CN1034921C - Producing process and device for high-purity ultra-fine aluminium oxide - Google Patents
Producing process and device for high-purity ultra-fine aluminium oxide Download PDFInfo
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- CN1034921C CN1034921C CN93110316A CN93110316A CN1034921C CN 1034921 C CN1034921 C CN 1034921C CN 93110316 A CN93110316 A CN 93110316A CN 93110316 A CN93110316 A CN 93110316A CN 1034921 C CN1034921 C CN 1034921C
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- kiln
- phase inversion
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- electric heating
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Abstract
The present invention relates to technology and a device for producing ultrafine aluminum oxide with high purity. The present invention has a continuous completion process that ammonium alum is decomposed to prepare gamma-Al2O3; then, the gamma-Al2O3 carries out phase inversion to prepare alpha-Al2O3. An electric heating pushed slab kiln is a device which is suitable for the technology. The ammonium alum is pushed into a kiln body by a material pushing device at definite time, and carries out preheating, dehydration, decomposition, phase inversion, cooling, and ultra-fine crushing, and then ultrafine aluminum oxide is prepared.
Description
The present invention relates to a kind of fine ceramics raw material---the production technique and the device of high-purity ultra-fine alumina.
High-purity ultra-fine alumina is a raw material of making the translucent ceramic tube of economize on electricity new type electro source-high-pressure mercury lamp, produces the method for high purity aluminium oxide with high-purity tschermigite pyrolysis.All adopt two-stage process both at home and abroad---intermittently unit operation is finished, and promptly tschermigite decomposes, γ-AL
2O
3Phase inversion carries out separately in decomposing furnace and phase inversion stove respectively, through the superfine grinding activation, makes high-purity superfine alumina powder again, and the main technique step is tschermigite → decomposition → phase inversion → coarse crushing → mixing → superfine grinding → mixing → packaging final prod.The technology of producing as domestic employing two-step approach is, the first step is decomposed, and contains in furnace pot or the crucible by alum with high-purity, carries out thermal dehydration in the chamber type electric resistance furnace of packing into and decomposes, and decomposition temperature is 1050 ℃, and constant temperature stops after 1～2 hour heating, and degradation production is γ-AL
2O
3, come out of the stove after allowing it naturally cool to room temperature.The second step phase inversion is with γ-AL
2O
3Pack into after sieving in the phase inversion stove.Progressively heat to 1200～1260 ℃, constant temperature 1～2 hour, γ-AL
2O
3Progressively phase inversion is α-AL
2O
3, stop heating, naturally cool to room temperature and come out of the stove, the back material powder of coming out of the stove sieves, and through the superfine grinding activation, just makes high-purity superfine alumina powder.Its AL
2O
3Content＞99.98%, granularity average out to 0.3～0.8 μ m.
" two-step approach " makes high-purity superfine alumina powder, operate loaded down with trivial details, decomposing furnace, phase inversion stove all will through intensification, temperature-fall period, the production cycle is long, the power consumption height.
The object of the present invention is to provide a kind of production technique and device of high-purity superfine alumina powder, simple to operate, with short production cycle, the low and constant product quality of power consumption.
The objective of the invention is to realize in the following way:
The high-purity ultra-fine alumina production technique is to be decomposed into γ-AL by tschermigite
2O
3, γ-AL
2O
3Phase inversion is α-AL
2O
3Form through superfine grinding, its technical characterstic is before superfine grinding again, and tschermigite is successively through following consecutive steps: be preheated to 200 ℃, 110～190 minutes, dewater 200～400 ℃, 70～120 minutes, decompose 400～1100 ℃, 80～140 minutes, 1200～1260 ℃ of phase inversions, 20～40 minutes, cooling.
A kind of device that is applicable to technology of the present invention---electric heating pushed bat kiln, comprise material puopulsion unit and kiln body, the material puopulsion unit comprises thruster, push pedal, crucible, kiln thorax bottom is equipped with frid, be divided into preheating section, dewatering period, decomposition section, phase inversion section, cooling section with temperature range in the kiln body, remove in each section of cooling section Heating element is housed, the different positions of kiln thorax is equipped with thermopair, and kiln body top has exhaust port.
Frid plays the track effect.Fill material in the crucible and place in the push pedal, thruster can adopt the leading screw thruster, is added with the time relay in the thruster motor circuit, and the self-timing propulsion functions is arranged, and push pedal enters in the kiln body, moves on frid.
Heating element, thermopair link to each other with electronic temperature controller, according to processing condition each section temperature in the kiln thorax are carried out automatic control.Each section kiln thorax one side has fixedly thermometric decorate thermopair.
Describe the present invention in detail below in conjunction with drawings and Examples:
Fig. 1 is the construction profile figure of electric heating pushed bat kiln;
Fig. 2 is each point for measuring temperature site plan of electric heating pushed bat kiln;
Fig. 3 is the A-A sectional view;
Fig. 4 is the B-B sectional view;
Fig. 5 produces the process flow diagram of high-purity superfine alumina powder for the hot pushed bat kiln of electricity consumption.
Among the figure: 1 crucible, 2 push pedals, 3 frids, 4 Heating elements---globars, 5 thrusters, 6 exhaust ports, 7 thermopairs, 8 kiln bodies, 9 shield caps.
The kiln body is made the insulation housing with high-alumina brick, light weeight alumina brick, vermiculite brick from inside to outside successively, and the kiln body is divided into preheating section, dewatering period, decomposition section, phase inversion section, cooling section successively, and each is intersegmental without obvious boundary, and the temperature of just controlling at each section is different.
Heater element adopts Elema, preheating section, dewatering period are temperature required low, in frid 3 bottoms the monolayer silicon carbon-point is housed radially, the temperature required height of phase inversion section also is heated evenly for ease of the material in the crucible, at the equal radially loading Elema in frid 3 bottoms and kiln thorax top, be parallel shape arranged side by side, decompose section and in frid 3 bottoms Elema is housed radially, according to the requirement of temperature conditions, can be at kiln thorax top also radially loading Elema.
Exhaust port 6 is located at kiln body top, connects tail gas discharge system. On the kiln body with protective cover 9.
Set fixedly point for measuring temperature at each section, as shown in Figure 2, set 6 points for measuring temperature, T1240℃、
T2900℃、T
31050℃、T
4、T
5、T
6Be 1200～1250 ℃, when temperature is higher than the point for measuring temperature temperature of setting, attemperating unit makes the heater element outage, and when temperature was not enough, attemperating unit made the heater element heat supply, and electronic temperature controller adopts the prior art that is comprised of thermometer, controllable silicon.
The chemical change that occurs at each section is:
Dewatering period: 200～400 ℃.
Decompose section: tschermigite, Tai-Ace S 150 decompose 400～1100 ℃
Phase inversion section: 1200～1260 ℃
γ-AL
2O
3＝α-AL
2O
3
Technical process is: fill high-purity crucible by alum, be positioned in the push pedal, regularly advanced by thruster, enter in the kiln thorax, in the preheating section preheating, dewatering period dehydration, decomposition section are decomposed the H that decomposites
2O, NH
3, SO
3Gas by exhaust port 6 through exhaust emissions system discharging, enter phase inversion section phase inversion after, through the cooling section cooling, by the discharge port kiln discharge, after coarse crushing, sieve, mixing, superfine grinding, mixing, packaging final prod.
Tschermigite periodicity is advanced automatically by thruster, and the push pedal cycle is relevant with the highest phase inversion temperature, and when the long timing of kiln, phase inversion temperature is high more, and the push pedal cycle is shorter, otherwise phase inversion temperature is low, and the push pedal cycle is long, and when push pedal cycle one timing, phase inversion temperature is high more, α-AL
2O
3Content high more, therefore can make the α-AL of different content according to different needs
2O
3High-purity superfine alumina powder.
Advantage of the present invention:
1, technology is tending towards rationally, and equipment is simple, and it is easy and simple to handle to take on material, saves time, laborsaving good operational environment;
2, economize on electricity, electric heating pushed bat kiln and batch furnace energy consumption compare:
(batch furnace refers to that decomposition, phase inversion two go on foot and carry out used decomposing furnace and phase inversion stove general name)
| Energy consumption of unit product (kwh/kg) | |
| Electric furnace intermittently | 93.0 |
| The electric heating pushed bat kiln | 68.5 |
By finding out in the table that pushed bat kiln is than batch furnace economize on electricity 26%.
3, stable and reliable product quality, the fine size activity is good, the translucent alumina ceramics pipe that the product that the present invention produces is made, its total light transmittance reaches 96%, and straight-line luminous transmittance reaches 8%.
Embodiment:
16 meters of electric heating pushed bat kiln length overalls, push pedal speed 60mm/ branch.
Preheating section accounts for 20% of length overall, and dewatering period accounts for 13% of length overall, and tschermigite Tai-Ace S 150 decomposes section and accounts for 15% of length overall, and the phase inversion section accounts for 4% of length overall, and cooling section accounts for 48% of length overall.
The push pedal cycle and the relation of high phase inversion temperature:
The highest phase inversion temperature of push pedal time
(branch/piece) (℃)
15 1240～1250
20 1235～1240
25 1230～1235
30 1225～1230
Charge 1.2～1.6kg in each crucible, be positioned in the push pedal, thruster regularly advances, the every every propelling of push pedal once traveled at the uniform speed 7 minutes in the kiln body, the material powder of (crucible is a periodic running in the kiln body) discharge port through coarse crushing, sieve, superfine grinding in the mixing, micronizer mill, mixing, packaging final prod.
Claims (4)
1, a kind of high-purity ultra-fine alumina production technique is to be decomposed into γ-AL by tschermigite
2O
3, γ-AL
2O
3Phase inversion is α-AL
2O
3, form through superfine grinding again, it is characterized in that before superfine grinding, tschermigite is successively through following successive processes, be preheated to 200 ℃, 110～190 minutes, dewater 200～400 ℃, 70～120 minutes, decompose 400～1100 ℃, 80～140 minutes, 1200～1260 ℃ of phase inversions, 20～40 minutes, cooling.
2, a kind of device that uses the described technology of claim 1---electric heating pushed bat kiln, it is characterized in that comprising material puopulsion unit and kiln body (8), the material puopulsion unit comprises thruster (5), push pedal (2), crucible (1), kiln thorax bottom is equipped with frid (3), be divided into preheating section, dewatering period, decomposition section, phase inversion section, cooling section with temperature range in the kiln body, remove in each section of cooling section Heating element (4) is housed, the different positions of kiln thorax is equipped with thermopair (7), and kiln body top has exhaust port (6).
3, electric heating pushed bat kiln according to claim 2, monolayer silicon carbon-point (4) radially is equipped with in frid (3) bottom that is characterised in that preheating section, dewatering period, monolayer silicon carbon-point (4) radially respectively is equipped with at frid (3) bottom and the kiln thorax top of decomposing section and phase inversion section, and each section kiln thorax one side has fixedly thermometric decorate thermopair.
4, electric heating pushed bat kiln according to claim 2 is characterised in that Heating element (4), thermopair (7) link to each other with electronic temperature controller.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110316A CN1034921C (en) | 1993-03-13 | 1993-03-13 | Producing process and device for high-purity ultra-fine aluminium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93110316A CN1034921C (en) | 1993-03-13 | 1993-03-13 | Producing process and device for high-purity ultra-fine aluminium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1092382A CN1092382A (en) | 1994-09-21 |
| CN1034921C true CN1034921C (en) | 1997-05-21 |
Family
ID=4988195
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93110316A Expired - Fee Related CN1034921C (en) | 1993-03-13 | 1993-03-13 | Producing process and device for high-purity ultra-fine aluminium oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1034921C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795650A (en) * | 2012-08-31 | 2012-11-28 | 福建鑫磊晶体有限公司 | Equipment and method for preparing gamma-Al2O3 through thermal decomposition of ammonium aluminum sulfate |
| CN102863000A (en) * | 2012-09-29 | 2013-01-09 | 浙江东晶光电科技有限公司 | Preparation method of high-purity aluminum oxide for growth of sapphire monocrystalline |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4377566A (en) * | 1980-07-01 | 1983-03-22 | Produits Chimiques Ugine Kuhlmann | Novel process for the preparation of high purity alumina from ammonium alum |
-
1993
- 1993-03-13 CN CN93110316A patent/CN1034921C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4377566A (en) * | 1980-07-01 | 1983-03-22 | Produits Chimiques Ugine Kuhlmann | Novel process for the preparation of high purity alumina from ammonium alum |
Non-Patent Citations (1)
| Title |
|---|
| 氧化铝生产工艺 R.W.Bartlete等 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1092382A (en) | 1994-09-21 |
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