CN102924092A - Low-cost and pollution-free preparation method for highly dispersed flaky alumina - Google Patents
Low-cost and pollution-free preparation method for highly dispersed flaky alumina Download PDFInfo
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- CN102924092A CN102924092A CN2012104080542A CN201210408054A CN102924092A CN 102924092 A CN102924092 A CN 102924092A CN 2012104080542 A CN2012104080542 A CN 2012104080542A CN 201210408054 A CN201210408054 A CN 201210408054A CN 102924092 A CN102924092 A CN 102924092A
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Abstract
The invention belongs to the technical field of the preparation of fine ceramic powder and particularly relates to a low-cost and pollution-free preparation method for highly dispersed flaky alumina. The method is characterized by comprising the following steps of: placing fluoride at the bottom in a ceramic crucible, adding aluminum oxide hydrate, and covering a crucible cover, wherein the mass ratio of the fluoride to the aluminum oxide hydrate is (1:50)-(1:20); sealing the crucible by using mud, and drying; and finally, calcining in a muffle furnace for 1 to 3 hours at the temperature of 1,100 to 1,300 DEG C to directly obtain the highly dispersed flaky alumina.
Description
Technical field
The invention belongs to the Fine Ceramic Powder preparing technical field, relate in particular to a kind of high dispersion flake aluminum oxide low cost, pollution-free preparation method.
Background technology
Tabular alumina has resistance to acids and bases, high temperature resistant, hardness is high, fusing point is high, the high a lot of good performances of thermal conductivity height and resistivity can be widely used in pigment, coating, makeup, automobile finish, printing ink, filler, abrasive material, refractory materials, slide gate nozzle, nozzle, sleeve pipe, cushion plate and casting liner, support of the catalyst, heat exchange medium, an electrical ignition element, fine ceramics etc. numerous areas.
At present, preparing the most frequently used method of tabular alumina is hydrothermal method, coating method, mechanical process and molten-salt growth method; Hydrothermal method is from published patent documentation [JP Pat, No.111239/1982, No.131517/1991, No.39362/1992] [US0522519A2/1992] and [Science Bulletin of paper document, 1997,42 (24): 2663] [J Dispersion Sci Techn, 2001,22 (2-3): 143] etc. can find out: the method apparatus expensive, cycle is long, tabular alumina by hydrothermal method preparation has thin hexagon sheet structure but exists particle diameter too small, radius-thickness ratio is little, and form easily twin and crystal reunion, dispersed relatively poor in water; [JP Pat, clear 61-295208/1986] and the powder impurity that obtains of [EP0236952A2/ 1987] report coating method few, the smooth surface of sheet, the various parameters of sheet (such as size, thickness, chemical constitution etc.) also are easy to control on technique, but the powder machinery intensity of gained is not high, particle size distribution is wider, needs stage treatment just can reach user's requirement; The mechanical process of [US3121623/1964] [CN194100796/1994] report is simple to operate, cost is low, but the powder purity that makes is low, have a considerable amount of broken platelets, and because mechanical force causes the variation of grain pattern and physicochemical property to make crystalline structure wayward; Molten-salt growth method is the most frequently used method of synthesizing flaky aluminum oxide, [Commun Am Ceram Soc, 2007,90:4070] [investigation of materials journal, 2008,22:205] existing a large amount of reports such as [US5296085/1994] [US5702519/1996] [CN101941728 B/2012] [CN101691302 B/2012], the tabular alumina technical process is complicated, energy consumption is high, cost is large but molten-salt growth method prepares, impurity is high, the shortcomings such as the tabular alumina that the tabular alumina of preparation has the hexagonal form also exists particle diameter little, and radius-thickness ratio is little; In addition, the indirect preparation method of liquid phase also is proved to be a kind of more feasible method, [the J Am Cer am Soc such as Richard F. Hill, 2001,84 (3): 514] take boehmite and hydrofluoric acid as raw material, prepare diameter greater than the sheet α of 25um-Al by colloidal sol-gel method at 1100 ℃
2O
3, Zhou Zhenjun etc. [silicate circular, 2003,22 (4): 11] on this basis, AlF in the pH value by control colloidal sol and the gel
3Content, having made diameter at 1100 ℃ of lower insulation 180min is tabular α-Al of 2um
2O
3, Wu etc. [Mater Lett, 2002,52 (2): 366] are with Al (NO
2)
39H
2O and NH
3H
2O solution is raw material, adopts high purity aluminium oxide ball milling original position to introduce crystal seed and interpolation ZnF
2, AlF
3Preparation technology, obtained the sheet α of median size＜50nm-Al
2O
3Coacervate, Chen Wei etc. [CN100594181C] mix hydrated aluminum oxide with polyoxyethylene glycol or polyvinyl alcohol water solution, calcining after dry, aluminum oxide and the aqueous solution that contains fluorochemical will be got, fluorochemical is adsorbed on the aluminum oxide, after drying 1200 ~ 1700 ℃ of calcinings, obtain the flaky alpha-alumina powder, the indirect preparation method of these liquid phases all relates to the multistep synthesis step, process is complicated, and has generally used fluorochemical in the report, does not take in actual applications counter-measure, the heating member of the hydrogen fluoride heavy corrosion sintering oven that sintering reaction is emitted enters in the air human body and surrounding environment is caused severe contamination.
Summary of the invention
The objective of the invention is the shortcoming that exists for present tabular alumina preparation method, provide that a kind of preparation process is simple, cost is low, the tabular alumina preparation method of safety and environmental protection, the tabular alumina radius-thickness ratio of preparation is large, and purity is high, good dispersity.
Goal of the invention of the present invention is achieved through the following technical solutions:
A kind of low cost of high dispersion flake aluminum oxide, pollution-free preparation method is characterized in that: first fluorochemical is placed the ceramic crucible inner bottom part, reinstall the hydrated aluminum oxide compound, the mass ratio of fluorochemical and hydrated aluminum oxide compound is 1:50 ~ 1:20, covers crucible cover; Then, with mud crucible is sealed oven dry; At last in retort furnace 1100 ~ 1300 ℃ the calcining 1 ~ 3 hour, directly obtain the high dispersion flake aluminum oxide.
Described hydrated aluminum oxide compound is a kind of in commercially available laminar aluminium hydroxide and the boehmite, diameter 0.2 ~ 2 um.
Described fluorochemical is AlF
3Or NH
4F.
Described mud is that a kind of and water in calcium carbonate, magnesiumcarbonate, calcium hydroxide, magnesium hydroxide and the white lime mixes.
Preparation method provided by the invention has following advantage:
1. preparation process is simple, and easily extension is produced, and cost is low;
2. prepared flaky alpha-alumina product diameter 5 ~ 10um, radius-thickness ratio is 5 ~ 10, good dispersity, pattern rule;
3. by fluorochemical being placed on alumina precursor bottom, and sealed crucible, fluorochemical is decomposed after F
-Ion is full of in the aluminum oxide slit gradually from the crucible bottom diffusion, makes the even oriented growth of aluminium oxide particles;
4. seal by calcium carbonate, magnesiumcarbonate, calcium hydroxide, magnesium hydroxide, white lime, the hydrogen fluoride that decomposites in the roasting process is absorbed substantially, forms stable Calcium Fluoride (Fluorspan) or magnesium fluoride, and can recycle, and makes whole process safety, and is pollution-free.
Description of drawings
Fig. 1 by in the embodiment of the invention 1 the electron scanning micrograph of employing raw material;
Fig. 2 by in the embodiment of the invention 2 the electron scanning micrograph of employing raw material;
Fig. 3 is the tabular alumina electron scanning micrograph that obtains in the embodiment of the invention 1;
Fig. 4 is the x-ray diffraction pattern of the tabular alumina that obtains in the embodiment of the invention 1;
Fig. 5 is the tabular alumina electron scanning micrograph that obtains in the embodiment of the invention 2.
Embodiment
Embodiment 1:
The 10g aluminum fluoride is placed the ceramic crucible inner bottom part, reinstall 500g hydroxide flake aluminium, particle size range 0.2 ~ 2um covers crucible cover; Then, the mud that mixes with white lime and water seals crucible, 80 ℃ of oven dry; At last 1100 ℃ of calcinings 3 hours in retort furnace obtain the tabular alumina product of high dispersive; Such as Fig. 1,3,4 are respectively the SEM photo of hydroxide flake aluminum feedstock, SEM photo and the XRD result of tabular alumina product, the result shows: the irregular hydroxide flake aluminium of pattern is after the present invention processes, obtain diameter 5 ~ 10um, the hexagonal plate Alpha-alumina of radius-thickness ratio 5 ~ 10, high dispersive, pattern rule.
Embodiment 2:
The 20g aluminum fluoride is placed the ceramic crucible inner bottom part, reinstall 400g sheet boehmite, particle size range 0.5 ~ 2um covers crucible cover; Then, the mud that mixes with calcium carbonate and water seals crucible, 80 ℃ of oven dry; At last in retort furnace 1300 ℃ the calcining 1 hour, obtain the tabular alumina product of high dispersive, such as Fig. 2,5 are respectively the SEM photo of sheet boehmite raw material and the SEM photo of tabular alumina product, the result shows: undersized sheet boehmite is after the present invention processes, obtain diameter 5 ~ 10um, the hexagonal plate Alpha-alumina of radius-thickness ratio 5 ~ 10, high dispersive, pattern rule.
Claims (5)
1. the low cost of a high dispersion flake aluminum oxide, pollution-free preparation method, it is characterized in that: first fluorochemical is placed the ceramic crucible inner bottom part, reinstall the hydrated aluminum oxide compound, the mass ratio of fluorochemical and hydrated aluminum oxide compound is 1:50 ~ 1:20, covers crucible cover; Then, with mud crucible is sealed oven dry; At last in retort furnace 1100 ~ 1300 ℃ the calcining 1 ~ 3 hour, directly obtain the high dispersion flake aluminum oxide.
2. the low cost of a kind of high dispersion flake aluminum oxide as claimed in claim 1, pollution-free preparation method is characterized in that: described hydrated aluminum oxide compound is a kind of in commercially available laminar aluminium hydroxide and the boehmite, diameter 0.2 ~ 2 um.
3. the low cost of a kind of high dispersion flake aluminum oxide as claimed in claim 1, pollution-free preparation method, it is characterized in that: described fluorochemical is AlF
3Or NH
4F.
4. the low cost of a kind of high dispersion flake aluminum oxide as claimed in claim 1, pollution-free preparation method, it is characterized in that: described mud is that a kind of and water in calcium carbonate, magnesiumcarbonate, calcium hydroxide, magnesium hydroxide and the white lime mixes.
5. the low cost of a kind of high dispersion flake aluminum oxide as claimed in claim 1, pollution-free preparation method, it is characterized in that: described high dispersion flake aluminum oxide is product diameter 5 ~ 10um, radius-thickness ratio is 5 ~ 10, good dispersity, the hexagonal plate aluminum oxide of pattern rule.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553096A (en) * | 2013-10-28 | 2014-02-05 | 郑州玉发精瓷科技有限公司 | Preparation method of tabular corundum phase aluminum oxide powder for electronic material polishing |
| CN103936044A (en) * | 2014-02-26 | 2014-07-23 | 贵州万方铝化科技开发有限公司 | Method for efficiently recycling fluoride in aluminum-containing compound preparation process |
| CN107722149A (en) * | 2017-11-16 | 2018-02-23 | 四川金核高分子材料有限公司 | A kind of ptfe micropowder and preparation method thereof |
| CN108560052A (en) * | 2018-04-26 | 2018-09-21 | 闽江学院 | A kind of preparation method and applications of six side's aluminium oxide of monocrystalline |
| CN110924234A (en) * | 2019-11-25 | 2020-03-27 | 浙江华丰纸业科技有限公司 | Printing two-section cigarette paper and preparation method thereof |
| CN114057505A (en) * | 2021-12-13 | 2022-02-18 | 西安邮电大学 | Preparation method of porous flaky alumina framework |
| CN115536369A (en) * | 2022-10-18 | 2022-12-30 | 湖北晶耐新材料有限公司 | Preparation method of self-toughening alumina ceramic material |
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| CN1050366A (en) * | 1989-09-21 | 1991-04-03 | 阿托化学公司 | Big xln of the Alpha-alumina of wafer form and method for making thereof |
| US5702519A (en) * | 1995-09-14 | 1997-12-30 | Merck Patent Gesellschaft Mit Ceschrankter Haftung | Flaky aluminum oxide and pearlescent pigment, and production thereof |
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2012
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| CN1050366A (en) * | 1989-09-21 | 1991-04-03 | 阿托化学公司 | Big xln of the Alpha-alumina of wafer form and method for making thereof |
| US5702519A (en) * | 1995-09-14 | 1997-12-30 | Merck Patent Gesellschaft Mit Ceschrankter Haftung | Flaky aluminum oxide and pearlescent pigment, and production thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103553096A (en) * | 2013-10-28 | 2014-02-05 | 郑州玉发精瓷科技有限公司 | Preparation method of tabular corundum phase aluminum oxide powder for electronic material polishing |
| CN103553096B (en) * | 2013-10-28 | 2015-02-11 | 郑州玉发精瓷科技有限公司 | Preparation method of tabular corundum phase aluminum oxide powder for electronic material polishing |
| CN103936044A (en) * | 2014-02-26 | 2014-07-23 | 贵州万方铝化科技开发有限公司 | Method for efficiently recycling fluoride in aluminum-containing compound preparation process |
| CN103936044B (en) * | 2014-02-26 | 2015-09-23 | 贵州天合国润高新材料科技有限公司 | Prepare efficient circulation in the process of aluminum contained compound and utilize the method for fluorochemical |
| CN107722149A (en) * | 2017-11-16 | 2018-02-23 | 四川金核高分子材料有限公司 | A kind of ptfe micropowder and preparation method thereof |
| CN108560052A (en) * | 2018-04-26 | 2018-09-21 | 闽江学院 | A kind of preparation method and applications of six side's aluminium oxide of monocrystalline |
| CN110924234A (en) * | 2019-11-25 | 2020-03-27 | 浙江华丰纸业科技有限公司 | Printing two-section cigarette paper and preparation method thereof |
| CN110924234B (en) * | 2019-11-25 | 2022-04-08 | 浙江华丰纸业科技有限公司 | Printing two-section cigarette paper and preparation method thereof |
| CN114057505A (en) * | 2021-12-13 | 2022-02-18 | 西安邮电大学 | Preparation method of porous flaky alumina framework |
| CN114057505B (en) * | 2021-12-13 | 2023-02-28 | 西安邮电大学 | Preparation method of porous flaky alumina framework |
| CN115536369A (en) * | 2022-10-18 | 2022-12-30 | 湖北晶耐新材料有限公司 | Preparation method of self-toughening alumina ceramic material |
| CN115536369B (en) * | 2022-10-18 | 2023-09-26 | 湖北晶耐新材料有限公司 | Preparation method of self-toughening alumina ceramic material |
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Application publication date: 20130213 |