CN101880396A - Preparation method of organic silicon rubber for encapsulating LED being convenient for vacuum defoamation - Google Patents
Preparation method of organic silicon rubber for encapsulating LED being convenient for vacuum defoamation Download PDFInfo
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- CN101880396A CN101880396A CN 201010191041 CN201010191041A CN101880396A CN 101880396 A CN101880396 A CN 101880396A CN 201010191041 CN201010191041 CN 201010191041 CN 201010191041 A CN201010191041 A CN 201010191041A CN 101880396 A CN101880396 A CN 101880396A
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- Prior art keywords
- methyl
- glue
- silicon
- phenyl
- vacuum defoamation
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- -1 methyl-phenyl hydrogen Chemical compound 0.000 claims abstract description 82
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 64
- 239000003054 catalyst Substances 0.000 claims abstract description 59
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 54
- 239000001257 hydrogen Substances 0.000 claims abstract description 52
- 239000010703 silicon Substances 0.000 claims abstract description 45
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 36
- 239000003921 oil Substances 0.000 claims abstract description 32
- 239000003112 inhibitor Substances 0.000 claims abstract description 27
- 239000000203 mixture Substances 0.000 claims abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003292 glue Substances 0.000 claims description 71
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 68
- 229920002554 vinyl polymer Polymers 0.000 claims description 67
- 238000006116 polymerization reaction Methods 0.000 claims description 54
- 239000000463 material Substances 0.000 claims description 53
- 238000005538 encapsulation Methods 0.000 claims description 50
- 229920002545 silicone oil Polymers 0.000 claims description 43
- 239000000178 monomer Substances 0.000 claims description 40
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 22
- 239000003153 chemical reaction reagent Substances 0.000 claims description 17
- 229920001296 polysiloxane Polymers 0.000 claims description 17
- 238000010792 warming Methods 0.000 claims description 17
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 15
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- 230000006837 decompression Effects 0.000 claims description 10
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 238000004513 sizing Methods 0.000 claims description 8
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 7
- 125000003944 tolyl group Chemical group 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 4
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 claims description 4
- 238000007151 ring opening polymerisation reaction Methods 0.000 claims description 4
- 239000004945 silicone rubber Substances 0.000 claims description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 3
- 239000003729 cation exchange resin Substances 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003930 superacid Substances 0.000 claims description 3
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims description 2
- IRVZFACCNZRHSJ-UHFFFAOYSA-N 2,4,6,8-tetramethyl-2,4,6,8-tetraphenyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound O1[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si]1(C)C1=CC=CC=C1 IRVZFACCNZRHSJ-UHFFFAOYSA-N 0.000 claims description 2
- BVTLTBONLZSBJC-UHFFFAOYSA-N 2,4,6-tris(ethenyl)-2,4,6-trimethyl-1,3,5,2,4,6-trioxatrisilinane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O1 BVTLTBONLZSBJC-UHFFFAOYSA-N 0.000 claims description 2
- XHSOUGYKMNMDQP-UHFFFAOYSA-N 3,3,4-trimethylpent-1-yn-1-ol Chemical compound CC(C(C#CO)(C)C)C XHSOUGYKMNMDQP-UHFFFAOYSA-N 0.000 claims description 2
- YJPBJCZCYXJXLS-UHFFFAOYSA-N C(=C)[Si]C.[Si] Chemical compound C(=C)[Si]C.[Si] YJPBJCZCYXJXLS-UHFFFAOYSA-N 0.000 claims description 2
- ICBWCWQMJGVTAW-UHFFFAOYSA-N C1(=CC=CC=C1)[Si]C=C.[Si] Chemical compound C1(=CC=CC=C1)[Si]C=C.[Si] ICBWCWQMJGVTAW-UHFFFAOYSA-N 0.000 claims description 2
- KUBFVEPCKQPQEF-UHFFFAOYSA-N CCC[Si](O[SiH2]O[SiH](C)O1)(O[Si]1(F)F)F Chemical compound CCC[Si](O[SiH2]O[SiH](C)O1)(O[Si]1(F)F)F KUBFVEPCKQPQEF-UHFFFAOYSA-N 0.000 claims description 2
- WTQAKAPKTROVFY-UHFFFAOYSA-N C[SiH]1O[Si](O[Si](O1)(CCC)F)(F)F Chemical compound C[SiH]1O[Si](O[Si](O1)(CCC)F)(F)F WTQAKAPKTROVFY-UHFFFAOYSA-N 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 2
- YFCGDEUVHLPRCZ-UHFFFAOYSA-N [dimethyl(trimethylsilyloxy)silyl]oxy-dimethyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C YFCGDEUVHLPRCZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- NWEKXBVHVALDOL-UHFFFAOYSA-N butylazanium;hydroxide Chemical compound [OH-].CCCC[NH3+] NWEKXBVHVALDOL-UHFFFAOYSA-N 0.000 claims description 2
- HAURRGANAANPSQ-UHFFFAOYSA-N cis-2,4,6-Trimethyl-2,4,6-triphenylcyclotrisiloxane Chemical compound O1[Si](C)(C=2C=CC=CC=2)O[Si](C)(C=2C=CC=CC=2)O[Si]1(C)C1=CC=CC=C1 HAURRGANAANPSQ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004132 cross linking Methods 0.000 claims description 2
- 125000003963 dichloro group Chemical group Cl* 0.000 claims description 2
- JEWCZPTVOYXPGG-UHFFFAOYSA-N ethenyl-ethoxy-dimethylsilane Chemical compound CCO[Si](C)(C)C=C JEWCZPTVOYXPGG-UHFFFAOYSA-N 0.000 claims description 2
- NUFVQEIPPHHQCK-UHFFFAOYSA-N ethenyl-methoxy-dimethylsilane Chemical group CO[Si](C)(C)C=C NUFVQEIPPHHQCK-UHFFFAOYSA-N 0.000 claims description 2
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 claims description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 2
- 125000005395 methacrylic acid group Chemical group 0.000 claims description 2
- RFGGTTPASBFBTB-UHFFFAOYSA-N methyl-[methyl(diphenyl)silyl]oxy-diphenylsilane Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(C)O[Si](C)(C=1C=CC=CC=1)C1=CC=CC=C1 RFGGTTPASBFBTB-UHFFFAOYSA-N 0.000 claims description 2
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 2
- UXRVNHHPRRDXJG-UHFFFAOYSA-M phosphane tetrabutylazanium hydroxide Chemical compound P.[OH-].C(CCC)[N+](CCCC)(CCCC)CCCC UXRVNHHPRRDXJG-UHFFFAOYSA-M 0.000 claims description 2
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 2
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 2
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 2
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 2
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N tetrahydrofuran Substances C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims 4
- 238000002834 transmittance Methods 0.000 abstract description 28
- 238000000034 method Methods 0.000 abstract description 7
- 229920001971 elastomer Polymers 0.000 abstract 2
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 abstract 2
- 229920005601 base polymer Polymers 0.000 description 37
- 239000000047 product Substances 0.000 description 25
- 150000002431 hydrogen Chemical class 0.000 description 20
- 125000004429 atom Chemical group 0.000 description 17
- 238000005987 sulfurization reaction Methods 0.000 description 15
- JQZGUQIEPRIDMR-UHFFFAOYSA-N 3-methylbut-1-yn-1-ol Chemical compound CC(C)C#CO JQZGUQIEPRIDMR-UHFFFAOYSA-N 0.000 description 14
- 239000003431 cross linking reagent Substances 0.000 description 14
- 238000005227 gel permeation chromatography Methods 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 14
- 238000005160 1H NMR spectroscopy Methods 0.000 description 13
- 238000009826 distribution Methods 0.000 description 13
- 238000001035 drying Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 238000000354 decomposition reaction Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 10
- 230000005855 radiation Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 239000003822 epoxy resin Substances 0.000 description 4
- 229920000647 polyepoxide Polymers 0.000 description 4
- 239000000565 sealant Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 235000010290 biphenyl Nutrition 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- NOKUWSXLHXMAOM-UHFFFAOYSA-N hydroxy(phenyl)silicon Chemical compound O[Si]C1=CC=CC=C1 NOKUWSXLHXMAOM-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229920000260 silastic Polymers 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 239000005046 Chlorosilane Substances 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- LAQFLZHBVPULPL-UHFFFAOYSA-N methyl(phenyl)silicon Chemical compound C[Si]C1=CC=CC=C1 LAQFLZHBVPULPL-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Abstract
The invention relates to a preparation method of organic silicon rubber for encapsulating LED being convenient for vacuum defoamation, which aims at solving the technical problems that the surface tension of LED encapsulating silicon rubber is reduced, so the LED encapsulating silicon rubber is convenient for the vacuum defoamation, and the transmittance of the product is improved. The method comprises the following steps that: 1) transparent vinyl silicon oil containing methyl trifluoropropyl silica chain link and methyl-phenyl silica chain link is prepared; 2) transparent vinyl silicon oil is configured with methyl-phenyl hydrogen-containing silicon oil, platinum catalyst and inhibitor to A/B rubber; the mol ratio of Si-H and Si-Vi is 0.8 to 3: 1; the hydrogen content of the methyl-phenyl hydrogen-containing silicon oil is 1.6 to 1.0*10<-6> percent by weight; 3) A/B rubber is uniformly mixed, after being vacuum defoamed at the room temperature, the mixture is vulcanized to a product.
Description
Technical field
The present invention relates to a kind of have no report, contain methyl trifluoro propyl silica chain link and aminomethyl phenyl silica chain link, be convenient to the LED encapsulation of vacuum defoamation with the preparation method of organic silicon rubber. Silicon rubber of the present invention has good performance, such as high refractive index, high transmission rate, radiation hardness, high-low temperature resistant, weather-proof, can be used as the LED encapsulating material, also is expected as other fluid sealant, casting glue and adhesive.
Background technology
The electric energy that the light emitting diode of super brightness (LED) consumes only is 1/10 of conventional light source, have the characteristics such as the mercury, the volume that do not use serious environment pollution are little, the life-span is long, at first enter the special lighting fields such as industrial equipment, instrument and meter, traffic lights, automobile, backlight. Along with the improvement of ultra-high brightness LED performance, power-type LED be expected to replace the conventional light source such as incandescent lamp, fluorescent lamp and become the 4th generation lighting source.
The LED encapsulating material need to have excellent light efficiency, high refractive index (n D 25 1.50) and high transmission rate (namely (in 400 ~ 800nm) scopes, light transmittance is greater than 98%, 10mm) at visible light. Have nearly 30 years history with the bisphenol A-type transparent epoxy resin as the common LED encapsulating material, but in the face of complicated environmental conditions such as the residing high temperature of power-type LED, high uitraviolet intensities, epoxy resin exposes the performance deficiencies such as easy xanthochromia, embrittlement, can't adapt to the power-type LED growth requirement.
Organosilicon material is comparatively ideal LED encapsulating material, and throw light on both at home and abroad relevant enterprise and scientific research institution have dropped into a large amount of manpower and materials one after another, and the LED organosilicon material for packaging is studied widely. Add-on type liquid silicon rubber can be made the LED encapsulating material. JP, 2006-324596 report 165 ℃ of lower injection mo(u)ldings, obtain shrinkage factor and are 3.37% with add-on type liquid silicon rubber, shrinkage ratio only 0.04, the encapsulating material of index of refraction 1.50 ~ 1.60. US2007-7291691 in addition also obtained Shao Er D hardness up to 50 degree, elastic modelling quantity 350 ~ 1500MPa, light transmittance 88% ~ 92%(wavelength 400nm, thickness of sample 4mm) the LED encapsulating material. In add-on type liquid silicon rubber, add heat resistance and the radiation resistance that an amount of inorganic filler (such as the oxide of boron, silicon, titanium, aluminium, zinc etc.) can improve material, with 450 ~ 470nm wavelength light irradiation 1000h, light transmittance is declined by less than 10% to gained LED encapsulating material under 140 ℃. Generally speaking, the LED encapsulating material need to vulcanize 2 ~ 5h at a certain temperature, and the production cycle is longer. US2008-7314770 D4With 1,3-divinyl-1,1,3,3 ,-tetramethyl disiloxane (vinyl double-seal head) ring-opening polymerisation under sulphuric acid catalysis obtains vinyl silicone oil; Then add in proportion containing hydrogen silicone oil, platinum catalyst and emulsion, mix and get final product completion of cure with visible light or UV-irradiation 2.5 ~ 20min afterwards, obtain preferably LED encapsulating material of performance.
Vinyl polysiloxane and containing hydrogen silicone oil can prepare organosilicon LED encapsulating material by the hydrosilylation sulfidization molding. In order to obtain high refractive index, radiation-resistant organosilicon encapsulating material, vinyl polysiloxane and containing hydrogen silicone oil generally need contain a certain amount of diphenyl silica chain link or aminomethyl phenyl silica chain link. US2004-0116640 and US2007-7294682 report make vinyl polysiloxane with chlorosilane cohydrolysis condensation process, then with itself and the containing hydrogen silicone oil sulfidization molding under platinum catalyst catalysis that contains phenyl silica chain link, obtain the LED encapsulating material。The index of refraction of this material can reach 1.51, Shao Er hardness D75 ~ 85 degree, bending strength 95 ~ 135MPa, and hot strength 5.4MPa, light transmittance reduces to 92% by 95% behind the ultraviolet radiation 500h. In order to reduce the shrinkage factor of this class organosilicon material, improve its cold-hot circulation impact performance, can improve the mass fraction of phenyl in the encapsulating material, thereby obtain that shrinkage factor is low, radiation hardness, heat-resisting, light transmittance reach 95% encapsulating material; Even can obtain to have excellent mechanical performance and adhesive property, can stand 1000-50 ℃/150 ℃ cold cycling and impact and indehiscent organosilicon encapsulating material. Owing to do not pass through reinforcement, the mechanical strength of these organosilicon encapsulating materials is relatively poor, still can not satisfy some specification requirement of LED encapsulating material. JP2005-0212008A1 and EP, 2004-1424363A1 adds fume colloidal silica, heat filling, light wave adjusting agent, fire retardant etc. in methyl and phenyl hydrogen-containing silicon oil and vinyl polysiloxane, behind 120 ~ 180 ℃ of lower curing 30 ~ 180min, the bending strength of encapsulating material is 95 ~ 100MPa, hot strength is 5.4MPa, Shao Er hardness D75 ~ 85 degree, index of refraction is up to 1.51; Light transmittance reduces to 92% from 95% behind 400nm radiation of light source 100h, still is 92% behind the irradiation 500h.
Blend and containing hydrogen silicone oil with vinyl polysiloxane and vinyl silicone oil vulcanize by silicon hydrogen additive process, can bring into play separately advantage of silicones and silicon rubber, obtain high-performance LED encapsulation material. The index of refraction 1.54 of the LED encapsulating material that US2007-7282270 obtains in this way, light transmittance 85 ~ 100%, shore a hardness 45 ~ 95 degree, hot strength 1.8MPa crackle just occurs on 150 ℃ of lower heating 100h surfaces.
The recent years correlative study also begins to enliven, (CN1978526 and CN101085855) such as the Huang Wei of Institute of Chemistry, Academia Sinica prepared the organic silicon epoxy resin composition of a kind of anti-ultraviolet and high temperature ageing, by blend, cast, curing molding, acquisition has good optical transparence and good uvioresistant, high-temperature aging resisting performance, can be used for the power type LED encapsulation material. The trip of Fudan University involves (CN101525466 and CN101525467) report epoxy resin, organic siliconresin, the acid inorganic nano-particles etc. such as Tang Yong, mix by simple physical, sulfidization molding under acid inorganic nano-particle catalytic action, obtain epoxy/organosilicon/inorganic, can be used as the LED encapsulating material. But these encapsulating materials all contain epoxide group, still have the defectives such as easy xanthochromia.
The Chengdu Guibao Technology Co., Ltd bear is graceful, Qiu Zehao, Yuan Sulan and Wang Youzhi (CN101544881) with α, alpha, omega-dihydroxy polydimethyl siloxane is primary raw material, with filler, plasticizer, crosslinking agent, coupling agent and catalyst mix, prepared silicone pouring sealant, it is simple to have technological process, and adhesive property is good, and heatproof and weather-resistant property are excellent, mobile performance is good, can be widely used in the embedding of the electronic devices such as LED photoelectric display device. Mainly take methyl silica chain link as main chain, index of refraction is lower for this class encapsulating material.
(CN101016446) such as the Su Junliu of Beiteli New Material Co., Ltd., Dongguan City prepares the LED organosilicon material for packaging with ethenyl blocking PSI, vinyl methyl silicon resin, poly-methyl hydrogen phenyl siloxane, catalyst and inhibitor mixed, light transmittance can reach 99%, refractive index can reach 1.49～1.53, is suitable for very much the encapsulation of the electronic products such as LED. (CN101381516) such as Lee Tsing-Hua University of Shanghai University invented the room temperature vulcanized organosilicon pouring sealant that a kind of LED uses, to be obtained by the addition of silicon hydrogen by ethenyl blocking PSI, vinyl-dimethyl base silyloxy end-blocking dimethyl silicone polymer, poly-methyl hydrogen phenyl siloxane and inhibitor methyl butynol, have good heat resistance, moisture-proof, light transmittance can reach 99%, and refractive index can reach 1.47 ~ 1.55. But these two patented product main chains are that its resistance to ultraviolet radiation can have much room for improvement with diphenyl silica chain link.
In the LED encapsulation process, need to carry out vacuum defoamation. If deaeration is unclean, the bubble difficulty is overflowed after the sizing material encapsulation, and meeting after the sulfuration affects light transmittance and the product quality of LED so that bubble is arranged in the encapsulating material. Silicon rubber for the low full methyl silica of index of refraction chain link because the surface tension of its raw material is lower, is easy to deaeration. And for the encapsulating material of high refractive index, because containing aminomethyl phenyl silica chain link or diphenyl silica chain link, because phenyl is sterically hindered larger, viscosity is larger, and its surface tension is large, and vacuum defoamation is just not too easy. Above-mentioned patent does not all relate to this point.
For the ease of vacuum defoamation, can add the material of low surface tension, but because index of refraction and the LED encapsulating material index of refraction difference of these materials are larger, can affect the light transmittance of encapsulating material, even can not get transparent encapsulating material. Reasonable way is to introduce some groups in the encapsulating material strand, reduces the surface tension of encapsulating material, can guarantee like this light transmittance of material, can be convenient to vacuum defoamation again. Usually, fluorine-containing polysiloxanes surface tension is lower. Therefore, the present invention uses in the organosilicon vinyl base polymer process, to dimethyl cyclosiloxane (D in preparation LED encapsulationn, n=3,4,5, etc), methyl ethylene cyclosiloxane (Dn Me，Vi, n=3,4,5, etc), methyl phenyl ring siloxane (Dn Me,PhN=3,4,5, etc) etc. add an amount of methyl trifluoro propyl cyclosiloxane, ring-opening copolymerization under catalyst action in the raw material, obtain on the one hand the vinyl base polymer of high refractive index, high transmission rate, in the product molecule, introduce methyl trifluoro propyl silica chain link on the other hand, reduced the surface tension of product, obtain to be convenient to the LED encapsulation organic silicon rubber of vacuum defoamation.
Summary of the invention
The technical issues that need to address of the present invention are that the surface tension of reduction LED encapsulation silicon rubber so that LED encapsulation silicon rubber is convenient to vacuum defoamation, reduces the defect rate during LED encapsulates, the light transmittance of raising product.
The LED encapsulation of the being convenient to vacuum defoamation of the present invention preparation method of organic silicon rubber is characterized in that in the steps below:
1) transparent vinyl base silicone oil preparation: at N2Protection is lower to add end-capping reagent in the polymerization single polymerization monomer that dewaters through decompression, carry out the ring-opening copolymerization reaction under catalyst action; By adding thermal decomposition or removing by filter catalyst, then the lower high temperature removal low molecular compound of decompression was cooled to room temperature, namely gets the transparent vinyl base silicone oil that contains methyl trifluoro propyl silica chain link and aminomethyl phenyl silica chain link after polymerisation was complete;
Above-mentioned polymerisation general formula is as follows:
D whereinn，D
n Me,Vi，D
n Me,Ph，D
n Me，FChemical structural formula is as follows:
The transparent vinyl base silicone oil structural formula that obtains is ViMe2(MeViSiO)
m(MePhSiO)
p(Me
2SiO)
q(MeCH
2CH
2CF
3SiO)
kMe
2Vi, wherein, m, p, q and K are 0 or positive integer, 0≤m≤580,0≤p≤3308,0≤q≤3289,0≤k≤384, and satisfy m/ (m+p+q+k)=0 ~ 0.1, p/ (m+p+q+k)=0.5 ~ 0.9, q/ (m+p+q+k)=0.1 ~ 0.5, k/ (m+p+q+k)=0 ~ 0.12; The vinyl silicone oil molecular weight is 500 ~ 50 * 104 。Transparent vinyl base silicone molecule amount is 500 ~ 50 * 104, refraction index nD 25Be 1.50 ~ 1.54, it can be used as the base polymer that silicon rubber is used in the LED encapsulation.
2) with gained transparent vinyl base silicone oil and crosslinking agent---methyl and phenyl hydrogen-containing silicon oil, platinum catalyst and inhibitor are mixed with A/B glue in the step 1); A glue is the mixture of transparent vinyl base silicone oil, platinum catalyst and inhibitor, and the platinum catalyst consumption is 2 ~ 50ppm of organic silicon rubber sizing material gross mass according to the pt atom quality, and the inhibitor consumption is 1 ~ 100:1 according to inhibitor and pt atom mol ratio; B glue is methyl and phenyl hydrogen-containing silicon oil, the perhaps mixture of methyl and phenyl hydrogen-containing silicon oil and transparent vinyl base silicone oil, and wherein the methyl and phenyl hydrogen-containing silicon oil consumption is 0.01 ~ 99.99% of B glue weight; Total consumption of transparent vinyl base silicone oil is in the A/B glue, after A/B glue mixes, make Si-H(silicon-hydrogen wherein) with Si-Vi(silicon-vinyl) mol ratio is that 0.8 ~ 3:1(is preferably 1 ~ 1.5:1); The hydrogen content of above-mentioned methyl and phenyl hydrogen-containing silicon oil is 1.6wt% ~ 1.0 * 10-6wt％；
3) A/B glue is mixed, at room temperature after the vacuum defoamation, sulfidization molding is made LED encapsulation organic silicon rubber;
In the step 1), described polymerization single polymerization monomer is comprised of dimethyl cyclosiloxane, methyl ethylene cyclosiloxane, methyl phenyl ring siloxane and methyl trifluoro propyl cyclosiloxane; Wherein, the dimethyl cyclosiloxane is 10 ~ 50mol% of polymerization single polymerization monomer total amount, and the methyl ethylene cyclosiloxane is 0.002 ~ 10mol% of polymerization single polymerization monomer total amount, and the methyl trifluoro propyl cyclosiloxane is 0.05 ~ 12mol% of polymerization single polymerization monomer total amount; Methyl phenyl ring siloxane be the polymerization single polymerization monomer total amount all the other the mole very;
Above-mentioned dimethyl cyclosiloxane is one or more in hexamethyl cyclotrisiloxane, octamethylcy-clotetrasiloxane, the decamethylcyclopentaandoxane, or dimethyl ring siloxane mixture (DMC); Above-mentioned methyl ethylene cyclosiloxane is one or more in trimethyl trivinyl cyclotrisiloxane, tetramethyl tetrem thiazolinyl cyclotetrasiloxane, the pentamethyl five vinyl D5s; Above-mentioned methyl phenyl ring siloxane is one or more in trimethyl triphenyl cyclotrisiloxane, tetramethyl tetraphenyl cyclotetrasiloxane, pentamethyl pentaphene basic ring five siloxanes, or the aminomethyl phenyl mixed methylcyclosiloxane; Above-mentioned methyl trifluoro propyl cyclosiloxane is one or more in methyl trifluoro propyl cyclotrisiloxane, methyl trifluoro propyl cyclotetrasiloxane, the methyl trifluoro propyl D5;
Described end-capping reagent is dimethyl vinyl methoxy silane, Vinyldimethylethoxysilane, 1,1,3,3-tetramethyl-1,3-divinyl disiloxane, α, ω-divinyl silicone oil, α, ω-three silicon methyl vinyl silicon oil, α, the silica-based vinyl silicone oil of ω-3,5-dimethylphenyl, α, ω-three silicon phenyl-vinyl silicon oil, HMDO, decamethyl tetrasiloxane, 1,3-dimethyl-1,1,3,3-tetraphenyl-disiloxane, α, ω-divinyl polysiloxanes, α, ω-three silicon methyl polysiloxane, α, the silica-based polysiloxanes of ω-3,5-dimethylphenyl, α, one or more in the ω-three silicon phenyl polysiloxane;
Described catalyst is 98% concentrated sulfuric acid, CF3SO
3Among H, phosphoric acid, Emathlite, storng-acid cation exchange resin, rare-earth solid superacid, TMAH, TMAH silicon alkoxide, tetraethyl ammonium hydroxide, tetraethyl ammonium hydroxide silicon alkoxide, TBAH, 4-n-butyl ammonium hydroxide, 4-n-butyl ammonium hydroxide silicon alkoxide, tetrabutylammonium hydroxide phosphine, tetrabutylammonium hydroxide phosphine silicon alkoxide, the KOH one or more;
Described platinum catalyst is chloroplatinic acid, H2PtCl
6Isopropyl alcohol (i-PrOH) solution, H2PtCl
6Oxolane (THF) solution, Pt (PPh3)
4、Cp
2PtCl
2, the coordination of ethylene methacrylic radical siloxane the platinum complex of platinum complex, dicyclopentadiene platinous chloride, dichloro two (triphenylphosphine) of platinum complex, diethyl phthalate coordination in a kind of;
Described inhibitor is a kind of in quinoline, pyridine, TBHP, propilolic alcohol, the tetramethyl butynol;
The polymeric reaction temperature of step 1) is 20 ~ 100 ℃, and polymerization reaction time is 1 ~ 20h; The lower high temperature removal low molecular compound of decompression progressively is warming up to 205 ℃ under-0.096MPa carries out;
The step 3) room temperature vacuum defoamation time is 1 ~ 60min, and curing temperature is 20 ~ 150 ℃.
As preferably, the temperature that the decompression of step 1) polymerization single polymerization monomer dewaters is that 35 ~ 45 ℃/pressure is 0.096Mpa; Polymeric reaction temperature is 80 ~ 100 ℃, and polymerization time is 1 ~ 5h; Decompression progressively is warming up to 205 ℃ when removing low molecular compound under-0.096MPa; The step 3) room temperature vacuum defoamation time is 5 ~ 40min, and curing temperature is 80 ~ 120 ℃.
As preferably, when platinum catalyst is H2PtCl
6Isopropyl alcohol (i-PrOH) solution, H2PtCl
6Oxolane (THF) solution, ethylene methacrylic radical siloxane platinum complex in a kind of the time, its consumption is that 2 ~ 30ppm(optimum of silicone rubber compounds gross mass is 2 ~ 10ppm) according to the pt atom quality.
For the deficiencies in the prior art, use in the vinyl base polymer preparation process of organic silicon rubber in the LED encapsulation, in the product molecule, introduce a certain amount of methyl trifluoro propyl silica chain link, reduced the surface tension of product, so that the LED organosilicon material for packaging is convenient to vacuum defoamation, solved that product is difficult to vacuum defoamation in the LED encapsulation, affected this problem of product quality.
With the silicon rubber of method preparation of the present invention, be a kind of report that has no, contain the methyl phenyl silicone rubber of methyl trifluoro propyl silica chain link and aminomethyl phenyl silica chain link.
Compare with background technology, the present invention introduces trifluoro propyl silica chain link in the vinyl silicone oil molecule that contains aminomethyl phenyl silica chain link, reduced the surface tension of LED encapsulation with silicon rubber, so that the LED encapsulating material of preparation is convenient to vacuum defoamation, improve the light transmittance of LED encapsulating material, reduced the defect rate of LED device. In addition, gained LED encapsulation also has good performance with organic silicon rubber, as has long operable time, high refractive index, high transmission rate, radiation hardness, high-low temperature resistant, weather-proof, also is expected as other fluid sealant, casting glue and adhesive.
Description of drawings
Fig. 1 is that the methyl trifluoro propyl silica chain link of different content is on the impact of sulfidization molding silastic product performance. The gained silastic product is that the methyl phenyl vinyl silicone oil that contains methyl trifluoro propyl silica chain link and aminomethyl phenyl silica chain link take the present invention preparation is as base polymer, mix according to Si-H:Si-Vi=1.2:1, and add sizing material 5ppm platinum catalyst and be the methyl butynol of 30:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, and respectively after 5min, 10min, 20min and 30min vacuum defoamation, get through room temperature vacuum row bubble and intensification curing molding. Wherein
Fig. 1 a is not for adding D3 Me,F；
Fig. 1 b is for adding 1mol%D3 Me,F, methyl trifluoro propyl silica chain link content 0.7mol% in the vinyl base polymer;
Fig. 1 c is for adding 3mol%D3 Me,F, methyl trifluoro propyl silica chain link content 1.44mol% in the vinyl base polymer;
Fig. 1 d is for adding 5mol%D3 Me,F, methyl trifluoro propyl silica chain link content 4.28mol% in the vinyl base polymer;
Fig. 1 e is for adding 7mol%D3 Me,F, methyl trifluoro propyl silica chain link content 5.3mol% in the vinyl base polymer.
The electron micrograph (100 times of multiplication factors) of sample can be found out after the above sulfuration, when methyl trifluoro propyl ring silica consumption is the 5-7mol% left and right sides, can remove well bubble.
Fig. 2 is different methyl trifluoro propyl silica chain link content and the capillary linear relationship of vinyl base polymer, can find out, along with the increase of methyl trifluoro propyl silica chain link content, the surface tension of vinyl base polymer reduces gradually.
The specific embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
The present invention can further specify by following embodiment, but embodiment is not limiting the scope of the invention.
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, gel chromatography (GPC, take THF as mobile phase, polystyrene is standard specimen, and is lower same) records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio (Ph/Si, lower same) are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to (thickness of sample 10mm, lower same) more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 1.2:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, add the 5ppm platinum catalyst, be the ratio adding methyl butynol of 30:1 according to inhibitor and pt atom mol ratio simultaneously, be mixed with A/B glue; Crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.1wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain the LED encapsulation and (see Fig. 1 a) with silicon rubber.
1) at N2Protection is lower to add monomer D in the there-necked flask of 250mL dryingn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4（9.305g，0.0314mol）、D
3 Me,F(1.1573g, 0.00247mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), the 6.23g rare-earth solid superacid is at N2Protection is lower, and then 100 ℃ of lower polymerization 5h remove by filter catalyst. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min, be cooled to room temperature, namely get the water white transparency product, be the vinyl base polymer of LED encapsulation silicon rubber, record its index of refraction n with abbe's refractometerD 25=1.5315, GPC records number-average molecular weight 0.65 * 104, molecular weight distribution width (MWD) is 1.64, warp1H-NMR records Si-Vi quality percentage composition 4.47 * 10-4Mol/g, Ph/Si are 0.784. Methyl trifluoro propyl silica chain link content 0.7mol% records surface tension 31.439mN/m with surface tension instrument, and light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) containing hydrogen silicone oil is mixed according to Si-H:Si-Vi=1.2:1 with gained vinyl base polymer, and add sizing material 5ppm platinum catalyst and be the methyl butynol of 30:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.1wt% of B glue gross mass in the B glue.
3) with gained A/B glue after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain the LED encapsulation with silicon rubber (seeing Fig. 1 b).
1) at N2Protection is lower to add monomer D in the there-necked flask of 250mL dryingn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（1.075g，0.035mol）、D
4（7.842g，0.02649mol）、D
3 Me,F(3.4719g, 0.00741mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), the 6.23g storng-acid cation exchange resin is at N2Protection is lower, and then 100 ℃ of lower polymerization 5h remove by filter catalyst. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min, be cooled to room temperature, namely get the water white transparency product, be the vinyl base polymer of LED encapsulation silicon rubber, record its index of refraction n with abbe's refractometerD 25=1.5305, GPC records number-average molecular weight 0.40 * 104, molecular weight distribution width (MWD) is 1.64, warp1It is 4.60 * 10 that H-NMR records Si-Vi content-4Mol/g, Ph/Si are 0.806, and methyl trifluoro propyl silica chain link content 1.44mol% records surface tension 29.318mN/m with surface tension instrument, and light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) containing hydrogen silicone oil is mixed according to Si-H:Si-Vi=1.2:1 with gained vinyl base polymer, and add sizing material 5ppm platinum catalyst and be the methyl butynol of 30:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.1wt% of B glue gross mass in the B glue.
3) with gained A/B glue after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain the LED encapsulation with silicon rubber (seeing Fig. 1 c).
Embodiment 4
1) at N2Protection is lower to add monomer D in the there-necked flask of 250mL dryingn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（1.075g，0.035mol）、D
4（6.379g，0.02155mol）、D
3 Me,F(5.7865g, 0.01235mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), 2.48g tetraethyl ammonium hydroxide silicon alkoxide is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min, be cooled to room temperature, namely get the water white transparency product, be the vinyl base polymer of LED encapsulation silicon rubber, record its index of refraction n with abbe's refractometerD 25=1.5290, GPC records number-average molecular weight 0.61 * 104, molecular weight distribution width (MWD) is 1.58, warp1H-NMR records Si-Vi quality percentage composition 3.6 * 10-4Mol/g, Ph/Si are 0.798, and methyl trifluoro propyl silica chain link content 4.28mol% records surface tension 26.869mN/m with surface tension instrument, and light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) containing hydrogen silicone oil is mixed according to Si-H:Si-Vi=1.2:1 with gained vinyl base polymer, and add sizing material 5ppm platinum catalyst and be the methyl butynol of 30:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.1wt% of B glue gross mass in the B glue.
3) with gained A/B glue after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain the LED encapsulation with silicon rubber (seeing Fig. 1 d).
1) at N2Protection is lower to add monomer D in the there-necked flask of 250mL dryingn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（1.075g，0.035mol）、D
4（4.917g，0.01661mol）、D
3 Me,F(8.1011g, 0.01729mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), the 6.23g Emathlite is at N2Protection is lower, and then 100 ℃ of lower polymerization 5h remove by filter catalyst. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5275, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 3.6 * 10 that H-NMR records Si-Vi content-4Mol/g, the Ph/Si(mol ratio) be 0.797, methyl trifluoro propyl silica chain link content 5.3mol% records surface tension 25.333mN/m with surface tension instrument, and light transmittance is up to 96% when recording 800nm with ultraviolet specrophotometer.
2) containing hydrogen silicone oil is mixed according to Si-H:Si-Vi=1.2:1 with gained vinyl base polymer, and add sizing material 5ppm platinum catalyst and be the methyl butynol of 30:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.1wt% of B glue gross mass in the B glue.
3) with gained A/B glue after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain the LED encapsulation with silicon rubber (seeing Fig. 1 e).
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 0.8:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, adding 15ppm platinum catalyst, while is the ratio adding methyl butynol of 50:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.08wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 120 ℃ of lower sulfuration 2h, obtain LED encapsulation silicon rubber.
Embodiment 7
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 1.5:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, adding 8ppm platinum catalyst, while is the ratio adding methyl butynol of 20:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 30wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain LED encapsulation silicon rubber.
Embodiment 8
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 2:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, adding 8ppm platinum catalyst, while is the ratio adding methyl butynol of 50:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 80wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain LED encapsulation silicon rubber.
Embodiment 9
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 3.5:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, adding 8ppm platinum catalyst, while is the ratio adding methyl butynol of 100:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 99.9wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain LED encapsulation silicon rubber.
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 1.2:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, adding the 8ppm platinum catalyst is the ratio adding propilolic alcohol of 30:1 simultaneously according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.01wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 100 ℃ of lower sulfuration 2h, obtain LED encapsulation silicon rubber.
Embodiment 11
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 1.5:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, adding 8ppm platinum catalyst, while is the ratio adding methyl butynol of 30:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 15wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 150 ℃ of lower sulfuration 1h, obtain LED encapsulation silicon rubber.
Embodiment 12
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 1.5:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, adding 8ppm platinum catalyst, while is the ratio adding methyl butynol of 1:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.1wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 80 ℃ of lower sulfuration 3h, obtain LED encapsulation silicon rubber.
Embodiment 13
1) at N2Protection is lower to add in the there-necked flask of 250mL dryingPolymerizationMonomer Dn Me,Ph（109.75g，0.2022mol）、D
4 Me,Vi（4.3g，0.035mol）、D
4(10.035g, 0.0339mol). 35 ℃ ~ 45 ℃/-remove the moisture content in the monomer under the 0.096MPa, then add end-capping reagent 1,1,3,3-tetramethyl-1,3-divinyl disiloxane (0.93g, 0.005mol), catalyst TMAH silicon alkoxide 2.48g is at N2Protection is lower, 100 ℃ of lower polymerization 5h, then at 150 ℃ of lower decomposition catalyst 3-4h until tail gas be neutrality. Be decompressed to-0.096MPa, be warming up to gradually 205 ℃ and remove low molecular compound, stopped heating when not having cut in the 5min is cooled to room temperature, gained water white transparency product is the vinyl base polymer of LED encapsulation silicon rubber, records its index of refraction n with abbe's refractometerD 25=1.5350, GPC records number-average molecular weight 0.83 * 104, molecular weight distribution width (MWD) is 1.81, warp1It is 4.56 * 10 that H-NMR records Si-Vi content-4Mol/g, aminomethyl phenyl silica chain link and silicon atom mol ratio are 0.784. Record surface tension 32.312mN/m with surface tension instrument, light transmittance is up to more than 98% when recording 800nm with ultraviolet specrophotometer.
2) be that 1.5:1 mixes with containing hydrogen silicone oil and gained vinyl base polymer according to the mol ratio of Si-H and Si-Vi, adding 2ppm platinum catalyst, while is the ratio adding methyl butynol of 1:1 according to inhibitor and pt atom mol ratio, be mixed with A/B glue, crosslinking agent methyl and phenyl hydrogen-containing silicon oil quality is the 0.1wt% of B glue gross mass in the B glue.
3) with gained A/B glue respectively after vacuum defoamation, at 80 ℃ of lower sulfuration 5h, obtain LED encapsulation silicon rubber.
Claims (6)
1. organic silicon rubber is used in a LED encapsulation of being convenient to vacuum defoamation, it is characterized in that in the steps below:
1) transparent vinyl base silicone oil preparation: at N2Protection is lower to add end-capping reagent in the polymerization single polymerization monomer that dewaters through decompression, carry out the ring-opening copolymerization reaction under catalyst action; By adding thermal decomposition or removing by filter catalyst, then the lower high temperature removal low molecular compound of decompression was cooled to room temperature, namely gets the transparent vinyl base silicone oil that contains methyl trifluoro propyl silica chain link and aminomethyl phenyl silica chain link after polymerisation was complete;
2) with gained transparent vinyl base silicone oil and crosslinking agent---methyl and phenyl hydrogen-containing silicon oil, platinum catalyst and inhibitor are mixed with A/B glue in the step 1); A glue is the mixture of transparent vinyl base silicone oil, platinum catalyst and inhibitor, and the platinum catalyst consumption is 2 ~ 50ppm of organic silicon rubber sizing material gross mass according to the pt atom quality, and the inhibitor consumption is 1 ~ 100:1 according to inhibitor and pt atom mol ratio; B glue is methyl and phenyl hydrogen-containing silicon oil, the perhaps mixture of methyl and phenyl hydrogen-containing silicon oil and transparent vinyl base silicone oil, and wherein the methyl and phenyl hydrogen-containing silicon oil consumption is 0.01 ~ 99.99% of B glue weight; Total consumption of transparent vinyl base silicone oil is in the A/B glue, and after A/B glue mixed, make wherein Si-H and Si-Vi mol ratio was 0.8 ~ 3:1; The hydrogen content of above-mentioned methyl and phenyl hydrogen-containing silicon oil is 1.6wt% ~ 1.0 * 10-6wt％；
3) A/B glue is mixed, at room temperature after the vacuum defoamation, sulfidization molding is made LED encapsulation organic silicon rubber;
In the step 1), described polymerization single polymerization monomer is comprised of dimethyl cyclosiloxane, methyl ethylene cyclosiloxane, methyl phenyl ring siloxane and methyl trifluoro propyl cyclosiloxane; Wherein, the dimethyl cyclosiloxane is 10 ~ 50mol% of polymerization single polymerization monomer total amount, and the methyl ethylene cyclosiloxane is 0.002 ~ 10mol% of polymerization single polymerization monomer total amount, and the methyl trifluoro propyl cyclosiloxane is 0.05 ~ 12mol% of polymerization single polymerization monomer total amount; Methyl phenyl ring siloxane be the polymerization single polymerization monomer total amount all the other the mole very;
Above-mentioned dimethyl cyclosiloxane is one or more in hexamethyl cyclotrisiloxane, octamethylcy-clotetrasiloxane, the decamethylcyclopentaandoxane, or the dimethyl ring siloxane mixture; Above-mentioned methyl ethylene cyclosiloxane is one or more in trimethyl trivinyl cyclotrisiloxane, tetramethyl tetrem thiazolinyl cyclotetrasiloxane, the pentamethyl five vinyl D5s; Above-mentioned methyl phenyl ring siloxane is one or more in trimethyl triphenyl cyclotrisiloxane, tetramethyl tetraphenyl cyclotetrasiloxane, pentamethyl pentaphene basic ring five siloxanes, or the aminomethyl phenyl mixed methylcyclosiloxane; Above-mentioned methyl trifluoro propyl cyclosiloxane is one or more in methyl trifluoro propyl cyclotrisiloxane, methyl trifluoro propyl cyclotetrasiloxane, the methyl trifluoro propyl D5;
Described end-capping reagent is dimethyl vinyl methoxy silane, Vinyldimethylethoxysilane, 1,1,3,3-tetramethyl-1,3-divinyl disiloxane, α, ω-divinyl silicone oil, α, ω-three silicon methyl vinyl silicon oil, α, the silica-based vinyl silicone oil of ω-3,5-dimethylphenyl, α, ω-three silicon phenyl-vinyl silicon oil, HMDO, decamethyl tetrasiloxane, 1,3-dimethyl-1,1,3,3-tetraphenyl-disiloxane, α, ω-divinyl polysiloxanes, α, ω-three silicon methyl polysiloxane, α, the silica-based polysiloxanes of ω-3,5-dimethylphenyl, α, one or more in the ω-three silicon phenyl polysiloxane;
Described catalyst is 98% concentrated sulfuric acid, CF3SO
3Among H, phosphoric acid, Emathlite, storng-acid cation exchange resin, rare-earth solid superacid, TMAH, TMAH silicon alkoxide, tetraethyl ammonium hydroxide, tetraethyl ammonium hydroxide silicon alkoxide, TBAH, 4-n-butyl ammonium hydroxide, 4-n-butyl ammonium hydroxide silicon alkoxide, tetrabutylammonium hydroxide phosphine, tetrabutylammonium hydroxide phosphine silicon alkoxide, the KOH one or more;
Described platinum catalyst is chloroplatinic acid, H2PtCl
6Aqueous isopropanol, H2PtCl
6Tetrahydrofuran solution, Pt (PPh3)
4、Cp
2PtCl
2, the coordination of ethylene methacrylic radical siloxane the platinum complex of platinum complex, dicyclopentadiene platinous chloride, dichloro two (triphenylphosphine) of platinum complex, diethyl phthalate coordination in a kind of;
Described inhibitor is a kind of in quinoline, pyridine, TBHP, propilolic alcohol, the tetramethyl butynol;
The polymeric reaction temperature of step 1) is 20 ~ 100 ℃, and polymerization reaction time is 1 ~ 20h; The lower high temperature removal low molecular compound of decompression progressively is warming up to 205 ℃ under-0.096MPa carries out;
The step 3) room temperature vacuum defoamation time is 1 ~ 60min, and curing temperature is 20 ~ 150 ℃.
2. the LED that is easy to vacuum defoamation according to claim 1 encapsulates the preparation method with organic silicon rubber, it is characterized in that step 2) in, total consumption of transparent vinyl base silicone oil is in the A/B glue, and after A/B glue mixed, the mol ratio of Si-H and Si-Vi was 1 ~ 1.5:1.
3. organic silicon rubber is used in the LED encapsulation that is easy to vacuum defoamation according to claim 1 and 2, it is characterized in that described transparent vinyl base silicone oil structural formula is ViMe2(MeViSiO)
m(MePhSiO)
p(Me
2SiO)
q(MeCH
2CH
2CF
3SiO)
kMe
2Vi, wherein, m, p, q and K are 0 or positive integer, 0≤m≤580,0≤p≤3308,0≤q≤3289,0≤k≤384, and satisfy m/ (m+p+q+k)=0 ~ 0.1, p/ (m+p+q+k)=0.5 ~ 0.9, q/ (m+p+q+k)=0.1 ~ 0.5, k/ (m+p+q+k)=0 ~ 0.12; The vinyl silicone oil molecular weight is 500 ~ 50 * 104 。
4. the LED encapsulation that the is easy to vacuum defoamation according to claim 1 and 2 preparation method of organic silicon rubber is characterized in that the temperature that the decompression of step 1) polymerization single polymerization monomer dewaters is that 35 ~ 45 ℃/pressure is 0.096Mpa; Polymeric reaction temperature is 80 ~ 100 ℃, and polymerization time is 1 ~ 5h; Decompression progressively is warming up to 205 ℃ when removing low molecular compound under-0.096MPa; The step 3) room temperature vacuum defoamation time is 5 ~ 40min, and curing temperature is 80 ~ 120 ℃.
5. the LED encapsulation that the is easy to vacuum defoamation according to claim 1 and 2 preparation method of organic silicon rubber is characterized in that described platinum catalyst is H2PtCl
6Aqueous isopropanol, H2PtCl
6Tetrahydrofuran solution, ethylene methacrylic radical siloxane platinum complex in a kind of, its consumption is 2 ~ 30ppm of silicone rubber compounds gross mass according to the pt atom quality.
6. the LED encapsulation that the is easy to vacuum defoamation according to claim 5 preparation method of organic silicon rubber is characterized in that described platinum catalyst is 2 ~ 10ppm of silicone rubber compounds gross mass.
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