CN104263305B - Quick packaging plastic of a kind of environment protection thermal stability LED light and preparation method thereof - Google Patents
Quick packaging plastic of a kind of environment protection thermal stability LED light and preparation method thereof Download PDFInfo
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- CN104263305B CN104263305B CN201410452764.4A CN201410452764A CN104263305B CN 104263305 B CN104263305 B CN 104263305B CN 201410452764 A CN201410452764 A CN 201410452764A CN 104263305 B CN104263305 B CN 104263305B
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Abstract
The invention provides quick packaging plastic of a kind of environment protection thermal stability LED light and preparation method thereof, the final cured product of described packaging plastic is PPF/PPF-DA crosslinking curing body, i.e. poly-fumaric acid propylene glycol ester/poly-fumaric acid propylene glycol ester diacrylate crosslinking curing body altogether, cured product nontoxicity, by the distance of regulating illumination intensity, light source and sample, can by curing time control within a short period of time, greatly meet the requirement of LED to set time, and the cured product of packaging plastic have higher transmittance, thermal stability and mechanical property.
Description
Technical field
The present invention relates to the quick packaging plastic of LED light of poly-fumaric acid propylene glycol ester sill, particularly relate to quick packaging plastic of a kind of environment protection thermal stability LED light and preparation method thereof.
Background technology
LED solid state light emitters, has compared with conventional light source that operating voltage is low, light efficiency is high, the life-span is long, monochromaticity is good, solid-state, an advantage of not objectionable impurities such as mercurous lead itself, is acknowledged as the forth generation light source replacing incandescent light.
Along with the fast development of electronic information industry, photocuring sizing agent there has also been significant progress.Photocuring sizing agent has that curing efficiency is high, power consumption less, solvent-free pollution, the advantage such as normal temperature solidified, development rapidly, has been widely used in the daily life field such as health care, electronic package.China's Mainland tackiness agent in 2006 and sealing agent output (not comprising urea aldehyde, phenolic aldehyde and melamino-formaldehyde tackiness agent) are 280.2 ten thousand tons, and sales volume 34,000,000,000 yuans, increased 11.32% and 24.13% than 2005 respectively.U.S.'s sealing agent sales volume in 2007 is 30.8 ten thousand tons, sales volume 1,800,000,000 dollars; The sales volume of tackiness agent is about 299.4 ten thousand tons for 2007, and market scale is 9,500,000,000 dollars.UV cure adhesive in various countries is developing with the annual growth of about 15%.
Along with the fast development of China's economy, energy consumption also grows with each passing day, the series of problems caused thus, and such as energy shortage, environmental pollution etc. are also more and more paid attention to.Photodiode (LED) is referred to as forth generation light source, and as cold light source, light source itself is the objectionable impurities such as mercurous lead not, so can not pollute to external world in production with in using.Compare with neon lamp with traditional incandescent light, photodiode have that operating voltage is low, working current is little, luminous efficiency is high, can planar package, shock resistance and anti-seismic performance is good, reliability is high, the life-span is long, just can regulate the advantages such as the power of luminescence easily by controlling electric current power.Therefore LED glue has considerable development prospect.The industry size of LED constantly expands, and the gross output value of China's Mainland LED in 2012 reaches 43,800,000,000 yuan, and compared with 2011, increasing degree is up to 53.68%.
This employing of LED matrix epoxy encapsulation glue in the market, PU urethane packaging plastic and condensed type silica gel etc.But there is the shortcomings such as the low or environmental-protecting performance of thermostability difference, tear strength is weak in these packaging plastics.A single component silica gel of SHIN-ETSU HANTOTAI of Japan, its cohesiveness and snappiness are fine, but because adding the powders such as white carbon black in glue, light transmission very poor (transmittance is lower than 90%).The Maneesh of Dow corning etc. adopt the Vinylphenyl silicon resin of branching and vinyl silicone oil and containing hydrogen silicone oil mixing cured, and its transmittance is better, but the physical strength of this type of organosilicon material is lower, and coefficient of thermal expansion is higher.
Summary of the invention
The object of the present invention is to provide quick packaging plastic of a kind of environment protection thermal stability LED light and preparation method thereof, this packaging plastic is short for set time, and cured product has features such as nontoxicity, good in optical property, mechanical property are strong, Heat stability is good.
For achieving the above object, present invention employs following technical scheme:
The quick packaging plastic of a kind of environment protection thermal stability LED light, this packaging plastic comprises light trigger, component A and B component, described component A is poly-fumaric acid propylene glycol ester (PPF), B component is poly-fumaric acid propylene glycol ester diacrylate (PPF-DA) altogether, in described packaging plastic, component A and the double bond of B component are than being 1:4 ~ 3:1, and the mass ratio of light trigger and component A is 0.01 ~ 0.05:1.
Described packaging plastic is made up of component A, B component and photoinitiator solution (0.05 ~ 0.1g/mL).
Described light trigger is acylphosphine oxide.
Described light trigger is BAPO ((2; 4; 6-trimethylbenzoyl) phenyl phosphine oxide), TEPO (2; 4; 6-trimethylbenzoyl ethoxyl phenenyl phosphine oxide) or TPO ((2; 4,6-trimethylbenzoyl) diphenyl phosphine oxide).
The number-average molecular weight of described poly-fumaric acid propylene glycol ester is 500 ~ 4000, and the number-average molecular weight that poly-fumaric acid propylene glycol ester is total to diacrylate is 500 ~ 4000.
The condition of cure of described packaging plastic is: the distance of packaging plastic and UV-light pointolite is 5 ~ 10cm, and ultraviolet wavelength is 200 ~ 450nm, and UV Light intensity is 300 ~ 574mW/cm
2, the UV Light time is < 5min.
The preparation method of the quick packaging plastic of above-mentioned environment protection thermal stability LED light, comprises the following steps:
1) add in methylene dichloride by component A and B component, then stir 0.5 ~ 1h, after stirring, rotary evaporation removing methylene dichloride obtains mixture under vacuum;
2) photoinitiator solution of preparation is added in mixture, then mixed by ultrasonic oscillation, obtain packaging plastic.
The time of described rotary evaporation is 1 ~ 2h, and the temperature of rotary evaporation is set in 35 ~ 40 DEG C.
Before photoinitiator solution adds mixture, to mixture at room temperature vacuum-drying 12 ~ 18h.(dry object removes moisture residual in mixture and removes methylene dichloride further, improves the purity of PPF and PPF-DA mixture)
The time of ultrasonic oscillation is 0.5 ~ 1h, and ultrasonic power is 180 ~ 500W (frequency: 20 ~ 130KHZ).
Beneficial effect of the present invention is embodied in:
The final cured product of packaging plastic of the present invention is PPF/PPF-DA crosslinking curing body, i.e. poly-fumaric acid propylene glycol ester/poly-fumaric acid propylene glycol ester diacrylate crosslinking curing body altogether, cured product nontoxicity, by the distance of regulating illumination intensity, light source and sample, can by curing time control within a short period of time, greatly meet the requirement of LED to set time, and the cured product of packaging plastic have higher transmittance, thermal stability and mechanical property.
Embodiment
Below in conjunction with embodiment, the present invention is elaborated.
The quick packaging plastic of the LED light adopting preparation technology of the present invention to make, its final cured product is PPF/PPF-DA crosslinking curing body, i.e. poly-fumaric acid propylene glycol ester/poly-fumaric acid propylene glycol ester diacrylate crosslinking curing body altogether.By the distance of regulating illumination intensity, light source and sample, by PPF and PPF-DA curing time control within a short period of time, meet the quick packaging plastic of LED light to the requirement of set time.Preparation different ratios PPF/PPF-DA, tests the physicals of this crosslinking curing body as the quick packaging plastic of LED light.Result shows that different double bond all has higher transmittance and thermal stability than crosslinking curing body, and mechanical property raises along with the reduction of double bond ratio.Be described as follows:
The preparation of component A: take a certain amount of DEF, 1 respectively, 2-propylene glycol, Zinc Chloride Anhydrous, Resorcinol (DEF: 1,2-propylene glycol: Zinc Chloride Anhydrous: the mol ratio of Resorcinol is 1:3:0.01:0.001), add in reactor, pass into nitrogen and reflux condensation mode water, it is 250 ~ 350r.m.p that stirring velocity controls, temperature of reaction controls at 130 DEG C, reaction 24h, final acquisition gathers fumaric acid propylene glycol ester (PPF), and molecular weight is 527.The preparation of component A can with reference to " FKurtisKasper, KazuhiroTanahashi, JohnPFisher & AntoniosGMikos; Synthesisofpoly (propylenefumarate), NATUREPROTOCOLS, VOL.4NO.4; 2009,518-525 ".
The preparation of B component: fumaryl chloride dropwise instills in the methylene dichloride mixing solutions of the propylene glycol of 0 DEG C and salt of wormwood (fumaryl chloride: propylene glycol: the mol ratio of salt of wormwood is 1:3:1.5) by (i), and fully stir, wait to dropwise, temperature of reaction is allowed to go back up to room temperature, stir 12h again, treated (distilled water, saturated nacl aqueous solution wash, extracted with diethyl ether, anhydrous sodium sulfate drying) obtains two (2-hydroxypropyl) fumaric acid intermediate product.(ii) under condition of ice bath, two (2-hydroxypropyl) fumaric acid is dissolved in methylene dichloride, and add triethylamine, then slowly acrylate chloride is dripped, in dropping process, temperature strictly controls to be no more than 0 DEG C, wherein two (2-hydroxypropyl) fumaric acid: triethylamine: the mol ratio of acrylate chloride is 1:3:2.1, treat that acrylate chloride dropwises, at room temperature reactant is stirred 12h, final acquisition gathers fumaric acid propylene glycol ester diacrylate (PPF-DA) altogether, and molecular weight is 1203.The preparation of component A can with reference to " S.He; M.D.Timmer; M.J.Yaszemski; A.W.Yasko; P.S.Engel; A.G.Mikos, Synthesisofbiodegradablepoly (propylenefumarate) networkswithpoly (propylenefumarate)-diacrylatemacromersascrosslinkingagentsandcharacterizati onoftheirdegradationproducts, Polymer42 (2001) 1251-1260 ".
Obtained component A and obtained B component are mixed than 1:2 ~ 2:1 according to double bond, is then mixed to get packaging plastic with light trigger.
Example 1: 1. take 2.00g component A (PPF) and 1.04g B component (PPF-DA) respectively, component A is 2:1 with the double bond ratio of B component, if PPF and PPF-DA viscosity is larger, be inconvenient to measure, can first in vacuum drying oven, its viscosity be reduced temperature furnishing 30 DEG C heating 5min, conveniently measure, when measuring, use same Erlenmeyer flask.Load weighted component A and B component are dissolved in the methylene dichloride of 20mL drying and are mixed to get mixing solutions.2. by mixing solutions magnetic stirrer, continuously stirring 0.5h.After stirring terminates, take out magneton.Mixing solutions is rotary evaporation under vacuumized conditions (-0.06MPa), and temperature is set in 37 DEG C, revolves continuously and steams 1h.3. the Erlenmeyer flask bottleneck coarse filter paper that the mixture after revolving steaming is housed is sealed, in case cause the volatilization of mixture, put into vacuum drying oven, vacuumize the mixture that (-0.06MPa) dry 12h obtains PPF and PPF-DA at ambient temperature.4. preparation (2,4,6-trimethylbenzoyl) phenyl phosphine oxide (BAPO) solution required for photocrosslinking.BAPO is dissolved in methylene dichloride by the concentration of 0.1g/mL.The mass ratio of BAPO and PPF is 0.03:1.5. the BAPO solution prepared is added in the mixture of PPF and PPF-DA, ultrasonic oscillation 0.5h (500W), initiator (BAPO) is mixed with mixture, obtains packaging plastic.6. the test event needed for crosslinking curing body, adds packaging plastic in corresponding mould and processes.As when needs are tested crosslinking curing body, with liquid-transfering needle, packaging plastic is added internal diameter 5mm, in the Glass tubing of length 2cm.Under 3000rpm rotating speed, centrifugal 10min obtains prefabricated sample to remove the defects such as bubble.7. be placed on pointolite uv curing machine Stage microscope by prefabricated sample, the distance arranging prefabricated sample and pointolite is 10cm, and wavelength is 200 ~ 450nm, and intensity of illumination is 574mW/cm
2.The ultraviolet lighting time is 3min.
Packaging plastic set time is the cured product that 3min obtains: cohesive strength is 2.71MPa, tensile shear strength is 1.27MPa, light transmission rate is greater than 90%, high temperature resistantly reach 271.60 DEG C.
Example 2: 1. take 2.00g component A (PPF) and 2.08g B component (PPF-DA) respectively, component A is 1:1 with the double bond ratio of B component, if PPF and PPF-DA viscosity is larger, be inconvenient to measure, can first in vacuum drying oven, its viscosity be reduced temperature furnishing 30 DEG C heating 5min, conveniently measure, when measuring, use same Erlenmeyer flask.Load weighted component A and B component are dissolved in the methylene dichloride of 20mL drying and are mixed to get mixing solutions.2. by mixing solutions magnetic stirrer, continuously stirring 0.5h.After stirring terminates, take out magneton.Mixing solutions is rotary evaporation under vacuumized conditions (-0.06MPa), and temperature is set in 37 DEG C, revolves continuously and steams 1h.3. the Erlenmeyer flask bottleneck coarse filter paper that the mixture after revolving steaming is housed is sealed, in case cause the volatilization of mixture, put into vacuum drying oven, vacuumize the mixture that (-0.06MPa) dry 12h obtains PPF and PPF-DA at ambient temperature.4. preparation (2,4,6-trimethylbenzoyl) phenyl phosphine oxide (BAPO) solution required for photocrosslinking.BAPO is dissolved in methylene dichloride by the concentration of 0.08g/mL.The mass ratio of BAPO and PPF is 0.024:1.5. the BAPO solution prepared is added in the mixture of PPF and PPF-DA, ultrasonic oscillation 1h (450W), initiator (BAPO) is mixed with mixture, obtains packaging plastic.6. the test event needed for crosslinking curing body, adds packaging plastic in corresponding mould and processes.As when needs are tested crosslinking curing body, with liquid-transfering needle, packaging plastic is added internal diameter 5mm, in the Glass tubing of length 2cm.Under 3000rpm rotating speed, centrifugal 10min obtains prefabricated sample to remove the defects such as bubble.7. be placed on pointolite uv curing machine Stage microscope by prefabricated sample, the distance arranging prefabricated sample and pointolite is 10cm, and wavelength is 200 ~ 450nm, and intensity of illumination is 574mW/cm
2.The ultraviolet lighting time is 4min.
Packaging plastic set time is the cured product that 4min obtains: cohesive strength is 1.87MPa, tensile shear strength is 1.53MPa, light transmission rate is greater than 90%, high temperature resistantly reach 285.26 DEG C.
Example 3: 1. take 1.00g component A (PPF) and 2.08g B component (PPF-DA) respectively, component A is 1:2 with the double bond ratio of B component, if PPF and PPF-DA viscosity is larger, be inconvenient to measure, can first in vacuum drying oven, its viscosity be reduced temperature furnishing 30 DEG C heating 5min, conveniently measure, when measuring, use same Erlenmeyer flask.Load weighted component A and B component are dissolved in the methylene dichloride of 20mL drying and are mixed to get mixing solutions.2. by mixing solutions magnetic stirrer, continuously stirring 0.5h.After stirring terminates, take out magneton.Mixing solutions is rotary evaporation under vacuumized conditions (-0.06MPa), and temperature is set in 37 DEG C, revolves continuously and steams 1h.3. the Erlenmeyer flask bottleneck coarse filter paper that the mixture after revolving steaming is housed is sealed, in case cause the volatilization of mixture, put into vacuum drying oven, vacuumize the mixture that (-0.06MPa) dry 12h obtains PPF and PPF-DA at ambient temperature.4. preparation (2,4,6-trimethylbenzoyl) phenyl phosphine oxide (BAPO) solution required for photocrosslinking.BAPO is dissolved in methylene dichloride by the concentration of 0.06g/mL.The mass ratio of BAPO and PPF is 0.018:1.5. the BAPO solution prepared is added in the mixture of PPF and PPF-DA, ultrasonic oscillation 0.5h (450W), initiator (BAPO) is mixed with mixture, obtains packaging plastic.6. the test event needed for crosslinking curing body, adds packaging plastic in corresponding mould and processes.As when needs are tested crosslinking curing body, with liquid-transfering needle, mixture is added internal diameter 5mm, in the Glass tubing of length 2cm.Under 3000rpm rotating speed, centrifugal 10min obtains prefabricated sample to remove the defects such as bubble.7. be placed on pointolite uv curing machine Stage microscope by prefabricated sample, the distance arranging prefabricated sample and pointolite is 10cm, and wavelength is 200 ~ 450nm, and intensity of illumination is 574mW/cm
2.The ultraviolet lighting time is 2min.
Packaging plastic set time is the cured product that 2min obtains: cohesive strength is 3.45MPa, tensile shear strength is 2.07MPa, light transmission rate is greater than 90%, high temperature resistantly reach 287.98 DEG C.
Through experiment, when the number-average molecular weight of poly-fumaric acid propylene glycol ester is 500 ~ 4000, the number-average molecular weight that poly-fumaric acid propylene glycol ester is total to diacrylate is 500 ~ 4000, all can obtain packaging plastic of good performance.
There is after LED light of the present invention quick packaging plastic products solidifying high transparency, snappiness be good, thermostability is high and the feature such as environmentally safe:
1. set time: be less than 5min
2. cohesive strength: be greater than 1.5MPa
3. tensile shear strength: be greater than 1MPa
4. light transmission performance: light transmission rate is greater than 90%
5. resistance toheat after solidification: high temperature resistantly reach 271.6 DEG C (PPF/PPF-DA double bond ratio=2:1) ~ 287.98 DEG C (PPF/PPF-DA double bond ratio=1:2).
6. cured product is to environment toxicological harmless effect.
Claims (7)
1. the quick packaging plastic of environment protection thermal stability LED light, it is characterized in that: this packaging plastic comprises light trigger, component A and B component, described component A is poly-fumaric acid propylene glycol ester, B component is poly-fumaric acid propylene glycol ester diacrylate altogether, in described packaging plastic, component A and the double bond of B component are than being 1:4 ~ 3:1, and the mass ratio of light trigger and component A is 0.01 ~ 0.05:1; Described light trigger is BAPO; The number-average molecular weight of described poly-fumaric acid propylene glycol ester is 500 ~ 4000, and the number-average molecular weight that poly-fumaric acid propylene glycol ester is total to diacrylate is 500 ~ 4000.
2. the quick packaging plastic of a kind of environment protection thermal stability LED light according to claim 1, is characterized in that: described packaging plastic is made up of component A, B component and photoinitiator solution.
3. the quick packaging plastic of a kind of environment protection thermal stability LED light according to claim 1, it is characterized in that: the condition of cure of described packaging plastic is: the distance of packaging plastic and UV-light pointolite is 5 ~ 10cm, ultraviolet wavelength is 200 ~ 450nm, and UV Light intensity is 300 ~ 574mW/cm
2, the UV Light time is < 5min.
4. prepare a method for the quick packaging plastic of environment protection thermal stability LED light as claimed in claim 1, it is characterized in that: comprise the following steps:
1) add in methylene dichloride by component A and B component, then stir 0.5 ~ 1h, after stirring, rotary evaporation removing methylene dichloride obtains mixture under vacuum;
2) photoinitiator solution of preparation is added in mixture, then mixed by ultrasonic oscillation, obtain packaging plastic.
5. a kind of method preparing the quick packaging plastic of environment protection thermal stability LED light according to claim 4, is characterized in that: the time of described rotary evaporation is 1 ~ 2h, and the temperature of rotary evaporation is set in 35 ~ 40 DEG C.
6. a kind of method preparing the quick packaging plastic of environment protection thermal stability LED light according to claim 4, is characterized in that: before photoinitiator solution adds mixture, to mixture at room temperature vacuum-drying 12 ~ 18h.
7. a kind of method preparing the quick packaging plastic of environment protection thermal stability LED light according to claim 4, is characterized in that: the time of ultrasonic oscillation is 0.5 ~ 1h, and ultrasonic power is 180 ~ 500W.
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| CN105860908B (en) * | 2016-04-08 | 2019-03-01 | 西安交通大学 | Environment-friendly type LED packaging plastic poly- fumaric acid butanediol ester sill and preparation method thereof |
| CN106729952B (en) * | 2016-12-23 | 2020-05-22 | 西安交通大学 | PPF/PPF-DA light-cured material bone adhesive tape |
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| CN102558521B (en) * | 2012-01-04 | 2013-10-02 | 清华大学 | Fumaric acid-diol polyester, copolyester of fumaric acid-diol polyester, polyester nucleating agent and application of fumaric acid-diol polyester |
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