CN109553774A - Led封装用高品质苯基乙烯基mtq硅树脂及制备方法 - Google Patents
Led封装用高品质苯基乙烯基mtq硅树脂及制备方法 Download PDFInfo
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- CN109553774A CN109553774A CN201811427916.XA CN201811427916A CN109553774A CN 109553774 A CN109553774 A CN 109553774A CN 201811427916 A CN201811427916 A CN 201811427916A CN 109553774 A CN109553774 A CN 109553774A
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- silicone resin
- phenyl vinyl
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- mtq silicone
- led encapsulation
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- 229920002050 silicone resin Polymers 0.000 title claims abstract description 81
- 238000005538 encapsulation Methods 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002105 nanoparticle Substances 0.000 claims abstract description 42
- -1 alkoxy silane Chemical compound 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 229910000077 silane Inorganic materials 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000005054 phenyltrichlorosilane Substances 0.000 claims abstract description 15
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 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 abstract description 9
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000010792 warming Methods 0.000 claims description 26
- 235000019441 ethanol Nutrition 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- 229960005489 paracetamol Drugs 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 238000013517 stratification Methods 0.000 claims description 5
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 4
- 239000003849 aromatic solvent Substances 0.000 claims description 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical group CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 4
- 150000002632 lipids Chemical class 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- XUIMIQQOPSSXEZ-RNFDNDRNSA-N silicon-32 atom Chemical compound [32Si] XUIMIQQOPSSXEZ-RNFDNDRNSA-N 0.000 claims description 4
- 125000003944 tolyl group Chemical group 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 8
- 230000007423 decrease Effects 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 238000011067 equilibration Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 13
- 229920001296 polysiloxane Polymers 0.000 description 12
- 238000002834 transmittance Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 7
- 229920002554 vinyl polymer Polymers 0.000 description 6
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000003028 elevating effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical compound CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000013213 extrapolation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- MEPLNBPJJKOWLV-UHFFFAOYSA-N hexanedioic acid;hydrazine Chemical compound NN.OC(=O)CCCCC(O)=O MEPLNBPJJKOWLV-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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Abstract
本发明涉及有机硅树脂制备技术领域,公开了一种LED封装用高品质苯基乙烯基MTQ硅树脂,以重量份数计,原料包括以下组分,一苯基三氯硅烷90‑120份;烷氧基硅烷100‑200份;双封头90‑120份;低级醇20‑50份;水200‑500份;溶剂100‑200份;改性无机纳米粒子30‑80份。本发明具有以下优点和效果:以一苯基三氯硅烷、烷氧基硅烷为原料,六甲基二硅氧烷与四甲基二乙烯基二硅氧烷以任意比例的混合物作为封端剂,在溶剂和低级醇形成的介质中平衡化反应,制得苯基乙烯基MTQ硅树脂。原料中的改性无机纳米粒子,在显著提高苯基乙烯基MTQ硅树脂折射率时,不会造成苯基乙烯基MTQ硅树脂透光性的下降,且对其力学性能影响较小,具有高折射率、高透光率和优异的耐热性能。
Description
技术领域
本发明属于有机硅树脂制备技术领域,特别涉及一种LED封装用高品质苯基乙烯基MTQ硅树脂。
技术背景
LED即发光二极管,是一种能够将电子转化为光子的半导体器件,主要由含镓、砷、磷、氮等的化合物制成,其核心是一个半导体晶片,通过改变半导体晶片的材质,可以实现不同波长可见光的生成,即可发出不同颜色的光。LED的基本特征决定了它是最理想的传统光源替代品,在指示灯、信号灯、景观照明领域受到广泛应用。LED产品需要针对不同封装和结构类型,设计出合理的封装形式,只有经过封装的LED才能最终成为产品,才能投入市场具有实际用途,因此,对LED发光二极管而言,封装的作用尤为重要。
LED封装用有机硅封装材料是LED封装材料中的一类,一般分为加成型硅树脂封装材料、含二官能度硅氧烷连段的硅树脂以及加成型液体硅橡胶等,MTQ硅树脂是LED封装用有机硅封装材料的补强填料,用于LED封装领域。在应用于LED封装材料领域时,需要MTQ硅树脂具有较好的光学性能及耐热性能,以满足封装时的要求。在现有技术中,为提高MTQ硅树脂的折射率,一种是在硅树脂中介入具有较大摩尔折射度的官能团如芳香环,其工艺条件复杂,并不利于工业化大规模生产。另一种则是直接通过共混的方式引入纳米粒子来提高材料的折射率,但纳米粒子虽然能较好地提高材料的折射率,但由于其团聚效应,会造成材料透光性的降低,导致制备的材料不能应用于LED封装领域。
发明内容
本发明的目的是提供一种LED封装用高品质苯基乙烯基MTQ硅树脂,具有高折射率、透光性好的效果。
本发明的上述技术目的是通过以下技术方案得以实现的:一种LED封装用高品质苯基乙烯基MTQ硅树脂,以重量份数计,原料包括以下组分,一苯基三氯硅烷90-120份;烷氧基硅烷100-200份;双封头90-120份;低级醇20-50份;水200-500份;溶剂100-200份;改性无机纳米粒子30-80份;所述双封头为六甲基二硅氧烷与四甲基二乙烯基二硅氧烷以任意比例的混合物,所述改性无机纳米制备方法如下:取无机纳米粒子投入N-乙酰基二氢鞘氨醇中,无机纳米粒子与N-乙酰基二氢鞘氨醇的质量比为2:3,升温到40-50℃,超声分散后,升温至55-60℃,保温3-6小时,得到改性无机纳米粒子。
通过采用上述技术方案,本发明以一苯基三氯硅烷、烷氧基硅烷为原料,六甲基二硅氧烷与四甲基二乙烯基二硅氧烷以任意比例的混合物作为封端剂,在溶剂和低级醇形成的介质中反应,化学反应方程式为mSi(OR)4+nPhSiCl3+p[R(3-x)VixSi]2O+qH2O→[R(3-x)ViSi0.5]a.[PhSi0.5]b.[(HO)ySiO(4-y)/2]c+3nHCl+4mROH,式中R为甲基或乙基,x为0或1,y为0-3的整数。[R(3-x)VixSi]2O为双封头。制得苯基乙烯基MTQ硅树脂。
在硅树脂原料中加入纳米粒子,虽然能够提高硅树脂的折射率,但由于纳米粒子的团聚效应,会造成硅树脂透光性降低,导致其无法应用于LED封装领域。现有技术中已有利用表面处理剂如偶联剂对纳米粒子进行改性,以提高纳米粒子在硅树脂原料的分散性,但还会出现另外一个问题,在树脂中加入纳米粒子会导致树脂本身变硬变脆,无法在实际中应用。
本发明经过反复研究,发现通过先将无机纳米粒子投入到N-乙酰基二氢鞘氨醇中,升温到40-50℃,超声分散后,再升温至55-60℃,保温3-6h得到的改性无机纳米粒子,不仅能在苯基乙烯基MTQ硅树脂原料中良好地分散,在显著提高苯基乙烯基MTQ硅树脂折射率时不会造成苯基乙烯基MTQ硅树脂透光性的下降,而且对其力学性能影响较小,不影响其使用。
本发明的进一步设置为:所述无机纳米粒子为纳米氧化锆、纳米二氧化钛、纳米二氧化硅中的一种。
通过采用上述技术方案,纳米氧化锆、纳米二氧化钛、纳米二氧化硅均具有较高的折射率,制成的改性无机纳米粒子能较好地提高苯基乙烯基MTQ硅树脂的折射率。
本发明的进一步设置为:以重量分数计,以重量份数计,原料包括一苯基三氯硅烷100份;双封头100份。
本发明的进一步设置为:以重量份数计,原料包括烷氧基硅烷120-150份;低级醇30-50份;溶剂120-150份。
本发明的进一步设置为:所述烷氧基硅烷为四甲氧基硅烷、四乙氧基硅烷、四乙氧基硅烷低聚物中的一种或多种,所述四乙氧基硅烷低聚物为硅32、硅40中的一种。
通过采用上述技术方案,四乙氧基硅烷又称硅酸乙酯、正硅酸乙酯,硅32又称硅酸乙酯32,硅40又称硅酸乙酯40。
本发明的进一步设置为:所述溶剂为芳烃溶剂或脂类环保溶剂,所述芳烃溶剂为甲苯或二甲苯,所述脂类环保溶剂为醋酸丁酯或PMA或DBE。
通过采用上述技术方案,PMA是丙二醇甲醚醋酸酯的英文缩写。DBE是二元酸酯,是一种低毒、低味,能生物降解的环保型溶剂。
本发明的进一步设置为:所述低级醇为甲醇、乙醇、异丙醇中的一种。
本发明的进一步设置为:以重量份数计,原料还包括己二酸二酰肼20-35份。
通过采用上述技术方案,己二酸二酰肼分子式为C6H14N4O2,为白色晶体,易溶于水。发明人在研究中发现,将其加入到苯基乙烯基MTQ硅树脂原料中,能提高改性无机纳米粒子的分散性,进一步减小改性无机纳米粒子对苯基乙烯基MTQ硅树脂透光性的影响,且还能进一步提高苯基乙烯基MTQ硅树脂的折射率;其次,己二酸二酰肼还能增强改性无机纳米粒子与苯基乙烯基MTQ硅树脂的粘结力,起到提高苯基乙烯基MTQ硅树脂的耐热性能。
本发明的进一步设置为:以重量份数计,原料还包括氨三亚甲基膦酸20-40份、对乙酰氨基酚25-40份。
通过采用上述技术方案,氨三亚甲基膦酸分子为C3H7NO9P3,可与水混溶,发明人将氨三亚甲基膦酸、对乙酰氨基酚加入到苯基乙烯基MTQ硅树脂原料中,能结合到苯基乙烯基MTQ硅树脂的分子链上,有效抑制苯基乙烯基MTQ硅树脂的热分解,显著提高苯基乙烯基MTQ硅树脂的耐热性能。
本发明的另一个目的在于提供一种上述LED封装用高品质苯基乙烯基MTQ硅树脂的制备方法,包括以下步骤,S1,将溶剂、水、低级醇、双封头、改性无机纳米粒子按比例投入反应釜中,控制釜温在20-50℃,滴加一苯基三氯硅烷,1-2小时滴完;升温到50-80℃,再滴加烷氧基硅烷,0.5-1.5小时滴完;S2,滴完后升温到70-90℃,维持回流2-4小时;S3,降温到50-55℃,静置分层;S4,往反应釜的料液中加碱中和或加水水洗到中性;S5,用活性炭对料液脱色、过滤;S6,升温到80-150℃,减压脱溶剂,得到苯基乙烯基MTQ硅树脂。
本发明的有益效果是:1、苯基乙烯基MTQ硅树脂原料中的改性无机纳米粒子,在显著提高苯基乙烯基MTQ硅树脂折射率时,不会造成苯基乙烯基MTQ硅树脂透光性的下降,且对其力学性能影响较小,兼具高折射率和高透光率;2、氨三亚甲基膦酸、对乙酰氨基酚加入到苯基乙烯基原料中,能有效抑制苯基乙烯基MTQ硅树脂的热分解,显著提高苯基乙烯基MTQ硅树脂的耐热性能,能用于LED封装材料领域或者用作有机硅压敏胶的增粘剂。
具体实施方式
实施例1:LED封装用高品质苯基乙烯基MTQ硅树脂,原料中各组分及含量如表1所示,其中表1中的组分含量单位为kg。烷氧基硅烷为四甲氧基硅烷,双封头为六甲基二硅氧烷与四甲基二乙烯基二硅氧烷的混合物,六甲基二硅氧烷与四甲基二乙烯基二硅氧烷的质量比为1:9。低级醇为甲醇,溶剂为甲苯。
改性无机纳米粒子制备方法如下:取纳米氧化锆投入N-乙酰基二氢鞘氨醇中,纳米氧化锆与N-乙酰基二氢鞘氨醇的质量比为2:3,升温到40℃,超声分散后,升温至55℃,保温3小时,得到改性无机纳米粒子。
LED封装用高品质苯基乙烯基MTQ硅树脂的制备方法如下:包括以下步骤,S1,将溶剂、水、低级醇、双封头、改性无机纳米粒子按比例投入反应釜中,控制釜温在20℃,滴加一苯基三氯硅烷,1小时滴完;升温到50℃,再滴加烷氧基硅烷,0.5小时滴完。S2,滴完后升温到70℃,维持回流2小时。S3,降温到50℃,静置分层。S4,往反应釜的料液中加碱中和到中性,碱为氢氧化钠溶液。S5,用活性炭对料液脱色、过滤。S6,升温到80℃,减压脱溶剂,得到苯基乙烯基MTQ硅树脂。
实施例2:LED封装用高品质苯基乙烯基MTQ硅树脂,原料中各组分及含量如表1所示,其中表1中的组分含量单位为kg。烷氧基硅烷为四乙氧基硅烷,双封头为六甲基二硅氧烷与四甲基二乙烯基二硅氧烷的混合物,六甲基二硅氧烷与四甲基二乙烯基二硅氧烷的质量比为1:1。低级醇为乙醇,溶剂为二甲苯。
改性无机纳米粒子制备方法如下:取纳米二氧化钛投入N-乙酰基二氢鞘氨醇中,纳米二氧化钛与N-乙酰基二氢鞘氨醇的质量比为2:3,升温到45℃,超声分散后,升温至60℃,保温4小时,得到改性无机纳米粒子。
LED封装用高品质苯基乙烯基MTQ硅树脂的制备方法如下:包括以下步骤,S1,将溶剂、水、低级醇、双封头、改性无机纳米粒子按比例投入反应釜中,控制釜温在30℃,滴加一苯基三氯硅烷,1.5小时滴完;升温到60℃,再滴加烷氧基硅烷,1小时滴完。S2,滴完后升温到50℃,维持回流3小时。S3,降温到50℃,静置分层。S4,往反应釜的料液中加水水洗到中性。S5,用活性炭对料液脱色、过滤。S6,升温到120℃,减压脱溶剂,得到苯基乙烯基MTQ硅树脂。
实施例3:LED封装用高品质苯基乙烯基MTQ硅树脂,原料中各组分及含量如表1所示,其中表1中的组分含量单位为kg。改性无机纳米粒子制备方法如下:取纳米二氧化硅投入N-乙酰基二氢鞘氨醇中,纳米二氧化硅与N-乙酰基二氢鞘氨醇的质量比为2:3,升温到50℃,超声分散后,升温至60℃,保温6小时,得到改性无机纳米粒子。烷氧基硅烷为硅40,双封头为六甲基二硅氧烷与四甲基二乙烯基二硅氧烷的混合物,六甲基二硅氧烷与四甲基二乙烯基二硅氧烷的质量比为9:1。低级醇为异丙醇,溶剂为醋酸丁酯。
LED封装用高品质苯基乙烯基MTQ硅树脂的制备方法如下:包括以下步骤,S1,将溶剂、水、低级醇、双封头、改性无机纳米粒子按比例投入反应釜中,控制釜温在50℃,滴加一苯基三氯硅烷,2小时滴完;升温到80℃,再滴加烷氧基硅烷,1.5小时滴完。S2,滴完后升温到90℃,维持回流4小时。S3,降温到55℃,静置分层。S4,往反应釜的料液中加碱中和到中性,碱为氢氧化钾溶液。S5,用活性炭对料液脱色、过滤。S6,升温到150℃,减压脱溶剂,得到苯基乙烯基MTQ硅树脂。
实施例4:LED封装用高品质苯基乙烯基MTQ硅树脂,与实施例1的区别在于,原料中各组分及含量如表1所示,溶剂为PMA,烷氧基硅烷为硅32。
实施例5:LED封装用高品质苯基乙烯基MTQ硅树脂,与实施例1的区别在于,原料中各组分及含量如表1所示,溶剂为DBE。
实施例6:LED封装用高品质苯基乙烯基MTQ硅树脂,与实施例1的区别在于,原料中各组分及含量如表1所示。LED封装用高品质苯基乙烯基MTQ硅树脂制备方法的步骤S1,将溶剂、水、低级醇、双封头、改性无机纳米粒子、己二酸二酰肼按比例投入反应釜中,控制釜温在20℃,滴加一苯基三氯硅烷,1小时滴完;升温到50℃,再滴加烷氧基硅烷,0.5小时滴完。
实施例7:LED封装用高品质苯基乙烯基MTQ硅树脂,与实施例6的区别在于,原料中各组分及含量如表1所示。
实施例8:LED封装用高品质苯基乙烯基MTQ硅树脂,与实施例1的区别在于,原料中各组分及含量如表1所示。LED封装用高品质苯基乙烯基MTQ硅树脂制备方法的步骤S1,将溶剂、水、低级醇、双封头、改性无机纳米粒子、氨三亚甲基膦酸、对乙酰氨基酚按比例投入反应釜中,控制釜温在20℃,滴加一苯基三氯硅烷,1小时滴完;升温到50℃,再滴加烷氧基硅烷,0.5小时滴完。
实施例9:LED封装用高品质苯基乙烯基MTQ硅树脂,与实施例8的区别在于,原料中各组分及含量如表1所示。
实施例10:LED封装用高品质苯基乙烯基MTQ硅树脂,与实施例4的区别在于,原料中各组分及含量如表1所示。LED封装用高品质苯基乙烯基MTQ硅树脂制备方法的步骤S1,将溶剂、水、低级醇、双封头、改性无机纳米粒子、己二酸二酰肼、氨三亚甲基膦酸、对乙酰氨基酚按比例投入反应釜中,控制釜温在20℃,滴加一苯基三氯硅烷,1小时滴完;升温到50℃,再滴加烷氧基硅烷,0.5小时滴完。
对比例1:苯基乙烯基MTQ硅树脂,与实施例1的不同之处在于,原料中各组分及含量如表1所示。LED封装用高品质苯基乙烯基MTQ硅树脂制备方法的步骤S1,将溶剂、水、低级醇、双封头按比例投入反应釜中,控制釜温在20℃,滴加一苯基三氯硅烷,1小时滴完;升温到50℃,再滴加烷氧基硅烷,0.5小时滴完。
对比例2:苯基乙烯基MTQ硅树脂,与实施例1的不同之处在于,用纳米氧化锆代替改性无机纳米粒子。
对比例3:一种固化物,制备方法如下:取苯基含氢硅油,加入15ppm浓度的PT785铂催化剂(购于南通安必亚特种有机硅公司)作为催化剂,进行固化,得到固化物。
表1实施例1-10、对比例1的苯基乙烯基MTQ硅树脂的原料组分及含量
各实施例、对比例中的苯基乙烯基MTQ硅树脂的性能测试与表征
红外分析:用美国Thermo公司Nicolet FT-IR-5700型红外光谱仪(KBr压片),扫描范围为400cm-1-4000cm-1,从得到的实施例1-10、对比例1-2的FT-IR谱图中,均在1600cm-1附近观察到乙烯基的特征峰、1000cm-1-1150cm-1处观察到硅树脂的特征吸收峰、1800cm-1-2400cm-1附近观察到苯基的特征吸收峰,可确定产物为带有苯基、乙烯基的苯基乙烯基MTQ硅树脂。
耐热性能测试:采用德国耐驰STA499C热重分析仪对各实施例及对比例的苯基乙烯基MTQ硅树脂进行分析,升温范围为300-800℃,氮气氛围,升温速率为15℃/min,记录苯基乙烯基MTQ硅树脂失重10%时的温度,并将结果于表2中列出。
折射率测定:将实施例1-10、对比例1-2中的苯基乙烯基MTQ硅树脂溶于乙酸乙酯溶液中,采用上海光学仪器厂2WA-J型阿贝折光仪测量不同浓度溶液的折射率,采用外推法确定苯基乙烯基MTQ硅树脂的折射率,将测定结果于表2中列出。
透光率测定:MTQ硅树脂作为一类结构特殊的硅树脂材料,将其单独作为高分子材料应用的场景很少,一般是将其作为填料去补强聚合物体系,以改进聚合物的性能。在透光率测试中,分别测定其本身的透光率及其补强聚合物后的透光率,以判断其能否在实际中应用。
苯基乙烯基MTQ硅树脂透光率:用日本岛津公司的UV3600型紫外分光光度计对实施例1-10、对比例1-2的苯基乙烯基MTQ硅树脂进行透光率测试,扫描范围为900nm-220nm,扫描速度为中速,光狭峰宽20nm,将测试结果于表3中列出。
固化物透光率:分别取实施例1-10、对比例1-2的苯基乙烯基MTQ硅树脂与苯基含氢硅油按质量比1:9混合,加入15ppm浓度的PT785铂催化剂(购于南通安必亚特种有机硅公司)作为催化剂,进行固化。将得到的固化物用日本岛津公司的UV3600型紫外分光光度计进行透光率测试,另外也对对比例3的固化物进行透光率测试,将测试结果于表3中列出。
表2实施例1-10、对比例1-2耐热性能测试结果和折射率测试结果
表3实施例1-10、对比例1-3的透光率测定
通过表2、表3的结果可知,改性无机纳米粒子能在显著提高苯基乙烯基MTQ硅树脂折射率的同时,其对苯基乙烯基MTQ硅树脂的透光率影响较小,能够较好地平衡苯基乙烯基MTQ硅树脂的折射率和透光率。未经改性的无机纳米粒子在加入苯基乙烯基MTQ硅树脂原料后,虽然其能提高苯基乙烯基MTQ硅树脂的折射率,但会造成透光率显著下降。己二酸二酰肼在加入苯基乙烯基MTQ硅树脂原料后,也能起到进一步提高苯基乙烯基MTQ硅树脂的折射率。氨三亚甲基膦酸、对乙酰氨基酚在加入苯基乙烯基MTQ硅树脂原料后,能显著提高苯基乙烯基MTQ硅树脂的耐热性能。
Claims (10)
1.一种LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于,以重量份数计,原料包括以下组分,
所述双封头为六甲基二硅氧烷与四甲基二乙烯基二硅氧烷以任意比例的混合物,所述改性无机纳米制备方法如下:取无机纳米粒子投入N-乙酰基二氢鞘氨醇中,无机纳米粒子与N-乙酰基二氢鞘氨醇的质量比为2:3,升温到40-50℃,超声分散后,升温至55-60℃,保温3-6小时,得到改性无机纳米粒子。
2.根据权利要求1所述的LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于:所述无机纳米粒子为纳米氧化锆、纳米二氧化钛、纳米二氧化硅中的一种。
3.根据权利要求1所述的LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于:以重量分数计,以重量份数计,原料包括一苯基三氯硅烷100份;双封头100份。
4.根据权利要求1所述的LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于:以重量份数计,原料包括烷氧基硅烷120-150份;低级醇30-50份;溶剂120-150份。
5.根据权利要求1所述的LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于:所述烷氧基硅烷为四甲氧基硅烷、四乙氧基硅烷、四乙氧基硅烷低聚物中的一种或多种,所述四乙氧基硅烷低聚物为硅32、硅40中的一种。
6.根据权利要求1所述的LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于:所述溶剂为芳烃溶剂或脂类环保溶剂,所述芳烃溶剂为甲苯或二甲苯,所述脂类环保溶剂为醋酸丁酯或PMA或DBE。
7.根据权利要求1所述的LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于:所述低级醇为甲醇、乙醇、异丙醇中的一种。
8.根据权利要求1所述的LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于:以重量份数计,原料还包括己二酸二酰肼20-35份。
9.根据权利要求1所述的LED封装用高品质苯基乙烯基MTQ硅树脂,其特征在于:以重量份数计,原料还包括氨三亚甲基膦酸20-40份、对乙酰氨基酚25-40份。
10.一种如权利要求1-9所述的任意一种LED封装用高品质苯基乙烯基MTQ硅树脂的制备方法,其特征在于:包括以下步骤,
S1,将溶剂、水、低级醇、双封头、改性无机纳米粒子按比例投入反应釜中,控制釜温在20-50℃,滴加一苯基三氯硅烷,1-2小时滴完;升温到50-80℃,再滴加烷氧基硅烷,0.5-1.5小时滴完;
S2,滴完后升温到70-90℃,维持回流2-4小时;
S3,降温到50-55℃,静置分层;
S4,往反应釜的料液中加碱中和或加水水洗到中性;
S5,用活性炭对料液脱色、过滤;
S6,升温到80-150℃,减压脱溶剂,得到苯基乙烯基MTQ硅树脂。
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