CN1861743A - Surface organic film coating process of long afterglow luminescent powder of alkaline earth aluminate - Google Patents
Surface organic film coating process of long afterglow luminescent powder of alkaline earth aluminate Download PDFInfo
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- CN1861743A CN1861743A CN 200610019317 CN200610019317A CN1861743A CN 1861743 A CN1861743 A CN 1861743A CN 200610019317 CN200610019317 CN 200610019317 CN 200610019317 A CN200610019317 A CN 200610019317A CN 1861743 A CN1861743 A CN 1861743A
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Abstract
A coating method of organic membrane made by long-after glow phosphor alkali soil aluminates powder, the characteristic of it is that: it is modified by silicon alkyl resin acceptor MAPS, then it is connected by the methenyl-methyl acrylate MMA, at last the composite MAPS/MMA modified phosphor powders are finished. The affective result of this invention is that: the preparation method is simple, the cost is low, and it is suitable to the industry produce. The phosphor powders are coated by MAPS/MMA not only can improve the water-resistant ability, and also it can increase the consistent ability between the powders and the organic mediator, and the phosphor ability of the powder can not be impaired.
Description
Technical field
The present invention relates to a kind of long afterglow luminescent powder of alkaline earth aluminate surface organic film coating process.
Background technology
Alkaline earth aluminate persistent luminescent material generally adopts high temperature solid-state method synthetic, grinds to form fines through the ball milling operation, thereby has higher specific surface area, when contacting with water, can hydrolysis reaction take place slowly, system pH is raise, generate aluminum hydroxide precipitation simultaneously.So not only gone bad the crystalline structure of material, reduced the long-persistence luminous characteristic of powder, influenced the acid base equilibrium of system again, thereby greatly limited the application of luminescent material in water-based system.In addition, luminescent powder often is applied to fields such as coating, printing ink and plastics as luminous pigment, material is carried out organic surface-coating handle, but not only protecting materials is avoided the erosion of water or chemical, also can improve the consistency of luminescent powder and organic system.At present, the long afterglow luminescent powder of alkaline earth aluminate surface coating modification mainly contains two kinds of inorganic coating modification and organic coating modifications, though inorganic coating modification can improve the water resistance of powder, products obtained therefrom and organic medium consistency are poor.
Summary of the invention
The purpose of this invention is to provide a kind of long afterglow luminescent powder of alkaline earth aluminate surface organic film coating process.
The present invention is achieved like this, and carries out modification with silane coupling agent X-methacryloyl one oxygen oxypropyl trimethyl silane (MAPS) earlier, and then grafting methyl methacrylate (MMA), finally obtains the composite modified luminescent powder of MAPS/MMA.When silane coupling agent MAPS carries out modification, with SrAl
2O
4: Eu
2+, Dy
3+Luminescent powder join in an amount of dehydrated alcohol (luminescent powder: ethanol=1: 4～6), ultrasonic dispersing 30 minutes.Add the silane coupling agent MAPS account for luminescent powder quality 1.0～3.0% then, with the sulphuric acid soln of 1mol/l pH value being transferred to is 1, moves in the thermostat water bath, reacts 2～6 hours at 60～100 ℃ times.After finishing, reaction carries out suction filtration, with standby behind the absolute ethanol washing 2 times.Get an amount of 50～100ml dimethylbenzene and put into the three-necked bottle that has reflux condensate device and agitator, feed the nitrogen deoxygenation.Add 0.5～1.0% Oxybenzene formyl (BPO), after stirring is dissolved it fully, add the SrAl that 10.0～20g handles through silane coupling agent MAPS
2O
4: Eu
2+, Dy
3+Luminescent powder, and make it to be uniformly dispersed, slowly splash into the MMA that accounts for luminescent powder weight 5～15% then stage by stage through dilution with toluene.Three-necked bottle is moved in the thermostat water bath, react 2～5h down for 80～120 ℃ in temperature.Reaction finishes the back suction filtration and removes removal xylene, uses absolute ethanol washing 2 times, puts into the vacuum drying oven Air drying 4～6 hours, can obtain the luminescent powder product of MAPS/MMA coating modification.
The invention has the beneficial effects as follows: technology is simple, and cost is low, is suitable for suitability for industrialized production.Not only can improve the water resistance of luminescent powder after MAPS/MMA coats, also can strengthen the consistency of luminescent powder and organic medium, not damage the long-persistence luminous performance of luminescent powder simultaneously.
Embodiment
Embodiment one, elder generation carry out modification with silane coupling agent MAPS, and then grafting methyl methacrylate MMA, finally obtain the composite modified luminescent powder of MAPS/MMA.When silane coupling agent MAPS carries out modification, with 10g SrAl
2O
4: Eu
2+, Dy
3+Luminescent powder joins in the 50g dehydrated alcohol, ultrasonic dispersing 30 minutes.Add the silane coupling agent MAPS account for luminescent powder quality 1.0% then, with the sulphuric acid soln of 1mol/l pH value being transferred to is 1, moves in the thermostat water bath, reacts 6 hours at 60 ℃ times.After finishing, reaction carries out suction filtration, with standby behind the absolute ethanol washing 2 times.Get 50ml dimethylbenzene and put into the three-necked bottle that has reflux condensate device and agitator, feed the nitrogen deoxygenation.Add 0.5% Oxybenzene formyl (BPO), after stirring is dissolved it fully, add the SrAl that 10.0g handles through silane coupling agent MAPS
2O
4: Eu
2+, Dy
3+Luminescent powder, and make it to be uniformly dispersed, slowly splash into the MMA that accounts for luminescent powder weight 5% then stage by stage through dilution with toluene.Three-necked bottle is moved in the thermostat water bath, react 5h down at certain 80～120 ℃.Reaction finishes the back suction filtration and removes removal xylene, uses absolute ethanol washing 2 times, puts into the vacuum drying oven Air drying 4 hours, can obtain the luminescent powder product of MAPS/MMA coating modification.
Embodiment two, elder generation carry out modification with silane coupling agent MAPS, and then grafting methyl methacrylate MMA, finally obtain the composite modified luminescent powder of MAPS/MMA.When silane coupling agent MAPS carries out modification, with 20g SrAl
2O
4: Eu
2+, Dy
3+Luminescent powder joins in the 120g dehydrated alcohol, ultrasonic dispersing 30 minutes.Add the silane coupling agent MAPS account for luminescent powder quality 2% then, with the sulphuric acid soln of 1mol/l pH value being transferred to is 1, moves in the thermostat water bath, reacts 4 hours at 80 ℃ times.After finishing, reaction carries out suction filtration, with standby behind the absolute ethanol washing 2 times.Get 80ml dimethylbenzene and put into the three-necked bottle that has reflux condensate device and agitator, feed the nitrogen deoxygenation.Add 1.0% Oxybenzene formyl (BPO), after stirring is dissolved it fully, add the SrAl that 15g handles through silane coupling agent MAPS
2O
4: Eu
2+, Dy
3+Luminescent powder, and make it to be uniformly dispersed, slowly splash into the MMA that accounts for luminescent powder weight 10% then stage by stage through dilution with toluene.Three-necked bottle is moved in the thermostat water bath, react 4h down for 100 ℃ in temperature.Reaction finishes the back suction filtration and removes removal xylene, uses absolute ethanol washing 2 times, puts into the vacuum drying oven Air drying 5 hours, can obtain the luminescent powder product of MAPS/MMA coating modification.
Embodiment three, elder generation carry out modification with silane coupling agent MAPS, and then grafting methyl methacrylate MMA, finally obtain the composite modified luminescent powder of MAPS/MMA.When silane coupling agent MAPS carries out modification, with 30g SrAl
2O
4: Eu
2+, Dy
3+Luminescent powder joins in the 120g dehydrated alcohol, ultrasonic dispersing 30 minutes.Add the silane coupling agent MAPS account for luminescent powder quality 3.0% then, with the sulphuric acid soln of 1mol/l pH value being transferred to is 1, moves in the thermostat water bath, reacts 2 hours at 100 ℃ times.After finishing, reaction carries out suction filtration, with standby behind the absolute ethanol washing 2 times.Get 100ml dimethylbenzene and put into the three-necked bottle that has reflux condensate device and agitator, feed the nitrogen deoxygenation.Add 1.0% Oxybenzene formyl (BPO), after stirring is dissolved it fully, add the SrAl that 20g handles through silane coupling agent MAPS
2O
4: Eu
2+, Dy
3+Luminescent powder, and make it to be uniformly dispersed, slowly splash into the MMA that accounts for luminescent powder weight 15% then stage by stage through dilution with toluene.Three-necked bottle is moved in the thermostat water bath, react 2h down for 120 ℃ in temperature.Reaction finishes the back suction filtration and removes removal xylene, uses absolute ethanol washing 2 times, puts into the vacuum drying oven Air drying 6 hours, can obtain the luminescent powder product of MAPS/MMA coating modification.
Claims (1)
1, a kind of long afterglow luminescent powder of alkaline earth aluminate surface organic film coating process is characterized in that: with SrAl
2O
4: Eu
2+, Dy
3+Luminescent powder joins in the dehydrated alcohol, luminescent powder: ethanol=1: 4～6, ultrasonic dispersing 30 minutes, add the silane coupling agent MAPS that accounts for luminescent powder quality 1.0～3.0% then, with the sulphuric acid soln of 1mol/l the pH value being transferred to is 1, move in the thermostat water bath, reacted 2～6 hours down at 60～100 ℃, carry out suction filtration after reaction finishes,, get 50～100ml dimethylbenzene and put into the three-necked bottle that has reflux condensate device and agitator with standby behind the absolute ethanol washing 2 times, feed the nitrogen deoxygenation, add 0.5～1.0% Oxybenzene formyl, after stirring is dissolved it fully, add the SrAl that 10.0～20g handles through silane coupling agent MAPS
2O
4: Eu
2+, Dy
3+Luminescent powder, and make it to be uniformly dispersed, slowly splash into the MMA that accounts for luminescent powder weight 5～15% then stage by stage through dilution with toluene, three-necked bottle is moved in the thermostat water bath, react 2～5h down for 80～120 ℃ in temperature; Reaction finishes the back suction filtration and removes removal xylene, uses absolute ethanol washing 2 times, puts into the vacuum drying oven Air drying 4～6 hours, can obtain the luminescent powder product of MAPS/MMA coating modification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610019317 CN1861743A (en) | 2006-06-09 | 2006-06-09 | Surface organic film coating process of long afterglow luminescent powder of alkaline earth aluminate |
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|---|---|---|---|
| CN 200610019317 CN1861743A (en) | 2006-06-09 | 2006-06-09 | Surface organic film coating process of long afterglow luminescent powder of alkaline earth aluminate |
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| CN1861743A true CN1861743A (en) | 2006-11-15 |
Family
ID=37389278
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440280B (en) * | 2008-12-12 | 2012-02-01 | 江苏博睿光电有限公司 | Surface-coated long-afterglow fluorescent powder and preparation method thereof |
| CN101486846B (en) * | 2009-02-16 | 2012-07-04 | 南京林业大学 | Method for improving compatibility of noctilucent powder in organic resin system |
| CN102899020A (en) * | 2012-10-25 | 2013-01-30 | 江苏博睿光电有限公司 | Silicate fluorescent powder for coating LED and coating method thereof |
| CN103589426A (en) * | 2013-11-08 | 2014-02-19 | 天津理工大学 | Preparation method of full-inorganic phosphor for near ultraviolet laser light conversion |
| CN106928999A (en) * | 2017-03-23 | 2017-07-07 | 江南大学 | The preparation method of photochromic adjustable warm colour light long afterglow luminous material |
| TWI610902B (en) * | 2015-08-28 | 2018-01-11 | 興亞玻璃股份有限公司 | Glass-covered photoluminescent material and method for producing glass-covered photoluminescent material |
| CN108059953A (en) * | 2017-11-24 | 2018-05-22 | 中国林业科学研究院木材工业研究所 | A kind of long-persistence luminous flexible nano cellulosic material, preparation method and applications |
| CN112080194A (en) * | 2020-08-14 | 2020-12-15 | 江苏固迈新材料技术有限公司 | Self-luminous pavement |
| CN113817458A (en) * | 2021-09-10 | 2021-12-21 | 贵州聚材科技有限公司 | Photoinduced energy storage luminescent powder coated with protective material and preparation method thereof |
| CN116144229A (en) * | 2023-02-17 | 2023-05-23 | 甘肃省交通科学研究院集团有限公司 | Acrylic acid-based weather-resistant energy storage self-luminous material for road and preparation method thereof |
| CN116814245A (en) * | 2023-07-07 | 2023-09-29 | 山东首明科技有限公司 | Composite material for manufacturing luminous plate and preparation method thereof |
-
2006
- 2006-06-09 CN CN 200610019317 patent/CN1861743A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440280B (en) * | 2008-12-12 | 2012-02-01 | 江苏博睿光电有限公司 | Surface-coated long-afterglow fluorescent powder and preparation method thereof |
| CN101486846B (en) * | 2009-02-16 | 2012-07-04 | 南京林业大学 | Method for improving compatibility of noctilucent powder in organic resin system |
| CN102899020A (en) * | 2012-10-25 | 2013-01-30 | 江苏博睿光电有限公司 | Silicate fluorescent powder for coating LED and coating method thereof |
| CN102899020B (en) * | 2012-10-25 | 2014-07-23 | 江苏博睿光电有限公司 | Silicate fluorescent powder for coating LED and coating method thereof |
| CN103589426A (en) * | 2013-11-08 | 2014-02-19 | 天津理工大学 | Preparation method of full-inorganic phosphor for near ultraviolet laser light conversion |
| TWI610902B (en) * | 2015-08-28 | 2018-01-11 | 興亞玻璃股份有限公司 | Glass-covered photoluminescent material and method for producing glass-covered photoluminescent material |
| CN106928999A (en) * | 2017-03-23 | 2017-07-07 | 江南大学 | The preparation method of photochromic adjustable warm colour light long afterglow luminous material |
| CN108059953A (en) * | 2017-11-24 | 2018-05-22 | 中国林业科学研究院木材工业研究所 | A kind of long-persistence luminous flexible nano cellulosic material, preparation method and applications |
| CN108059953B (en) * | 2017-11-24 | 2020-05-22 | 中国林业科学研究院木材工业研究所 | Long-afterglow luminous flexible nano-cellulose material, and preparation method and application thereof |
| CN112080194A (en) * | 2020-08-14 | 2020-12-15 | 江苏固迈新材料技术有限公司 | Self-luminous pavement |
| CN112080194B (en) * | 2020-08-14 | 2022-02-11 | 江苏固迈新材料技术有限公司 | Self-luminous pavement |
| CN113817458A (en) * | 2021-09-10 | 2021-12-21 | 贵州聚材科技有限公司 | Photoinduced energy storage luminescent powder coated with protective material and preparation method thereof |
| CN116144229A (en) * | 2023-02-17 | 2023-05-23 | 甘肃省交通科学研究院集团有限公司 | Acrylic acid-based weather-resistant energy storage self-luminous material for road and preparation method thereof |
| CN116814245A (en) * | 2023-07-07 | 2023-09-29 | 山东首明科技有限公司 | Composite material for manufacturing luminous plate and preparation method thereof |
| CN116814245B (en) * | 2023-07-07 | 2023-12-19 | 山东首明科技有限公司 | Composite material for manufacturing luminous plate and preparation method thereof |
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Open date: 20061115 |