CN1607179A - Preparation technology of size controllable incompact superfine alumina powder material - Google Patents
Preparation technology of size controllable incompact superfine alumina powder material Download PDFInfo
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- CN1607179A CN1607179A CN 200310100398 CN200310100398A CN1607179A CN 1607179 A CN1607179 A CN 1607179A CN 200310100398 CN200310100398 CN 200310100398 CN 200310100398 A CN200310100398 A CN 200310100398A CN 1607179 A CN1607179 A CN 1607179A
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Abstract
A process for preparing ultrafine powdered aluminium oxide wherein aluminium nitrate and ammonia water are use as raw material added with dispersant, adsorbent, reducer and chelant to obtain the product by adjusting the added quantity and proportion of adsorbent and chelant. The technological characteristics is low cost, stable quality, short productive period, controllable products grain diameter and distribution, directly forming powder with ball milling. The products prepared by said invention can be widely used in precision ceramics, chemical catalyst, rearearth fluorescent dye, aviation light source device, moisture sensitive sensor and infrared absorption material etc.
Description
Technical field
The invention belongs to the compound technical field of aluminium, be specifically related to aluminum oxide.
Technical background
Superfine alumina powder as one of special type function material, because excellent characteristics such as having high strength, high rigidity, resistance to wear, corrosion-resistant, high temperature resistant, anti-oxidant, good insulating and specific surface area are big has obtained using widely in fields such as high technology ceramics, chemical catalyst, fluorescent RE powder, aviation light source device, wet quick property transmitter and infrared absorbing materials at present.
According to the retrieval, the method for making of at present domestic and international ultra-fine alumina mainly comprises following method:
Mercury chloride activated water solution, as Chinese patent 95105843.6, Chinese patent ZL92104368.6, Chinese patent 1079718A, United States Patent (USP) 2872096, United States Patent (USP) 3042628, German Patent 2604083 and German Patent 2604083, this method highly toxic substance HgCl
2As catalyzer, be unfavorable for environmental protection and health.
The exsiccated ammonium alum pyrolysis method, as English Patent 514538, German Patent 2215594 and German Patent 2419544, this method expense is big, and the treatment time is long.
The aluminium alcoholates hydrolysis method, as Chinese patent 1195646A and Chinese patent 1342609A, this method poor reproducibility, processing condition are wayward.
The activated aluminum powder hydrolysis method, as Chinese patent 1286235A Chinese patent 1394807A, this method equipment complexity, the production cycle is long.
Summary of the invention
At present, the superfine alumina powder material at home and abroad has broad prospects on the market as a kind of emerging high-tech product, be in great demand, and in rising trend year by year.Because developing rapidly and actual needs of science and technology, it is controlled to press for a kind of yardstick, and form is loose, with low cost, preparation technology simple and the method for favorable reproducibility prepares the superfine alumina powder material.The object of the present invention is to provide a kind of yardstick controlled, form is loose, with low cost, preparation technology simple and the preparation method of the ultra-fine alumina of favorable reproducibility.Technical problem underlying to be solved by this invention and the technical scheme that solves its technical problem comprise:
1, preparation process comprises:
1) a kind of organic polymer dispersion agent is joined Al (NO
3)
39H
2Make modified solution in the O solution;
2) with NH
3H
2O splashes in the modified solution, stirs simultaneously, progressively generates white flocks in the solution, until pH=7～11;
3) add the sorbent material carbon black powder, add a kind of poly-hydroxy aldehyde then, the foreign ion in the reduction colloidal sol, high-speed stirring 30 minutes～2 hours as reductive agent;
4) add sequestrant rapidly after, make itself and aluminum ion be combined into stable chelate, stirred 10 minutes～1 hour, it is dispersed in the sol system, then suction filtration;
5) the gained filter cake can obtain ultra-fine γ-Al in 2～4 hours 600～900 ℃ of following roastings
2O
3, granularity is at 8～11nm; Calcined 4～8 hours down at 900～1400 ℃, can obtain ultra-fine α-Al
2O
3, granularity is at 42～100nm.
2, above-mentioned steps 1) described in the organic polymer dispersion agent can be polypropylene acid ammonium, one or more in polyoxyethylene glycol (PEG) and the polyoxyethylene groups phenyl ether (OP-10).
3, above-mentioned steps 3) described in reductive agent poly-hydroxy aldehyde can be in glucose, sucrose and the starch one or more, described carbon black powder is 1: 1～4: 1 with the virtual mass ratio of reductive agent.
4, above-mentioned steps 3) in utilize the absorption buttressing effect of organic network dispersion effect of organic high molecular compound and high-specific surface area carbon black powder to combine synergy, intercept the reunion and the combination of ultrafine particulate, described carbon black powder is 1: 1～8: 1 with the virtual mass ratio of dispersion agent.
5, above-mentioned steps 4) described in sequestrant can be a kind of or several among polyvinyl alcohol, citric acid and the EDTA.
6, above-mentioned steps 4) in by uniting addition and the ratio of adjusting carbon black powder and sequestrant, make that the particle diameter of product and distribution are controlled, described carbon black powder is 1: 1～3: 1 with the virtual mass ratio of sequestrant.
Superfine alumina powder material preparation technology of the present invention has following characteristics:
1) utilize cheap aluminum nitrate and ammoniacal liquor as raw materials for production, raw materials cost is cheap; 2) in the colloidal sol that generates, add sorbent material and sequestrant,, make that the particle diameter of product and distribution are controlled, and do not need ball milling directly to become powder by the addition and the ratio of comprehensive adjustment sorbent material and sequestrant; 3) adopt poly-hydroxy aldehyde to reduce impurity element in the colloidal sol as reductive agent, significantly improved the purity of product, making cheap low pure raw material be applied in the preparation of nano material becomes possibility; 4) synergy of utilizing the buttressing effect of organic network dispersion effect of organic high molecular compound and the inorganic solid-phase media of high-specific surface area to combine intercepts the reunion and the combination of nanoparticle; 5) compare with existing production technology, owing to gel, absorption, reduce, be sequestered in the same liquid phase and carry out, and adopt the dehydration of suction filtration technology, so this explained hereafter is reappeared, the cycle is short, saves the energy, reduces cost.
Embodiment
The present invention is described in more detail below in conjunction with embodiment, but the invention is not restricted to these embodiment.
Embodiment 1:
155 gram aluminum nitrates are joined in 1 premium on currency, add 20 gram polyoxyethylene glycol, stir and dissolve fully, in mixing solutions, splash into saturated ammoniacal liquor until aluminum nitrate, until pH=11, add carbon black powder 50 grams and sucrose 25 grams, stirred 90 minutes, add 20 gram citric acids then, stirred suction filtration 40 minutes.The gained filter cake can obtain ultra-fine γ-Al in 3 hours 800 ℃ of following roastings
2O
3
Embodiment 2:
155 gram aluminum nitrates are joined in 1 premium on currency, add 10 gram polypropylene acid ammoniums, stirring is dissolved fully until aluminum nitrate, in mixing solutions, splash into saturated ammoniacal liquor,, add carbon black powder 30 grams and starch 30 grams until pH=7, stirred 50 minutes, add 30 gram polyvinyl alcohol then, stirred suction filtration 20 minutes.The gained filter cake can obtain ultra-fine γ-Al in 2 hours 900 ℃ of following roastings
2O
3
Embodiment 3:
155 gram aluminum nitrates are joined in 1 premium on currency, add 5 gram polyoxyethylene groups phenyl ethers, stirring is dissolved fully until aluminum nitrate, in mixing solutions, splash into saturated ammoniacal liquor,, add carbon black powder 40 grams and glucose 30 grams until pH=11, stirred 30 minutes, add 30 gram EDTA then, stirred suction filtration 30 minutes.The gained filter cake can obtain ultra-fine α-Al in 4 hours 1200 ℃ of calcinings
2O
3
Claims (6)
1. the preparation method of a controllable size, ultra-fine alumina that form is loose is characterized in that preparation process comprises: 1) a kind of organic polymer dispersion agent is joined Al (NO
3)
39H
2Make modified solution in the O solution; 2) with NH
3H
2O splashes in the modified solution, stirs simultaneously, progressively generates white flocks in the solution, until pH=7～11; 3) add the sorbent material carbon black powder, add a kind of poly-hydroxy aldehyde then, the foreign ion in the reduction colloidal sol, high-speed stirring 10 minutes～2 hours as reductive agent; 4) add sequestrant rapidly after, stirred 10 minutes～1 hour, it is dispersed in the sol system, then suction filtration; 5) the gained filter cake can obtain ultra-fine γ-Al in 2～4 hours 600～900 ℃ of following roastings
2O
3, granularity is at 8～11nm; Calcined 4～8 hours down at 900～1400 ℃, can obtain ultra-fine α-Al
2O
3, granularity is at 42～100nm.
2. by the described method of claim 1, it is characterized in that the organic polymer dispersion agent in the step 1) can be a polypropylene acid ammonium, one or more in polyoxyethylene glycol (PEG) and the polyoxyethylene groups phenyl ether (OP-10).
3. by the described method of claim 1, it is characterized in that reductive agent poly-hydroxy aldehyde in the step 3) can be one or more in glucose, sucrose and the starch, described carbon black powder is 1: 1～4: 1 with the virtual mass ratio of reductive agent.
4. by the described method of claim 1, the synergy that it is characterized in that utilizing in the step 3) absorption buttressing effect of organic network dispersion effect of organic high molecular compound and high-specific surface area carbon black powder to combine, intercept the reunion and the combination of ultrafine particulate, described carbon black powder is 1: 1～8: 1 with the virtual mass ratio of dispersion agent.
5. by the described method of claim 1, it is characterized in that sequestrant in the step 4) can be a kind of or several among polyvinyl alcohol, citric acid and the EDTA.
6. by the described method of claim 1, it is characterized in that in the step 4) addition and the ratio of adjusting carbon black powder and sequestrant by uniting making that the particle diameter of product and distribution are controlled that described carbon black powder is 1: 1～3: 1 with the virtual mass ratio of sequestrant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310100398 CN1607179A (en) | 2003-10-15 | 2003-10-15 | Preparation technology of size controllable incompact superfine alumina powder material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310100398 CN1607179A (en) | 2003-10-15 | 2003-10-15 | Preparation technology of size controllable incompact superfine alumina powder material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1607179A true CN1607179A (en) | 2005-04-20 |
Family
ID=34755943
Family Applications (1)
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|---|---|---|---|
| CN 200310100398 Pending CN1607179A (en) | 2003-10-15 | 2003-10-15 | Preparation technology of size controllable incompact superfine alumina powder material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102240803A (en) * | 2011-07-15 | 2011-11-16 | 郑州大学 | Surface treatment method for improving hydration resistance of aluminum powder |
| CN101327944B (en) * | 2008-07-16 | 2012-11-28 | 孙志昂 | Production process for preparing superfine crystal alpha-aluminum oxide by directly using aluminum sulfate |
| US8343415B2 (en) | 2007-01-15 | 2013-01-01 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic particulate material and processes for forming same |
| CN101746786B (en) * | 2008-12-08 | 2013-08-14 | 中国科学院福建物质结构研究所 | Method for preparing high-purity alpha-Al2O3 nano-crystalline material |
| CN103833377A (en) * | 2014-03-21 | 2014-06-04 | 景德镇陶瓷学院 | Particle size control method of ceramic powder prepared by wet chemical method |
| CN109231970A (en) * | 2018-10-25 | 2019-01-18 | 河南东风新研材科技有限公司 | A kind of nanocrystalline ceramics corundum abrasive and preparation method thereof |
| CN110143606A (en) * | 2019-06-03 | 2019-08-20 | 吉林省人工影响天气办公室 | Nano-aluminium oxide raw powder's production technology |
-
2003
- 2003-10-15 CN CN 200310100398 patent/CN1607179A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8343415B2 (en) | 2007-01-15 | 2013-01-01 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic particulate material and processes for forming same |
| CN101327944B (en) * | 2008-07-16 | 2012-11-28 | 孙志昂 | Production process for preparing superfine crystal alpha-aluminum oxide by directly using aluminum sulfate |
| CN101746786B (en) * | 2008-12-08 | 2013-08-14 | 中国科学院福建物质结构研究所 | Method for preparing high-purity alpha-Al2O3 nano-crystalline material |
| CN102240803A (en) * | 2011-07-15 | 2011-11-16 | 郑州大学 | Surface treatment method for improving hydration resistance of aluminum powder |
| CN102240803B (en) * | 2011-07-15 | 2012-12-26 | 郑州大学 | Surface treatment method for improving hydration resistance of aluminum powder |
| CN103833377A (en) * | 2014-03-21 | 2014-06-04 | 景德镇陶瓷学院 | Particle size control method of ceramic powder prepared by wet chemical method |
| CN109231970A (en) * | 2018-10-25 | 2019-01-18 | 河南东风新研材科技有限公司 | A kind of nanocrystalline ceramics corundum abrasive and preparation method thereof |
| CN110143606A (en) * | 2019-06-03 | 2019-08-20 | 吉林省人工影响天气办公室 | Nano-aluminium oxide raw powder's production technology |
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