CN110951451A - Packaging adhesive for LED and preparation method thereof - Google Patents
Packaging adhesive for LED and preparation method thereof Download PDFInfo
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- CN110951451A CN110951451A CN201911314235.7A CN201911314235A CN110951451A CN 110951451 A CN110951451 A CN 110951451A CN 201911314235 A CN201911314235 A CN 201911314235A CN 110951451 A CN110951451 A CN 110951451A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 57
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 57
- 238000004806 packaging method and process Methods 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 86
- 229920005989 resin Polymers 0.000 claims abstract description 72
- 239000011347 resin Substances 0.000 claims abstract description 72
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 60
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 45
- 239000001257 hydrogen Substances 0.000 claims abstract description 45
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 43
- 239000010703 silicon Substances 0.000 claims abstract description 43
- -1 vinyl hydrogen Chemical compound 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 22
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003112 inhibitor Substances 0.000 claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 239000008213 purified water Substances 0.000 claims description 11
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 239000012074 organic phase Substances 0.000 claims description 9
- 229920002050 silicone resin Polymers 0.000 claims description 9
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 8
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical group C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 8
- 229910000077 silane Inorganic materials 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000000178 monomer Substances 0.000 claims description 7
- 238000006068 polycondensation reaction Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical group CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 6
- 229920001971 elastomer Polymers 0.000 claims description 6
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 6
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 abstract description 8
- 239000000565 sealant Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000003014 reinforcing effect Effects 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 11
- 238000002156 mixing Methods 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000002390 adhesive tape Substances 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 239000005022 packaging material Substances 0.000 description 5
- 238000011056 performance test Methods 0.000 description 5
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 125000003700 epoxy group Chemical group 0.000 description 4
- 229920002379 silicone rubber Polymers 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910018557 Si O Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910021485 fumed silica Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 239000004636 vulcanized rubber Substances 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Power Engineering (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a packaging adhesive for an LED and a preparation method thereof, the preparation method firstly prepares vinyl hydrogen MQ silicon resin, and then adds the vinyl hydrogen MQ silicon resin into a pouring sealant to obtain the packaging adhesive for the LED, which is composed of AB two components prepared by the vinyl hydrogen MQ silicon resin and the vinyl resin, wherein the mass ratio of the component A to the component B is 10: 1; the component A is prepared from vinyl hydrogen based MQ silicon resin, vinyl silicon resin and an inhibitor according to the mass ratio of 100: 10-30: 0.01-0.3; the component B is prepared from vinyl resin, an adhesive and a catalyst according to a mass ratio of 100: 10-25: 1-3. The LED packaging adhesive has a reasonable and simple formula, not only improves the reinforcing effect of the LED packaging adhesive, but also has good light transmittance and fluidity, and is beneficial to construction and adhesive dispensing; in addition, the raw materials are easy to obtain, the operation is easy, the product quality is easy to control, and the method is suitable for large-scale industrial production and has popularization and application prospects.
Description
Technical Field
The invention relates to preparation and application of a packaging material, in particular to packaging glue for an LED (light emitting diode) and a preparation method thereof.
Background
In recent years, with the ever-increasing attention on environmental protection and the deep mind of energy-saving concept, LED devices are used as new generation of environmental protection and energy-saving lighting technology and green light source, and show increasing market demand worldwide.
The organic silicon has the advantages of high light transmittance, high refractive index, high heat resistance, low internal stress, low hygroscopicity and the like, and the performance of the organic silicon is far superior to that of epoxy resin when being used as an LED packaging material. A great deal of manpower and material resources are successively input by countries and lighting enterprises in the world to research the organic silicon material for LED packaging. The high-power white light LED packaging material is required to have certain hardness and tensile strength besides high refractive index, light transmittance and ultraviolet radiation resistance.
The MQ silicone resin is a silicone resin consisting of a monofunctional Si-O unit (M unit "mono") and a tetrafunctional Si-O unit (SiQZ is called Q unit "quad"), and has a compact sphere with a double-layer structure. MQ silicon resin is commonly used as a reinforcing agent of silicone rubber, and generally, the MQ silicon resin is powder and is not easy to disperse when being directly used. Meanwhile, the common MQ silicon resin synthesis process is complex, the subsequent treatment process is complicated, and the like, so that the quality stability of the product is difficult to ensure.
Except for MQ silicon resin, most of the prior art adopts the silicon rubber reinforced by adding white carbon black. Although the method can effectively improve the strength of the silicon rubber, the processing is complicated due to the difficult mixing, large dust and easy structurization of the white carbon black by the gas phase method; in addition, the price of the high-tearing white carbon black is quite expensive, and the cost is greatly increased. More importantly, the refractive index difference between the fumed silica and the organosilicon material is large, and the light transmittance of the LED packaging material is reduced after the fumed silica is added.
Disclosure of Invention
Aiming at the defects of the prior art, the invention develops the preparation of the vinyl hydrogen-based MQ silicon resin and adds the vinyl hydrogen-based MQ silicon resin into the pouring sealant for use, and provides the LED packaging sealant and the preparation method thereof.
In order to achieve the above object of the invention, the embodiments are as follows:
the invention provides an LED packaging adhesive, which mainly comprises A, B two components prepared from vinyl hydrogen-based MQ silicon resin and vinyl resin, wherein the mass ratio of the component A to the component B is 10: 1; the component A is vinyl hydrogen based MQ silicon resin, vinyl silicon resin and an inhibitor which are prepared according to the mass ratio of 100: 10-30: 0.01-0.3; the component B is prepared from vinyl resin, an adhesive and a catalyst according to a mass ratio of 100: 10-25: 1-3.
The invention also provides a preparation method of the LED packaging adhesive, the preparation method adds the vinyl hydrogen group MQ silicon resin into the packaging adhesive, and the preparation method comprises the following steps and process conditions:
the method comprises the following steps: preparation of vinyl hydrogen-based MQ silicon resin
Feeding a silane monomer, a vinyl end-capping agent and a hydrogen-containing end-capping agent in a mass ratio of 100: 10-20: 15-20 to prepare a mixed system, dripping a catalyst into the mixed system under stirring, keeping the temperature between 0 and 40 ℃ during dripping, heating for hydrolytic polycondensation after dripping is finished, keeping the reaction temperature between 50 and 80 ℃, and keeping the reaction time for 3 to 8 hours; cooling and standing the reaction liquid for layering, taking a lower organic phase, repeatedly washing the lower organic phase with water to be neutral, and distilling under reduced pressure to remove low molecular substances under the conditions of 120-160 ℃ and-0.09-0.1 MP to obtain the MQ silicon resin containing hydrogen of 0.16-0.3%, vinyl of 2.5-4% and viscosity of 1000-5000 mPa.s at 25 ℃;
the catalyst is a mixed solution of purified water and concentrated hydrochloric acid, and the mass ratio of the silane monomer to the vinyl end capping agent to the hydrogen-containing end capping agent to the purified water to the concentrated hydrochloric acid is 100: 10-20: 15-20: 62.5-98: 37.5-70, wherein the amount of the purified water is 50-70% of the total amount of reactants, and the amount of the concentrated hydrochloric acid is 30-50% of the total amount of the reactants;
step two: preparation of packaging adhesive for LED
Preparing a component A from vinyl hydrogen based MQ silicon resin, vinyl silicon resin and an inhibitor according to a mass ratio of 100: 10-30: 0.01-0.3; the component B is prepared from vinyl resin, an adhesive and a catalyst according to the mass ratio of 100: 10-25: 1-3; the mass ratio of the component A to the component B is 10:1, the components are uniformly mixed and defoamed in vacuum to obtain packaging virgin rubber for the LED, and the packaging virgin rubber is cured for 2-5 hours at 120-160 ℃ to prepare adhesive strips, so that the packaging rubber for the LED is obtained;
the vinyl silicone resin has a vinyl content of 4-6%, and a viscosity of 10000-30000mPa.s at 25 ℃; preferably vinyl silicone resin having a vinyl content of 5% and a viscosity of 20000 at 25 ℃;
the inhibitor is one or a mixture of more than one of 1-ethynyl-1-cyclohexanol and 2-methyl-3-butynol-2-ol; preferably 1-ethynyl-1-cyclohexanol;
the adhesive is an adhesive containing vinyl, hydroxyl and epoxy functional structures;
the catalyst is chloroplatinic acid or a Karster catalyst, wherein the Karster catalyst has a platinum content of 3000-5000 ppm, preferably 5000 ppm;
the silane monomer is methyl orthosilicate or ethyl orthosilicate; preferably methyl orthosilicate;
the vinyl end-capping agent is tetramethyl divinyl disiloxane or dimethyl divinyl ethoxysilane; preferably tetramethyldivinyldisiloxane;
the hydrogen-containing end-capping reagent is tetramethyl dihydrodisiloxane or dimethyl dihydroethoxysilane; preferably tetramethyldihydrodisiloxane;
the curing conditions are preferably 150 ℃ for 3 hours.
Compared with the prior art, the invention has the following advantages:
1. the LED packaging adhesive containing the vinyl hydrogen group MQ silicon resin is reasonable and simple in formula, not only improves the reinforcing effect of the LED packaging adhesive, but also has good light transmittance and fluidity, and is beneficial to construction and adhesive dispensing.
2. The LED packaging adhesive prepared by the invention can obtain an LED packaging product with higher hardness and excellent mechanical property and tear strength without adding a reinforcing material. The performance test results of the cured LED packaging products prepared in the embodiments 1 to 5 are shown in Table 1, and all the performance test results meet or even exceed the requirements of the packaging adhesive used as an environment-friendly and energy-saving new-generation lighting technology and a green light source LED.
3. The reasonable formula and feasible technical route of the invention are further illustrated by the relevant data of comparative examples 1 and 2 and the performance test results shown in Table 1; in addition, the raw materials are easy to obtain, the operation is easy, the product quality is easy to control, and the method is suitable for large-scale industrial production and has popularization and application prospects.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The present invention is further illustrated by the following examples, which are intended to provide those skilled in the art with a full understanding and appreciation of the invention. Any combination or substitution of features in the embodiments without departing from the principle of the present invention shall be deemed to be within the scope of the present invention.
Example 1
A preparation method of packaging adhesive for LED comprises the following steps and process conditions:
the method comprises the following steps: preparation of vinyl hydrogen-based MQ silicon resin
The preparation method comprises the steps of feeding tetraethoxysilane, tetramethyl divinyl disiloxane and tetramethyl dihydro disiloxane according to the mass ratio of 100:10:15 to prepare a mixed system, dripping a mixed solution of 62.5 parts of purified water and 37.5 parts of hydrochloric acid with the concentration of 36% into the mixed system under the stirring condition, keeping the temperature between 0 and 40 ℃ during dripping, heating up for hydrolytic polycondensation reaction after dripping is finished, keeping the reaction temperature at 70 ℃, and keeping the reaction time at 3.5 hours; cooling the reaction liquid, standing for layering, taking a lower-layer organic phase, repeatedly washing with water to be neutral, and distilling under reduced pressure to remove low molecular substances under the conditions of 150 ℃ and-0.09 MP to obtain the vinyl hydrogen-containing MQ silicon resin with the hydrogen content of 0.16 percent, the vinyl content of 2.5 percent and the viscosity of 5000mPa.s at 25 ℃;
step two: preparation of packaging adhesive for LED
Preparing a component A from the vinylhydride MQ silicon resin prepared in the step one, the vinyl silicon resin with the vinyl content of 5% and the viscosity of 20000mPa.s at 25 ℃ and an inhibitor 1-ethynyl-1-cyclohexanol according to the mass ratio of 100:20: 0.01; a vinyl silicon resin with 5 percent of vinyl content and 20000mPa.s of viscosity at 25 ℃, an adhesive HM-160 (21.5 percent of epoxy group content with 25.5 percent of hydroxyl group content) and a Karster catalyst with 5000ppm of platinum content are prepared into a component B according to the mass ratio of 100:10: 1; the mass ratio of the component A to the component B is 10:1, the components are uniformly mixed, defoamed in vacuum, and cured for 3 hours at 150 ℃ to prepare the packaging adhesive tape for the LED, and the test performance is shown in Table 1.
Example 2
A preparation method of packaging adhesive for LED comprises the following steps and process conditions:
the method comprises the following steps: preparation of vinyl hydrogen-based MQ silicon resin
The preparation method comprises the steps of feeding methyl orthosilicate, tetramethyl divinyl disiloxane and tetramethyl dihydro disiloxane according to a mass ratio of 100:10:20 to prepare a mixed system, dripping a mixed solution of 65 parts of purified water and 65 parts of hydrochloric acid with a concentration of 36% into the mixed system under a stirring condition, keeping the temperature between 0 and 40 ℃ during dripping, heating up for hydrolytic polycondensation reaction after dripping is finished, keeping the reaction temperature at 60 ℃, and keeping the reaction time at 6 hours; cooling the reaction liquid, standing for layering, taking a lower-layer organic phase, repeatedly washing with water to be neutral, and distilling under reduced pressure at 120 ℃ and under the reduced pressure condition of-0.1 MP to remove low molecular substances to obtain the MQ silicon resin containing vinyl hydrogen with the hydrogen content of 0.3 percent, the vinyl content of 2.7 percent and the viscosity of 1000mPa.s at 25 ℃;
step two: preparation of packaging adhesive for LED
Mixing the vinyl hydrogen group MQ silicon resin prepared in the step one, vinyl silicon resin with the vinyl content of 4% and the viscosity of 30000mPa.s at 25 ℃, and inhibitor 2-methyl-3-butynol-2-ol according to the proportion of 100: 30: 0.3 of component A; a vinyl silicon resin with 5 percent of vinyl content and viscosity of 30000mPa.s at 25 ℃, an adhesive HM-513 (vinyl 5 percent and epoxy group 4.3 percent) and a Karster catalyst with 5000ppm of platinum content are prepared into a component B according to the mass ratio of 100:10: 2; the mass ratio of the component A to the component B is 10:1, the components are uniformly mixed, defoamed in vacuum, and cured for 5 hours at 120 ℃ to prepare the packaging adhesive tape for the LED, and the test performance is shown in Table 1.
Example 3
A preparation method of packaging adhesive for LED comprises the following steps and process conditions:
the method comprises the following steps: preparation of vinyl hydrogen-based MQ silicon resin
The preparation method comprises the steps of feeding methyl orthosilicate, dimethyl divinyl ethoxysilane and dimethyl dihydro ethoxysilane according to the mass ratio of 100:20:20 to prepare a mixed system, dripping a mixed solution of 98 parts of purified water and 42 parts of hydrochloric acid with the concentration of 36% into the mixed system under the condition of stirring, keeping the temperature between 0 and 40 ℃ during dripping, heating up for hydrolytic polycondensation reaction after dripping is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time for 3 hours; cooling the reaction liquid, standing for layering, taking a lower-layer organic phase, repeatedly washing with water to neutrality, distilling under reduced pressure at 150 ℃ and under the reduced pressure condition of-0.1 MP to remove low molecular substances, and obtaining the hydrogen-containing MQ silicon resin with the hydrogen content of 0.27 percent, the vinyl content of 4 percent and the viscosity of 3300mPa.s at 25 ℃;
step two: preparation of packaging adhesive for LED
Mixing the vinyl hydrogen group MQ silicon resin prepared in the step one, vinyl silicon resin with the vinyl content of 4% and the viscosity of 30000mPa.s at 25 ℃, and inhibitor 2-methyl-3-butynol-2-ol according to the proportion of 100:15: 0.1 mass ratio of component A; a vinyl silicon resin with 4 percent of vinyl content and 30000mPa.s of viscosity at 25 ℃, an adhesive HM-160 (21.5 percent of epoxy group content with 25.5 percent of hydroxyl content) and a Karster catalyst with 3000ppm of platinum content are prepared into a component B according to the mass ratio of 100:10: 3; the mass ratio of the component A to the component B is 10:1, the components are uniformly mixed, defoamed in vacuum, cured for 4 hours at 130 ℃ and prepared into the packaging adhesive tape for the LED, and the test performance is shown in Table 1.
Example 4
A preparation method of packaging adhesive for LED comprises the following steps and process conditions:
the method comprises the following steps: preparation of vinyl hydrogen-based MQ silicon resin
Preparing a mixed system by feeding methyl orthosilicate, tetramethyl divinyl disiloxane and tetramethyl dihydro disiloxane according to a mass ratio of 100:20:15, dripping a mixed solution of 62.5 parts of purified water and 37.5 parts of hydrochloric acid with a concentration of 36% into the mixed system under a stirring condition, keeping the temperature between 0 and 40 ℃ during dripping, heating up for hydrolytic polycondensation reaction after dripping is finished, keeping the reaction temperature at 60 ℃, and keeping the reaction time at 8 hours; cooling the reaction liquid, standing for layering, taking a lower-layer organic phase, repeatedly washing with water to be neutral, and distilling under reduced pressure at 150 ℃ and under the reduced pressure condition of-0.1 MP to remove low molecular substances to obtain the MQ silicon resin containing the vinyl hydrogen with the hydrogen content of 0.17 percent, the vinyl content of 3.8 percent and the viscosity of 4300mPa.s at 25 ℃;
step two: preparation of packaging adhesive for LED
The vinyl hydrogen-based MQ silicon resin prepared in the first step, vinyl silicon resin with the vinyl content of 6% and the viscosity of 10000mPa.s at 25 ℃ and an inhibitor are mixed according to the weight ratio of 100:10: 0.2, preparing the component A, wherein the inhibitor is a mixture of 1-ethynyl-1-cyclohexanol and 2-methyl-3-butynol-2-ol (in a mass ratio of 1: 1); a vinyl silicon resin with the vinyl content of 6 percent and the viscosity of 10000mPa.s at 25 ℃, an adhesive HM-513 (vinyl 5 percent and epoxy group 4.3 percent) and a Karster catalyst with the platinum content of 3000ppm are prepared into a component B according to the mass ratio of 100:10: 3; the mass ratio of the component A to the component B is 10:1, the components are uniformly mixed, defoamed in vacuum, and cured for 3 hours at 150 ℃ to prepare the packaging adhesive tape for the LED, and the test performance is shown in Table 1.
Example 5
A preparation method of packaging adhesive for LED comprises the following steps and process conditions:
the method comprises the following steps: preparation of vinyl hydrogen-based MQ silicon resin
The preparation method comprises the steps of feeding tetraethoxysilane, tetramethyl divinyl disiloxane and tetramethyl dihydro disiloxane according to the mass ratio of 100:15:15 to prepare a mixed system, dripping a mixed solution of 65 parts of purified water and 65 parts of hydrochloric acid with the concentration of 36% into the mixed system under the stirring condition, keeping the temperature between 0 and 40 ℃ during dripping, heating up for hydrolytic polycondensation reaction after dripping is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time for 3 hours; cooling the reaction liquid, standing for layering, taking a lower-layer organic phase, repeatedly washing with water to neutrality, distilling under reduced pressure at 150 ℃ and under the reduced pressure condition of-0.1 MP to remove low molecular substances, and obtaining the MQ silicon resin containing the vinyl hydrogen with the hydrogen content of 0.18 percent, the vinyl content of 3.2 percent and the viscosity of 3100mPa.s at 25 ℃;
step two: preparation of packaging adhesive for LED
The vinyl hydrogen-based MQ silicon resin prepared in the first step, vinyl silicon resin with 5% of vinyl content and 20000mPa.s of viscosity at 25 ℃ and inhibitor 2-methyl-3-butynol-2-ol are mixed according to the proportion of 100: 25: 0.3 of component A; vinyl silicone resin with 5% vinyl content and viscosity of 20000mPa.s at 25 ℃, adhesive HM-513 (vinyl 5% epoxy 4.3%), chloroplatinic acid catalyst with 5000ppm platinum content, wherein the weight ratio of the vinyl silicone resin to the adhesive HM-513 is 100:10:2, preparing a component B; the mass ratio of the component A to the component B is 10:1, the components are uniformly mixed, defoamed in vacuum, cured for 2 hours at 160 ℃ and prepared into the packaging adhesive tape for the LED, and the test performance is shown in Table 1.
Comparative example 1
Sequentially mixing vinyl MQ silicon resin (viscosity of 8000mPa.s at 25 ℃) with vinyl content of 5%, hydrogen-containing silicon resin (viscosity of 5000mPa.s at 25 ℃) with hydrogen content of 0.3%, and 2-methyl-3-butynol-2-ol according to the proportion of 10: 40: 0.3 weight ratio to prepare glue A; mixing vinyl MQ silicon resin (viscosity 8000mPa.s at 25 ℃) with vinyl content of 2%, adhesive HM-160 (hydroxyl content 25.5% and epoxy content 21.5%), Karster catalyst with platinum content 5000ppm according to a proportion of 50: 1.5: 0.2 weight ratio to prepare glue B;
and uniformly mixing the component A and the component B according to the weight ratio of 1:1, and defoaming in vacuum to prepare the packaging adhesive for the LED. The encapsulation adhesive was cured at 150 ℃ for 3 hours and tested for performance. The test results are shown in table 1.
Comparative example 2
Sequentially mixing hydrogen group MQ silicon resin (viscosity is 3000mPa.s at 25 ℃) with hydrogen content of 0.5%, vinyl silicon resin (viscosity is 10000mPa.s at 25 ℃) with vinyl content of 6%, 2-methyl-3-butynol-2-ol according to the weight ratio of 30: 20: 0.3 weight ratio to prepare glue A; vinyl silicone resin (viscosity 10000mPa.s at 25 ℃), adhesive HM-513 (vinyl 5% epoxy 4.3%), Karster catalyst with platinum content 5000ppm were mixed according to a ratio of 50: 15: 2 is prepared into glue B;
and uniformly mixing the component A and the component B according to the weight ratio of 1:1, and defoaming in vacuum to prepare the packaging adhesive for the LED. The encapsulation adhesive was cured at 150 ℃ for 3 hours and tested for performance. The test results are shown in table 1.
TABLE 1 post cure Performance test results for resins
The product performance test methods in table 1 are as follows:
hardness: and (4) measuring the hardness of the silicone rubber according to the standard GB/T531-2008.
Tensile strength and elongation at break: and testing the tensile strength and the elongation at break of the vulcanized rubber according to GB/T528-2009.
Tear strength test: and testing the tearing strength of the vulcanized rubber according to GB/T528-2008.
Light transmittance: and testing the light transmittance in the visible wavelength range of 200-800 nm by using an ultraviolet-visible spectrophotometer at the temperature of 25 ℃.
Table 1 shows that, after the vinyl hydrogen-containing MQ resin prepared by the present invention is added, the hardness and tear strength of the encapsulation adhesive are both greatly improved compared with those of the pure vinyl MQ resin or the hydrogen-containing MQ resin, and the tensile strength of the encapsulation adhesive is significantly increased. Meanwhile, the resin obtained by the invention has good compatibility with vinyl resin, and the prepared LED packaging material has higher light transmittance.
Claims (4)
1. The LED packaging adhesive is characterized by mainly comprising A, B two components prepared from vinyl hydrogen-based MQ silicone resin and vinyl resin, wherein the mass ratio of the component A to the component B is 10: 1; the component A is vinyl hydrogen based MQ silicon resin, vinyl silicon resin and an inhibitor which are prepared according to the mass ratio of 100: 10-30: 0.01-0.3; the component B is prepared from vinyl resin, an adhesive and a catalyst according to a mass ratio of 100: 10-25: 1-3.
2. A preparation method of a packaging adhesive for an LED is characterized in that a vinyl hydrogen group MQ silicon resin is added into a pouring adhesive, and the preparation method comprises the following steps and process conditions:
the method comprises the following steps: preparation of vinyl hydrogen-based MQ silicon resin
Feeding a silane monomer, a vinyl end-capping agent and a hydrogen-containing end-capping agent in a mass ratio of 100: 10-20: 15-20 to prepare a mixed system, dripping a catalyst into the mixed system under stirring, keeping the temperature between 0 and 40 ℃ during dripping, heating for hydrolytic polycondensation after dripping is finished, keeping the reaction temperature between 50 and 80 ℃, and keeping the reaction time for 3 to 8 hours; cooling and standing the reaction liquid for layering, taking a lower organic phase, repeatedly washing the lower organic phase with water to be neutral, and distilling under reduced pressure to remove low molecular substances under the conditions of 120-160 ℃ and-0.09-0.1 MP to obtain the MQ silicon resin containing hydrogen of 0.16-0.3%, vinyl of 2.5-4% and viscosity of 1000-5000 mPa.s at 25 ℃;
the catalyst is a mixed solution of purified water and concentrated hydrochloric acid, and the mass ratio of the silane monomer to the vinyl end capping agent to the hydrogen-containing end capping agent to the purified water to the concentrated hydrochloric acid is 100: 10-20: 15-20: 62.5-98: 37.5-70, wherein the amount of the purified water is 50-70% of the total amount of reactants, and the amount of the concentrated hydrochloric acid is 30-50% of the total amount of the reactants;
step two: preparation of packaging adhesive for LED
Preparing a component A from vinyl hydrogen based MQ silicon resin, vinyl silicon resin and an inhibitor according to a mass ratio of 100: 10-30: 0.01-0.3; the component B is prepared from vinyl resin, an adhesive and a catalyst according to the mass ratio of 100: 10-25: 1-3; the mass ratio of the component A to the component B is 10:1, the components are uniformly mixed and defoamed in vacuum to obtain packaging virgin rubber for the LED, and the packaging virgin rubber is cured for 2-5 hours at 120-160 ℃ to prepare adhesive strips, so that the packaging rubber for the LED is obtained;
the vinyl silicone resin has a vinyl content of 4-6%, and a viscosity of 10000-30000mPa.s at 25 ℃;
the inhibitor is one or a mixture of more than one of 1-ethynyl-1-cyclohexanol and 2-methyl-3-butynol-2-ol;
the adhesive is an adhesive containing vinyl, hydroxyl and epoxy functional structures;
the catalyst is chloroplatinic acid or a Karster catalyst, wherein the platinum content is 3000-5000 ppm.
3. The method for preparing the packaging adhesive for the LED according to claim 2, wherein the method comprises the following steps:
the silane monomer is methyl orthosilicate or ethyl orthosilicate;
the vinyl end-capping agent is tetramethyl divinyl disiloxane or dimethyl divinyl ethoxysilane;
the hydrogen-containing end-capping reagent is tetramethyl dihydrodisiloxane or dimethyl dihydroethoxy silane.
4. The method for preparing the packaging adhesive for the LED according to claim 2 or 3, wherein the method comprises the following steps: the silane monomer is methyl orthosilicate;
the vinyl end-capping agent is tetramethyl divinyl disiloxane;
the hydrogen-containing end-capping reagent is tetramethyldihydrodisiloxane;
the inhibitor is 1-ethynyl-1-cyclohexanol;
the vinyl silicon resin is vinyl silicon resin with 5% of vinyl content and 20000 viscosity;
the catalyst is a Karster catalyst with platinum content of 5000 ppm;
the curing condition is 150 ℃ for 3 hours.
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| CN112694865A (en) * | 2020-12-18 | 2021-04-23 | 广东普赛达密封粘胶有限公司 | Single-component thermosetting organic silicon adhesive for adhering electric kettle and preparation method thereof |
| CN115926738A (en) * | 2022-12-14 | 2023-04-07 | 烟台德邦科技股份有限公司 | Heat-conducting insulating silica gel for high-strength semiconductor packaging and preparation method thereof |
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