CN1696060A - Method for preparing Nano powder of alumina from industrial waste - Google Patents
Method for preparing Nano powder of alumina from industrial waste Download PDFInfo
- Publication number
- CN1696060A CN1696060A CN 200510024601 CN200510024601A CN1696060A CN 1696060 A CN1696060 A CN 1696060A CN 200510024601 CN200510024601 CN 200510024601 CN 200510024601 A CN200510024601 A CN 200510024601A CN 1696060 A CN1696060 A CN 1696060A
- Authority
- CN
- China
- Prior art keywords
- ammonium
- solution
- aluminum
- sulfate
- mentioned
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
A process for preparing the aluminium oxide nanoparticles from the industrial waste (used Al catalyst or rejected A-alloy) includes grinding, reacting on fused ammonium hydrogen sulfate or its solution, filtering, thermal concentrating, recrystallzing to obtain ammonium aluminium sulfate crystals, preparing its solution, dripping it in the solution of ammonium dicarbonate containing polyethanediol to generate alkaline ammonium aluminium carbonate, drying, and burning.
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
3Industrial waste, as contain 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 solution;
C. with above-mentioned salic 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 are 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 fused solution cooling of being reacted by spent catalyst, 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, 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
3pPowder, 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
3Industrial waste, as contain aluminium spent catalyst or scrap aluminium alloy car bits and 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 solution;
C. with above-mentioned salic 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 are 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 fused solution cooling of being reacted by spent catalyst, 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, 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.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2005100246017A CN100431963C (en) | 2005-03-24 | 2005-03-24 | Method for preparing Nano powder of alumina from industrial waste |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNB2005100246017A CN100431963C (en) | 2005-03-24 | 2005-03-24 | Method for preparing Nano powder of alumina from industrial waste |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1696060A true CN1696060A (en) | 2005-11-16 |
CN100431963C CN100431963C (en) | 2008-11-12 |
Family
ID=35348975
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNB2005100246017A Expired - Fee Related CN100431963C (en) | 2005-03-24 | 2005-03-24 | Method for preparing Nano powder of alumina from industrial waste |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN100431963C (en) |
Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101870482A (en) * | 2010-05-21 | 2010-10-27 | 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 for gamma-alumina with gradient distribution holes |
CN103449492A (en) * | 2013-01-15 | 2013-12-18 | 深圳信息职业技术学院 | Low-cost nano aluminum oxide powder preparation method and nano aluminum oxide powder |
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 |
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 |
CN104891542A (en) * | 2015-06-24 | 2015-09-09 | 山东大学 | Preparation method of ultrafine alpha-Al2O3 powder |
CN104891541A (en) * | 2015-06-18 | 2015-09-09 | 成都华泽晶体材料有限公司 | Method for preparing flaky alpha alumina with ammonium aluminum carbonate hydroxide pyrolysis method |
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 |
CN109455747A (en) * | 2018-11-28 | 2019-03-12 | 陕西好化工科技有限公司 | A method of aluminium oxide is prepared using methanol-to-olefins dead catalyst and containing phosphatic manure |
CN113321230A (en) * | 2020-02-28 | 2021-08-31 | 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 |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1177761C (en) * | 2002-03-12 | 2004-12-01 | 中国科学院上海硅酸盐研究所 | Process for preparing alumina powder with high sinter activity |
CN1448340A (en) * | 2002-04-04 | 2003-10-15 | 苏州市宇光特种陶瓷材料厂 | Process for preparing high-purity ultra-fine alumina powder |
CN1186261C (en) * | 2003-06-05 | 2005-01-26 | 上海大学 | Preparation method of nano alumina material |
CN1273384C (en) * | 2004-06-02 | 2006-09-06 | 武汉大学 | Preparation of nano aluminum oxide without hard coacervation |
-
2005
- 2005-03-24 CN CNB2005100246017A patent/CN100431963C/en not_active Expired - Fee Related
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101870482A (en) * | 2010-05-21 | 2010-10-27 | 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 |
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 for gamma-alumina with gradient distribution holes |
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 |
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 |
CN103449492A (en) * | 2013-01-15 | 2013-12-18 | 深圳信息职业技术学院 | Low-cost nano aluminum oxide powder preparation method and nano aluminum oxide powder |
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 |
CN104891541A (en) * | 2015-06-18 | 2015-09-09 | 成都华泽晶体材料有限公司 | Method for preparing flaky alpha alumina with ammonium aluminum carbonate hydroxide pyrolysis method |
CN104891542A (en) * | 2015-06-24 | 2015-09-09 | 山东大学 | Preparation method of ultrafine alpha-Al2O3 powder |
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 |
CN109455747A (en) * | 2018-11-28 | 2019-03-12 | 陕西好化工科技有限公司 | A method of aluminium oxide is prepared using methanol-to-olefins dead catalyst and containing phosphatic manure |
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 |
CN113321230A (en) * | 2020-02-28 | 2021-08-31 | 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 |
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 |
Also Published As
Publication number | Publication date |
---|---|
CN100431963C (en) | 2008-11-12 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN1696060A (en) | Method for preparing Nano powder of alumina from industrial waste | |
EP1934384B1 (en) | Coating method of metal oxide superfine particles on the surface of metal oxide and coating produced therefrom | |
EP2824200B1 (en) | Process for the comprehensive recovery of metal cobalt, ruthenium and aluminum from waste catalyst co-ru/al2o3 in fischer-tropsch synthesis | |
Li et al. | Microwave-assisted Sol− Gel synthesis and photoluminescence characterization of LaPO4: Eu3+, Li+ nanophosphors | |
CN106865618B (en) | One kind " peanut shape " Mn2O3The preparation method of/C particles | |
CN1403375A (en) | Synthesis process of nanostring and nanopowder of RE hydroxide or oxide | |
CN1923686A (en) | Synthesis method of nano hexaboride | |
US8979974B2 (en) | Composition for collecting metal component | |
EP4368575A1 (en) | Method for partially reducing vanadium pentoxide using ammonia solution, and vanadium dioxide powder prepared thereby | |
CN1237006C (en) | In2O3 and ITO monodisperse nano powder hydrothermal preparation method | |
Kaithwas et al. | Structural features of Ce doped YAG nanoparticles synthesized by modified sol–gel method | |
Kamat et al. | Synthesis of yttrium aluminium garnet by the gel entrapment technique using hexamine | |
CN1150130C (en) | Prepn. of nano RE oxide powder | |
JPH11292538A (en) | Production of zirconia-ceria composition | |
Kanezaki et al. | Solid-state chemistry of thermally induced yellow colouring in synthetic hydrous titanium oxide from TiCl 3 | |
CN112342450B (en) | Production process of high-refractive-index coating mixed material | |
JPH04154621A (en) | Production of electrically conductive titanium dioxide powder | |
Fu et al. | La2Sn2O7: Eu3+ micronanospheres: hydrothermal synthesis and luminescent properties | |
Yagmurlu et al. | Solid-State Conversion of Scandium Phosphate into Scandium Oxide with Sodium Compounds | |
Qi et al. | Hydrothermal synthesis and luminescence properties of TiO2: Eu3+ submicrospheres | |
CN100393623C (en) | Large particle rare-earth oxide and its preparing method | |
CN102344156A (en) | Method for preparing superfine alumina by solid-phase reaction | |
JP4359531B2 (en) | Zirconium-based oxide production method and automobile exhaust gas purification catalyst | |
CN1386700A (en) | Process for synthesizing superfine hydroxyapatite powder by self combustion method | |
CN112047355B (en) | Method for preparing aluminum borate crystal whisker by precipitation method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20081112 Termination date: 20110324 |