CN102034923B - High wet-heat resistance transparent light-emitting diode packaging material and preparation method thereof - Google Patents
High wet-heat resistance transparent light-emitting diode packaging material and preparation method thereof Download PDFInfo
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- CN102034923B CN102034923B CN2010102727309A CN201010272730A CN102034923B CN 102034923 B CN102034923 B CN 102034923B CN 2010102727309 A CN2010102727309 A CN 2010102727309A CN 201010272730 A CN201010272730 A CN 201010272730A CN 102034923 B CN102034923 B CN 102034923B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000005022 packaging material Substances 0.000 title abstract 2
- 239000003822 epoxy resin Substances 0.000 claims abstract description 38
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 38
- 239000000178 monomer Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- FCVNATXRSJMIDT-UHFFFAOYSA-N trihydroxy(phenyl)silane Chemical group O[Si](O)(O)C1=CC=CC=C1 FCVNATXRSJMIDT-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 11
- 238000001746 injection moulding Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 16
- 239000012043 crude product Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 9
- 239000005054 phenyltrichlorosilane Substances 0.000 claims description 9
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 8
- 239000004593 Epoxy Substances 0.000 claims description 5
- HBGPNLPABVUVKZ-POTXQNELSA-N (1r,3as,4s,5ar,5br,7r,7ar,11ar,11br,13as,13br)-4,7-dihydroxy-3a,5a,5b,8,8,11a-hexamethyl-1-prop-1-en-2-yl-2,3,4,5,6,7,7a,10,11,11b,12,13,13a,13b-tetradecahydro-1h-cyclopenta[a]chrysen-9-one Chemical compound C([C@@]12C)CC(=O)C(C)(C)[C@@H]1[C@H](O)C[C@]([C@]1(C)C[C@@H]3O)(C)[C@@H]2CC[C@H]1[C@@H]1[C@]3(C)CC[C@H]1C(=C)C HBGPNLPABVUVKZ-POTXQNELSA-N 0.000 claims 4
- PFRGGOIBYLYVKM-UHFFFAOYSA-N 15alpha-hydroxylup-20(29)-en-3-one Natural products CC(=C)C1CCC2(C)CC(O)C3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 PFRGGOIBYLYVKM-UHFFFAOYSA-N 0.000 claims 4
- SOKRNBGSNZXYIO-UHFFFAOYSA-N Resinone Natural products CC(=C)C1CCC2(C)C(O)CC3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 SOKRNBGSNZXYIO-UHFFFAOYSA-N 0.000 claims 4
- 229920001577 copolymer Polymers 0.000 claims 4
- 229920005989 resin Polymers 0.000 abstract description 11
- 239000011347 resin Substances 0.000 abstract description 11
- 239000011159 matrix material Substances 0.000 abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052710 silicon Inorganic materials 0.000 abstract description 6
- 239000010703 silicon Substances 0.000 abstract description 6
- 229920001187 thermosetting polymer Polymers 0.000 abstract description 5
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 5
- 238000002834 transmittance Methods 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 229910018557 Si O Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000005375 organosiloxane group Chemical group 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000192 social effect Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Silicon Polymers (AREA)
- Epoxy Resins (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Abstract
The invention relates to a high wet-heat resistance transparent light-emitting diode (LED) packaging material and a preparation method thereof. The method comprises the following steps: a thermosetting epoxy resin (EP) is used as the matrix resin, the synthesized organic silicon monomer and the matrix resin are used to perform a grafting polycondensation reaction in proportion, a curing system is added in the product to stir evenly, then injection molding is performed, vacuum-pumping is performed, and a cured sample is obtained through curing, wherein the organic silicon monomer is phenyl silanetriol monomer which is obtained by hydrolyzing phenyl trichloro silicane. The synthesized CAB and EP directly react to prepare an EP-CAB copolymer. The method has the following outstanding advantages: the wet-heat resistance of EP can be effectively increased, the transparency can be improved, the reaction time can be reduced and the reaction complexity can be lowered; and the method has an important theoretical significance and application value in the practical study of the civilian industry.
Description
Technical field
The invention belongs to LED encapsulating material field, be specifically related to the technology of preparing of the transparent LED encapsulating material of high moisture-proof heat.
Background technology
LED is as the novel illumination light source, no matter from energy savings still from reducing the angle of polluting, all have the potentiality of alternative traditional lighting light source, be one of approach that solves present China energy crisis.
At present, LED encapsulates with epoxy resin (EP), and the effect of LED encapsulation back resin enclosure mainly contains: 1) protection tube core etc. does not receive extraneous the erosion; 2) take different shapes and material character (mixing or do not mix color dispersing agent), play lens or diffusing lens function; 3) select for use the epoxy resin of respective indices of refraction to do transition, with the light outgoing efficient that improves tube core etc.Epoxy resin has good comprehensive mechanical properties, adhesive strength high, bonding wide, shrinkage is low, good stability, excellent electrical insulating property, good processability etc., is widely used in LED encapsulating material field.Yet, mobile poor because the viscosity of epoxy resin is big, solidify back crosslink density height, so exist internal stress big, shortcoming such as fatigue durability, thermal endurance and moisture-proof are relatively poor has restricted the application of epoxy resin aspect structural material to a great extent.Therefore, strengthen the design and development of epoxy resin encapsulating material, improve the wet-hot aging performance of epoxy resin, improve its properties of transparency and have economy and social effect.
Because the organosilicon main chain is made up of the Si-O key, the bond energy of Si-O key is bigger than the bond energy of C-C key and C-O key, therefore should effectively improve its wet-hot aging performance with modifying epoxy resin by organosilicon; Owing to contain the organosilyl good heat resistance of phenyl in the organosilicon that contains other group such as methyl, contain the phenyl modifying epoxy resin by organosilicon so select for use, more can improve the wet-hot aging performance of epoxy resin significantly.At present; The common way of modifying epoxy resin by organosilicon is earlier the organosiloxane polycondensation to be become prepolymer; Again with prepolymer and epoxy resin reaction; Materials Science and Engineering journal " the synthetic and performance of modifying epoxy resin by organosilicon " delivered in February, 2009 for example, not enough below just existing: reactions step is many, not easy to operate, the time is long; And first pre-polymerization afterreaction influences the heat resistance of modified epoxy.
Summary of the invention
The one phenyl silanetriol monomer (CAB) of the object of the present invention is to provide that reactions step is few, the reaction time is short directly with hot transparent LED encapsulating material of high moisture-proof of epoxy resin (EP) prepared in reaction EP-CAB copolymer and preparation method thereof.
The preparation method of the transparent LED encapsulating material of high moisture-proof heat provided by the invention, specific as follows:
The first step, in mixture of ice and water, in the mixed solution of deionized water and acetone, dropwise add a phenyl trichlorosilane, behind the sufficient reacting; Filtration obtains crude product; Further crude product is dissolved in the acetone, utilizes a large amount of deionized waters and sodium carbonate to regulate PH, filter to neutral; 50～70 ℃ of following vacuumize 1～3h obtain a phenyl silanetriol monomer;
Second step, under 80～90 ℃ of conditions of reaction temperature, with epoxy resin 100 weight portions be less than a phenyl silanetriol monomer generation grafting polycondensation reaction 1～2h of 20 weight portions, make the EP-CAB copolymer;
The 3rd step, in the EP-CAB copolymer, add 100 weight portion curing systems, the back injection molding that stirs vacuumizes, be cured behind 0.5～1.5h, condition of cure be earlier 75～85 ℃ solidify 0.5～1.5h, 115～125 ℃ of curing 1.5～2.5h again.
Preferred reaction conditions is:
The first step, in mixture of ice and water, in the mixed solution of deionized water and acetone, dropwise add a phenyl trichlorosilane, behind the sufficient reacting; Filtration obtains crude product; Further crude product is dissolved in the acetone, utilizes a large amount of deionized waters and sodium carbonate to regulate PH, filter to neutral; 60 ℃ of following vacuumize 2h obtain a phenyl silanetriol monomer;
Second the step, under 80～90 ℃ of conditions of reaction temperature, the phenyl silanetriol monomer generation grafting polycondensation reaction 1.5h with epoxy resin 100 weight portions and 2～10 weight portions makes the EP-CAB copolymer;
The 3rd step, in the EP-CAB copolymer, add 100 weight portion curing systems, the back injection molding that stirs vacuumizes, be cured behind the 1h, condition of cure be earlier 80 ℃ solidify 1h, 120 ℃ of curing 2h again.
By the transparent LED encapsulating material of high moisture-proof heat that said method makes, it can reach water absorption rate is 0.2125%～0.3456%, and heat decomposition temperature is 221 ℃～228 ℃, and light transmittance is 86.93%～90.1% superperformance simultaneously.
The application has following innovative point:
With elder generation the organosiloxane polycondensation is become prepolymer, again prepolymer is compared with the method for epoxy resin reaction, the direct and epoxy resin prepared in reaction EP-CAB copolymer of the synthetic phenyl silanetriol monomer of the present invention; Modifier one phenyl silanetriol monomer is through a phenyl trichlorosilane hydrolysis gained; Shorten the reaction time, reduced the complexity of reaction, and easy operating; The wet-hot aging performance of epoxy resin is obviously improved, and properties of transparency improves.
Description of drawings
Fig. 1 is the process chart of the transparent LED encapsulating material preparation of high moisture-proof heat.
Embodiment
Embodiment 1: with thermosetting epoxy resin (EP) is matrix resin, with synthetic organic silicon monomer and matrix resin reaction, prepares the transparent LED encapsulating material of high moisture-proof heat, and it is following that it specifically prepares process:
The first step, in mixture of ice and water, in the mixed solution of 150ml deionized water and 10ml acetone, dropwise add 10g～30g one phenyl trichlorosilane, the reaction 30min; Filtration obtains crude product; Further it is dissolved in the acetone, utilizes a large amount of deionized waters and sodium carbonate to regulate PH, filter to neutral; 60 ℃ of following vacuumize 2h obtain a phenyl silanetriol monomer (CAB);
Second step, under 80～90 ℃ of reaction temperatures, be 2～5 weight portion generation grafting polycondensation reaction 1.5h with epoxy resin 100 weight portions and a phenyl silanetriol monomer, prepare the EP-CAB copolymer;
The 3rd step, in the EP-CAB copolymer, add 100 weight portion curing systems, the back injection molding that stirs vacuumizes, be cured behind the 1h, condition of cure be earlier 80 ℃ solidify 1h, 120 ℃ of curing 2h again, obtain solidified sample;
The 4th step, carry out performance test according to international standard GB/T1034-1998, the actual measurement water absorption rate is 0.3456%, and heat decomposition temperature is 228 ℃, and simultaneously light transmittance is 86.93%.
Embodiment 2: they with the thermosetting epoxy resin matrix resin, and with synthetic organic silicon monomer and matrix resin reaction, the hot LED encapsulating material of preparation high transparent moisture-proof, it is following that it specifically prepares process:
The first step, in mixture of ice and water, in the mixed solution of 150ml deionized water and 10ml acetone, dropwise add 10g～30g one phenyl trichlorosilane, the reaction 30min; Filtration obtains crude product; Further it is dissolved in the acetone, utilizes a large amount of deionized waters and sodium carbonate to regulate PH, filter to neutral; 60 ℃ of following vacuumize 2h obtain a phenyl silanetriol monomer (CAB);
Second step, under 80～90 ℃ of reaction temperatures, be 7～10 weight portion generation grafting polycondensation reaction 1.5h with epoxy resin 100 weight portions and a phenyl silanetriol monomer, prepare the EP-CAB copolymer;
The 3rd step, in the EP-CAB copolymer, add 100 weight portion curing systems, the back injection molding that stirs vacuumizes, be cured behind the 1h, condition of cure be earlier 80 ℃ solidify 1h, 120 ℃ of curing 2h again, obtain solidified sample;
The 4th step, carry out performance test according to international standard GB/T1034-1998, the actual measurement water absorption rate is 0.2125%, and heat decomposition temperature is 221 ℃, and simultaneously light transmittance is 90.14%.
Embodiment 3: with thermosetting epoxy resin (EP) is matrix resin, with synthetic organic silicon monomer and matrix resin reaction, prepares the transparent LED encapsulating material of high moisture-proof heat, and it is following that it specifically prepares process:
The first step, in mixture of ice and water, in the mixed solution of 150ml deionized water and 10ml acetone, dropwise add 10g～30g one phenyl trichlorosilane, the reaction 30min; Filtration obtains crude product; Further it is dissolved in the acetone, utilizes a large amount of deionized waters and sodium carbonate to regulate PH, filter to neutral; 60 ℃ of following vacuumize 2h obtain a phenyl silanetriol monomer (CAB);
Second step, under 80～90 ℃ of reaction temperatures, be 20 weight portion generation grafting polycondensation reaction 2h with epoxy resin 100 weight portions and a phenyl silanetriol monomer, prepare the EP-CAB copolymer;
The 3rd step, in the EP-CAB copolymer, add 100 weight portion curing systems, the back injection molding that stirs vacuumizes, be cured behind the 1.5h, condition of cure be earlier 85 ℃ solidify 1.5h, 125 ℃ of curing 2.5h again, obtain solidified sample;
The 4th step, carry out performance test according to international standard GB/T1034-1998, the actual measurement water absorption rate is 0.2015%, and heat decomposition temperature is 219 ℃, and simultaneously light transmittance is 84.93%.
Embodiment 4: with thermosetting epoxy resin (EP) is matrix resin, with synthetic organic silicon monomer and matrix resin reaction, prepares the transparent LED encapsulating material of high moisture-proof heat, and it is following that it specifically prepares process:
The first step, in mixture of ice and water, in the mixed solution of 150ml deionized water and 10ml acetone, dropwise add 10g～30g one phenyl trichlorosilane, the reaction 30min; Filtration obtains crude product; Further it is dissolved in the acetone, utilizes a large amount of deionized waters and sodium carbonate to regulate PH, filter to neutral; 60 ℃ of following vacuumize 2h obtain a phenyl silanetriol monomer (CAB);
Second step, under 80～90 ℃ of reaction temperatures, be 15 weight portion generation grafting polycondensation reaction 1h with epoxy resin 100 weight portions and a phenyl silanetriol monomer, prepare the EP-CAB copolymer;
The 3rd step, in the EP-CAB copolymer, add 100 weight portion curing systems, the back injection molding that stirs vacuumizes, be cured behind the 0.5h, condition of cure be earlier 75 ℃ solidify 0.5h, 115 ℃ of curing 1.5h again, obtain solidified sample;
The 4th step, carry out performance test according to international standard GB/T1034-1998, the actual measurement water absorption rate is 0.2018%, and heat decomposition temperature is 216 ℃, and simultaneously light transmittance is 84.56%.
Claims (4)
1. the preparation method of the transparent LED encapsulating material of one kind high moisture-proof heat, specific as follows:
The first step, in mixture of ice and water, in the mixed solution of deionized water and acetone, dropwise add a phenyl trichlorosilane, behind the sufficient reacting; Filtration obtains crude product; Further crude product is dissolved in the acetone, utilizes a large amount of deionized waters and sodium carbonate to regulate PH, filter to neutral; 60 ℃ of following vacuumize 1～3h obtain a phenyl silanetriol monomer;
Second step, under 80～90 ℃ of conditions of reaction temperature, with epoxy resin 100 weight portions be less than a phenyl silanetriol monomer generation grafting polycondensation reaction 1～2h of 20 weight portions, make epoxy resin-one phenyl silanetriol copolymer;
The 3rd goes on foot, in epoxy resin-one phenyl silanetriol copolymer, adds 100 weight portion curing systems; The back injection molding stirs; Vacuumize, be cured behind 0.5～1.5h, condition of cure be earlier 75～85 ℃ solidify 0.5～1.5h, again 115～125 ℃ solidify 1.5～2.5h.
2. the method for claim 1 is characterized in that step is following:
The first step, in mixture of ice and water, in the mixed solution of deionized water and acetone, dropwise add a phenyl trichlorosilane, behind the sufficient reacting; Filtration obtains crude product; Further crude product is dissolved in the acetone, utilizes a large amount of deionized waters and sodium carbonate to regulate PH, filter to neutral; 60 ℃ of following vacuumize 2h obtain a phenyl silanetriol monomer;
Second the step, under 80～90 ℃ of conditions of reaction temperature, the phenyl silanetriol monomer generation grafting polycondensation reaction 1.5h with epoxy resin 100 weight portions and 2 ~ 10 weight portions makes epoxy resin-one phenyl silanetriol copolymer;
The 3rd step, in epoxy resin-one phenyl silanetriol copolymer, add 100 weight portion curing systems, the back injection molding that stirs vacuumizes, be cured behind the 1h, condition of cure be earlier 80 ℃ solidify 1h, 120 ℃ of curing 2h again.
3. method as claimed in claim 2 is characterized in that:
In said second step, a phenyl silanetriol monomer is 2 ~ 5 weight portions.
4. method as claimed in claim 2 is characterized in that:
In said second step, a phenyl silanetriol monomer is 7 ~ 10 weight portions.
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| CN109384905A (en) * | 2017-08-03 | 2019-02-26 | 湘潭大学 | A kind of over-expense SiClx skeleton bisphenol-a derivative epoxy acrylic resin and preparation method |
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| CN1560106A (en) * | 2004-03-10 | 2005-01-05 | 中国科学院广州化学研究所 | Modified epoxy resin by organic silicon and its electronic packag material and preparation process thereof |
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| CN1560106A (en) * | 2004-03-10 | 2005-01-05 | 中国科学院广州化学研究所 | Modified epoxy resin by organic silicon and its electronic packag material and preparation process thereof |
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| Title |
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| 刘宝成.环氧改性有机硅树脂技术研究.《涂料工业》.2008,第38卷(第12期),第26-29页. * |
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