CN102617119A - Method for reshaping small-granularity alumina power - Google Patents
Method for reshaping small-granularity alumina power Download PDFInfo
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- CN102617119A CN102617119A CN2012100883725A CN201210088372A CN102617119A CN 102617119 A CN102617119 A CN 102617119A CN 2012100883725 A CN2012100883725 A CN 2012100883725A CN 201210088372 A CN201210088372 A CN 201210088372A CN 102617119 A CN102617119 A CN 102617119A
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Abstract
The invention relates to a method for reshaping small-granularity alumina power. The small-granularity alumina power is characterized in that alumina in China in the prior art meets the granularity required by tri-phosphor fluorescent powder, and the alumina subjected to air flow pulverization is graded to generate small parts of small-granularity power. The granularity of the power is generally between 0.8mum and 3.0mum. Through the specific re-calcination method, the granularity of the small-granularity alumina can reach the requirement of serving as tri-phosphor fluorescent powder raw materials. The product quality influence caused by adding the small-granularity alumina power into normal-granularity powder is avoided, or the production cost increase caused by secondary product formation is avoided.
Description
Technical field
The alumina powder jointed method that reshapes of small grain size belongs to the aluminum oxide powder preparing technical field.
Background technology
The required aluminum oxide grain size D50 of present domestic three primary colors fluorescent powder generally is controlled between 4.0～7.0 μ m, but present domestic aluminum oxide will meet the required granularity of three primary colors fluorescent powder, all will pass through comminution by gas stream basically; Aluminum oxide after the pulverizing can produce the powder of small portion small grain size through classification, all can discharging in bagroom, and the granularity D50 of this part powder is generally between 0.8～3.0 μ m; If add this part small grain size powder in the powder of normal particle sizes, can influence size-grade distribution, thereby influence quality product; If do not add; Just form seconds, can not be used on the fluorescent material, cause production cost to increase.The present invention becomes powder to make it can reach production requirement through the reprocessing to this part small grain size aluminum oxide again, cuts the waste.
Summary of the invention
The technical problem that the present invention will solve is: overcome the deficiency of prior art, provide a kind of and can make behind the comminution by gas stream or the alumina powder jointed alumina powder jointed method that reshapes of the small grain size that meets the required size-grade distribution of three primary colors fluorescent powder that becomes of small grain size that alternate manner causes.
For overcoming the problem that prior art causes, the present invention proposes the alumina powder jointed method that reshapes of a kind of small grain size, and the small grain size aluminum oxide powder is become powder again, makes its size-grade distribution can reach the requirement of making the three primary colors fluorescent powder raw material.
The process step of this method is:
1, mixing of materials: mix by weight 1: 3～6 with deionized water small grain size is alumina powder jointed, add little additive and fall LMP, said additive is ammonium chloride and mebor or Neutral ammonium fluoride and mebor;
2, material is handled: adopt pressurized air to stir 20～60min, separate through plate-and-frame filter press, water cut is controlled at 20～40%;
3, reshape: after press filtration separates with drying materials; Oven dry back material is calcined again, and calcining temperature is 1000～1400 ℃, obtains the aluminum oxide powder of granularity D50=4.0～7.0 μ m behind calcining 2～5h.
The powder of the small portion small grain size that the aluminum oxide of the alumina powder jointed finger comminution by gas stream of described small grain size produces through classification, discharging in bagroom, granularity D50=0.8～3.0 μ m's is alumina powder jointed.
The add-on of said ammonium chloride or Neutral ammonium fluoride is 0.2～1% of a deionized water weight.
The add-on of said boric acid is 1～5% of a deionized water weight.
Said bake out temperature is 100～200 ℃.
Preferably, small grain size is alumina powder jointed mixes by weight 1: 4～5 with deionized water.
Preferably, the pressurized air churning time is 40～50min; The separation time-division is dried up to be controlled at 30～35%.
Preferably, calcining temperature is 1100～1250 ℃, and calcination time is 3～4h.
Again become the aluminum oxide powder of powder as shown in the table through sample detection each item index according to the present invention:
Again become the aluminum oxide powder of powder to make the light-emitting data of green emitting phosphor according to the present invention
Data can be seen through the present invention and become the aluminum oxide of powder to satisfy the requirement of three primary colors fluorescent powder again from table, and the fluorescent material that the performance of the three primary colors fluorescent powder of working it out is worked it out than normal particle sizes powder in relative brightness is good.
Description of drawings
Fig. 1 makes the SEM photo of aluminum oxide powder for present method satisfies condition down.Product brightness as can be seen from the figure of the present invention is higher, and the particle median size is about 6 μ m, and the intergranular space is less, arranges closely knit.
Embodiment
Embodiment 1
The alumina powder jointed method practical implementation that reshapes of small grain size is following:
1, gets small grain size high purity alumina powder 100kg, add the 500kg ionized water.
2, the boric acid that adds 3.5kg ammonium chloride and 15kg.
3, the pressurized air of the material for preparing more than the general under 0.2Mpa pressure stirs 50min.
4, separate with plate-and-frame filter press after stirring is accomplished, separate moisture controlled about 30%.
5, separate after through 100～200 ℃ of oven dry.
6, oven dry back material is calcined 4h after 1200 ℃.
After detecting calcining, obtain aluminum oxide powder granularity: D10,4.46 μ m; D50,6.23 μ m; D90,14.81 μ m.
Embodiment 2
The alumina powder jointed method practical implementation that reshapes of small grain size is following:
1, gets small grain size high purity alumina powder 100kg, add the 300kg ionized water.
2, the boric acid that adds 0.6kg ammonium chloride and 3kg.
3, the pressurized air of the material for preparing more than the general under 0.2Mpa pressure stirs 20min.
4, separate with plate-and-frame filter press after stirring is accomplished, separate moisture controlled about 20%.
5, separate after through 100～120 ℃ of oven dry.
6, oven dry back material is calcined 2h after 1100 ℃.
After detecting calcining, obtain aluminum oxide powder granularity: D10,3.47 μ m; D50,6.12 μ m; D90,12.98 μ m.
Embodiment 3
The alumina powder jointed method practical implementation that reshapes of small grain size is following:
1, gets small grain size high purity alumina powder 100kg, add the 600kg ionized water.
2, the boric acid that adds 6kg ammonium chloride and 30kg.
3, the pressurized air of the material for preparing more than the general under 0.2Mpa pressure stirs 60min.
4, separate with plate-and-frame filter press after stirring is accomplished, separate moisture controlled about 40%.
5, separate after through 180～200 ℃ of oven dry.
6, oven dry back material is calcined 5h after 1250 ℃.
After detecting calcining, obtain aluminum oxide powder granularity: D10,3.86 μ m; D50,6.28 μ m; D90,14.46 μ m.
Embodiment 4
The alumina powder jointed method practical implementation that reshapes of small grain size is following:
1, gets small grain size high purity alumina powder 100kg, add the 450kg ionized water.
2, the boric acid that adds 2.7kg ammonium chloride and 13.5kg.
3, the pressurized air of the material for preparing more than the general under 0.2Mpa pressure stirs 40min.
4, separate with plate-and-frame filter press after stirring is accomplished, separate moisture controlled about 30%.
5, separate after through 140～160 ℃ of oven dry.
6, oven dry back material is calcined 4h after 1175 ℃.
After detecting calcining, obtain aluminum oxide powder granularity: D10,3.64 μ m; D50,6.18 μ m; D90,13.42 μ m.
Embodiment 5
The alumina powder jointed method practical implementation that reshapes of small grain size is following:
1, gets small grain size high purity alumina powder 100kg, add the 300kg ionized water.
2, the boric acid that adds 0.6kg Neutral ammonium fluoride and 3kg.
3, the pressurized air of the material for preparing more than the general under 0.2Mpa pressure stirs 20min.
4, separate with plate-and-frame filter press after stirring is accomplished, separate moisture controlled about 20%.
5, separate after through 100～120 ℃ of oven dry.
6, oven dry back material is calcined 2h after 1100 ℃.
After detecting calcining, obtain aluminum oxide powder granularity: D10,3.45 μ m; D50,6.14 μ m; D90,13.02 μ m.
Embodiment 6
The alumina powder jointed method practical implementation that reshapes of small grain size is following:
1, gets small grain size high purity alumina powder 100kg, add the 500kg ionized water.
2, the boric acid that adds 6kg Neutral ammonium fluoride and 30kg.
3, the pressurized air of the material for preparing more than the general under 0.2Mpa pressure stirs 45min.
4, separate with plate-and-frame filter press after stirring is accomplished, separate moisture controlled about 30%.
5, separate after through 140～160 ℃ of oven dry.
6, oven dry back material is calcined 4h after 1175 ℃.
After detecting calcining, obtain aluminum oxide powder granularity: D10,3.48 μ m; D50,6.25 μ m; D90,13.63 μ m.
Embodiment 7
The alumina powder jointed method practical implementation that reshapes of small grain size is following:
1, gets small grain size high purity alumina powder 100kg, add the 450kg ionized water.
2, the boric acid that adds 2.7kg Neutral ammonium fluoride and 13.5kg.
3, the pressurized air of the material for preparing more than the general under 0.2Mpa pressure stirs 40min.
4, separate with plate-and-frame filter press after stirring is accomplished, separate moisture controlled about 30%.
5, separate after through 140～160 ℃ of oven dry.
6, oven dry back material is calcined 4h after 1200 ℃.
After detecting calcining, obtain aluminum oxide powder granularity: D10,3.52 μ m; D50,6.20 μ m; D90,13.87 μ m.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any professional and technical personnel of being familiar with possibly utilize the technology contents of above-mentioned announcement to change or be modified as the equivalent embodiment of equivalent variations.But everyly do not break away from technical scheme content of the present invention, to any simple modification, equivalent variations and remodeling that above embodiment did, still belong to the protection domain of technical scheme of the present invention according to technical spirit of the present invention.
Claims (8)
1. the alumina powder jointed method that reshapes of small grain size is characterized in that, comprises following process step:
1.1, mixing of materials: mix by weight 1: 3～6 with deionized water small grain size is alumina powder jointed, add little additive and fall LMP, said additive is ammonium chloride and mebor or Neutral ammonium fluoride and mebor;
1.2, material handles: adopt pressurized air to stir 20～60min, separate through plate-and-frame filter press, water cut is controlled at 20～40%;
1.3, reshape: after press filtration separates with drying materials; Oven dry back material is calcined again, and calcining temperature is 1000～1400 ℃, obtains the aluminum oxide powder of granularity D50=4.0～7.0 μ m behind calcining 2～5h.
2. the alumina powder jointed method that reshapes of small grain size according to claim 1; It is characterized in that the powder of the aluminum oxide of the alumina powder jointed finger comminution by gas stream of small grain size described in the process step 1.1 through the small portion small grain size of classification generation; Discharging in bagroom, granularity D50=0.8～3.0 μ m's is alumina powder jointed.
3. the alumina powder jointed method that reshapes of small grain size according to claim 1, its characteristic are mixed by weight 1: 4～5 with deionized water in that small grain size described in the process step 1.1 is alumina powder jointed.
4. the alumina powder jointed method that reshapes of small grain size according to claim 1, the add-on that it is characterized in that ammonium chloride described in the process step 1.1 or Neutral ammonium fluoride is 0.2～1% of a deionized water weight.
5. the alumina powder jointed method that reshapes of small grain size according to claim 1, the add-on that it is characterized in that boric acid described in the process step 1.1 is 1～5% of a deionized water weight.
6. the alumina powder jointed method that reshapes of small grain size according to claim 1 is characterized in that the pressurized air churning time is 40～50min in the process step 1.2; The separation time-division is dried up to be controlled at 30～35%.
7. the alumina powder jointed method that reshapes of small grain size according to claim 1 is characterized in that calcining temperature is 1100～1250 ℃ in the process step 1.3, and calcination time is 3～4h.
8. the alumina powder jointed method that reshapes of small grain size according to claim 1 is characterized in that bake out temperature described in the process step 1.3 is 100～200 ℃.
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| CN2012100883725A CN102617119A (en) | 2012-03-30 | 2012-03-30 | Method for reshaping small-granularity alumina power |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076732A (en) * | 1992-03-25 | 1993-09-29 | 兰州电瓷厂 | The method of purification that contains the commercial alumina waste residue |
| WO2003055803A2 (en) * | 2001-12-27 | 2003-07-10 | Showa Denko K.K. | Particulate alumina, method for producing particulate alumina and composition containing particulate alumina |
| CN1686807A (en) * | 2005-05-18 | 2005-10-26 | 中国铝业股份有限公司 | Method for preparing alpha-Al2O3 from dust powder collected by electricity |
| CN1830789A (en) * | 2006-03-10 | 2006-09-13 | 潮州三环（集团）股份有限公司 | Preparation method of ultrafine alpha-Al2O3 powder and obtained product |
-
2012
- 2012-03-30 CN CN2012100883725A patent/CN102617119A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076732A (en) * | 1992-03-25 | 1993-09-29 | 兰州电瓷厂 | The method of purification that contains the commercial alumina waste residue |
| WO2003055803A2 (en) * | 2001-12-27 | 2003-07-10 | Showa Denko K.K. | Particulate alumina, method for producing particulate alumina and composition containing particulate alumina |
| CN1686807A (en) * | 2005-05-18 | 2005-10-26 | 中国铝业股份有限公司 | Method for preparing alpha-Al2O3 from dust powder collected by electricity |
| CN1830789A (en) * | 2006-03-10 | 2006-09-13 | 潮州三环（集团）股份有限公司 | Preparation method of ultrafine alpha-Al2O3 powder and obtained product |
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Application publication date: 20120801 |