CN109517175A - LED encapsulation high-quality phenyl vinyl MTQ silicone resin and preparation method - Google Patents
LED encapsulation high-quality phenyl vinyl MTQ silicone resin and preparation method Download PDFInfo
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- CN109517175A CN109517175A CN201811427880.5A CN201811427880A CN109517175A CN 109517175 A CN109517175 A CN 109517175A CN 201811427880 A CN201811427880 A CN 201811427880A CN 109517175 A CN109517175 A CN 109517175A
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- silicone resin
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- phenyl vinyl
- mtq silicone
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- 229920002050 silicone resin Polymers 0.000 title claims abstract description 83
- 238000005538 encapsulation Methods 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 39
- -1 alkoxy silane Chemical compound 0.000 claims abstract description 38
- 229910000077 silane Inorganic materials 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000002904 solvent Substances 0.000 claims abstract description 27
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 25
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 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 13
- 239000005054 phenyltrichlorosilane Substances 0.000 claims abstract description 13
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 235000019441 ethanol Nutrition 0.000 claims description 32
- 238000010792 warming Methods 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 8
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 claims description 8
- WDSCBUNMANHPFH-UHFFFAOYSA-N acexamic acid Chemical compound CC(=O)NCCCCCC(O)=O WDSCBUNMANHPFH-UHFFFAOYSA-N 0.000 claims description 8
- 229960004582 acexamic acid Drugs 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 8
- QEHNNAQSHBJMTJ-UHFFFAOYSA-N 2,2,3,3,4,4-hexamethyl-1h-naphthalene Chemical compound C1=CC=C2C(C)(C)C(C)(C)C(C)(C)CC2=C1 QEHNNAQSHBJMTJ-UHFFFAOYSA-N 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 238000013517 stratification Methods 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 125000001231 benzoyloxy group Chemical group C(C1=CC=CC=C1)(=O)O* 0.000 claims description 5
- 238000006386 neutralization reaction Methods 0.000 claims description 5
- 239000003849 aromatic solvent Substances 0.000 claims description 4
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical group CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 4
- 150000002632 lipids Chemical class 0.000 claims description 4
- 238000002156 mixing 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 4
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims 1
- 239000005052 trichlorosilane Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000011067 equilibration Methods 0.000 abstract description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 11
- 239000000463 material Substances 0.000 description 10
- 229920001296 polysiloxane Polymers 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 6
- 239000002585 base Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- CGMFKBXPQJJHBR-UHFFFAOYSA-N [SiH3]O[SiH](C=C)C=C Chemical compound [SiH3]O[SiH](C=C)C=C CGMFKBXPQJJHBR-UHFFFAOYSA-N 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- 239000005046 Chlorosilane Substances 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 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 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- SESFRYSPDFLNCH-UHFFFAOYSA-N benzyl benzoate Chemical compound C=1C=CC=CC=1C(=O)OCC1=CC=CC=C1 SESFRYSPDFLNCH-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000000051 benzyloxy group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])O* 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- OTKJDMGTUTTYMP-UHFFFAOYSA-N dihydrosphingosine Natural products CCCCCCCCCCCCCCCC(O)C(N)CO OTKJDMGTUTTYMP-UHFFFAOYSA-N 0.000 description 1
- 230000003028 elevating effect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 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
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 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
- 230000035939 shock Effects 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- OTKJDMGTUTTYMP-ZWKOTPCHSA-N sphinganine Chemical compound CCCCCCCCCCCCCCC[C@@H](O)[C@@H](N)CO OTKJDMGTUTTYMP-ZWKOTPCHSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G77/06—Preparatory processes
- C08G77/10—Equilibration processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/52—Encapsulations
- H01L33/56—Materials, e.g. epoxy or silicone resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Silicon Polymers (AREA)
Abstract
The present invention relates to organic siliconresin preparation technical fields, disclose a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin, and based on parts by weight, raw material includes following components, 90-120 parts of a phenyl trichlorosilane；100-200 parts of alkoxy silane；90-120 parts of double-seal head；20-50 parts of lower alcohol；200-500 parts of water；100-200 parts of solvent；The double-seal head is hexamethyldisiloxane and tetramethyl divinyl disiloxane with the mixture of arbitrary proportion.The present invention has the following advantages and effects: using a phenyl trichlorosilane, alkoxy silane as raw material, hexamethyldisiloxane and tetramethyl divinyl disiloxane are using the mixture of arbitrary proportion as end-capping reagent, the equilibration reaction in the medium that solvent and lower alcohol are formed, the refractive index of phenyl vinyl MTQ silicone resin is improved by the modifying titanium dioxide of high refractive index, phenyl vinyl MTQ silicone resin is made, with very good heat resistance and high refractive index；It can be used in the LED encapsulation of high-quality, high request.
Description
Technical field
The invention belongs to organosilicon preparation technical field, in particular to a kind of LED encapsulation high-quality phenyl vinyl MTQ
Silicone resin and preparation method.
Technical background
LED is a kind of solid state semiconductor devices that can convert electrical energy into visible light, have energy consumption is small, the service life is long,
It is pollution-free etc. it is a series of a little, for meeting the needs of mankind are in terms of energy conservation and environmental protection and alleviating the energy and environmental crisis very
It is beneficial.For LED, encapsulating material is most important, because the quality of encapsulating material influences whether the encapsulation of LED light, assembles
And the reliability and service life etc. of device.Therefore, heat shock resistance, the encapsulating material without xanthochromia, high refractive index are developed
It is technology very crucial in LED manufacture.MTQ silicone resin is a kind of encapsulating material applied to LED encapsulation, by MQ silicon tree
Rouge modification obtains, and the organic group of three-functionality-degree (R1SiO3/2, T chain link) is introduced MQ molecule, is formed by single functionality M chain link
The MTQ silicone resin constituted with three-functionality-degree T chain link and tetra functional Q chain link.MTQ silicone resin in the prior art is being applied to half
When conductor encapsulates, heat-resistant aging, optical property are all difficult to meet the requirement of semiconductor packages, it is necessary to provide a kind of modification
MTQ silicone resin, have excellent heat-resisting, optical property, with for the LED of high-quality encapsulate.
Summary of the invention
The object of the present invention is to provide a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin, with excellent resistance to
Heat, the effect of high refractive index can be used for LED encapsulation.
Above-mentioned technical purpose of the invention has the technical scheme that a kind of LED encapsulation high-quality
Phenyl vinyl MTQ silicone resin, based on parts by weight, raw material include following components, 90-120 parts of a phenyl trichlorosilane；Alcoxyl
100-200 parts of base silane；90-120 parts of double-seal head；20-50 parts of lower alcohol；200-500 parts of water；100-200 parts of solvent；It is described double
End socket is hexamethyldisiloxane and tetramethyl divinyl disiloxane with the mixture of arbitrary proportion.
By using above-mentioned technical proposal, the present invention is using a phenyl trichlorosilane, alkoxy silane as raw material, hexamethyl two
Siloxanes and tetramethyl divinyl disiloxane are formed using the mixture of arbitrary proportion as end-capping reagent in solvent and lower alcohol
Medium in react, chemical equation be 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, R is methyl or ethyl in formula, and x is 0 or 1, and y is
The integer of 0-3.[R(3-x)VixSi]2O is double-seal head.Phenyl vinyl MTQ silicone resin is made, with excellent heat resistance
And high refractive index, it can be used in the LED encapsulation of high-quality, high request.
The further setting of the present invention are as follows: based on parts by weight, raw material includes 100 parts of a phenyl trichlorosilane；Double-seal head
100 parts.
The further setting of the present invention are as follows: based on parts by weight, raw material includes 120-150 parts of alkoxy silane；Lower alcohol
30-50 parts；120-150 parts of solvent.
The further setting of the present invention are as follows: the alkoxy silane is tetramethoxy-silicane, tetraethoxysilane, four ethoxies
One of base silane oligomer is a variety of, and the tetraethoxysilane oligomer is one of silicon 32, silicon 40.
By using above-mentioned technical proposal, tetraethoxysilane is also known as silester, ethyl orthosilicate, and silicon 32 is also known as silicic acid
Ethyl ester 32, silicon 40 are also known as ethyl silicate 40.
The further setting of the present invention are as follows: the solvent is aromatic solvent or lipid environmentally friendly solvent, and the aromatic solvent is
Toluene or dimethylbenzene, the lipid environmentally friendly solvent are butyl acetate or PMA or DBE.
By using above-mentioned technical proposal, PMA is the english abbreviation of propylene glycol methyl ether acetate.DBE is dibasic acid ester, is
A kind of less toxic, low taste, can biodegradable environment-friendly type solvent.
The further setting of the present invention are as follows: the lower alcohol is one of methanol, ethyl alcohol, isopropanol.
By using above-mentioned technical proposal, lower alcohol, that is, short carbon chain alcohol, lower alcohol of the invention is methanol, ethyl alcohol, isopropyl
One of alcohol.
The further setting of the present invention are as follows: based on parts by weight, raw material further includes 20-40 parts of Acetaminocaproic Acid, benzene
25-30 parts of formyloxy Ergol.
By using above-mentioned technical proposal, Acetaminocaproic Acid molecular formula is C8H15NO3, with benzoxy yl benzoic acid
Benzyl ester is scattered in phenyl vinyl MTQ silicone raw, is participated in the synthesis of phenyl vinyl MTQ silicone resin, can be significantly improved
The heat resistance of the phenyl vinyl MTQ silicone resin of production inhibits phenyl vinyl MTQ silicone resin strand in thermal environment
Fracture and decomposition.
The further setting of the present invention are as follows: based on parts by weight, raw material further includes acetyl group hexamethyl tetrahydronaphthalene 10-20
Part.
By using above-mentioned technical proposal, it is former that acetyl group hexamethyl tetrahydronaphthalene is scattered in phenyl vinyl MTQ silicone resin
In material, it can be combined with phenyl vinyl MTQ silicone resin strand, significantly inhibit phenyl vinyl MTQ silicone resin strand
Fracture, to improve the thermal stability of phenyl vinyl MTQ silicone resin；In addition, acetyl group hexamethyl tetrahydronaphthalene with 6- second
When acylamino- caproic acid, benzoyloxy Ergol are collectively resided in phenyl vinyl MTQ silicone raw, benzene is being improved
Three can also play synergistic effect in base vinyl MTQ silicone resin heat resistance.
The further setting of the present invention are as follows: based on parts by weight, raw material further includes 15-35 parts of modifying titanium dioxide；It is described
Modifying titanium dioxide the preparation method is as follows: take nano-titanium dioxide investment N- acetyldihydro sphingol in, be warming up to 40-50
DEG C, 3-6h is kept the temperature after mixing evenly, obtains modifying titanium dioxide, wherein nano-titanium dioxide and N- acetyldihydro sphingol
Mass ratio is 2:3.
By using above-mentioned technical proposal, in LED encapsulation field, the refractive index of LED chip is usually 2.2-2.4, and one
As organosilicon material refractive index be 1.4 or so.Therefore, the refractive index for improving encapsulating material is conducive to passing through for light, Jin Erneng
Improve the efficiency of LED light.Generally using the group for introducing high refraction in silicone molecules structure in currently available technology, to mention
The optical property of high polymer itself.The present invention is then using the inorganic matter that high refraction is added, and the refractive index of titanium dioxide is general
In 2.55-2.76 or so, refractive index is higher.But directly titanium dioxide is added in phenyl vinyl MTQ silicone raw, one
It is that compatibility is bad, second is that the intermolecular attachment force of titanium dioxide and phenyl vinyl MTQ silicone resin is weak, causes titanium dioxide easy
It is detached from from MTQ silicone resin.The present invention is first modified nano-titanium dioxide surface, mixed with N- acetyldihydro sphingol
After conjunction, is being kept the temperature after heating, obtaining modifying titanium dioxide, can be preferably compatible with phenyl vinyl MTQ silicone raw, and table
Face has more binding sites, it is easier to be connected with phenyl vinyl MTQ silicone resin molecule, play raising phenyl vinyl
The effect of MTQ silicone resin refractive index, to meet requirement of the LED encapsulation material to high optical property.
The present invention also provides a kind of preparation methods of above-mentioned LED encapsulation high-quality phenyl vinyl MTQ silicone resin, including
Solvent, water, lower alcohol, double-seal head are put in proportion into reaction kettle by following steps, S1, are controlled kettle temperature at 20-50 DEG C, are added dropwise
One phenyl trichlorosilane drips off for 1-2 hours；It is warming up to 50-80 DEG C, then alkoxy silane is added dropwise, is dripped off within 0.5-1.5 hours；S2,
It is warming up to 70-90 DEG C after dripping off, maintains reflux 2-4 hours；S3 cools to 50-55 DEG C, stratification；S4, toward the material of reaction kettle
Add alkali neutralization in liquid or adds water washing to neutrality；S5, with active carbon to feed liquid decoloration, filtering；S6 is warming up to 80-150 DEG C, subtracts
Pressure-off solvent obtains phenyl vinyl MTQ silicone resin.
The beneficial effects of the present invention are: 1, of the invention using a phenyl trichlorosilane, alkoxy silane as raw material, hexamethyl two
Siloxanes and tetramethyl divinyl disiloxane are formed using the mixture of arbitrary proportion as end-capping reagent in solvent and lower alcohol
Medium in equilibration reaction, phenyl vinyl MTQ silicone resin is made, with very good heat resistance and high refraction
Rate；It can be used in the LED encapsulation of high-quality, high request；2,20-40 parts of the Acetaminocaproic Acid in MTQ silicone raw, benzene
Formyloxy Ergol can effectively inhibit fracture and decomposition of the phenyl vinyl MTQ silicone resin strand in thermal environment,
Play the role of improving phenyl vinyl MTQ silicone resin heat resistance；3, by adding in phenyl vinyl MTQ silicone raw
Enter the modifying titanium dioxide of high refractive index, the refractive index of phenyl vinyl MTQ silicone resin can be significantly improved, to meet LED encapsulation
Requirement of the material to optical property.
Specific embodiment
Embodiment 1:LED, which is encapsulated, uses high-quality phenyl vinyl MTQ silicone resin, and each component is as shown in table 1 in raw material, wherein
The unit of each component content is kg in table 1, and alkoxy silane is tetramethoxy-silicane, and double-seal head is hexamethyldisiloxane and four
The mixture of divinyl disiloxane, the wherein quality of hexamethyldisiloxane and tetramethyl divinyl disiloxane
Than for 1:9.Lower alcohol is methanol, and solvent is toluene.
The preparation method of LED encapsulation high-quality phenyl vinyl MTQ silicone resin is as follows, includes the following steps, S1, will be molten
Agent, water, lower alcohol, double-seal head are put in proportion into reaction kettle, control feed liquid temperature in reaction kettle and a phenyl three is added dropwise at 20 DEG C
Chlorosilane drips off for 1 hour；50 DEG C are warming up to, then alkoxy silane is added dropwise, is dripped off within 0.5 hour.
S2, alkoxy silane are warming up to 70 DEG C after dripping off, maintain reflux 2 hours.
S3 cools to 50 DEG C, stratification.
S4, into the feed liquid of reaction kettle plus alkali neutralization is to neutrality, and alkali is sodium hydroxide solution.
S5, with active carbon to feed liquid decoloration, filtering.
S6 is warming up to 80 DEG C, depressurizes desolventizing, obtains phenyl vinyl MTQ silicone resin.
Embodiment 2:LED, which is encapsulated, uses high-quality phenyl vinyl MTQ silicone resin, and each component is as shown in table 1 in raw material, wherein
The unit of each component content is kg in table 1, and alkoxy silane is tetraethoxysilane, and double-seal head is hexamethyldisiloxane and four
The mixture of divinyl disiloxane, the wherein quality of hexamethyldisiloxane and tetramethyl divinyl disiloxane
Than for 1:6.Lower alcohol is ethyl alcohol, and solvent is dimethylbenzene.
The preparation method of LED encapsulation high-quality phenyl vinyl MTQ silicone resin is as follows, includes the following steps, S1, will be molten
Agent, water, lower alcohol, double-seal head are put in proportion into reaction kettle, control feed liquid temperature in reaction kettle and a phenyl three is added dropwise at 30 DEG C
Chlorosilane drips off for 1.5 hours；60 DEG C are warming up to, then alkoxy silane is added dropwise, is dripped off within 1 hour.
S2, alkoxy silane are warming up to 80 DEG C after dripping off, maintain reflux 3 hours.
S3 cools to 50 DEG C, stratification.
S4, into the feed liquid of reaction kettle plus water is washed to neutrality.
S5, with active carbon to feed liquid decoloration, filtering.
S6 is warming up to 120 DEG C, depressurizes desolventizing, obtains phenyl vinyl MTQ silicone resin.
Embodiment 3:LED, which is encapsulated, uses high-quality phenyl vinyl MTQ silicone resin, and each component is as shown in table 1 in raw material, wherein
The unit of each component content is kg in table 1, and alkoxy silane is tetraethoxysilane, and double-seal head is hexamethyldisiloxane and four
The mixture of divinyl disiloxane, the wherein quality of hexamethyldisiloxane and tetramethyl divinyl disiloxane
Than for 1:1.Lower alcohol is isopropanol, solvent butyl acetate.
The preparation method of LED encapsulation high-quality phenyl vinyl MTQ silicone resin is as follows, includes the following steps, S1, will be molten
Agent, water, lower alcohol, double-seal head are put in proportion into reaction kettle, control feed liquid temperature in reaction kettle and a phenyl three is added dropwise at 50 DEG C
Chlorosilane drips off for 2 hours；80 DEG C are warming up to, then alkoxy silane is added dropwise, is dripped off within 1.5 hours.
S2, alkoxy silane are warming up to 90 DEG C after dripping off, maintain reflux 4 hours.
S3 cools to 55 DEG C, stratification.
S4, into the feed liquid of reaction kettle plus alkali neutralization is to neutrality, and alkali is potassium hydroxide solution.
S5, with active carbon to feed liquid decoloration, filtering.
S6 is warming up to 150 DEG C, depressurizes desolventizing, obtains phenyl vinyl MTQ silicone resin.
Embodiment 4:LED encapsulation high-quality phenyl vinyl MTQ silicone resin, the difference with embodiment 3 is, in raw material
Each component is as shown in table 1, and the mass ratio of hexamethyldisiloxane and tetramethyl divinyl disiloxane in double-seal head is 1:
1, solvent PMA, alkoxy silane are silicon 32.
Embodiment 5:LED encapsulation high-quality phenyl vinyl MTQ silicone resin, the difference with embodiment 3 is, in raw material
Each component is as shown in table 1, and alkoxy silane is silicon 40, hexamethyldisiloxane and two silicon of tetramethyl divinyl in double-seal head
The mass ratio of oxygen alkane is 8:1, and solvent DBE, alkoxy silane is silicon 40.
Embodiment 6:LED, which is encapsulated, uses high-quality phenyl vinyl MTQ silicone resin, and each component is as shown in table 1 in raw material, wherein
The unit of each component content is kg in table 1, and alkoxy silane is tetramethoxy-silicane, and double-seal head is hexamethyldisiloxane and four
The mixture of divinyl disiloxane, the wherein quality of hexamethyldisiloxane and tetramethyl divinyl disiloxane
Than for 1:9.Lower alcohol is methanol, and solvent is toluene.
The preparation method of LED encapsulation high-quality phenyl vinyl MTQ silicone resin is as follows, includes the following steps, S1, will be molten
Agent, water, lower alcohol, double-seal head, Acetaminocaproic Acid, benzoyloxy Ergol are put in proportion into reaction kettle, control
Feed liquid temperature is added dropwise a phenyl trichlorosilane, drips off within 1 hour at 20 DEG C in reaction kettle processed；50 DEG C are warming up to, then alkoxy is added dropwise
Silane drips off for 0.5 hour.
S2, alkoxy silane are warming up to 70 DEG C after dripping off, maintain reflux 2 hours.
S3 cools to 50 DEG C, stratification.
S4, into the feed liquid of reaction kettle plus water is washed to neutrality.
S5, with active carbon to feed liquid decoloration, filtering.
S6 is warming up to 80 DEG C, depressurizes desolventizing, obtains phenyl vinyl MTQ silicone resin.
Embodiment 7:LED encapsulation high-quality phenyl vinyl MTQ silicone resin, the difference with embodiment 6 is, in raw material
Each component is as shown in table 1.
Embodiment 8:LED encapsulation high-quality phenyl vinyl MTQ silicone resin, the difference from example 2 is that, in raw material
Each component is as shown in table 1.Step S2 in the preparation method of LED encapsulation high-quality phenyl vinyl MTQ silicone resin is as follows,
Solvent, water, lower alcohol, double-seal head, acetyl group hexamethyl tetrahydronaphthalene are put in proportion into reaction kettle by S1, control reaction kettle
Middle feed liquid temperature is added dropwise a phenyl trichlorosilane, drips off within 1.5 hours at 30 DEG C；60 DEG C are warming up to, then alkoxy silane is added dropwise, 1
Hour drips off.
Embodiment 9:LED encapsulation high-quality phenyl vinyl MTQ silicone resin, the difference from example 2 is that, in raw material
Each component is as shown in table 1.Step S2 in the preparation method of LED encapsulation high-quality phenyl vinyl MTQ silicone resin is as follows,
S1, by solvent, water, lower alcohol, double-seal head, Acetaminocaproic Acid, benzoyloxy Ergol, acetyl group hexamethyl four
Hydrogenated naphthalene is put in proportion into reaction kettle, is controlled feed liquid temperature in reaction kettle and a phenyl trichlorosilane is added dropwise, 1.5 is small at 30 DEG C
When drip off；60 DEG C are warming up to, then alkoxy silane is added dropwise, is dripped off within 1 hour.
Embodiment 10:LED, which is encapsulated, uses high-quality phenyl vinyl MTQ silicone resin, and each component is as shown in table 1 in raw material,
The unit of each component content is kg in middle table 1, and alkoxy silane is tetraethoxysilane, double-seal head be hexamethyldisiloxane with
The mixture of tetramethyl divinyl disiloxane, the wherein matter of hexamethyldisiloxane and tetramethyl divinyl disiloxane
Amount is than being 1:6.Lower alcohol is ethyl alcohol, and solvent is dimethylbenzene.
Modifying titanium dioxide is the preparation method is as follows: take in nano-titanium dioxide investment N- acetyldihydro sphingol, heating
To 40-50 DEG C, 3-6h is kept the temperature after mixing evenly, obtains modifying titanium dioxide, wherein nano-titanium dioxide and N- acetyldihydro
The mass ratio of sphingol is 2:3.
The preparation method of LED encapsulation high-quality phenyl vinyl MTQ silicone resin is as follows, includes the following steps, S1, will be molten
Agent, water, lower alcohol, double-seal head, modifying titanium dioxide are put in proportion into reaction kettle, and feed liquid temperature is 30 in control reaction kettle
DEG C, a phenyl trichlorosilane is added dropwise, drips off within 1.5 hours；60 DEG C are warming up to, then alkoxy silane is added dropwise, is dripped off within 1 hour.
S2, alkoxy silane are warming up to 80 DEG C after dripping off, maintain reflux 3 hours.
S3 cools to 50 DEG C, stratification.
S4, into the feed liquid of reaction kettle plus alkali neutralization is to neutrality, and alkali is sodium bicarbonate solution.
S5, with active carbon to feed liquid decoloration, filtering.
S6 is warming up to 120 DEG C, depressurizes desolventizing, obtains phenyl vinyl MTQ silicone resin.
Embodiment 11:LED, which is encapsulated, uses high-quality phenyl vinyl MTQ silicone resin, and the difference with embodiment 10 is, raw material
Middle each component is as shown in table 1.Modifying titanium dioxide is the preparation method is as follows: take nano-titanium dioxide to put into N- acetyldihydro sheath ammonia
In alcohol, it is warming up to 40-50 DEG C, keeps the temperature 3-6h after mixing evenly, obtain modifying titanium dioxide, wherein nano-titanium dioxide and N- second
The mass ratio of acyl group dihydrosphingosine is 2:3.
Step S1 in the LED encapsulation preparation method of high-quality phenyl vinyl MTQ silicone resin is as follows, S1, by solvent,
Water, double-seal head, Acetaminocaproic Acid, benzoyloxy Ergol, acetyl group hexamethyl tetrahydronaphthalene, changes lower alcohol
Property titanium dioxide be put in proportion into reaction kettle, control reaction kettle in feed liquid temperature at 30 DEG C, be added dropwise a phenyl trichlorosilane,
It drips off within 1.5 hours；60 DEG C are warming up to, then alkoxy silane is added dropwise, is dripped off within 1 hour.
Comparative example 1: phenyl vinyl MTQ silicone resin, the difference with embodiment 10 are, with the nanometer of non-modified processing
Titanium dioxide replaces modifying titanium dioxide.
Comparative example 2: phenyl vinyl MTQ silicone resin, the difference with embodiment 11 are, with the nanometer of non-modified processing
Titanium dioxide replaces modifying titanium dioxide.
The raw material components of phenyl vinyl MTQ silicone resin in each embodiment of table 1
The performance test of MTQ silicone resin and characterization of each embodiment
Infrared analysis: U.S. Thermo company Nicolet FT-IR-5700 type infrared spectrometer (KBr tabletting), scanning are used
Range is 400cm-1-4000cm-1, from the FT-IR spectrogram of obtained each embodiment, second is observed near 1600cm-1
Observe that the characteristic absorption peak of silicone resin, 1800cm-1-2400cm-1 are attached at the characteristic peak of alkenyl, 1000cm-1-1150cm-1
Close up observes the characteristic absorption peak of phenyl, it may be determined that product is the phenyl vinyl MTQ silicone resin with phenyl, vinyl.
Heat resistance test: using the resistance to STA499C thermogravimetric analyzer of speeding of Germany to the phenyl second of each embodiment and comparative example
Alkenyl MTQ silicone resin is analyzed, and temperature elevating range is 300-800 DEG C, nitrogen atmosphere, and heating rate is 15 DEG C/min, records benzene
Temperature when base vinyl MTQ silicone resin weightlessness 10%, and result is listed in table 2.
Detecting refractive index: the phenyl vinyl MTQ silicone resin in embodiment 1-11, comparative example 1-2 is dissolved in ethyl acetate
In solution, using the refractive index of Shanghai optical instrument factory 2WA-J type abbe's refractometer measurement various concentration solution, using extrapolation
The refractive index for determining phenyl vinyl MTQ silicone resin lists measurement result in table 2.
Each embodiment heat resistance test result of table 2 and detecting refractive index result
By the result in table 2 it is found that the refractive index of the phenyl vinyl MTQ silicone resin in embodiment 1-5 is higher, adding
After entering modifying titanium dioxide, the refractive index of phenyl vinyl MTQ silicone resin can be significantly improved.Phenylethylene in comparative example 1-2
The detecting refractive index of base MTQ silicone resin is the results show that the nano-titanium dioxide of non-modified processing can also mention to a certain extent
High phenyl vinyl MTQ silicone resin, but the effect of not no modifying titanium dioxide is good.Acetaminocaproic Acid, benzoyloxy benzene
Benzyl formate can effectively improve the heat resistance of phenyl vinyl MTQ silicone resin, and acetyl group hexamethyl tetrahydronaphthalene can also improve
The heat resistance of phenyl vinyl MTQ silicone resin, and in the presence of three is common, improving, phenyl vinyl MTQ silicone resin is heat-resisting
Aspect of performance can play synergistic effect.
Claims (10)
1. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin, it is characterised in that: based on parts by weight, raw material includes
Following components,
The double-seal head is hexamethyldisiloxane and tetramethyl divinyl disiloxane with the mixture of arbitrary proportion.
2. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin according to claim 1, it is characterised in that: with
Parts by weight meter, raw material include 100 parts of a phenyl trichlorosilane；100 parts of double-seal head.
3. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin according to claim 1, it is characterised in that: with
Parts by weight meter, raw material include 120-150 parts of alkoxy silane；30-50 parts of lower alcohol；120-150 parts of solvent.
4. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin according to claim 1, it is characterised in that: institute
State alkoxy silane be one of tetramethoxy-silicane, tetraethoxysilane, tetraethoxysilane oligomer or a variety of, it is described
Tetraethoxysilane oligomer is one of silicon 32, silicon 40.
5. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin according to claim 1, it is characterised in that: institute
Stating solvent is aromatic solvent or lipid environmentally friendly solvent, and the aromatic solvent is toluene or dimethylbenzene, and the lipid environmentally friendly solvent is
Butyl acetate or PMA or DBE.
6. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin according to claim 1, it is characterised in that: institute
Stating lower alcohol is one of methanol, ethyl alcohol, isopropanol.
7. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin according to claim 1, it is characterised in that: with
Parts by weight meter, raw material further include 20-40 parts of Acetaminocaproic Acid, 25-30 parts of benzoyloxy Ergol.
8. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin according to claim 1, it is characterised in that: with
Parts by weight meter, raw material further include 10-20 parts of acetyl group hexamethyl tetrahydronaphthalene.
9. a kind of LED encapsulation high-quality phenyl vinyl MTQ silicone resin according to claim 1, it is characterised in that: with
Parts by weight meter, raw material further include 15-35 parts of modifying titanium dioxide；The modifying titanium dioxide is the preparation method is as follows: take nanometer
Titanium dioxide is put into N- acetyldihydro sphingol, is warming up to 40-50 DEG C, is kept the temperature 3-6h after mixing evenly, obtains modified two
Titanium oxide, wherein the mass ratio of nano-titanium dioxide and N- acetyldihydro sphingol is 2:3.
10. the system that high-quality phenyl vinyl MTQ silicone resin is used in a kind of any one LED encapsulation as claimed in claims 1-9
Preparation Method, it is characterised in that: include the following steps,
Solvent, water, lower alcohol, double-seal head are put in proportion into reaction kettle by S1, control kettle temperature at 20-50 DEG C, a phenyl is added dropwise
Trichlorosilane drips off for 1-2 hours；It is warming up to 50-80 DEG C, then alkoxy silane is added dropwise, is dripped off within 0.5-1.5 hours；
S2 is warming up to 70-90 DEG C after dripping off, maintain reflux 2-4 hours；
S3 cools to 50-55 DEG C, stratification；
S4 adds alkali neutralization into the feed liquid of reaction kettle or adds water washing to neutrality；
S5, with active carbon to feed liquid decoloration, filtering；
S6 is warming up to 80-150 DEG C, depressurizes desolventizing, obtains phenyl vinyl MTQ silicone resin.
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