CN108976609A - A kind of luminescent plastic to shine and energy storage effect is excellent - Google Patents
A kind of luminescent plastic to shine and energy storage effect is excellent Download PDFInfo
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- CN108976609A CN108976609A CN201810926617.4A CN201810926617A CN108976609A CN 108976609 A CN108976609 A CN 108976609A CN 201810926617 A CN201810926617 A CN 201810926617A CN 108976609 A CN108976609 A CN 108976609A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/774—Borates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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Abstract
The present invention relates to new function material technical fields, disclose a kind of luminescent plastic to shine and energy storage effect is excellent, centered on europium oxide, it is coated using cadmium oxide, carried magnetic iron oxide, obtained stable core-shell structure is as luminescent material, the good dispersion in polypropylene, performance is not damaged in extrusion, fluorescence intensity is high, it can excite and generate a large amount of quantum dot, light storage performance is high, it can adapt to environmental change, so that luminescent plastic luminous intensity and fluorescent lifetime are guaranteed, the luminous and excellent energy storage effect luminescent plastic that the present invention is prepared solves fluorescent powder used in existing luminescent plastic under adverse circumstances variation, the problem of causing the mechanical property of luminescent plastic and luminescent properties to be severely impacted, it can be realized the realistic meaning for improving luminescent material luminescent properties and extending luminescent plastic suitable application area , it is a kind of technical solution being extremely worth of widely use.
Description
Technical field
The invention belongs to new function material technical fields, and in particular to a kind of luminous modeling to shine and energy storage effect is excellent
Material.
Background technique
Luminescent plastic refers to the plastics that aobvious luminous effect is generated in dark or light.Not according to the luminous pigment being added
Together, and the different type such as self luminous plastic and stimulated luminescence plastics can be divided into.Luminescent plastic communication, optical information processing,
The optoelectronic areas such as video parts, measurement and control instrument, inorganic semiconductor electroluminescent device are widely applied, especially with complete
The development of ball letter highway more obtains fast development as the application of information terminal display device.Another application of luminescent plastic
Field is entirely lighting optical fiber.Entirely lighting optical fiber is the novel optic luminescence medium to grow up the 1990s, and
One Ge Xin branch of polymer optical fiber, it has also become the emerging high-tech product of this century decoration, Lighting Industry.Its main feature is that: light
Fine effective clear aperture is big, transmission range is long, long using safe life, energy saving, non-maintaining, pollution-free, in illumination, dress
The industries such as decorations, decoration, advertisement, medical treatment and measurement are applied.
Existing luminescent plastic is to be added to fluorescent powder in plastic master batch to carry out using and fluorescent powder is as luminescent material
Other than needing that there are excellent luminescent properties, it is also necessary to which the preparation process that can adapt to plastic products meets the use of plastics
Property.In fact, in luminescent plastic in use, will receive ultraviolet light irradiation, difference variation, hydro-thermal corrode etc. in environment, and glimmering
The luminescent properties of light powder are closely related with variations such as temperature, irradiation, weathers again, and rugged environment variation will cause luminescent plastic
Mechanical property and luminescent properties are severely impacted.And the energy storage effect of existing luminescent plastic is poor, and service life is short, effect
Rate is low.
Summary of the invention
The purpose of the present invention is providing a kind of luminescent plastic to shine and energy storage effect is excellent for existing problem,
Fluorescence intensity is high, can excite and generate a large amount of quantum dot, and light storage performance is high, can adapt to environmental change, so that luminescent plastic
Luminous intensity and fluorescent lifetime are guaranteed.
The present invention is achieved by the following technical solutions:
A kind of luminescent plastic to shine and energy storage effect is excellent, is made of following component: polypropylene 500-510 in parts by weight
Part, 35-40 parts of dihexyl phthalate, 24-28 parts of luminescent material, 10-12 parts of polyethylene wax, stearic acid pentaerythritol ester
3.5-4.0 parts, 1.4-1.6 parts of stearic amide, 0.6-0.8 parts of titanate coupling agent；The preparation method packet of the luminescent material
Include following steps:
(1) it weighs 5.5-6.0 grams of europium oxide to be placed in a beaker, 30-35 milliliters of concentrated nitric acids is added, are stirred to obtain transparent molten
Then the caddy aqueous solution that 10-12 milliliters of molar concentrations are 0.32-0.34 mol/L is added, at room temperature in liquid into beaker
Continuing magnetic force stir 60-70 minute, formation homogeneous mixture solotion, and by mixed solution in ultrasonic cleaner sonic oscillation 3-
5 minutes；
(2) 45-50 milliliters of hydrochloric acid solutions are added in three-necked flask, weigh 2.3-2.5 grams of pretreated ferroso-ferric oxide powder
End and 2.6-2.8 grams of Boratex are added in flask, add 10-15 milliliters of dehydrated alcohols, stirring and dissolving, heating water bath is extremely
40-45 DEG C, it is passed through nitrogen, reacts 40-50 minutes under oxygen-free environment, then adds the dispersion liquid being prepared in step (1)
Entering into three-necked flask, stirs evenly, water-bath is warming up to 85-90 DEG C, is stirred to react 1.0-1.5 hours, 3-4 hours are stood,
Obtain colloidal sol；
(3) colloidal sol that step (2) is prepared is transferred in Muffle furnace, preheats 1-2 hours at 160-180 DEG C, then rises
Temperature calcines 18-20 minutes to 560-600 DEG C, cools to room temperature with the furnace, and it is small to be placed in 70-80 DEG C of vacuum oven dry 6-8
When, it pulverizes.
It is further described as to above scheme, step (1) the concentrated nitric acid molar concentration is 13-15 mol/L.
It is further described as to above scheme, step (2) the hydrochloric acid solution pH value is between 3.8-4.0.
It is further described as to above scheme, the processing side of step (2) the pretreated ferroferric oxide powder
Method are as follows: by ferroferric oxide powder be added to 4-5 times of volume molar concentration be 0.15-0.18 mol/L hydrochloric acid solution in,
Ultrasonic disperse 10-15 minutes, filtering made to be washed with deionized to filtrate neutrality, filtrate is then placed in 6-8 times of volume
Dehydrated alcohol in, ultrasonic disperse 15-20 minutes at 3-5 DEG C, filter, it is dry.
It is further described as to above scheme, the luminescent material particle size that step (3) is prepared is received in 10-20
Between rice.
It is further described as to above scheme, the luminescent plastic extrusion temperature is 195-200 DEG C, and extrusion pressure is
3.6-3.8MPa。
The present invention is had the advantage that compared with prior art for bad, the energy storage effect that solves existing luminescent plastic luminescent properties
The problem of difference, the present invention provides a kind of luminous and excellent energy storage effect luminescent plastics to use oxidation centered on europium oxide
Cadmium cladding, carried magnetic iron oxide, obtained stable core-shell structure is as luminescent material, the good dispersion in polypropylene, squeezes
Middle performance is not damaged out, and fluorescence intensity is high, can excite and generate a large amount of quantum dot, and light storage performance is high, can adapt to environment
Variation, so that luminescent plastic luminous intensity and fluorescent lifetime are guaranteed, the luminous and energy storage effect that the present invention is prepared is excellent
Different luminescent plastic solves fluorescent powder used in existing luminescent plastic under adverse circumstances variation, causes the power of luminescent plastic
The problem of performance and luminescent properties are severely impacted, and light storage with higher, have taken into account luminescent properties and use
The promotion in service life improves the development and utilization of luminescent plastic, can be realized and improves luminescent material luminescent properties and extend luminous
The realistic meaning of plastics suitable application area is a kind of technical solution being extremely worth of widely use.
Specific embodiment
To make the purpose of the present invention, technical solution and effect clearer, clear and definite, combined with specific embodiments below to this hair
It is bright to be described further, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, is not used to limit
Technical solution provided by the present invention.
Embodiment 1
A kind of luminescent plastic to shine and energy storage effect is excellent, is made of following component in parts by weight: 500 parts of polypropylene,
35 parts of dihexyl phthalate, 24 parts of luminescent material, 10 parts of polyethylene wax, 3.5 parts of stearic acid pentaerythritol ester, stearic acid acyl
1.4 parts of amine, 0.6 part of titanate coupling agent；The preparation method of the luminescent material the following steps are included:
(1) 5.5 grams of europium oxides are weighed to be placed in a beaker, 30 milliliters of concentrated nitric acids are added, are stirred to obtain clear solution, then to
The caddy aqueous solution that 10 milliliters of molar concentrations are 0.32 mol/L is added in beaker, continuing magnetic force stirs 60 points at room temperature
Clock, formed homogeneous mixture solotion, and by mixed solution in ultrasonic cleaner sonic oscillation 3 minutes；
(2) 45 milliliters of hydrochloric acid solutions are added in three-necked flask, weigh 2.3 grams of pretreated ferroferric oxide powders and 2.6
Gram Boratex is added in flask, adds 10 milliliters of dehydrated alcohols, stirring and dissolving, and heating water bath is passed through nitrogen to 40 DEG C,
It reacts 40 minutes under oxygen-free environment, then the dispersion liquid being prepared in step (1) is added in three-necked flask, stirring is equal
Even, water-bath is warming up to 85 DEG C, is stirred to react 1.0 hours, stands 3 hours, obtains colloidal sol；
(3) colloidal sol that step (2) is prepared is transferred in Muffle furnace, is preheated 1 hour at 160 DEG C, then heats to 560
DEG C, it calcines 18 minutes, cools to room temperature with the furnace, be placed in drying 6 hours in 70 DEG C of vacuum ovens, pulverize.
It is further described as to above scheme, step (1) the concentrated nitric acid molar concentration is 13 mol/Ls.
It is further described as to above scheme, step (2) the hydrochloric acid solution pH value is between 3.8-4.0.
It is further described as to above scheme, the processing side of step (2) the pretreated ferroferric oxide powder
Method are as follows: ferroferric oxide powder is added to the molar concentration of 4 times of volumes as in the hydrochloric acid solution of 0.15 mol/L, ultrasound is divided
It dissipates 10 minutes, filtering, makes to be washed with deionized to filtrate neutrality, then filtrate is placed in the dehydrated alcohol of 6 times of volumes
In, ultrasonic disperse 15 minutes at 3 DEG C are filtered, dry.
It is further described as to above scheme, the luminescent material particle size that step (3) is prepared is received in 10-20
Between rice.
It is further described as to above scheme, the luminescent plastic extrusion temperature is 195 DEG C, and extrusion pressure is
3.6MPa。
Embodiment 2
A kind of luminescent plastic to shine and energy storage effect is excellent, is made of following component in parts by weight: 505 parts of polypropylene,
38 parts of dihexyl phthalate, 26 parts of luminescent material, 11 parts of polyethylene wax, 3.8 parts of stearic acid pentaerythritol ester, stearic acid acyl
1.5 parts of amine, 0.7 part of titanate coupling agent；The preparation method of the luminescent material the following steps are included:
(1) 5.8 grams of europium oxides are weighed to be placed in a beaker, 33 milliliters of concentrated nitric acids are added, are stirred to obtain clear solution, then to
The caddy aqueous solution that 11 milliliters of molar concentrations are 0.33 mol/L is added in beaker, continuing magnetic force stirs 65 points at room temperature
Clock, formed homogeneous mixture solotion, and by mixed solution in ultrasonic cleaner sonic oscillation 4 minutes；
(2) 48 milliliters of hydrochloric acid solutions are added in three-necked flask, weigh 2.4 grams of pretreated ferroferric oxide powders and 2.7
Gram Boratex is added in flask, adds 12 milliliters of dehydrated alcohols, stirring and dissolving, and heating water bath is passed through nitrogen to 42 DEG C,
It reacts 43 minutes under oxygen-free environment, then the dispersion liquid being prepared in step (1) is added in three-necked flask, stirring is equal
Even, water-bath is warming up to 88 DEG C, is stirred to react 1.2 hours, stands 3.5 hours, obtains colloidal sol；
(3) colloidal sol that step (2) is prepared is transferred in Muffle furnace, preheats 1.5 hours, then heats at 170 DEG C
It 580 DEG C, calcines 19 minutes, cools to room temperature with the furnace, be placed in drying 7 hours in 75 DEG C of vacuum ovens, pulverize.
It is further described as to above scheme, step (1) the concentrated nitric acid molar concentration is 14 mol/Ls.
It is further described as to above scheme, step (2) the hydrochloric acid solution pH value is between 3.8-4.0.
It is further described as to above scheme, the processing side of step (2) the pretreated ferroferric oxide powder
Method are as follows: by ferroferric oxide powder be added to 4.5 times of volumes molar concentration be 0.16 mol/L hydrochloric acid solution in, ultrasound
Dispersion 12 minutes, filtering make to be washed with deionized to filtrate neutrality, then filtrate are placed in the anhydrous second of 7 times of volumes
In alcohol, ultrasonic disperse 18 minutes at 4 DEG C are filtered, dry.
It is further described as to above scheme, the luminescent material particle size that step (3) is prepared is received in 10-20
Between rice.
It is further described as to above scheme, the luminescent plastic extrusion temperature is 195-200 DEG C, and extrusion pressure is
3.7MPa。
Embodiment 3
A kind of luminescent plastic to shine and energy storage effect is excellent, is made of following component in parts by weight: 510 parts of polypropylene,
40 parts of dihexyl phthalate, 28 parts of luminescent material, 12 parts of polyethylene wax, 4.0 parts of stearic acid pentaerythritol ester, tristearin
1.6 parts of sour amide, 0.8 part of titanate coupling agent；The preparation method of the luminescent material the following steps are included:
(1) 6.0 grams of europium oxides are weighed to be placed in a beaker, 35 milliliters of concentrated nitric acids are added, are stirred to obtain clear solution, then to
The caddy aqueous solution that 12 milliliters of molar concentrations are 0.34 mol/L is added in beaker, continuing magnetic force stirs 70 points at room temperature
Clock, formed homogeneous mixture solotion, and by mixed solution in ultrasonic cleaner sonic oscillation 5 minutes；
(2) 50 milliliters of hydrochloric acid solutions are added in three-necked flask, weigh 2.5 grams of pretreated ferroferric oxide powders and 2.8
Gram Boratex is added in flask, adds 15 milliliters of dehydrated alcohols, stirring and dissolving, and heating water bath is passed through nitrogen to 45 DEG C,
It reacts 50 minutes under oxygen-free environment, then the dispersion liquid being prepared in step (1) is added in three-necked flask, stirring is equal
Even, water-bath is warming up to 90 DEG C, is stirred to react 1.5 hours, stands 4 hours, obtains colloidal sol；
(3) colloidal sol that step (2) is prepared is transferred in Muffle furnace, is preheated 2 hours at 180 DEG C, then heats to 600
DEG C, it calcines 20 minutes, cools to room temperature with the furnace, be placed in drying 8 hours in 80 DEG C of vacuum ovens, pulverize.
It is further described as to above scheme, step (1) the concentrated nitric acid molar concentration is 15 mol/Ls.
It is further described as to above scheme, step (2) the hydrochloric acid solution pH value is between 3.8-4.0.
It is further described as to above scheme, the processing side of step (2) the pretreated ferroferric oxide powder
Method are as follows: ferroferric oxide powder is added to the molar concentration of 5 times of volumes as in the hydrochloric acid solution of 0.18 mol/L, ultrasound is divided
It dissipates 15 minutes, filtering, makes to be washed with deionized to filtrate neutrality, then filtrate is placed in the dehydrated alcohol of 8 times of volumes
In, ultrasonic disperse 20 minutes, are filtered at 5 DEG C, dry.
It is further described as to above scheme, the luminescent material particle size that step (3) is prepared is received in 10-20
Between rice.
It is further described as to above scheme, the luminescent plastic extrusion temperature is 200 DEG C, and extrusion pressure is
3.8MPa。
Comparative example 1
Difference with embodiment 1 is only that in luminescent material preparation, the addition for omitting caddy aqueous solution in step (1) makes
With remaining is consistent.
Comparative example 2
Difference with embodiment 2 is only that, in luminescent material preparation, omits pretreated ferroso-ferric oxide powder in step (2)
The addition at end uses, remaining is consistent.
Comparative example 3
Difference with embodiment 3 is only that, in luminescent material preparation, the dispersion that will be prepared in step (1) in step (2)
Liquid is added in three-necked flask, is stirred evenly, and water-bath is warming up to 70 DEG C, is stirred to react 2.5 hours, remaining is consistent.
Comparative example 4
Difference with embodiment 3 is only that, in luminescent material preparation, 650 DEG C are warming up in step (3), is calcined 25 minutes, with
Furnace is cooled to room temperature, remaining is consistent.
Comparative experiments
Luminous and excellent energy storage effect luminescent plastic is prepared, using the method for embodiment 1-3 and comparative example 1-4 respectively to use
Long after glow luminous material (additive amount is the 7% of polypropylene plastics quality) prepares the method for luminescent plastic as a control group, each group system
Standby is polypropylene luminescent plastic, prepares luminescent plastic according to each group method processing, and be processed as identical disc-shaped sample
(every group of preparation 5), thickness of sample are 10 millimeters, and diameter is 25 millimeters, carry out mechanics and luminescent properties test, while measuring sample
The heat resistance of product, keeps in test that irrelevant variable is consistent, assesses each group properties of sample being prepared, counts effectively flat
Mean value, as a result as shown in the table:
(it is 1000lx that exciting light, which shines, in test, and firing time is 10 minutes；Measured quantity when initial luminescence is 10 seconds)
The luminous and excellent energy storage effect luminescent plastic that the present invention is prepared solves glimmering used in existing luminescent plastic
Light powder is under adverse circumstances variation, the problem of causing the mechanical property of luminescent plastic and luminescent properties to be severely impacted, and
Light storage with higher has taken into account the promotion of luminescent properties and service life, improves the development and utilization of luminescent plastic, can
It realizes the realistic meaning for improving luminescent material luminescent properties and extending luminescent plastic suitable application area, is that one kind is extremely worthy to be popularized
The technical solution used.
Claims (6)
1. a kind of luminescent plastic to shine and energy storage effect is excellent, which is characterized in that be made in parts by weight of following component:
500-510 parts of polypropylene, 35-40 parts of dihexyl phthalate, 24-28 parts of luminescent material, 10-12 parts of polyethylene wax, tristearin
Sour pentaerythritol ester 3.5-4.0 parts, 1.4-1.6 parts of stearic amide, 0.6-0.8 parts of titanate coupling agent；The luminescent material
Preparation method the following steps are included:
(1) it weighs 5.5-6.0 grams of europium oxide to be placed in a beaker, 30-35 milliliters of concentrated nitric acids is added, are stirred to obtain transparent molten
Then the caddy aqueous solution that 10-12 milliliters of molar concentrations are 0.32-0.34 mol/L is added, at room temperature in liquid into beaker
Continuing magnetic force stir 60-70 minute, formation homogeneous mixture solotion, and by mixed solution in ultrasonic cleaner sonic oscillation 3-
5 minutes；
(2) 45-50 milliliters of hydrochloric acid solutions are added in three-necked flask, weigh 2.3-2.5 grams of pretreated ferroso-ferric oxide powder
End and 2.6-2.8 grams of Boratex are added in flask, add 10-15 milliliters of dehydrated alcohols, stirring and dissolving, heating water bath is extremely
40-45 DEG C, it is passed through nitrogen, reacts 40-50 minutes under oxygen-free environment, then adds the dispersion liquid being prepared in step (1)
Entering into three-necked flask, stirs evenly, water-bath is warming up to 85-90 DEG C, is stirred to react 1.0-1.5 hours, 3-4 hours are stood,
Obtain colloidal sol；
(3) colloidal sol that step (2) is prepared is transferred in Muffle furnace, preheats 1-2 hours at 160-180 DEG C, then rises
Temperature calcines 18-20 minutes to 560-600 DEG C, cools to room temperature with the furnace, and it is small to be placed in 70-80 DEG C of vacuum oven dry 6-8
When, it pulverizes.
2. a kind of luminescent plastic to shine and energy storage effect is excellent as described in claim 1, which is characterized in that step (1) is described
Concentrated nitric acid molar concentration is 13-15 mol/L.
3. a kind of luminescent plastic to shine and energy storage effect is excellent as described in claim 1, which is characterized in that step (2) is described
Hydrochloric acid solution pH value is between 3.8-4.0.
4. a kind of luminescent plastic to shine and energy storage effect is excellent as described in claim 1, which is characterized in that step (2) is described
The processing method of pretreated ferroferric oxide powder are as follows: ferroferric oxide powder is added to the molar concentration of 4-5 times of volume
In hydrochloric acid solution for 0.15-0.18 mol/L, ultrasonic disperse 10-15 minutes, filtering made to be washed with deionized to filtrate
For neutrality, then filtrate is placed in the dehydrated alcohol of 6-8 times of volume, ultrasonic disperse 15-20 minutes at 3-5 DEG C, filtering,
Drying.
5. a kind of luminescent plastic to shine and energy storage effect is excellent as described in claim 1, which is characterized in that step (3) preparation
Obtained luminescent material particle size is between 10-20 nanometers.
6. a kind of luminescent plastic to shine and energy storage effect is excellent as described in claim 1, which is characterized in that the luminescent plastic
Extrusion temperature is 195-200 DEG C, extrusion pressure 3.6-3.8MPa.
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| CN201810926617.4A CN108976609A (en) | 2018-08-15 | 2018-08-15 | A kind of luminescent plastic to shine and energy storage effect is excellent |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5797669A (en) * | 1995-02-15 | 1998-08-25 | Nihon Kagaku Hakko K.K. | Chemical luminescence apparatus |
| CN1403375A (en) * | 2002-10-11 | 2003-03-19 | 清华大学 | Synthesis process of nanostring and nanopowder of RE hydroxide or oxide |
| CN107573718A (en) * | 2017-09-22 | 2018-01-12 | 安徽裕泰环保科技有限公司 | A kind of novel plastic for improving luminescent plastic mechanical property |
-
2018
- 2018-08-15 CN CN201810926617.4A patent/CN108976609A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5797669A (en) * | 1995-02-15 | 1998-08-25 | Nihon Kagaku Hakko K.K. | Chemical luminescence apparatus |
| CN1403375A (en) * | 2002-10-11 | 2003-03-19 | 清华大学 | Synthesis process of nanostring and nanopowder of RE hydroxide or oxide |
| CN107573718A (en) * | 2017-09-22 | 2018-01-12 | 安徽裕泰环保科技有限公司 | A kind of novel plastic for improving luminescent plastic mechanical property |
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| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20181211 |
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| WW01 | Invention patent application withdrawn after publication |