CN1301274C - Method for preparing illuminant organic glass in long persistence, and organic glass prepared by the method - Google Patents
Method for preparing illuminant organic glass in long persistence, and organic glass prepared by the method Download PDFInfo
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- CN1301274C CN1301274C CNB2005100117853A CN200510011785A CN1301274C CN 1301274 C CN1301274 C CN 1301274C CN B2005100117853 A CNB2005100117853 A CN B2005100117853A CN 200510011785 A CN200510011785 A CN 200510011785A CN 1301274 C CN1301274 C CN 1301274C
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Abstract
The present invention provides a preparing method of illuminant organic glass with long persistence. The method comprises two steps of prepolymerization and polymerization. The present invention is characterized in that in the processes of prepolymerization and/or polymerization, ultrasonic waves are used for stirring; as a result, illuminant powder with long persistence is uniformly dispersed in methyl methacrylate substrata; the weight ratio of the methyl methacrylate to the illuminant powder with long persistence is equal to 100:10 to 100:50. The preparing method can cause the illuminant powder with long persistence to be uniformly dispersed in the methyl methacrylate substrata. Illuminant organic glass with long persistence, which is prepared by adopting the method, has the good combination properties such as high dispersancy of illuminat powder, no precipitation, uniform luminous intensity, long persistence time, good appearance quality, etc.
Description
Technical field
The present invention relates to synthetic glass, particularly relate to light emissive plastic.
Background technology
Long-persistence luminous phenomenon is meant that certain material can absorb ambient light radiating energy, and this material discharges the phenomenon of these stored energys more slowly with the form of visible light then.Material with this performance can be applied in fields such as reading of low light level guidance lighting, object identification and instrument under the dark situation.Common long-afterglow material is mainly rear-earth-doped aluminate and silicate compound system.Because this type of material has characteristics such as "dead", time of persistence of length, luminous intensity height, is widely used in each fields such as national defence, industry, building, daily lifes at present.
The material of main part of long after glow luminous material is Powdered, during use the powdery luminescent material is sneaked in the different substrates materials such as coating, printing ink, plastics, synthetic glass, can make above-mentioned materials have long-persistence luminous function, thereby enlarge the scope of application of long after glow luminous material greatly, the industrialization product of existing multiple this material of application comes out at present.In above-mentioned substrate material, synthetic glass has characteristics such as the transparency is good, intensity is high, easy to process, is widely used in industry and daily life field.With the characteristics of luminescence of synthetic glass in conjunction with rare earth long-afterglow luminescent material, make synthetic glass with long-persistence luminous performance, will indicate at dark situation, obtain good application aspect the practical application such as road indication, ad decoration.
In synthetic glass is produced, exist the process of passing through bulk polymerization composite solid state synthetic glass (PMMA) by the methyl methacrylate monomer (MMA) of liquid state.In polymerization process; be added on the long afterglow light-emitting particles in the liquid methyl methacrylate monomer because gravity settling effect meeting inevitably produces precipitation, reunion; influence the dispersed homogeneous degree of luminescent material in liquid methyl methacrylate monomer; the luminescent material particle of Tian Jiaing can produce certain inhibition simultaneously, prolongs monomeric polymerization process.Simple mechanical stirring is handled, as stirring rod, blade etc., can partly address the above problem, but because general rare earth long afterglow luminescent powder particle thin (200-500 order), general mechanical stirring dispersing mode still can not effectively solve the agglomeration traits of luminescent powder, therefore rare earth long-afterglow luminescent material can't be evenly dispersed in the synthetic glass matrix, non-uniform light appears, luminous intensity is low, problems such as visual appearance difference, mechanical stirring can produce in liquid methyl methacrylate monomer and cause a large amount of bubbles simultaneously, is unfavorable for gas purging in the synthetic glass.
Summary of the invention
The present invention is directed to above-mentioned defective, a kind of preparation method of long-persistence luminous synthetic glass is provided, long after glow luminous material is evenly dispersed in the synthetic glass matrix.
Long-persistence luminous synthetic glass with this method preparation is provided simultaneously.Adopt the long-persistence luminous synthetic glass of this method preparation to have excellent comprehensive performances such as the luminescent powder dispersiveness is high, nothing precipitation, luminous intensity is even, time of persistence is long, visual appearance is good.
A kind of preparation method of long-persistence luminous synthetic glass, adopt two-stage polymerization process, comprise two steps of prepolymerization and polymerization, it is characterized in that, in prepolymerization and/or polymerization process, adopt ultrasonic stirring, long-afterglow luminescent powder is dispersed in the methyl methacrylate matrix, the weight ratio of methyl methacrylate and long-afterglow luminescent powder is 100: 10-100: 50.
Described prepolymerized temperature is under 60-90 ℃, and frequency of ultrasonic is 10-30kHz, sound intensity 10-15W/cm
2, the right 20%-40% that reaches of pre-polymerization.
Described polymerization temperature is 50-90 ℃, and frequency of ultrasonic is 1-10kHz, sound intensity 15-20W/cm
2
Described ultrasonic transducer is piezoelectric ceramic piece transverter or aluminium alloy transverter.
Described long-afterglow luminescent powder solvent treatment is removed luminescent powder surface organic impurity and moisture.Described solvent is methyl alcohol preferably.
Described long-afterglow luminescent powder is " strontium aluminate: europium, dysprosium ", " calcium aluminate: europium, dysprosium ", " strontium silicate: europium, dysprosium ", " manosil AS strontium: europium, dysprosium " or " yttrium oxysulfide: europium ", powder size is 100 orders-1000 orders.
Also be added with in the described methyl methacrylate monomer slurries and account for the initiator that the methyl methacrylate weight ratio is 0.05%-0.1%, the softening agent of 4%-7%, remover or its combination of 0.3%-0.8%.
Described initiator benzoyl peroxide (BPO), Diisopropyl azodicarboxylate (ABN) or peroxidation carbonic acid diisopropyl ester (IPP).Preferred Diisopropyl azodicarboxylate.
Described softening agent is dibutyl phthalate (DBP), dioctyl ester, Uniflex DBS.Preferred dibutyl phthalate.
Described remover is stearic acid, silicone oil.Preferred stearic acid.
The preparation method of the long-persistence luminous synthetic glass of the present invention comprises two steps of prepolymerization and polymerization.Long-afterglow luminescent powder and methyl methacrylate monomer slurries are mixed stirring in proportion, heat mixed organic hyaline monomer slurry then and carry out prepolymerization, under the about 60-80 of prepolymerization temperature ℃, in mechanical stirring after for some time (about 30 minutes), use ultrasonic wave instead and stir and disperse.Open the transverter of ultrasonic generator, frequency of ultrasonic is 10-30kHz, sound intensity 10-15W/cm
2, because in the ultrasonic agitation process, a part of sound wave mechanical energy is converted to heat energy, so should adjust the operating power of ultrasonic generator in the ultra-sonic dispersion process, the prepolymerization slurry temperature is maintained below 90 ℃, the final right 20%-40% that reaches of pre-polymerization.Last polymerization forming should carry out in the mould of preparation synthetic glass, and bath temperature is 50-60 ℃, and (frequency of ultrasonic is 1-10kHz, sound intensity 10-20W/cm with the low frequency high-energy ultrasonic in water-bath
2) vibrate polymerization, the time is 1-2 hour, slurries are gel state in mould, stop ultrasonicly, with warming-in-water to 90 ℃, are incubated about 2 hours, until the synthetic glass moulding.In pre-polymerization process, produced a large amount of bubbles owing to stir, therefore the slip after the prepolymerization is injected the vacuum vessel chamber, to remove the gas in the slip.
In the above-mentioned pre-polymerization process, because of ferro element can weaken the luminous intensity of rare earth inspired long-lasting phosphor, so prepolymerization container and initial mechanical stirrer should not adopt the material that contains ferro element.
Above-mentioned ultrasonic transducer in order to have optimum dispersed with stirring effect, should be installed in the transverter setting aggregation container bottom, preferably places a plurality of transverters; Simultaneously, for avoiding the influence of ferro element to long-afterglow material, present method is selected the piezoelectric ceramic piece transverter for use, perhaps the aluminium alloy transverter.
Long-persistence luminous powder material is the alkali earth metal aluminate (for example, strontium aluminate, calcium aluminate) that rare earth elements europium, dysprosium excite, silicate (for example, strontium silicate), silico-aluminate (manosil AS strontium), and the oxysulfide (for example, yttrium oxysulfide) that excites of europium.
In the methyl methacrylate monomer slurries, can selectivity add initiator, softening agent and releasing agent.Initiator can be accelerated polymerization velocity, shorten polymerization time, the normal selection with benzoyl peroxide (BPO), Diisopropyl azodicarboxylate (ABN), peroxidation carbonic acid diisopropyl ester (IPP) etc., because of BPO and IPP have certain oxidisability, therefore preferential to select initiator be Diisopropyl azodicarboxylate (ABN).Softening agent can increase the workability of synthetic glass, can select dibutyl phthalate (DBP), dioctyl ester, Uniflex DBS etc., and the present invention preferentially uses dibutyl phthalate.Releasing agent can be selected stearic acid, silicone oil etc. for use, and present method is selected stearic acid for use.The add-on of each above-mentioned auxiliary agent (with synthetic glass MMA monomer weight portion rate): initiator is 0.05%-0.1%, and softening agent is 4%-7%, and releasing agent is 0.3%-0.8%.
The preparation method of the long-persistence luminous synthetic glass of the present invention, in long afterglow luminescent powder and organic hyaline monomer prepolymerization and/or polymerization process, introduce acoustic energy, it is ultrasonic wave, utilize hyperacoustic cavitation effect, radiation pressure, physical propertys such as acoustic streaming stir the mixture of long-afterglow luminescent powder and organic hyaline monomer, in the liquid organic glass monomer, produce a large amount of small cavitys, these cavitys can make liquid produce violent concussion in generation and cancellation process, drive and produce motion mutually between the luminescent powder particle, because cavity uniform distribution in liquid that ultrasonic wave produces, therefore can make between the luminescent powder particle homodisperse in liquid phase.Adopt ultra-sonic dispersion technology can obtain the finely dispersed long-persistence luminous pmma material of luminescent powder.Accompanying drawing 1 is the section sample Photomicrograph of the long-persistence luminous pmma material of employing present method preparation, and as shown in the figure, the luminescent powder particles dispersed is good, is evenly distributed, and does not have aggregation phenomenon.Supersound process also can be used to remove the bubble that mixed slurry produces after mechanical stirring, thereby reaches the purpose of degasification.
Ultrasonic wave also is a kind of energy, and it can quicken the polymerization process of synthetic glass, thereby shortens the long-persistence luminous synthetic glass cycle, and cuts down the consumption of energy.The required polymerization time of present method is 4-6 hour, is lower than common synthetic glass polymerization required 8-12 hour.
The ultrasonic interface that can activate between luminescent powder particle and the synthetic glass matrix, make between the two in conjunction with tight, luminescent powder effectively is wrapped in the synthetic glass, has blocked the influence of outside air and moisture effectively luminescent powder luminous efficiency and time of persistence; While has guaranteed the luminous efficiency of luminescent material owing to the high transmission rate feature (transmittance can reach 91%-93%) that pmma material has the biglyyest.Experiment confirm can guarantee that be 10-20 hour time of persistence.
Adopt the long-persistence luminous synthetic glass of this method preparation to have excellent comprehensive performances such as the luminescent powder dispersiveness is high, nothing precipitation, luminous intensity is even, time of persistence is long, visual appearance is good.
Description of drawings
Fig. 1: the deployment conditions photo of the steady persistence synthetic glass internal illumination powder particles of ultrasonic aid preparation
Embodiment
The present invention is described in further detail below in conjunction with embodiment.
Embodiment 1
Strontium aluminate: europium, dysprosium 2Kg, buff powder, 1000 orders, commercially available.
Methyl methacrylate 10Kg, colourless liquid, commercially available.
The adding parts by weight are 10: 2 " strontium aluminate: europium, dysprosium " in methyl methacrylate monomer, put into the prepolymerization reactor, be heated to 80 ℃, imposed mechanical stirring 15 minutes, put into ultrasonic transducer probe then, ultra-sonic dispersion 30 minutes, temperature of reaction remains on 90 ℃, the operating frequency of used ultra-sonic generator is 20kHz, and the sound intensity is 15W/cm
2Treat that prepolymerization reaches 30%, viscosity reaches requirement, stop the supersound process process, the prepolymerization slip is put into the vacuum cavity degasification, then slip is injected in the mould that the dull and stereotyped silex glass by two cleanings constitutes, seal the back and in 60 ℃ of water-baths, carry out mass polymerization, in water-bath, use low frequency high-energy ultrasonic (operating frequency 1kHz, sound intensity 15W/cm simultaneously instead
2) slip in the mould is disperseed and vibrates polymerization, the time is 2 hours, reaches gelation state to feed liquid, stop supersound process, warming-in-water to 90 ℃ was incubated after 2 hours, and cooling and demolding promptly obtains the finely dispersed long-persistence luminous methacrylate sheet of luminescent material.
Embodiment 2
Strontium silicate: europium, dysprosium 1Kg, buff powder, 500 orders, commercially available.Use washed with methanol, remove surperficial organic impurity and moisture, dry then, 60 ℃ of bakings 2 hours.
Methyl methacrylate 10Kg, colourless liquid, commercially available.
Diisopropyl azodicarboxylate (ABN) 5g, colourless liquid, commercially available.
The adding parts by weight are 10: 1 " strontium silicate: europium, dysprosium " in methyl methacrylate monomer, add initiator Diisopropyl azodicarboxylate (ABN) then, put into the prepolymerization reactor, are heated to 70 ℃, impose mechanical stirring.Treating that pre-polymerization is right reaches 20%, viscosity reaches requirement, the prepolymerization slip is put into the vacuum cavity degasification, then slip is injected in the mould that the dull and stereotyped silex glass by two cleanings constitutes, seal the back and in 50 ℃ of water-baths, carry out mass polymerization, in water-bath, use simultaneously low frequency high-energy ultrasonic (operating frequency 5kHz, sound intensity 20W/cm instead
2) slip in the mould is disperseed and vibrates polymerization, the time is 1 hour, reaches gelation state to feed liquid, stop supersound process, warming-in-water to 90 ℃ was incubated after 2 hours, and cooling and demolding promptly obtains the finely dispersed long-persistence luminous methacrylate sheet of luminescent material.
Embodiment 3
The manosil AS strontium: europium, dysprosium 3Kg, buff powder, 200 orders, commercially available.
Methyl methacrylate 10Kg, colourless liquid, commercially available.
Diisopropyl azodicarboxylate (ABN) 10g, colourless liquid, commercially available.
Dibutyl phthalate 400g, colourless liquid, commercially available.
Stearic acid 30g, white solid, commercially available.
The adding parts by weight are 10: 3 manosil AS strontium in methyl methacrylate monomer: europium, dysprosium, add initiator Diisopropyl azodicarboxylate (ABN) then, plasticizer phthalic acid dibutylester, stearic acid release agent, put into the prepolymerization reactor, be heated to 60 ℃, imposed mechanical stirring simultaneously 30 minutes, put into ultrasonic transducer probe then, ultra-sonic dispersion 60 minutes, temperature of reaction remains on 90 ℃, and the operating frequency of used ultra-sonic generator is 25kHz, and the sound intensity is 10W/cm
2Treat that prepolymerization reaches 40%, viscosity reaches requirement, stop the supersound process process, the prepolymerization slip is put into the vacuum cavity degasification, then slip is injected in the mould that the dull and stereotyped silex glass by two cleanings constitutes, seal the back and in 60 ℃ of left and right sides water-baths, carry out mass polymerization, reach gelation state to feed liquid, warming-in-water to 90 ℃ was incubated after 2 hours, and cooling and demolding promptly obtains the finely dispersed long-persistence luminous methacrylate sheet of luminescent material.
Embodiment 4
Yttrium oxysulfide: europium 5Kg, buff powder, 100 orders, commercially available.Use washed with methanol, remove surperficial organic impurity and moisture, dry then, 80 ℃ of bakings 2 hours.
Methyl methacrylate 10Kg, colourless liquid, commercially available.
Dibutyl phthalate 700g, colourless liquid, commercially available.
Stearic acid 80g, white solid, commercially available.
The adding parts by weight are 10: 5 " yttrium oxysulfide: europium " in methyl methacrylate monomer, add the plasticizer phthalic acid dibutylester, stearic acid release agent is put into the prepolymerization reactor, is heated to 70 ℃, imposed mechanical stirring simultaneously 30 minutes, put into ultrasonic transducer probe then, ultra-sonic dispersion 60 minutes, temperature of reaction remains on 90 ℃, the operating frequency of used ultra-sonic generator is 30kHz, and the sound intensity is 12W/cm
2Treat that prepolymerization reaches 30%, viscosity reaches requirement, stop the supersound process process, the prepolymerization slip is put into the vacuum cavity degasification, then slip is injected in the mould that the dull and stereotyped silex glass by two cleanings constitutes, seal the back and in 50 ℃ of water-baths, carry out mass polymerization, in water-bath, use low frequency high-energy ultrasonic (operating frequency 8kHz, sound intensity 20W/cm simultaneously instead
2) slip in the mould is disperseed and vibrates polymerization, the time is 1.5 hours, reaches gelation state to feed liquid, stop supersound process, warming-in-water to 90 ℃ was incubated after 2 hours, and cooling and demolding promptly obtains the finely dispersed long-persistence luminous methacrylate sheet of luminescent material.
Experimental example
The above-mentioned organic glass products that makes under D65 standard light source (illumination 1000LX), is excited 10min, remove light source, measure its 60 seconds original intensities, 10 minutes after-glow brightnesses and the total time of persistence when reaching visible brightness 0.3 milli candela/metre2.
Brightness tester: Minolta LS-110 luminance meter.
Claims (9)
1, a kind of preparation method of long-persistence luminous synthetic glass, comprise two steps of prepolymerization and polymerization, it is characterized in that, in prepolymerization and/or polymerization process, use ultrasonic stirring, long-afterglow luminescent powder is dispersed in the methyl methacrylate matrix, and the weight ratio of methyl methacrylate and long-afterglow luminescent powder is 100: 10-100: 50.
2, the preparation method of long-persistence luminous synthetic glass according to claim 1, described prepolymerized temperature are 60 ℃-90 ℃, and frequency of ultrasonic is 10-30kHz, sound intensity 10-15W/cm
2, the right 20%-40% that reaches of pre-polymerization.
3, the preparation method of long-persistence luminous synthetic glass according to claim 1, described polymerization temperature is 50 ℃-90 ℃, frequency of ultrasonic is 1-10kHz, sound intensity 15-20W/cm
2
4, according to the preparation method of each described long-persistence luminous synthetic glass of claim 1-3, described ultrasonic wave is produced by piezoelectric ceramic piece transverter or aluminium alloy transverter.
5, the preparation method of long-persistence luminous synthetic glass according to claim 1, described long-afterglow luminescent powder solvent treatment is removed surperficial organic impurity and moisture.
6, the preparation method of long-persistence luminous synthetic glass according to claim 5, described long-afterglow luminescent powder is " strontium aluminate: europium, dysprosium ", " calcium aluminate: europium, dysprosium ", " strontium silicate: europium, dysprosium ", " manosil AS strontium: europium, dysprosium " or " yttrium oxysulfide: europium ", powder size are 100 orders-1000 orders.
7, the preparation method of long-persistence luminous synthetic glass according to claim 1 also is added with in the described methyl methacrylate monomer slurries and accounts for the initiator that the methyl methacrylate weight ratio is 0.05%-0.1%, plasticising dosage, 0.3%-0.8% remover or its combination of 4%-7%.
8, the preparation method of long-persistence luminous synthetic glass according to claim 7, described initiator is benzoyl peroxide, Diisopropyl azodicarboxylate or peroxidation carbonic acid diisopropyl ester, described softening agent is dibutyl phthalate, dioctyl phthalate (DOP) or Uniflex DBS, and described remover is stearic acid or silicone oil.
9, the preparation method of long-persistence luminous synthetic glass according to claim 8, described initiator is a Diisopropyl azodicarboxylate, and described softening agent is a dibutyl phthalate, and described remover is a stearic acid.
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| CNB2005100117853A CN1301274C (en) | 2005-05-25 | 2005-05-25 | Method for preparing illuminant organic glass in long persistence, and organic glass prepared by the method |
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| CN104097369A (en) * | 2014-06-05 | 2014-10-15 | 安徽物宝光电材料有限公司 | Organic glass screen |
| CN104479437B (en) * | 2015-01-06 | 2017-01-25 | 东华大学 | Preparation method for super-hydrophobic self-luminous coating |
| CN104926965A (en) * | 2015-05-20 | 2015-09-23 | 安徽力华光电玻璃科技有限公司 | Process for preparing solar glass tube |
| CN106519093B (en) * | 2016-11-27 | 2018-11-23 | 天津城建大学 | A kind of preparation method of temperature sensing color changing organic glass |
| CN106589754A (en) * | 2016-12-20 | 2017-04-26 | 安徽亚克力实业有限公司 | Impact-resistant organic glass and preparation method thereof |
| CN108727531A (en) * | 2018-05-24 | 2018-11-02 | 安徽新涛光电科技有限公司 | Advertisement light emitting word photoelectric functional method for glass preparation and its product |
| CN110483667A (en) * | 2018-08-29 | 2019-11-22 | 含山县金中环装饰材料有限公司 | A kind of composite modification material improving organic glass resistance to soiling |
| CN114874367B (en) * | 2022-05-11 | 2023-09-29 | 江苏汉瓷新材料科技有限公司 | Long-afterglow luminous acrylic material and preparation method thereof |
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Effective date of registration: 20120217 Address after: Five, building 3, No. 518-519 Desheng East Road, Daliang street, Shunde District, Guangdong, Foshan 528300 Co-patentee after: BEIJING AGLAIA TECHNOLOGY & DEVELOPMENT Co.,Ltd. Patentee after: GUANGDONG AGLAIA OPTOELECTRONIC MATERIALS Co.,Ltd. Address before: Five, building 3, No. 518-519 Desheng East Road, Daliang street, Shunde District, Guangdong, Foshan 528300 Patentee before: GUANGDONG AGLAIA OPTOELECTRONIC MATERIALS Co.,Ltd. |