CN104910902A - Surface treatment method of zinc-manganese silicate green fluorescent powder - Google Patents
Surface treatment method of zinc-manganese silicate green fluorescent powder Download PDFInfo
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- CN104910902A CN104910902A CN201510292760.9A CN201510292760A CN104910902A CN 104910902 A CN104910902 A CN 104910902A CN 201510292760 A CN201510292760 A CN 201510292760A CN 104910902 A CN104910902 A CN 104910902A
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Abstract
The invention provides a surface treatment method of zinc-manganese silicate green fluorescent powder. The method comprises the process steps of preparing a precursor solution, performing butyl titanate surface treatment and performing reduction repairing. According to the method provided by the invention, the zinc-manganese silicate green fluorescent powder is added into the precursor solution prepared from butyl titanate, diethanolamine, glycerol and ethanol, and the mixture is dried at 80-120 DEG C, then is burnt for 4-8 hours at 300-600 DEG C in a hydrogen atmosphere, and then is screened to obtain the fluorescent powder for surface treatment. The method provided by the invention has the advantages that the process steps are simple, the product is superior in degradation resistance and the like; and the method can be used for surface treatment of the synthesized zinc-manganese silicate green fluorescent powder.
Description
Technical field
The invention belongs to fluorescent material preparing technical field, be specifically related to a kind of surface treatment method of manganese zinc silicate green fluorescent powder.
Background technology
Since manganese zinc silicate green fluorescent powder in 1938 is applied in luminescent lamp, it is widely used in lighting field and display device as the green color component in three primary colors fluorescent powder.In recent years, along with the development in epoch, the night life of people is also more and more abundanter, and night, the neon light of flicker became an indispensable part in city, and manganese zinc silicate green fluorescent powder is the important component part of its Green neon light.Because the duration of service of neon light is longer, and change trouble, so its anti-light performance requriements that declines is very high, and wherein topmost light decay derives from the light decay of fluorescent material.At present, this type of fluorescent material sold in market is Japanese powder substantially, and the powder that exploitation has oneself intellecture property is badly in need of in China.The commercial manganese zinc silicate green fluorescent powder shortcoming that ubiquity powder dispersity is poor in the use procedure of neon light, resist degradation ability is low.How to prepare the dispersiveness had, the manganese zinc silicate green fluorescent powder of strong resist degradation ability become current be badly in need of solve technical problem.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of surface treatment method of manganese zinc silicate green fluorescent powder, can prepare dispersed better, the commercial manganese zinc silicate green fluorescent powder of resist degradation superior performance.
To achieve these goals, the technical solution used in the present invention is:
A surface treatment method for manganese zinc silicate green fluorescent powder, comprises the steps: step one, prepares precursor solution:
By butyl (tetra) titanate, diethanolamine, glycerol, ethanol according to 1.00g:(5.00-30.00) ml:(1.00-10.00) ml:(50.00-300.00) mixing of ml ratio, at 50-70 DEG C, dust technology is used to regulate ph value to be 2.00-3.50, stir 50-80 hour, be mixed with precursor solution;
Step 2, butyl (tetra) titanate surface treatment:
Manganese zinc silicate green fluorescent powder to be joined in step one in the made precursor solution got ready, in manganese zinc silicate green fluorescent powder add-on and precursor solution, the mass ratio of butyl (tetra) titanate is 100.00:(0.05-2.00), stir and obtain aqueous fluorescent material in 6-20 hour, by this aqueous fluorescent material dry 24-48 hour at 80-120 DEG C, form fluorescent material powder agglomates;
Step 3, reduction is repaired:
Fluorescent material powder agglomates drying formed afterwards crosses 100 mesh sieves, puts into alumina crucible, under pure hydrogen atmosphere, in 300-600 DEG C of calcination 4-8 hour, after cooling, fluorescent material is crossed 100 mesh sieves, obtains surface treatment product.
The described dust technology concentration for the preparation of precursor solution is 0.02-0.06mol/L.
In described step 3, pure hydrogen atmosphere refers to that hydrogen flowing quantity is 30.00-100.00 cube m/h.
Compared with prior art, because the present invention adopts distinctive precursor solution when surface treatment, then adopt hydrogen atmosphere calcination reparation, thus produce dispersed better, the commercial manganese zinc silicate green fluorescent powder of resist degradation superior performance.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment one
A surface treatment method for manganese zinc silicate green fluorescent powder, comprises the steps:
Step one, prepare precursor solution:
2.36g butyl (tetra) titanate is joined in 120.00ml ethanol, then adds 13.00ml diethanolamine and 3.00ml glycerol, stir, at 50 DEG C, working concentration is the nitric acid of 0.02mol/L, regulates ph value to be 2.10, continue stirring 50 hours, be mixed with precursor solution;
Step 2, butyl (tetra) titanate surface treatment:
236.00g manganese zinc silicate green fluorescent powder is joined in step one in the made precursor solution got ready, stir and obtain aqueous fluorescent material in 10 hours, by this aqueous fluorescent material at 120 DEG C dry 24 hours, form fluorescent material powder agglomates;
Step 3, reduction is repaired:
Fluorescent material powder agglomates drying formed afterwards crosses 100 mesh sieves, puts into alumina crucible, and under pure hydrogen atmosphere, hydrogen flowing quantity is 30.00 cubes ms/h, in 300 DEG C of calcinations 8 hours, after cooling, fluorescent material is crossed 100 mesh sieves, obtains surface treatment product.
Embodiment two
A surface treatment method for manganese zinc silicate green fluorescent powder, comprises the steps:
Step one, prepare precursor solution:
Joined in 5.60L ethanol by 56.00g butyl (tetra) titanate, then add 0.56L diethanolamine and 0.28L glycerol, stir, at 60 DEG C, working concentration is the nitric acid of 0.03mol/L, regulates ph value to be 2.5, continues stirring 56 hours, is mixed with precursor solution;
Step 2, butyl (tetra) titanate surface treatment:
3733.00g manganese zinc silicate green fluorescent powder is joined in step one in the made precursor solution got ready, stir and obtain aqueous fluorescent material in 12 hours, by this aqueous fluorescent material at 100 DEG C dry 36 hours, form fluorescent material powder agglomates;
Step 3, reduction is repaired:
Fluorescent material powder agglomates drying formed afterwards crosses 100 mesh sieves, puts into alumina crucible, and under pure hydrogen atmosphere, hydrogen flowing quantity is 35.00 cubes ms/h, in 600 DEG C of calcinations 4 hours, after cooling, fluorescent material is crossed 100 mesh sieves, obtains surface treatment product.
Embodiment three
A surface treatment method for manganese zinc silicate green fluorescent powder, comprises the steps:
Step one, prepare precursor solution:
100.00g butyl (tetra) titanate is joined in 10.00L ethanol, then adds 0.50L diethanolamine and 1.00L glycerol, stir, at 70 DEG C, working concentration is the nitric acid of 0.05mol/L, regulates ph value to be 2.80, continue stirring 60 hours, be mixed with precursor solution;
Step 2, butyl (tetra) titanate surface treatment:
5.00kg manganese zinc silicate green fluorescent powder is joined in step one in the made precursor solution got ready, stir and obtain aqueous fluorescent material in 12 hours, by this aqueous fluorescent material at 120 DEG C dry 48 hours, form fluorescent material powder agglomates;
Step 3, reduction is repaired:
Fluorescent material powder agglomates drying formed afterwards crosses 100 mesh sieves, puts into alumina crucible, and under pure hydrogen atmosphere, hydrogen flowing quantity is 70.00 cubes ms/h, in 500 DEG C of calcinations 8 hours, after cooling, fluorescent material is crossed 100 mesh sieves, obtains surface treatment product.
Embodiment four
A surface treatment method for manganese zinc silicate green fluorescent powder, comprises the steps:
Step one, prepare precursor solution:
Joined in 10.00L ethanol by 40.00g butyl (tetra) titanate, then add 0.5L diethanolamine and 0.32L glycerol, stir, at 70 DEG C, working concentration is the nitric acid of 0.05mol/L, regulates ph value to be 2.80, continues stirring 68 hours, is mixed with precursor solution;
Step 2, butyl (tetra) titanate surface treatment:
5.00kg manganese zinc silicate green fluorescent powder is joined in step one in the made precursor solution got ready, stir and obtain aqueous fluorescent material in 12 hours, by this aqueous fluorescent material at 120 DEG C dry 28 hours, form fluorescent material powder agglomates;
Step 3, reduction is repaired:
Fluorescent material powder agglomates drying formed afterwards crosses 100 mesh sieves, puts into alumina crucible, and under pure hydrogen atmosphere, hydrogen flowing quantity is 46.00 cubes ms/h, in 450 DEG C of calcinations 8 hours, after cooling, fluorescent material is crossed 100 mesh sieves, obtains surface treatment product.
Embodiment five
A surface treatment method for manganese zinc silicate green fluorescent powder, comprises the steps:
Step one, prepare precursor solution:
65.00g butyl (tetra) titanate is joined in 10.00L ethanol, then adds 0.50L diethanolamine and 1.00L glycerol, stir, at 70 DEG C, working concentration is the nitric acid of 0.03mol/L, regulates ph value to be 3.50, continue stirring 63 hours, be mixed with precursor solution;
Step 2, butyl (tetra) titanate surface treatment:
5.00kg manganese zinc silicate green fluorescent powder is joined in step one in the made precursor solution got ready, stir and obtain aqueous fluorescent material in 12 hours, by this aqueous fluorescent material at 120 DEG C dry 30 hours, form fluorescent material powder agglomates;
Step 3, reduction is repaired:
Fluorescent material powder agglomates drying formed afterwards crosses 100 mesh sieves, puts into alumina crucible, and under pure hydrogen atmosphere, hydrogen flowing quantity is 50.00 cubes ms/h, in 600 DEG C of calcinations 8 hours, after cooling, fluorescent material is crossed 100 mesh sieves, obtains surface treatment product.
Claims (3)
1. a surface treatment method for manganese zinc silicate green fluorescent powder, is characterized in that, comprises the steps:
Step one, prepare precursor solution:
By butyl (tetra) titanate, diethanolamine, glycerol, ethanol according to 1.00g:(5.00-30.00) ml:(1.00-10.00) ml:(50.00-300.00) mixing of ml ratio, at 50-70 DEG C, dust technology is used to regulate ph value to be 2.00-3.50, stir 50-80 hour, be mixed with precursor solution;
Step 2, butyl (tetra) titanate surface treatment:
Manganese zinc silicate green fluorescent powder to be joined in step one in the made precursor solution got ready, in manganese zinc silicate green fluorescent powder add-on and precursor solution, the mass ratio of butyl (tetra) titanate is 100.00:(0.05-2.00), stir and obtain aqueous fluorescent material in 6-20 hour, by this aqueous fluorescent material dry 24-48 hour at 80-120 DEG C, form fluorescent material powder agglomates;
Step 3, reduction is repaired:
Fluorescent material powder agglomates drying formed afterwards crosses 100 mesh sieves, puts into alumina crucible, under pure hydrogen atmosphere, in 300-600 DEG C of calcination 4-8 hour, after cooling, fluorescent material is crossed 100 mesh sieves, obtains surface treatment product.
2. the surface treatment method of manganese zinc silicate green fluorescent powder according to claim 1, is characterized in that, the described dust technology concentration for the preparation of precursor solution is 0.02-0.06mol/L.
3. the surface treatment method of manganese zinc silicate green fluorescent powder according to claim 1, is characterized in that, in described step 3, pure hydrogen atmosphere refers to that hydrogen flowing quantity is 30.00-100.00 cube m/h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040559A (en) * | 2019-12-25 | 2020-04-21 | 湖南航天三丰科工有限公司 | Water-based fluorescent paint and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1254739A (en) * | 1998-11-24 | 2000-05-31 | 中国科学院长春物理研究所 | Coated electrofluorescent powder and its coating method |
| CN1510102A (en) * | 2002-12-20 | 2004-07-07 | 殷忠梅 | Diolame fluorescent powder and preparing method thereof |
| CN102895965A (en) * | 2012-10-31 | 2013-01-30 | 辽宁大学 | Er<3+>: Y3Al5O12/TiO2 composite membrane and application thereof in catalytic degradation of organic dye |
| CN103022467A (en) * | 2011-09-28 | 2013-04-03 | 北京当升材料科技股份有限公司 | Lithium manganate material for surface treatment and preparation method thereof |
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- 2015-06-01 CN CN201510292760.9A patent/CN104910902A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1254739A (en) * | 1998-11-24 | 2000-05-31 | 中国科学院长春物理研究所 | Coated electrofluorescent powder and its coating method |
| CN1510102A (en) * | 2002-12-20 | 2004-07-07 | 殷忠梅 | Diolame fluorescent powder and preparing method thereof |
| CN103022467A (en) * | 2011-09-28 | 2013-04-03 | 北京当升材料科技股份有限公司 | Lithium manganate material for surface treatment and preparation method thereof |
| CN102895965A (en) * | 2012-10-31 | 2013-01-30 | 辽宁大学 | Er<3+>: Y3Al5O12/TiO2 composite membrane and application thereof in catalytic degradation of organic dye |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040559A (en) * | 2019-12-25 | 2020-04-21 | 湖南航天三丰科工有限公司 | Water-based fluorescent paint and preparation method thereof |
| CN111040559B (en) * | 2019-12-25 | 2021-09-03 | 湖南航天三丰科工有限公司 | Water-based fluorescent paint and preparation method thereof |
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Application publication date: 20150916 |