CN1312042C - Method of preparing fibre powder body of nano alumina in high purity - Google Patents
Method of preparing fibre powder body of nano alumina in high purity Download PDFInfo
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- CN1312042C CN1312042C CNB2003101061288A CN200310106128A CN1312042C CN 1312042 C CN1312042 C CN 1312042C CN B2003101061288 A CNB2003101061288 A CN B2003101061288A CN 200310106128 A CN200310106128 A CN 200310106128A CN 1312042 C CN1312042 C CN 1312042C
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- alumina fiber
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- 239000000843 powder Substances 0.000 title claims abstract description 42
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000000835 fiber Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 30
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000004411 aluminium Substances 0.000 claims abstract description 26
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 14
- 238000007664 blowing Methods 0.000 claims abstract description 12
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000004090 dissolution Methods 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims description 15
- 230000004913 activation Effects 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 150000007522 mineralic acids Chemical class 0.000 abstract 1
- 238000010792 warming Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 241000024287 Areas Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000007073 chemical hydrolysis Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Images
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Fibers (AREA)
Abstract
The present invention relates to a method for preparing high purity nanometer alumina fiber powder. HV-1 catalysts are dissolved in distilled water, and the dissolution can be promoted by inorganic acid addition and slight warming. Metallic aluminium is soaked in the catalyst solution for 1 to 30 minutes to be activated, aluminum is extracted, and the aluminum surface is washed by distilled water to wash out surface impurities. Then, the metallic aluminium is put at an air blowing inlet and is blown by an air compressor. The aluminum is placed for several hours, and at the moment, the aluminium surface generates gas-solid reaction with oxygen in the air to generate nanometer alumina fiber. The fibrous alumina powder generated on the aluminum surface is collected, and the steps are repeated. Finally, the generated solid powder is calcined for 0.5 to 5 hours at the temperature of about 500 DEG C, the catalysts are evaporated into gas, and the catalysts and the powder can be separated with the catalysts recovered.
Description
One, technical field
The present invention relates to the preparation of high purity nanometer alumina fiber powder, especially utilize chemical gas-solid phase reaction method to produce the preparation method of high purity nanometer alumina fiber powder.
Two, background technology
Existing relate to the method that the high purity nanometer alumina preparation method adopts the chemical hydrolysis reactive crystallization more, starting material adopt titanium tetrachloride etc. more.As relate to the preparation of high purity nanometer alumina fiber powder, then need to adopt the technology of High Temperature High Pressure.Aforesaid method has certain pollution generally.High purity nanometer alumina fiber powder performance is better than spherical high purity nanometer alumina powder, and original purposes is arranged, and does not see the preparation method's that the high purity nanometer alumina fiber powder is arranged report.
Three, summary of the invention
The present invention seeks to: a kind of high purity nanometer alumina fiber powder preparation method is provided, especially utilizes chemical gas-solid phase reaction method to produce.
The object of the present invention is achieved like this:
1, with the HV-1 catalyst dissolution to distilled water, add mineral acid and heat slightly and can promote its dissolving.
2, metallic aluminium is soaked in above-mentioned catalyst solution carried out activation treatment in 1-30 minute, aluminium is taken out,, wash surface impurity off with its surface of distilled water flushing.
3, then aluminium is placed into the air-blowing air port, by air compressor to the metallic aluminium air-blowing.Place some hrs, this moment, the surface and the one solid reaction of airborne oxygen generation gas of aluminium generated nano-alumina fiber.Collect fibrous alumina powder jointed that the aluminium surface generates then, see accompanying drawing, repeat above-mentioned 1-3 step.
4, at last with the pressed powder that generates under 500 ℃ of left and right sides temperature, under the condition of logical protection gas roasting 0.5-5 hour.Catalyzer flashes to gas, can make wherein catalyzer and powder separation, and catalyzer is cool can be used after coagulating repeatedly.
Then as required, under＜950 ℃ of conditions, roasting can obtain the gama-alumina fiber powder of different nano-scales, at 1000 ℃ of left and right sides roasting temperature different times, can obtain the Alpha-alumina of different size.
5, final product packing.
Catalyzer is recycling after condensation.Catalyst solution behind the aluminium dipping needs in time to replenish new catalyzer.
Characteristics of the present invention are:
1, non-crystalline state high purity nanometer alumina fiber powder can generate under normal temperature condition fully.
2, by control heat treated temperature, temperature rise rate and constant temperature soaking time,, constant temperature 6-10 hour, can obtain polycrystalline gama-alumina nanometer fibre powder 500 ℃ of left and right sides temperature.
3, because have only the consumption of starting material aluminium in reaction process, catalyzer can be reused, and production cost is lower.
4, the productive rate height of product, yield rate reaches 98%, so remarkable in economical benefits.
The present invention is starting material with the rafifinal, in free of contamination environment, under normal temperature condition, pass through gas-solid phase reaction synthesis of nano fiber powder by activation, according to the market requirement, can produce product purity＞99.9 and＞99.99% fibrous high purity nanometer alumina powder, this product has high added value, and domestic still do not have a manufacturer.
Application Areas of the present invention is extensive: its surface-area of nano-alumina fiber is big, has stronger adsorptive power, the heavy metal ion in can being used for purifying waste water.Can be used as the toughener of matrix materials such as electronic ceramic substrate, ceramic fine filter, ceramic membrane and metal matrix, ceramic base, plastic base.Have stronger biological activity, can be used as catalyzer and support of the catalyst and catch new Application Areass such as virus.In traditional industries, high-purity, ultra-fine alumina is the important source material of optics monocrystalline and fine ceramics, rather well received in high-tech areas such as material, microelectronics and aerospace industries, be commonly used to make nose cone, antenna windows and the biological ceramics of using as rotor, piston, high-pressure sodium fluorescent tube, multilevel integration substrate, multi-layer capacitor, microwave device, laser apparatus, chemical sensor, guided missile window and satellite etc., its application prospect is very wide.
The present invention can obtain diameter at the gama-alumina fiber of 5-10 nanometer and the Alpha-alumina rod-shpaed particle about particle diameter 30 nanometers by controlling heat treated temperature, time and temperature rise rate.Comparison with other preparation method: the system of high purity nanometer alumina fiber powder respectively has: the simple to operation and control of 1 processing unit, energy consumption is low.Product purity is adjustable.The fiber powder color is pure white, and is mobile strong.Invert point between each phase reduces about 100 degree than traditional product.Production cost reduces.
Four, description of drawings
Fig. 1 is a process flow sheet of the present invention
Five, embodiment
To distilled water, the adding mineral acid reaches heats slightly with the HV-1 catalyst dissolution, and heating is no more than 40 ℃, can promote its dissolving.The concentration of catalyzer HV-1 is lower than at 3% o'clock and wants timely make-up catalyst at 3%-8%, and catalyzer is produced by rain profit nanosecond science and technology engineering center of Nanjing Nanjing University.
Fine aluminium soaks in above-mentioned catalyst solution and carried out activation treatment in 1-30 minute, and aluminium is taken out the back with its surface of distilled water flushing, washes surface impurity off.Then aluminium is placed into the air-blowing air port, by air compressor to the metallic aluminium air-blowing.The temperature that can also control air-blowing is to 35-40 ℃.The temperature of air-blowing is high more, and the time is just short, generally needs 10-60 minute.Placed then 1-10 hour, this moment, the surface and the one solid reaction of airborne oxygen generation gas of aluminium generated nano-alumina fiber.Collect fibrous alumina powder jointed that the aluminium surface generates with physical method then, repeat above-mentioned steps and gather a certain amount of work in-process.At last with the pressed powder that generates under 500 ℃ of left and right sides temperature, roasting 0.5-5 hour.Catalyzer flashes to gas, can make wherein catalyzer and powder separation, and catalyzer is cool can be used after coagulating repeatedly.
Then as required, under＜950 ℃ of conditions (generally 450-550 ℃ condition), roasting can obtain the gama-alumina fiber powder of different nano-scales, at 1000 ℃ of left and right sides roasting temperature different times, can obtain the Alpha-alumina of different size.
In the preparation process and high purity nanometer alumina fiber powder Performance Influence Factor
Several Factors below in the preparation process: temperature rise rate etc. influences diameter, length-to-diameter ratio and the intensity of sapphire whisker powder in activation treatment time, surface adsorption impurity, gas velocity, temperature of reaction, moisture and the heat treatment process.The activation treatment time is moderate, otherwise can increase raw-material loss.The purity of the impurity effect product of surface adsorption will be used distilled water and chemical pure above sulfuric acid or hydrochloric acid.With moisture removal, the existence of moisture makes that when thermal treatment process the sapphire whisker powder lumps seriously in heat treatment process with the method for air blast and hot blast, and forms part A lOOH, rather than pure aluminum oxide.Gas velocity has a significant impact the length and the intensity of fiber.Temperature rise rate is too fast in the heat treatment process just ruptures in the fiber crystallization process, forms nano particle.
Temperature rise rate in the heat treatment process:
Temperature rise rate generally is controlled in 100-150 ℃/hour the scope in heat treatment process, and when temperature rise rate surpasses 200 ℃/hour, fiber will be fractured into nano level particle in crystallization process, and its particle diameter is in the scope of 10-30 nanometer.
The influence of gas velocity
Gas velocity has a significant impact the length and the intensity of fiber.Gas velocity control will be regulated according to the amount of actual production aluminium.In general gas velocity is more little, and the particle diameter of fiber is thin more, and length is long more.But output is lower.
Heat treatment period
Heat treatment period is long more, and the crystallization degree of its fiber is high more.During as lower 450-550 ℃, constant temperature 6-10 hour, its fiber was converted into polycrystalline gama-alumina nanometer fibre powder fully.In the time of 950-1300 ℃, constant temperature 15-30 hour, it was converted into alpha-phase aluminum oxide fully.And its purity also improves a lot.Especially 950-1050 ℃ the time, better effects if.
Claims (5)
1, high purity nanometer alumina fiber powder preparation method is characterized in that the HV-1 catalyst dissolution to distilled water, adds mineral acid and heat slightly to promote its dissolving; Metallic aluminium soaked in above-mentioned catalyst solution carried out activation treatment in 1-30 minute, aluminium is taken out,, wash surface impurity off with its surface of distilled water flushing; Then aluminium is placed into the air-blowing air port, by air compressor to the metallic aluminium air-blowing; Place some hrs, this moment, the surface and the one solid reaction of airborne oxygen generation gas of aluminium generated nano-alumina fiber; Collect fibrous alumina powder jointed that the aluminium surface generates then, repeat above-mentioned steps; At last with the pressed powder that generates under the condition of 500 ℃ of left and right sides temperature, roasting 0.5-5 hour, catalyzer flashed to gas, made wherein catalyzer and powder separation, and reclaimed catalyzer.
2,, it is characterized in that in the time of 450-550 ℃ constant temperature 6-10 hour, its fiber was converted into polycrystalline gama-alumina nanometer fibre powder fully by the described high purity nanometer alumina fiber powder of claim 1 preparation method; Carry out roasting being lower than under 950 ℃ of temperature, obtain the gama-alumina fiber powder of different nano-scales.
3,, it is characterized in that temperature rise rate in the pressed powder roasting process is controlled in 100-150 ℃/hour the scope by claim 1 or 2 described high purity nanometer alumina fiber powder preparation methods.
4, by claim 1 or 2 described high purity nanometer alumina fiber powder preparation methods, it is characterized in that fine aluminium soaks in above-mentioned catalyst solution carried out activation treatment in 1-30 minute.
5, by claim 1 or 2 described high purity nanometer alumina fiber powder preparation methods, it is characterized in that aluminium is placed into the air-blowing air port, the temperature of air-blowing is to 35-40 ℃, the time 10-60 of air-blowing minute.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101061288A CN1312042C (en) | 2003-10-24 | 2003-10-24 | Method of preparing fibre powder body of nano alumina in high purity |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101061288A CN1312042C (en) | 2003-10-24 | 2003-10-24 | Method of preparing fibre powder body of nano alumina in high purity |
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| CN1539737A CN1539737A (en) | 2004-10-27 |
| CN1312042C true CN1312042C (en) | 2007-04-25 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100342966C (en) * | 2005-09-06 | 2007-10-17 | 南开大学 | Loaded palladium catalyst and preparing method and its use |
| US20080176075A1 (en) | 2007-01-15 | 2008-07-24 | Saint-Gobain Ceramics & Plastics, Inc. | Ceramic particulate material and processes for forming same |
| CN102311132B (en) * | 2010-07-07 | 2013-08-28 | 中国石油化工股份有限公司 | Rod-like one-dimensional polycrystalline gamma-Al2O3 nanocrystal grains and preparation method thereof |
| CN102491393B (en) * | 2011-12-14 | 2013-07-10 | 昆明马克西姆科技有限公司 | Method for preparing high-purity ultrafine Al2O3 powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034768A (en) * | 1987-11-23 | 1989-08-16 | 帝国化学工业公司 | Inorganic oxide fibres and manufacturing thereof |
| JPH0491225A (en) * | 1990-08-02 | 1992-03-24 | Taimei Kagaku Kogyo Kk | Polycrystalline alumina fiber and production thereof |
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2003
- 2003-10-24 CN CNB2003101061288A patent/CN1312042C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034768A (en) * | 1987-11-23 | 1989-08-16 | 帝国化学工业公司 | Inorganic oxide fibres and manufacturing thereof |
| JPH0491225A (en) * | 1990-08-02 | 1992-03-24 | Taimei Kagaku Kogyo Kk | Polycrystalline alumina fiber and production thereof |
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