CN102502739B - Method for producing high-purity alpha-aluminum oxide - Google Patents
Method for producing high-purity alpha-aluminum oxide Download PDFInfo
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- CN102502739B CN102502739B CN 201110357749 CN201110357749A CN102502739B CN 102502739 B CN102502739 B CN 102502739B CN 201110357749 CN201110357749 CN 201110357749 CN 201110357749 A CN201110357749 A CN 201110357749A CN 102502739 B CN102502739 B CN 102502739B
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Abstract
The invention relates to a method for producing high-purity alpha-aluminum oxide, in particular to a method for producing high-purity alpha-aluminum oxide with the purity of more than 99.999 percent by taking industrial aluminum hydroxide or sodium metaaluminate as a raw material. The method comprises the following steps: performing reaction of the industrial aluminum hydroxide or sodium metaaluminate and hydrochloric acid in a sealed reaction tank to obtain an aluminum trichloride solution; filtering, evaporating and crystallizing the aluminum trichloride solution to obtain an aluminum chloride hexahydrate crystal; dehydrating the aluminum chloride hexahydratecrystal in a protection of hydrogen chloride gas at high temperature to obtain anhydrous aluminum trichloride powder; sublimating and purifying the aluminum trichloride powder in a vacuum furnace to obtain aluminum trichloride with the purity of more than 99.999 percent; dissolving the high-purity aluminum trichloride in an ammonia solution, concentrating, crystallizing, filtering and drying to obtain high-purity aluminum hydroxide crystal; and calcining the aluminum hydroxide crystal at high temperature to obtain the high-purity alpha-aluminum oxide powder.
Description
Technical field
The present invention relates to a kind of production method of pure alpha-aluminum oxide, is raw material by industrial aluminium hydroxide or industrial sodium metaaluminate particularly, and production purity is greater than the method for 99.999% pure alpha-aluminum oxide.
Background technology
High purity aluminium oxide be purity at the aluminum oxide more than 99.99%, be mainly used in fluorescent material, high-purity ceramic, circuit substrate, artificial substrate, be widely used in fields such as metallurgy, machinery, chemical industry, electronics, aviation and national defence.
Because the high purity aluminium oxide powder is with a wide range of applications, all will prepare the high purity aluminium oxide powder in recent years all over the world as one of main direction of field of new, it is numerous to produce the high purity aluminium oxide method, mainly contain choline aluminium hydrolysis method, exsiccated ammonium alum pyrolysis method, volatile salt pyrolysis method, the method that is in pilot scale and laboratory stage also has mercury chloride activated water solution, plasma method, spray pyrolysis, low-carbon alkyl aluminium hydrolysis method, hydrothermal method, elutriation complexometry, sol-gel method etc.There are deficiencies such as product foreign matter content height, energy consumption height, environmental pollution be serious more or less in above-mentioned several production method.Therefore be necessary to explore a kind of effective means for the preparation of high purity aluminium oxide, the purity of aluminum oxide is reached more than 99.999%, reach the requirement of high purity aluminium oxide.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method for preparing the pure alpha-aluminum oxide powder, its production efficiency height, facility investment is few, energy consumption is low, and smaller to the influence of environment, cost is low, the product purity height can satisfy the requirement of pure alpha-aluminum oxide.
Solving the technical scheme that technical problem of the present invention adopts is: adopt purity to be not less than 80% industrial aluminium hydroxide or industrial sodium metaaluminate and hydrochloric acid in the reactive tank internal reaction that seals, obtain aluminum trichloride solution; After aluminum trichloride solution filters, generate six water aluminum chloride crystal through evaporation, crystallization.Six water aluminum chloride crystal high temperature dehydration under the protection of hydrogen chloride gas obtains the aluminum trichloride (anhydrous) powder.The purification that distils in vacuum oven of aluminum chloride powder obtains purity and surpasses 99.999% aluminum chloride.After high-purity aluminum chloride is dissolved in ammonia soln, through having obtained high-purity aluminum hydroxide crystals after concentrated, crystallization, filtration, the drying.Aluminum hydroxide crystals has generated the pure alpha-aluminum oxide powder through after the high-temperature calcination.
Described hydrochloric acid and industrial aluminium hydroxide or industrial sodium metaaluminate by volume weight liquid-solid ratio are 1 ~ 10:1 when reaction, and the used salt acid concentration is 10 ~ 36%, and temperature of reaction is 30 ~ 90 ℃, and the reaction times is 1 ~ 20h.
Described aluminum chloride filtrate evaporative crystallization through 3 ~ 10h under 80 ~ 150 ℃ of temperature generates six water aluminum chloride crystal.
Described six water aluminum chloride crystal are at flow 2 ~ 10 m
3Under the hydrogen chloride gas protection of/h, 120 ~ 250 ℃ of following high temperature dehydrations obtain the aluminum trichloride (anhydrous) powder.Return in the hydrochloric acid soln behind the hydrogen chloride gas bulk absorption moisture.Vacuum tightness when described aluminum chloride powder distils in vacuum oven is 10
-2~ 10
3Pa, sublimation temperature is 150 ~ 177 ℃.
When described high-purity aluminum chloride powder was dissolved in ammonia soln ammonia and soaks operation, temperature of reaction was controlled at 20 ~ 50 ℃; Being dried to water ratio after the filtration is lower than 5% and obtains aluminum hydroxide crystals.
The temperature of described high-temperature calcination aluminum hydroxide crystals is 800 ~ 1200 ℃.
The inner lining material of described hydrochloric acid reaction groove, vacuum oven associated conduit all adopts polytetrafluoroethylmaterial material.
The invention has the beneficial effects as follows: industrial aluminium hydroxide or industrial sodium metaaluminate obtain the high purity aluminium oxide powder soak processing such as crystallization through hydrochloric acid leaching, drying and dehydrating, vacuum-sublimation purification, ammonia after.This technical process is short, realize suitability for industrialized production easily, and equipment is simple, and security is good, and energy consumption is low, and production cost is low, and environmental pollution is little.The alumina content of the pure alpha-aluminum oxide that obtains is greater than 99.999%.
Description of drawings:
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment one
Using purity is that 98.5 ~ 99% industrial aluminium hydroxide is raw material.With the hydrochloric acid soln of raw material and 15 ~ 25% according to liquid-solid ratio be 5:1 at reactive tank internal reaction 3h, obtain aluminum trichloride solution.After aluminum trichloride solution filtered, filtrate through evaporation, the crystallization of 3 ~ 4h, obtained six water aluminum chloride crystal under 80 ~ 90 ℃, and six water aluminum chloride crystal are at flow 2 ~ 5m
3The hydrogen chloride gas protection of/h down; obtain the aluminum trichloride (anhydrous) powder in 120 ~ 150 ℃ of following high temperature dehydrations; the aluminum trichloride (anhydrous) powder places in the vacuum oven; maintenance vacuum tightness is 1 ~ 10Pa; 165 ℃ of control sublimation temperatures obtain purity and surpass 99.999% aluminum chloride after vacuum tightness significantly decreases.High-purity aluminum chloride that distillation obtains is dissolved in ammoniacal liquor and reacts, and keeping temperature of reaction is 20 ~ 30 ℃, is dried to water ratio after the filtration and is lower than 5%, and obtain the pure alpha-aluminum oxide powder after 800 ℃ of high-temperature calcinations.
Result of implementation: the purity of pure alpha-aluminum oxide powder is 99.9995%, and the product total impurities is 0.0004%.Wherein the residual volume of Si is 1 ppmw, and the residual volume of Ca is 0.5 ppmw, and the residual volume of Na is 1 ppmw, other foreign matter contents less than
1 ppmw.
Embodiment two
Using purity is that 90 ~ 95% industrial sodium metaaluminate is raw material.With the hydrochloric acid soln of raw material and 20 ~ 30% according to liquid-solid ratio be 8:1 at reactive tank internal reaction 10h, obtain aluminum trichloride solution.After aluminum trichloride solution filtered, filtrate through evaporation, the crystallization of 5 ~ 6h, obtained six water aluminum chloride crystal under 90 ~ 100 ℃, and six water aluminum chloride crystal are at flow 5 ~ 8m
3The hydrogen chloride gas protection of/h obtains the aluminum trichloride (anhydrous) powder in 150 ~ 200 ℃ of following high temperature dehydrations down, and the aluminum trichloride (anhydrous) powder places in the vacuum oven, and keeping vacuum tightness is 10 ~ 10
2Pa, 175 ℃ of control sublimation temperatures obtain purity and surpass 99.999% aluminum chloride after vacuum tightness significantly decreases.High-purity aluminum chloride that distillation obtains is dissolved in ammoniacal liquor and reacts, and keeping temperature of reaction is 30 ~ 40 ℃, is dried to water ratio after the filtration and is lower than 5%, and obtain the pure alpha-aluminum oxide powder after 1000 ℃ of high-temperature calcinations.
Result of implementation: the purity of pure alpha-aluminum oxide powder is 99.9997%, and the product total impurities is 0.0003%.Wherein the residual volume of Si is 1 ppmw, and the residual volume of Ca is 0.5 ppmw, and the residual volume of Na is 0.5 ppmw, other foreign matter contents less than
1 ppmw.
Embodiment three
Using purity is that 85 ~ 90% industrial aluminium hydroxide is raw material.With the hydrochloric acid soln of raw material and 10 ~ 20% according to liquid-solid ratio be 8:1 at reactive tank internal reaction 2h, obtain aluminum trichloride solution.After aluminum trichloride solution filtered, filtrate through evaporation, the crystallization of 6 ~ 8h, obtained six water aluminum chloride crystal under 110 ~ 130 ℃, and six water aluminum chloride crystal are at flow 8 ~ 10m
3The hydrogen chloride gas protection of/h down; obtain the aluminum trichloride (anhydrous) powder in 200 ~ 250 ℃ of following high temperature dehydrations; the aluminum trichloride (anhydrous) powder places in the vacuum oven; maintenance vacuum tightness is 0.1 ~ 1Pa; 168 ℃ of control sublimation temperatures obtain purity and surpass 99.999% aluminum chloride after vacuum tightness significantly decreases.High-purity aluminum chloride that distillation obtains is dissolved in ammoniacal liquor and reacts, and keeping temperature of reaction is 50 ~ 60 ℃, is dried to water ratio after the filtration and is lower than 5%, and obtain the pure alpha-aluminum oxide powder after 1200 ℃ of high-temperature calcinations.
Result of implementation: the purity of pure alpha-aluminum oxide powder is 99.9993%, and the product total impurities is 0.0007%.Wherein the residual volume of Si is 3 ppmw, and the residual volume of Ca is 0.5 ppmw, and the residual volume of Na is 1ppmw, other foreign matter contents less than
1 ppmw.
Claims (2)
1. the production method of a pure alpha-aluminum oxide is characterized in that step is as follows:
(1) industrial aluminium hydroxide or industrial sodium metaaluminate and hydrochloric acid obtain aluminum trichloride solution in the reactive tank internal reaction of sealing;
(2) after aluminum trichloride solution filters, through evaporative crystallization, generate six water aluminum chloride crystal;
(3) six water aluminum chloride crystal high temperature dehydration under the protection of hydrogen chloride gas obtains the aluminum trichloride (anhydrous) powder;
(4) the aluminum trichloride (anhydrous) powder purification that distils in vacuum oven obtains purity and surpasses 99.999% aluminum chloride;
(5) after high-purity aluminum chloride is dissolved in ammonia soln, obtain high-purity aluminum hydroxide crystals through after condensing crystal, filtration and the drying;
(6) aluminum hydroxide crystals is through generating the pure alpha-aluminum oxide powder after the high-temperature calcination;
In step 1) hydrochloric acid and industrial aluminium hydroxide or industrial sodium metaaluminate by volume the weight liquid-solid ratio be 1 ~ 10:1 when reaction, the used salt acid concentration is 10 ~ 36%, temperature of reaction is 30 ~ 90 ℃, the reaction times is 1 ~ 20h;
In step 2) in after aluminum trichloride solution filters, filtrate evaporative crystallization through 3 ~ 10h under 80 ~ 150 ℃ of temperature generates six water aluminum chloride crystal;
Six water aluminum chloride crystal are at flow 2 ~ 10 m in the step 3)
3The hydrogen chloride gas protection of/h obtains the aluminum trichloride (anhydrous) powder in 120 ~ 250 ℃ of following high temperature dehydrations down;
Vacuum tightness when the aluminum chloride powder distils in vacuum oven in step 4) is 10
-2~ 10
3Pa, sublimation temperature is 150 ~ 177 ℃;
When high-purity aluminum chloride powder was dissolved in ammonia soln ammonia and soaks operation in step 5), temperature of reaction was controlled at 20 ~ 50 ℃; Being dried to water ratio after the filtration is lower than 5% and obtains aluminum hydroxide crystals;
The temperature of high-temperature calcination aluminum hydroxide crystals is 800 ~ 1200 ℃ in step 6).
2. method according to claim 1 is characterized in that: adopting purity to be not less than high-purity industrial aluminium hydroxide of 80% or purity, to be not less than 80% high-purity industrial sodium metaaluminate be raw material.
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| AU2012385519B2 (en) * | 2012-07-20 | 2017-01-05 | Obshchestvo S Ogranichennoy Otvetstvennost'yu "Obedinennaya Kompaniya Rusal Inzhenerno-Tekhnologicheskiy Tsentr" | Method for producing alumina |
| CN107572569A (en) * | 2012-12-17 | 2018-01-12 | 波拉尔蓝宝石有限公司 | The method for manufacturing high-purity alpha-alumina |
| CA2900261C (en) * | 2013-02-04 | 2017-03-07 | Obshchestvo S Ogranichennoy Otvetstvennost'yu "Obedinennaya Kompaniya Rusal Inzhenerno-Tekhnologicheskiy Tsentr" | Porous aluminum oxide powders with a honeycomb structure |
| US10023472B2 (en) * | 2013-02-04 | 2018-07-17 | United Company RUSAL Engineering and Technology Centre LLC | Aluminum oxide production method |
| CN103204530B (en) * | 2013-05-14 | 2014-10-22 | 昆明冶金研究院 | Method for removing sodium in preparation of high-purity alumina |
| CN103351012A (en) * | 2013-06-27 | 2013-10-16 | 中国铝业股份有限公司 | Preparation method of aluminum oxide powder |
| CN104016389A (en) * | 2014-06-17 | 2014-09-03 | 扬州大学 | Method for preparing high-purity aluminum oxide by sublimation |
| US20170260062A1 (en) * | 2014-10-03 | 2017-09-14 | Orbite Technologies Inc. | Methods for purifying aluminium ions |
| CN105621468B (en) * | 2014-11-27 | 2017-03-29 | 中国科学院过程工程研究所 | A kind of preparation method of high purity aluminium oxide |
| CN111453752A (en) * | 2020-06-09 | 2020-07-28 | 孙雪梅 | High-purity alumina and preparation method thereof |
| CN112374516A (en) * | 2020-11-19 | 2021-02-19 | 衡阳鸿宇化工有限责任公司 | Evaporation concentration crystallization device of aluminum trichloride solution and use method thereof |
| CN114455607B (en) * | 2022-03-08 | 2023-04-25 | 重庆工贸职业技术学院 | Purification method of industrial byproduct ammonium chloride |
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Address after: 650031 No. 86 Yuantong North Road, Yunnan, Kunming Patentee after: Kunming Metallurgical Research Institute Co., Ltd Address before: 650031, 86 North Tong Road, Wuhua District, Yunnan, Kunming Patentee before: Kunming Metallurgical Research Institute |