous salt-aluminum are reduced as much as possible.
- the purity of anhydrous salt-aluminum obtained by subtracting the total of impurity components is 999% by weight or more, and all the main impurity components except gallium (Ga) are substantially below the detection limit. It is to provide a salty aluminum.
- Another object of the present invention is to provide a method for producing high-purity anhydrous salt-aluminum that can easily produce such high-purity anhydrous salt-aluminum industrially. It is in.
- the present invention relates to anhydrous salt aluminum in which main impurity components (impurity metals) derived from aluminum raw materials used in the production of industrial anhydrous salt aluminum are reduced as much as possible.
- the content of major impurity components excluding gallium (Ga) is 1 ppm or less, and the purity of anhydrous sodium chloride obtained by subtracting the total of impurity components is 99.99% by weight or more.
- the high purity anhydrous salty aluminum characterized in that the purity of the anhydrous salty aluminum obtained by subtracting the total of the impurity components is 99.999% by weight or more.
- the present invention provides a temperature controllable sublimation furnace for sublimating an anhydrous salt-aluminum vapor and a molten salt bath power of salt-aluminum and salt-sodium and an anhydrous salt connected to the sublimation furnace.
- a temperature controllable sublimation furnace for sublimating an anhydrous salt-aluminum vapor and a molten salt bath power of salt-aluminum and salt-sodium and an anhydrous salt connected to the sublimation furnace.
- the ambient temperature of the condenser is controlled to 160 ° C or higher, and the bath temperature of the mixed molten salt bath is 170 to 185 ° C.
- the atmospheric temperature of the condenser is controlled to 40 to 80 ° C, and purified anhydrous aluminum chloride is recovered in the condenser, and the mixed molten salt bath with a bath temperature exceeding 185 ° C is left as the residue in the sublimation furnace.
- High purity anhydrous chloride Miniu is a non-manufacturing method of.
- the chlorine compound of the impurity metal has a boiling point lower than that of anhydrous salt-aluminum, such as salt-cathenium, salt-titanium, vanadium chloride, etc.
- anhydrous salt-aluminum such as salt-cathenium, salt-titanium, vanadium chloride, etc.
- the high boiling point metal chlorine compound include salt sodium, magnesium chloride, salt calcium, salt ferric iron and the like.
- purity of anhydrous salt-aluminum obtained by subtracting the sum of impurity components means an impurity component that can be detected by an analysis method usually provided It means that everything except the (impurity metal) concentration is regarded as pure! This means that the purity of this anhydrous aluminum chloride is 99.99% by weight or more, preferably 99.999% by weight or more.
- the weight composition ratio of aluminum chloride in the mixed molten salt bath is 90 wt% or more and 98 wt% or less, preferably 93 wt% or more and 97 wt% or less.
- the bath temperature of the mixed molten salt bath is less than 170 ° C, preferably less than 175 ° C
- the ambient temperature of the condenser is 160 ° C or higher, preferably 1 70 ° C or higher and 175 ° C.
- the condenser ambient temperature is 40 ° C or higher and 80 ° C or lower.
- purified anhydrous sodium chloride aluminum is recovered in a condenser by controlling to 50 ° C or higher and 70 ° C or lower, and sublimation is performed using a mixed molten salt bath having a bath temperature of 185 ° C, preferably 183 ° C, as the residue. It must be left in the furnace.
- the temperature of the condenser when the temperature of the condenser is lower than 160 ° C when the bath temperature is lower than 170 ° C, impurity components having a boiling point lower than that of aluminum chloride such as salty titanium and salty vanadium are contained in the purified anhydrous salty aluminum. If the ambient temperature of the condenser is lower than 40 ° C when the bath temperature is 170 to 185 ° C, the purified anhydrous aluminum chloride becomes powdery and bulky. As a result, the volume production efficiency of the condenser is increased. It falls and is no longer suitable for industrial production.
- the condenser ambient temperature at a bath temperature of 170 to 185 ° C exceeds 80 ° C, the purified anhydrous salt-aluminum becomes hard and takes time to recover the vessel power, and the condensation efficiency (Recovery rate) decreases significantly. Furthermore, sublimation of anhydrous salt-aluminum stops when the bath temperature when recovering purified anhydrous aluminum chloride in the condenser is lower than 170 ° C, and anhydrous salt-aluminum when higher than 185 ° C. The problem arises that the impurities with higher boiling points increase.
- a salt having a vapor pressure close to that of aluminum chloride is preferably obtained by adding a metal reducing agent such as metal aluminum or metal magnesium, preferably metal aluminum, into the mixed molten salt bath.
- a metal reducing agent such as metal aluminum or metal magnesium, preferably metal aluminum
- Metallic aluminum used as a metal reducing agent Is charged into a sublimation furnace having a purity of 99% by weight or more, preferably 99.9% by weight or more, and having a powdery, thin-film, or thin-plate shape, preferably a powdery shape. It is usually in the range of 1 to 3% by weight, preferably 1.5 to 2.5% by weight, based on the aluminum chloride.
- salt-aluminum is newly supplied to the residue of the unmixed molten salt remaining in the sublimation furnace, and repeatedly purified anhydrous salt-aluminum is recovered.
- unmixed molten salt remaining in the sublimation furnace repeatedly in this way, the recovery rate of anhydrous salt-aluminum with respect to salt-sodium and metal reducing agent is increased and the basic unit is improved! There is.
- the high-purity anhydrous salt-aluminum of the present invention is a major impurity component derived from an aluminum raw material used in the production of industrial anhydrous salt-aluminum, namely sodium (Na), potassium (K), lithium ( Li), magnesium (Mg), silicon (Si), calcium (Ca), beryllium (Be), titanium (Ti), vanadium (V), chromium (Cr), scandium (Sc), manganese (Mn), Anhydrous salt aluminum that has reduced iron (Fe), cobalt (Co), nickel (Ni), copper (Cu), zinc (Zn), gallium (Ga) and germanium (Ge) as much as possible.
- the purity of anhydrous aluminum chloride obtained by subtracting the total of impurity components is 99.99% by weight or more, and the content of major impurity components excluding gallium (Ga) is 1ppm or less.
- the total of impurity components Anhydrous salt obtained by subtracting the purity of aluminum is 99.999% by weight or more.
- FIG. 1 is an explanatory diagram for explaining a sublimation purification apparatus to which a method for producing high purity anhydrous aluminum chloride of the present invention is applied.
- the sublimation purification apparatus used in the following examples and comparative examples includes a sublimation furnace 1 that has a heating device la and can be controlled in temperature, and a thermal insulation treatment in the sublimation furnace 1.
- the condenser 2 is connected to the heat pipe 3 and has a heating / cooling device 2a and the temperature can be controlled.
- the condenser 2 traps low-boiling impurity components (not shown).
- the apparatus is provided with a pipe 4 that guides this low-boiling impurity component.
- the sublimation furnace 1 was charged with 622 g (96.1 wt%) of crude anhydrous aluminum chloride with a purity of 99 wt% and 25 g (3.9 wt%) of sodium chloride with a purity of 99 wt%.
- a mixed molten salt bath (salt-aluminum weight composition ratio 96. lwt%) was prepared by melting aluminum and salt sodium.
- the heating device la is set to 195 ° C. Set the bath temperature to rise, observe the rise in bath temperature, further set the heating device la to 225 ° C and raise the bath temperature, and when this bath temperature exceeds 183 ° C, the heating device Heating with la was stopped.
- the atmospheric temperature of the condenser 2 is controlled to 160 ° C by the heating and cooling device 2a, and the bath temperature is 170 ° C.
- the temperature of the condenser 2 was controlled to 50 ° C. by the heating / cooling device 2a until reaching 183 ° C. from the time when it reached ° C.
- nitrogen gas was introduced from pipe 4 and the exhaust gas was guided to an abatement device (not shown) by an aspirator.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in this way is 185 g, its powder shape is toothpick, and the impurity component (impurity metal) concentration is shown in Table 1. It was as shown in.
- the recovery time of purified anhydrous sodium chloride aluminum was 1 hour.
- Example 2 200 g of the same crude anhydrous aluminum chloride as in Example 1 was charged into the residual molten molten salt remaining in the sublimation furnace 1 in Example 1 above, and the mixed aluminum salt weight composition ratio was 96.2% by weight. In the same manner as in Example 1 above, crude anhydrous sodium chloride was purified.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in Example 2 was 180 g, the powder shape was toothpick, and the impurity component (impurity metal) concentration was As shown in 1.
- the recovery time of purified anhydrous sodium chloride aluminum was 1 hour.
- sublimation furnace 1 was charged with 630 g (9 6.5 wt%) of the same crude anhydrous salt-aluminum as Example 1 and 23 g (3.5 wt%) of the same salt salt sodium as Example 1. Further, 12 g of a 99.9 wt% metal aluminum sheet (1.9 wt% with respect to anhydrous aluminum chloride) was added to form a mixed molten salt bath, and the heating operation of the sublimation furnace 1 and the condenser as in Example 1 were performed. The heating and cooling operations of 2 were performed, and the crude anhydrous salt-aluminum was purified.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in Example 3 was 190 g, the powder shape was toothpick, and the impurity component (impurity metal) concentration was As shown in 1.
- the recovery time of purified anhydrous sodium chloride aluminum was 1 hour.
- the atmospheric temperature of condenser 2 is controlled to 170 ° C by heating and cooling device 2a, and the bath temperature is adjusted to 175 ° C. From the point of arrival, until the temperature reaches 183 ° C, the atmospheric temperature of the condenser 2 is controlled to 50 ° C by the heating and cooling device 2a. Purification was performed.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in this way is 185 g, its powder shape is toothpick, and the impurity component (impurity metal) concentration is shown in Table 1. It was as shown in.
- the recovery time of purified anhydrous sodium chloride aluminum was 1 hour.
- Example 4 200 g of the same crude water-free aluminum chloride as in Example 4 is charged into the residual molten molten salt remaining in the sublimation furnace 1 in Example 4 above, and the mixed molten salt bath has an aluminum chloride weight composition ratio of 96.2% by weight.
- the crude anhydrous salt-aluminum was purified.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in Example 5 was 180 g, the powder shape was toothpick, and the impurity component (impurity metal) concentration was It was as shown in 1.
- the recovery time of purified anhydrous sodium chloride aluminum was 1 hour.
- sublimation furnace 1 was charged with 630 g (9 6.5 wt%) of the same crude anhydrous salt-aluminum as in Example 1 and 23 g (3.5 wt%) of the same salt as sodium salt as in Example 1. Further, 12 g of 99.9% by weight pure metal aluminum sheet (1.9 wt% with respect to anhydrous aluminum chloride) was added to form a mixed molten salt bath, and the heating operation and condenser of the sublimation furnace 1 as in Example 4 were performed. The heating and cooling operations of No. 2 were performed to purify the crude anhydrous salt-aluminum.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in Example 6 was 190 g, the powder shape was toothpick, and the impurity component (impurity metal) concentration was As shown in 1.
- the recovery time of purified anhydrous sodium chloride aluminum was 1 hour.
- Sublimation furnace 1 was charged with 495 g (94.3 wt%) of the same crude anhydrous salt-aluminum as in Example 1 and 30 g (5.7 wt%) of the same salt-sodium as in Example 1, and further with the same metal aluminum powder as in Example 1. 9 g (1.8 wt% with respect to anhydrous salt-aluminum) was added, and a mixed molten salt bath (salt-aluminum weight composition ratio 94.3 wt%) was prepared in the same manner as in Example 1.
- Example 2 As for the heating operation, the same operation as in Example 1 was performed, and for the condenser 2, the temperature inside the condenser reached normal temperature (20 ° C) by air cooling and increased to 80 ° C, and the crude anhydrous salt solution was heated. ⁇ Aluminum was refined.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in Comparative Example 1 was 55 g, the powder shape was toothpick, and the impurity component (impurity metal) concentration was As shown in 1.
- the recovery time of purified anhydrous sodium chloride aluminum was 1 hour.
- Sublimation furnace 1 was charged with 580 g (95.7 wt%) of the same crude anhydrous salt-aluminum as in Example 1 and 26 g (4.3 wt%) of the same salt-sodium as in Example 1, and mixed molten salt as in Example 1.
- a bath (aluminum chloride weight composition ratio 95.7 wt%) was prepared, and in the same manner as in Example 1, crude anhydrous salt aluminum was prepared. Purification was performed.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in Comparative Example 2 is 165 g, the powder shape is toothpick, and the impurity component (impurity metal) concentration is As shown in 1.
- the recovery time of purified anhydrous sodium chloride aluminum was 1 hour.
- Sublimation furnace 1 was charged with 595 g (95.5 wt%) of the same crude anhydrous salt-aluminum as in Example 1 and 28 g (4.5 wt%) of the same salt-sodium as in Example 1, and further with the same metal aluminum powder as in Example 1. 10 g (1.7 wt% with respect to anhydrous salt-aluminum) was added, and a mixed molten salt bath (salt-aluminum weight composition ratio 95.5 wt%) was prepared in the same manner as in Example 1.
- the crude anhydrous salt film was purified in the same manner as in Example 1 except that the heating with the heating device la was stopped when the temperature exceeded 190 ° C.
- the purified anhydrous salt-aluminum recovered in the condenser 2 in Comparative Example 3 is 250 g, the powder shape is toothpick, and the impurity component (impurity metal) concentration is As shown in 1.
- the recovery time of purified anhydrous salt-aluminum was 1.5 hours.
- the high-purity anhydrous salt-aluminum of the present invention is obtained by reducing as much as possible the impurity components derived from the aluminum raw materials found in the special grade reagents sold and subtracting the total of the impurity components.
- the purity of anhydrous aluminum chloride is 99.99% by weight or higher, preferably 99.999% by weight or higher, so that it can be used for chemical vapor deposition (CV D) and EL devices in the manufacture of fuel cells, semiconductors, ICs, etc. High purity, starting with applications such as Al O insulating film by ALE method etc.
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- Life Sciences & Earth Sciences (AREA)
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- Manufacture And Refinement Of Metals (AREA)
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Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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JP2007511228A JP5125504B2 (ja) | 2005-04-04 | 2006-04-03 | 高純度無水塩化アルミニウムの製造方法 |
US11/887,785 US20090028766A1 (en) | 2005-04-04 | 2006-04-03 | High Purity Anhydrous Aluminium Chloride and Process for Production Thereof |
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JP2005107719 | 2005-04-04 | ||
JP2005-107719 | 2005-04-04 |
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WO2006107020A1 true WO2006107020A1 (ja) | 2006-10-12 |
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US (1) | US20090028766A1 (ja) |
JP (1) | JP5125504B2 (ja) |
CN (1) | CN101155759A (ja) |
TW (1) | TW200702304A (ja) |
WO (1) | WO2006107020A1 (ja) |
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US9368848B2 (en) * | 2011-07-21 | 2016-06-14 | Nippon Soda Ltd., Co. | Aluminum-halogen fuel cell |
CN102557097B (zh) * | 2011-10-20 | 2014-04-16 | 常州亚环环保科技有限公司 | 一种饮用水级聚合氯化铝中铁离子的去除方法 |
CN103365952B (zh) * | 2012-04-06 | 2017-04-12 | 东芝医疗系统株式会社 | 医疗信息检索装置 |
US9449068B2 (en) * | 2012-06-13 | 2016-09-20 | Oracle International Corporation | Information retrieval and navigation using a semantic layer and dynamic objects |
CN103708518B (zh) * | 2012-09-29 | 2015-04-29 | 贵阳铝镁设计研究院有限公司 | 一种无水氯化铝制备方法 |
CN103803621A (zh) * | 2012-11-06 | 2014-05-21 | 贵阳铝镁设计研究院有限公司 | 一种复盐法由结晶氯化铝脱水制备无水氯化铝的方法 |
CN103351012A (zh) * | 2013-06-27 | 2013-10-16 | 中国铝业股份有限公司 | 一种氧化铝粉体的制备方法 |
CN103818942B (zh) * | 2014-01-22 | 2015-03-18 | 中国科学院上海硅酸盐研究所 | 一种高纯无水碘化锶的制备方法 |
CN103942266A (zh) * | 2014-03-27 | 2014-07-23 | 上海巨数信息科技有限公司 | 一种基于olap能自定义复杂业务计算逻辑的数据分析方法 |
CN104402032A (zh) * | 2014-11-17 | 2015-03-11 | 宁夏中远天宇科技有限公司 | 一种新型的无水三氯化铝的生产方法 |
CN107311213A (zh) * | 2017-07-13 | 2017-11-03 | 中国恩菲工程技术有限公司 | 高纯无三水氯化铝的制备方法 |
CN112357885A (zh) * | 2020-12-02 | 2021-02-12 | 中国科学院上海应用物理研究所 | 一种氯化物熔盐中单一组分的提纯方法 |
CN112915575A (zh) * | 2021-01-22 | 2021-06-08 | 华融化学股份有限公司 | 一种三氯化铝的捕集方法 |
US11996281B1 (en) | 2023-06-07 | 2024-05-28 | Applied Materials, Inc. | System and method for introducing aluminum to an ion source |
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JPH061607A (ja) * | 1992-06-22 | 1994-01-11 | Mitsubishi Materials Corp | 高純度塩化アルミニウムの製造方法 |
JPH06263438A (ja) * | 1993-03-09 | 1994-09-20 | Mitsubishi Petrochem Co Ltd | 高純度無水塩化アルミニウムの製造方法 |
JPH09301714A (ja) * | 1996-05-09 | 1997-11-25 | Nippon Light Metal Co Ltd | 高純度無水塩化アルミニウムの製造方法 |
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US3378338A (en) * | 1965-05-27 | 1968-04-16 | Imp Smelting Corp Ltd | Production of high-purity aluminium chloride |
US3694170A (en) * | 1970-03-30 | 1972-09-26 | Nippon Soda Co | Process for production of spherical granules or lumps of anhydrous aluminum chloride |
JPS63112416A (ja) * | 1986-10-31 | 1988-05-17 | Toshiba Corp | 高純度アルミニウム化合物の製造方法 |
-
2006
- 2006-04-03 US US11/887,785 patent/US20090028766A1/en not_active Abandoned
- 2006-04-03 TW TW095111809A patent/TW200702304A/zh unknown
- 2006-04-03 WO PCT/JP2006/307048 patent/WO2006107020A1/ja active Application Filing
- 2006-04-03 CN CNA2006800110575A patent/CN101155759A/zh active Pending
- 2006-04-03 JP JP2007511228A patent/JP5125504B2/ja active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH061607A (ja) * | 1992-06-22 | 1994-01-11 | Mitsubishi Materials Corp | 高純度塩化アルミニウムの製造方法 |
JPH06263438A (ja) * | 1993-03-09 | 1994-09-20 | Mitsubishi Petrochem Co Ltd | 高純度無水塩化アルミニウムの製造方法 |
JPH09301714A (ja) * | 1996-05-09 | 1997-11-25 | Nippon Light Metal Co Ltd | 高純度無水塩化アルミニウムの製造方法 |
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JPWO2006107020A1 (ja) | 2008-09-25 |
JP5125504B2 (ja) | 2013-01-23 |
TW200702304A (en) | 2007-01-16 |
CN101155759A (zh) | 2008-04-02 |
US20090028766A1 (en) | 2009-01-29 |
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