CN100431963C - Method for preparing Nano powder of alumina from industrial waste - Google Patents
Method for preparing Nano powder of alumina from industrial waste Download PDFInfo
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- CN100431963C CN100431963C CNB2005100246017A CN200510024601A CN100431963C CN 100431963 C CN100431963 C CN 100431963C CN B2005100246017 A CNB2005100246017 A CN B2005100246017A CN 200510024601 A CN200510024601 A CN 200510024601A CN 100431963 C CN100431963 C CN 100431963C
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Abstract
The present invention relates to a method for utilizing industrial waste to prepare nanometer alumina powder, which belongs to the technical field of chemical engineering. The method of the present invention mainly comprises: industrial waste at least containing 70 wt% of aluminum or Al2O3, such as aluminium containing spent catalysts or scrap aluminium alloy turnings, is used as raw material, the raw material is ground into powder to react with molten ammonium bisulfate solution or ammonium bisulfate solution, and products are filtered, concentrated by heating and recrystallized to obtain aluminium ammonium sulfate crystals with purity higher than 99.9%; the obtained aluminium ammonium sulfate crystals are prepared into solution with the concentration of 0.1 to 0.5 mol/L, ammonium bicarbonate solution with the concentration of 1 to 5 mol/L is prepared simultaneously, and 1 to 5% of polyethylene glycol as dispersing agents is added into the ammonium bicarbonate solution; the aluminium ammonium sulfate solution is added into the prepared ammonium bicarbonate solution drip by drip to obtain basic aluminum ammonium carbonate, and the obtained basic aluminum ammonium carbonate is dried and burned to finally obtain nanometer alumina powder with the particle diameter of 50 to 100 nm.
Description
Technical field
The present invention relates to a kind ofly prepare nano alumina powder jointed method by industrial waste.Belong to technical field of chemistry and chemical engineering.
Background technology
Nano alumina material is the nano material that significant application value and development prospect are arranged.Nano aluminium oxide is because of having high rigidity, high strength, characteristic such as heat-resisting, corrosion-resistant, heat-stable material, guided missile window and high-pressure mercury lamp fluorescent tube material, computer integrate circuit substrate, high-abrasive material and bioceramic material have been widely used as, and the catalyzer of petrochemical industry or support of the catalyst, in handling, vehicle exhaust also can be used as carrier.Nano alumina powder jointed is the raw material of making nano ceramics, and nano ceramics hard wear resistant and to a certain degree toughness is arranged is the structured material with major application prospect.
The at present external nano alumina powder jointed raw material of mass preparation mostly is expensive alkoxide or more expensive fine aluminium salt (as aluminum chloride, aluminum nitrate etc.), and the cost height causes nano aluminium oxide to hold at high price, and has seriously limited its application and industrialization process.
Summary of the invention
The object of the present invention is to provide and a kind ofly prepare the nano alumina powder jointed method that purity meets the requirements with industrial waste.Another purpose of the present invention is to provide a kind of simple technology, and promptly wet-chemical synthetic liquid phase method prepares nano alumina powder jointed method.
The present invention a kind ofly prepares nano alumina powder jointed method by industrial waste, it is characterized in that this method has following technological process and step:
A. will contain 70wt% aluminium or Al at least
2O
3Contain aluminium spent catalyst or scrap aluminium alloy car bits, be ground into powder;
B. be to take by weighing monoammonium sulfate in 1: 6～1: 10 according to the mol ratio of aluminum oxide and monoammonium sulfate; Be heated fusion or be mixed with saturated solution;
C. with above-mentioned contain aluminium spent catalyst powder with on a small quantity repeatedly mode be incorporated in slowly in the fused monoammonium sulfate liquation; Perhaps scrap aluminium alloy car bits powder is incorporated in the monoammonium sulfate solution of above-mentioned preparation, after powder all added, heating was fully reacted it, and the time is 0.5～1 hour;
D. with above-mentioned liquation cooling of being reacted by the spent catalyst powder, be dissolved in water, the elimination throw out is got filtrate; Perhaps directly take the solution that was reacted by scrap aluminium alloy car bits powder, the elimination throw out is got filtrate; Respectively the filtrate heating is concentrated, recrystallization 2～5 times, products therefrom promptly gets purity at the ammonium aluminum sulfate crystal more than 99.9% 50～70 ℃ of oven dry 2～6 hours;
E. the gained ammonium aluminum sulfate crystal is mixed with the solution that concentration is 0.1～0.5mol/L, simultaneously in addition compound concentration is the ammonium bicarbonate soln of 1～5mol/L, and adds 1～5% polyoxyethylene glycol make dispersion agent in ammonium bicarbonate soln;
F. with above-mentioned aluminum ammonium sulfate solution, dropwise be incorporated in the above-mentioned ammonium bicarbonate soln for preparing; The mol ratio of aluminum ammonium sulfate solution and ammonium bicarbonate soln is 1: 8～1: 15; And with ammoniacal liquor control pH value between 9～11, vigorous stirring simultaneously, the reaction after-filtration that finishes with the throw out of gained with deionized water wash for several times, until the approaching neutrality of pH value, promptly gets the Aluminum Carbonate Basic ammonium;
G. gained Aluminum Carbonate Basic ammonium was descended dry 1～3 hour at 80～120 ℃,, finally make the nano alumina powder jointed of particle diameter 50～100nm then 1050～1200 ℃ of following calcinations 1～3 hour.
The advantage of the inventive method is: technology is simple, easy and simple to handle, equipment is simple, and cost is low, and free from environmental pollution.Prepared alumina powder jointed purity height, good uniformity, fine size.
Embodiment
Embodiment one: the technological process and the step of present embodiment are as follows:
1. at first will contain the aluminium spent catalyst and pulverize, take by weighing the spent catalyst 51g that this contains 80% aluminum oxide;
2. take by weighing monoammonium sulfate 346.85g, heating and melting on electric furnace;
With the powder of above-mentioned salic spent catalyst with on a small quantity repeatedly mode slowly add in the fused monoammonium sulfate liquation, after treating all to add, heating makes it continue reaction, the time is 30 minutes;
4. after treating that it naturally cools to room temperature, add water and fully dissolve, remove by filter bits, get filtrate.The heating of gained filtrate is concentrated, and cooling is left standstill and is made it separate out crystal; The ammonium aluminum sulfate crystal that obtains is leached, and recrystallization is 3 times repeatedly, and the ammonium aluminum sulfate crystal that obtains is ground, and dries 4 hours, and promptly gets highly purified ammonium aluminum sulfate crystal for 65 ℃;
5. take by weighing the above-mentioned exsiccated ammonium alum 23.7g that makes, be mixed with the solution that concentration is 0.2mol/L.Simultaneously in addition compound concentration is the ammonium bicarbonate soln of 2mol/L, and to take by weighing molecular weight be that 2000 polyoxyethylene glycol PEG1.26g dissolves in the ammonium bicarbonate soln;
6. above-mentioned aluminum ammonium sulfate solution is slowly dripped in above-mentioned ammonium bicarbonate soln, and to control its pH value with ammoniacal liquor be 9; Vigorous stirring has been reacted after-filtration simultaneously, with the gained throw out with deionized water wash for several times, near neutral, promptly gets Aluminum Carbonate Basic ammonium precipitation until the pH value;
7. the Aluminum Carbonate Basic ammonium after 2 hours, in 1100 ℃ of calcinations 2 hours, is promptly got the α-Al about particle diameter 50nm at 105 ℃ of following freeze-day with constant temperature
2O
3Nano-powder.
Embodiment two: the technological process and the step of present embodiment and the foregoing description 1 are basic identical, and different is:
1. the industrial waste of Cai Yonging is to contain the aluminium scrap car bits of aluminium more than 80%, takes by weighing these aluminium scrap car bits 45g;
2. these aluminium scrap car bits are repeatedly joined in the saturated solution that is made into by the 346.85g monoammonium sulfate on a small quantity;
3. reacting by heating is 1 hour, has reacted after-filtration, gets filtrate;
4. the filtrate heating concentrates, and cooling is left standstill, and makes it separate out crystal.Recrystallization is 4 times so repeatedly, and the gained ammonium aluminum sulfate crystal is ground, and dries 3 hours, and promptly gets highly purified ammonium aluminum sulfate crystal for 70 ℃;
5. take by weighing exsiccated ammonium alum 23.7g, be mixed with the solution that concentration is 0.1mol/L.The concentration of the bicarbonate of ammonia of preparation is 1mol/L in addition, and adds polyoxyethylene glycol 0.95g, and it is fully dissolved;
6. be 10 with ammoniacal liquor control pH value;
7. gained Aluminum Carbonate Basic ammonium is under 100 ℃ of temperature, after dry 3 hours, in 1200 ℃ of calcinations 1.5 hours; Finally make the α-Al about particle diameter 50nm
2O
3Nano powder.
By prepared aluminum oxide among above-mentioned two embodiment is α-Al
2O
3Powder, purity can reach 99.99%, and particle form is mainly spherical and bar-shaped, and the median size of alumina particle is 50nm.
Claims (1)
1. one kind prepares nano alumina powder jointed method by industrial waste, it is characterized in that this method has following technological process and step:
A. will contain 70wt% aluminium or Al at least
2O
3Aluminium spent catalyst or the scrap aluminium alloy car bits that contain be raw material, be ground into powder;
B. be to take by weighing monoammonium sulfate in 1: 6～1: 10 according to the mol ratio of aluminum oxide and monoammonium sulfate; Be heated fusion or be mixed with saturated solution;
C. with above-mentioned contain aluminium spent catalyst powder with on a small quantity repeatedly mode be incorporated in slowly in the fused monoammonium sulfate liquation; Perhaps scrap aluminium alloy car bits powder is incorporated in the monoammonium sulfate saturated solution of above-mentioned preparation, after powder all added, heating was fully reacted it, and the reaction times is 0.5～1 hour;
D. with above-mentioned liquation cooling of being reacted by the spent catalyst powder, be dissolved in water, the elimination throw out is got filtrate; Perhaps directly take the solution that was reacted by scrap aluminium alloy car bits powder, the elimination throw out is got filtrate; Respectively the filtrate heating is concentrated, recrystallization 2～5 times, products therefrom promptly gets purity at the ammonium aluminum sulfate crystal more than 99.9% 50～70 ℃ of oven dry 2～6 hours;
E. the gained ammonium aluminum sulfate crystal is mixed with the solution that concentration is 0.1～0.5mol/L, simultaneously in addition compound concentration is the ammonium bicarbonate soln of 1～5mol/L, and adds 1～5% polyoxyethylene glycol make dispersion agent in ammonium bicarbonate soln;
F. with above-mentioned aluminum ammonium sulfate solution, dropwise be incorporated in the above-mentioned ammonium bicarbonate soln for preparing; The mol ratio of aluminum ammonium sulfate solution and ammonium bicarbonate soln is 1: 8～1: 15; And with ammoniacal liquor control pH value between 9～11, vigorous stirring simultaneously, the reaction after-filtration that finishes with the throw out of gained with deionized water wash for several times, until the approaching neutrality of pH value, promptly gets the Aluminum Carbonate Basic ammonium;
G. gained Aluminum Carbonate Basic ammonium was descended dry 1～3 hour at 80～120 ℃,, finally make the nano alumina powder jointed of particle diameter 50～100nm then 1050～1200 ℃ of following calcinations 1～3 hour.
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| CNB2005100246017A CN100431963C (en) | 2005-03-24 | 2005-03-24 | Method for preparing Nano powder of alumina from industrial waste |
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| CNB2005100246017A CN100431963C (en) | 2005-03-24 | 2005-03-24 | Method for preparing Nano powder of alumina from industrial waste |
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| CN100431963C true CN100431963C (en) | 2008-11-12 |
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Families Citing this family (11)
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| CN101870482B (en) * | 2010-05-21 | 2012-05-23 | 焦作市宏程先进陶瓷科技有限公司 | High-purity ammonium aluminum carbonate hydroxide as precursor of high-purity easy-sintering aluminum oxide ceramic powder and preparation process thereof |
| CN102849763A (en) * | 2012-09-07 | 2013-01-02 | 中国石油天然气股份有限公司 | Solid-phase preparation method of gamma-alumina with gradient distribution holes |
| CN103449493A (en) * | 2013-01-15 | 2013-12-18 | 深圳信息职业技术学院 | Low-cost nano aluminum oxide film preparation method and nano aluminum oxide film |
| CN103449492B (en) * | 2013-01-15 | 2016-01-13 | 深圳信息职业技术学院 | A kind of nano alumina powder jointed preparation method of low cost and nano alumina powder jointed |
| CN103693666A (en) * | 2013-12-24 | 2014-04-02 | 北京佳逸创景科技有限公司 | Method for extracting aluminum oxide |
| CN104891541B (en) * | 2015-06-18 | 2016-09-28 | 成都华泽晶体材料有限公司 | The method that aluminium carbonate ammonium pyrolysismethod prepares flaky alumina |
| CN104891542B (en) * | 2015-06-24 | 2017-03-29 | 山东大学 | A kind of ultra-fine α Al2O3Raw powder's production technology |
| CN106115755A (en) * | 2016-06-28 | 2016-11-16 | 上海滃泽科技有限公司 | A kind of method utilizing aluminium scrap goods upgrading to prepare high purity aluminium oxide |
| CN107055583A (en) * | 2017-05-02 | 2017-08-18 | 常熟理工学院 | The method that ammonia-alum is prepared by raw material of dead catalyst |
| CN109455747B (en) * | 2018-11-28 | 2021-01-05 | 陕西好一化工科技有限公司 | Method for preparing alumina and phosphorus-containing fertilizer by using methanol-to-olefin waste catalyst |
| CN113321230B (en) * | 2020-02-28 | 2022-06-14 | 国家能源投资集团有限责任公司 | Method for preparing aluminum oxide and silicon fertilizer by using fly ash |
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