CN114456383A - Organic silicon adhesion promoter for LED packaging and preparation method and application thereof - Google Patents
Organic silicon adhesion promoter for LED packaging and preparation method and application thereof Download PDFInfo
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- CN114456383A CN114456383A CN202210136697.XA CN202210136697A CN114456383A CN 114456383 A CN114456383 A CN 114456383A CN 202210136697 A CN202210136697 A CN 202210136697A CN 114456383 A CN114456383 A CN 114456383A
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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
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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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
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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Abstract
The invention discloses an organic silicon adhesion promoter for LED packaging and a preparation method and application thereof. Epoxy silane, acrylic acid hydroxy ester and a catalyst are mixed and react to obtain epoxy silane containing an acrylate group; 1,3,5, 7-tetramethylcyclotetrasiloxane, noble metal catalyst and organic solvent are uniformly mixed, and the mixed solution of acetoacetic acid alkenyl ester and epoxy silane containing acrylate group is dripped into the mixed solution for reaction to obtain the adhesion promoter. The adhesion promoter simultaneously contains alkoxy, epoxy, ester, beta-dicarbonyl and hydrogen, is added into addition type organic silicon packaging glue, has good adhesion performance to metals such as aluminum, copper, stainless steel and the like and substrates such as PPA, PBT, PCB and the like, and can meet the use requirements of most LED substrates and electronic devices.
Description
Technical Field
The invention relates to a material for LED packaging, in particular to an organic silicon bonding promoter for LED packaging and a preparation method and application thereof.
Background
The addition type organic silicon resin for LED packaging has the characteristics of high temperature yellowing resistance, good ultraviolet aging resistance and the like, so that the addition type organic silicon resin has wide application in high-power indicator lamps. The LED base materials are various, and the bonding force between the common addition type packaging adhesive and the base materials is weaker after the common addition type packaging adhesive is cured. Moisture and sulfur dioxide in the air easily enter the device through the gap to cause failure. The current common method is to increase the adhesion between the packaging adhesive and the substrate by adding an adhesion promoter.
With the development of LED packaging technology, the invention patents related to the adhesion promoter of LED addition type packaging glue are increased year by year. For example, chinese patent publication No. CN105482120A reports an adhesive obtained by reacting hydrogen-containing silicone oil or tetramethylcyclotetrasiloxane with vinylsilane and methacryloxysilane, which has excellent adhesion to metallic aluminum, polyphthalamide and polycarbonate, but has poor adhesion to other substrates, and is only applicable to a system having a refractive index of about 1.42, and has a narrow application range. Chinese patent publication No. CN108129845A reports an adhesive obtained by reacting silane, hydroxyl-terminated polysiloxane and end-cap under the conditions of deionized water and catalyst, and then adding epoxysilane, estersilane and end-cap to continue the reaction, which has good compatibility with the system and good adhesion to metal aluminum, polyphthalamide and carbonate, but the synthesis process is complicated, the post-treatment is more, and the applicability to other base materials is not strong. Chinese patent publication No. CN105524282A reports an adhesive obtained by reacting diphenylsilanediol, epoxysilane, estersilane, borate and solvent under the catalysis of titanate, which has good adhesion to plastic substrates such as polyphthalamide, poly (1, 4-cyclohexanedimethanol terephthalate) and polycarbonate, but residual catalyst titanate is easy to yellow the addition type packaging adhesive and has poor storage stability in the packaging adhesive.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of an organic silicon adhesion promoter for LED packaging.
Another object of the present invention is to provide the silicone adhesion promoter for LED encapsulation obtained by the above production method.
The invention further aims to provide application of the organic silicon adhesion promoter for LED packaging.
The purpose of the invention is realized by the following technical scheme: a preparation method of an organic silicon adhesion promoter for LED packaging comprises the following steps:
(1) mixing epoxy silane, acrylic acid hydroxy ester and a catalyst, heating to 60-100 ℃, reacting for 3-10 hours, reacting under the conditions that the vacuum degree is-0.06-0.09 MPa and the temperature is 80-100 ℃ until no fraction flows out, and obtaining epoxy silane containing acrylate groups;
(2) uniformly mixing 1,3,5, 7-tetramethylcyclotetrasiloxane, a noble metal catalyst and an organic solvent to obtain a mixed solution A; mixing alkenyl acetoacetate with the epoxy silane containing the acrylate group obtained in the step (1) to obtain a mixed solution B; and heating the mixed solution A to 60-80 ℃, dropwise adding the mixed solution B into the mixed solution A for reaction, and removing low-boiling-point substances under the condition of-0.06-0.09 MP after the reaction is finished to obtain the adhesion promoter.
The epoxysilane in step (1) is preferably at least one selected from the group consisting of 3- (2, 3-epoxypropoxy) propyltrimethoxysilane, 3- (2, 3-epoxypropoxy) propylmethyldimethoxysilane, 3- (2, 3-epoxypropoxy) propyltriethoxysilane, 3- (2, 3-epoxypropoxy) propylmethyldiethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethylmethyldimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltriethoxysilane and 2- (3, 4-epoxycyclohexyl) ethylmethyldiethoxysilane.
The hydroxyl acrylate in the step (1) is preferably at least one of hydroxyethyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate and hydroxypropyl methacrylate.
The catalyst in the step (1) is an ester exchange catalyst, and preferably at least one of dibutyltin dilaurate, dibutyltin diacetate, triethyl borate, isopropyl borate and tributyl borate.
The reaction substances in the step (1) are epoxy silane and acrylic hydroxyl ester, and the epoxy silane and the acrylic hydroxyl ester are preferably matched according to the molar ratio of 1 (1-1.2); more preferably, the molar ratio is 1 (1-1.1).
The dosage of the catalyst in the step (1) is conventional dosage, and is preferably 0.1-1% of the total mass of the reaction substances (epoxy silane and acrylic acid hydroxy ester).
The noble metal catalyst in the step (2) is at least one of platinum, palladium, rhodium and complex compounds thereof; preferably at least one of chloroplatinic acid and 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum.
The dosage of the noble metal catalyst in the step (2) is conventional dosage, and is preferably 0.01-0.3% of the mass of 1,3,5, 7-tetramethylcyclotetrasiloxane.
The alkenyl acetoacetate in step (2) is at least one of allyl acetoacetate, ethylene glycol acetoacetate methacrylate, and ethylene glycol acetoacetate acrylate.
The organic solvent in the step (2) is at least one of toluene, cyclohexane and methylcyclohexane.
The organic solvent does not participate in the reaction and is used for dissolving reaction substances; the amount of the compound is preferably 1 to 2 times of the mass of 1,3,5, 7-tetramethylcyclotetrasiloxane.
The amount of the reaction substance in the step (2) is preferably 1,3,5, 7-tetramethylcyclotetrasiloxane: alkenyl acetoacetate: molar ratio of acrylate group-containing epoxy silane ═ 1: 1: (1-2).
The reaction time in the step (2) is preferably 5-16 hours.
An organic silicon adhesion promoter for LED packaging is obtained by the preparation method.
The organic silicon bonding accelerant for LED packaging is applied to addition type organic silicon packaging glue.
Compared with the prior art, the invention has the following advantages and effects:
1. the invention provides an organic silicon packaging adhesive bonding accelerant for an LED, which contains alkoxy, epoxy, ester, beta-dicarbonyl and hydrogen radicals in the structure, and the structure is added into addition type organic silicon packaging adhesive, so that the bonding of the organic silicon packaging adhesive to various metals (aluminum, copper and stainless steel) and plastic base materials (polyphthalamide (PPA), polybutylene terephthalate (PBT) and Printed Circuit Board (PCB)) can be greatly improved, the application range is wider than that of the existing adhesive, and the use of most LED base materials and electronic devices can be met.
2. The organic silicon packaging adhesive bonding accelerant for the LED prepared by the invention is carried out under a non-aqueous phase condition, and side reactions such as epoxy ring opening and the like can be prevented. Meanwhile, the reaction condition is mild, and the production and the control are easy.
3. The organic silicon packaging adhesive bonding promoter for the LED, which is prepared by the invention, has a siloxane structure similar to the packaging adhesive in structure, so that the organic silicon packaging adhesive bonding promoter has good compatibility with a system and cannot influence the light transmittance.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
(1) Preparation of adhesion promoter
236g (1mol) of 3- (2, 3-epoxypropoxy) propyltrimethoxysilane (silane coupling agent KH-560), 116g (1mol) of hydroxyethyl acrylate and 0.35g of dibutyltin dilaurate are stirred uniformly at room temperature, heated to 100 ℃ for reaction for 3 hours, and decompressed to-0.09 MP at the current temperature to remove low-boiling-point substances, thus obtaining 310g of colorless transparent intermediate product 1.
Adding 120g (0.5mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane and 0.36g of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst into a reaction vessel, adding 120g of cyclohexane, uniformly mixing, heating to 80 ℃, dropwise adding a mixture of 71g (0.5mol) of allyl acetoacetate and 160g (0.5mol) of intermediate product 1 into the reaction vessel within 1 hour, preserving heat at 80 ℃ for 5 hours, and then removing low-boiling-point substances under the condition of-0.09 MP to obtain the adhesion promoter 1.
(2) Preparation of addition type packaging adhesive sample for LED
85 parts by mass of vinyl methyl silicone resin with the viscosity of 6000mPa s vinyl content of 1.31 wt%, 15 parts by mass of vinyl silicone oil with the viscosity of 10000mPa s vinyl content of 0.12 wt%, 4.3 parts by mass of hydrogen-containing silicone oil with the active hydrogen content of 1.0 wt%, 2 parts by mass of adhesion promoter 1 and 0.01 part by mass of 1-ethynyl-1-cyclohexanol are uniformly mixed under the action of a high-speed centrifuge (1000RPM), then 0.1 part by mass of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst is added, the mixture is uniformly mixed, vacuum defoaming is carried out, curing is carried out for 1 hour at 80 ℃, curing is carried out for 3 hours at 150 ℃, and the properties of the sample are shown in Table 1.
Example 2
(1) Preparation of adhesion promoter
278g (1mol) of 3- (2, 3-epoxypropoxy) propyltriethoxysilane, 139g (1.2mol) of hydroxyethyl acrylate and 4.17g of triethyl borate are stirred uniformly at room temperature, heated to 60 ℃ for reaction for 10 hours, and decompressed to-0.09 MP at the temperature of 90 ℃ to remove low-boiling substances, thus obtaining 353g of colorless transparent intermediate product 2.
Adding 120g (0.5mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane and 0.012g of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst into a reaction vessel, adding 120g of cyclohexane, uniformly mixing, heating to 60 ℃, dropwise adding a mixture of 71g (0.5mol) of allyl acetoacetate and 181g (0.5mol) of intermediate product 2 into the reaction vessel within 1 hour, preserving heat at 60 ℃ for 16 hours after dropwise adding, and then removing low-boiling-point substances under the condition of-0.09 MP to obtain the adhesion promoter 2.
(2) Preparation of addition type packaging adhesive sample for LED
The preparation method of the sample of the addition type packaging adhesive for the LED in the embodiment is basically the same as that of the embodiment 1, except that the adhesion promoter 1 in the embodiment 1 is changed into the adhesion promoter 2, and the properties of the sample are shown in the table 1.
Example 3
(1) Preparation of adhesion promoter
246g (1mol) of 2- (3, 4-epoxy cyclohexyl) ethyl trimethoxy silane, 116g (1mol) of hydroxyethyl acrylate and 1.00g of dibutyltin diacetate are stirred uniformly at room temperature, the temperature is raised to 60 ℃ for reaction for 6 hours, and low-boiling-point substances are removed by reducing the pressure to-0.06 MP at the temperature of 80 ℃ to obtain 319g of colorless transparent intermediate product 3.
60g (0.25mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane and 0.18g of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst are added into a reaction vessel, 120g of toluene is added, the mixture is uniformly mixed, the temperature is raised to 80 ℃, a mixture of 53g (0.25mol) of acetoacetic acid ethylene glycol methacrylate and 165g (0.5mol) of intermediate product 3 is dripped into the reaction vessel within 1 hour, the temperature is kept at 80 ℃ for 8 hours after the dripping is finished, and then low-boiling substances are removed under the condition of-0.06 MP, so that the adhesion promoter 3 is obtained.
(2) Preparation of addition type packaging adhesive sample for LED
The preparation method of the sample of the addition type packaging adhesive for the LED in the embodiment is basically the same as that of the embodiment 1, except that the adhesion promoter 1 in the embodiment 1 is changed into the adhesion promoter 3, and the properties of the sample are shown in the table 1.
Example 4
(1) Preparation of adhesion promoter
236g (1mol) of 3- (2, 3-epoxypropoxy) propyltrimethoxysilane, 130g (1mol) of hydroxyethyl methacrylate and 1.00g of dibutyltin diacetate are stirred uniformly at room temperature, the temperature is raised to 60 ℃ for reaction for 6 hours, and the low-boiling-point substances are removed at the temperature of 90 ℃ under reduced pressure of-0.06 MP, so that 315g of colorless transparent intermediate product 4 is obtained.
Adding 120g (0.5mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane and 0.36g of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst into a reaction container, adding 120g of toluene, uniformly mixing, heating to 80 ℃, dropwise adding a mixture of 107g (0.5mol) of acetoacetic acid ethylene glycol methacrylate and 167g (0.5mol) of intermediate product 4 into the reaction container within 1 hour, keeping the temperature at 80 ℃ for 8 hours after the dropwise adding is completed, and then removing low-boiling-point substances under the condition of-0.06 MP to obtain the adhesion promoter 4.
(2) Preparation of addition type packaging adhesive sample for LED
The preparation method of the sample of the addition type packaging adhesive for the LED in the embodiment is basically the same as that of the embodiment 1, except that the adhesion promoter 1 in the embodiment 1 is changed into the adhesion promoter 4, and the properties of the sample are shown in the table 1.
Example 5
(1) Preparation of adhesion promoter
236g (1mol) of 3- (2, 3-epoxypropoxy) propyltrimethoxysilane, 130g (1mol) of hydroxyethyl methacrylate and 0.35g of dibutyltin dilaurate are stirred uniformly at room temperature, heated to 70 ℃ for reaction for 10 hours, and reduced pressure to-0.09 MP at the temperature of 90 ℃ to remove low-boiling-point substances, thus obtaining 319g of colorless transparent intermediate product 5.
Adding 120g (0.5mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane and 0.36g of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst into a reaction vessel, adding 120g of toluene, uniformly mixing, heating to 80 ℃, dripping a mixture of 71g (0.5mol) of allyl acetoacetate and 167g (0.5mol) of intermediate product 5 into the reaction vessel within 1 hour, preserving heat for 8 hours after finishing dripping, and removing low-boiling-point substances under the condition of-0.06 MP after the reaction is finished to obtain the adhesion promotion 5.
(2) Preparation of addition type packaging adhesive sample for LED
The preparation method of the sample of the addition type packaging adhesive for the LED in the embodiment is basically the same as that of the embodiment 1, except that the adhesion promoter 1 in the embodiment 1 is changed into the adhesion promoter 5, and the properties of the sample are shown in the table 1.
Comparative example 1
85 parts by mass of vinyl methyl silicone resin with the viscosity of 6000mPa s vinyl content of 1.31 wt%, 15 parts by mass of vinyl silicone oil with the viscosity of 10000mPa s vinyl content of 0.12 wt%, 4.3 parts by mass of hydrogen-containing silicone oil with the active hydrogen content of 1.0 wt%, 2 parts by mass of adhesive KH560(3- (2, 3-epoxypropoxy) propyltrimethoxysilane), and 0.01 part by mass of 1-ethynyl-1-cyclohexanol were uniformly mixed under the action of a high-speed centrifuge (1000RPM), and then 0.1 part by mass of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst was added, and the mixture was uniformly mixed, vacuum defoamed, cured at 80 ℃ for 1 hour, and cured at 150 ℃ for 3 hours, and the sample properties are shown in Table 1.
Comparative example 2
(1) Preparation of adhesion promoter
Adding 120g (0.5mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane and 0.36g of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst into a reaction vessel, adding 120g of toluene, uniformly mixing, heating to 80 ℃, dripping 71g (0.5mol) of allyl acetoacetate into the reaction vessel within 1 hour, preserving the temperature for 8 hours after finishing dripping, and then removing low-boiling-point substances under the condition of-0.06 MP to obtain adhesion promotion 6.
(2) Preparation of addition type packaging adhesive sample for LED
The preparation method of the addition type packaging adhesive sample for the LED in the embodiment is basically consistent with the preparation method of the LED in the embodiment 1, the difference is that the adhesion promoter 1 in the embodiment 1 is changed into the adhesion promoter 6, and the properties of the sample are shown in the table 1.
Comparative example 3
(1) 236g (1mol) of 3- (2, 3-epoxypropoxy) propyltrimethoxysilane, 130g (1mol) of hydroxyethyl methacrylate (1mol) and 1.00g of dibutyltin diacetate are stirred uniformly at room temperature, the temperature is raised to 60 ℃ for reaction for 6 hours, and the low-boiling-point substances are removed by reducing the pressure to-0.06 MP at the temperature of 90 ℃ to obtain 319g of colorless transparent intermediate products.
Adding 120g (0.5mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane and 0.18g of 1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane platinum (platinum content 5000PPM) catalyst into a reaction vessel, adding 120g of toluene, uniformly mixing, heating to 80 ℃, dripping 167g (0.5mol) of intermediate product into the reaction vessel within 1 hour, preserving heat for 8 hours after finishing dripping, and then removing low-boiling-point substances under the condition of-0.06 MP to obtain the adhesion promoter 7.
(2) Preparation of addition type packaging adhesive sample for LED
The preparation method of the addition type packaging adhesive sample for the LED in the embodiment is basically consistent with the preparation method of the LED in the embodiment 1, the difference is that the adhesion promoter 1 in the embodiment 1 is changed into the adhesion promoter 7, and the properties of the sample are shown in the table 1.
TABLE 1 test results of the cured Performance of the addition type Silicone encapsulant
The method for testing the performance of the packaging adhesive in table 1 is as follows:
hardness: the hardness of the silicone packaging adhesive is measured according to GB/T531.1-2008.
Tensile shear strength: the tensile shear strength of the bond of the addition silicone packaging adhesive to the substrate was determined in accordance with GB/T13936-1992.
Light transmittance: and testing the light transmittance in the visible light wavelength range of 200-800 nm by using an ultraviolet-visible light photometer at 25 ℃ according to GB/T2410-2008.
As shown in Table 1 and comparative example 1, after the adhesion promoter prepared by the invention is added, the hardness and the light transmittance of the packaging adhesive are basically unchanged, and the adhesion to metal is obviously improved, probably because the structure contains a beta-dicarbonyl functional group which can generate complexation with the metal, and meanwhile, alkoxy in the structure can also react with a small amount of hydroxyl on the surface of the metal to form stronger acting force. From comparative example 2, it can be seen that the single beta-dicarbonyl group and hydrogen group bonding to metal is general and poor, and the ratio of hydrogen and vinyl in the formulation is changed due to the large amount of hydrogen remaining in the structure, resulting in the decrease of hardness. From comparative example 3, it is clear that the functional groups such as active epoxy group and strongly polar ester group in the structure can exert strong force with plastic and can form strong adhesion with the substrate, but the adhesion with metal is slightly poor, and the hardness is reduced due to too high hydrogen content in the adhesive.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of an organic silicon adhesion promoter for LED packaging is characterized by comprising the following steps:
(1) mixing epoxy silane, acrylic acid hydroxy ester and a catalyst, heating to 60-100 ℃, reacting for 3-10 hours, reacting under the conditions that the vacuum degree is-0.06-0.09 MPa and the temperature is 80-100 ℃ until no fraction flows out, and obtaining epoxy silane containing acrylate groups;
(2) uniformly mixing 1,3,5, 7-tetramethylcyclotetrasiloxane, a noble metal catalyst and an organic solvent to obtain a mixed solution A; mixing alkenyl acetoacetate with the epoxy silane containing the acrylate group obtained in the step (1) to obtain a mixed solution B; and heating the mixed solution A to 60-80 ℃, dropwise adding the mixed solution B into the mixed solution A for reaction, and removing low-boiling-point substances under the condition of-0.06-0.09 MP after the reaction is finished to obtain the adhesion promoter.
2. The method for preparing the silicone adhesion promoter for LED encapsulation according to claim 1, characterized in that:
the epoxy silane in the step (1) is at least one of 3- (2, 3-epoxypropoxy) propyltrimethoxysilane, 3- (2, 3-epoxypropoxy) propylmethyldimethoxysilane, 3- (2, 3-epoxypropoxy) propyltriethoxysilane, 3- (2, 3-epoxypropoxy) propylmethyldiethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethylmethyldimethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltriethoxysilane and 2- (3, 4-epoxycyclohexyl) ethylmethyldiethoxysilane;
the hydroxyl acrylate in the step (1) is at least one of hydroxyethyl methacrylate, hydroxyethyl acrylate, hydroxypropyl acrylate and hydroxypropyl methacrylate.
3. The method for preparing the silicone adhesion promoter for LED encapsulation according to claim 1, characterized in that:
the catalyst in the step (1) is at least one of dibutyltin dilaurate, dibutyltin diacetate, triethyl borate, isopropyl borate and tributyl borate.
4. The method for preparing the silicone adhesion promoter for LED encapsulation according to claim 1, characterized in that:
the reaction substance in the step (1) is epoxy silane and acrylic hydroxyl ester, and the epoxy silane and the acrylic hydroxyl ester are matched according to the molar ratio of 1 (1-1.2);
the amount of the catalyst used in the step (1) is 0.1-1% of the total mass of the epoxy silane and the acrylic hydroxyl ester.
5. The method for preparing the silicone adhesion promoter for LED encapsulation according to claim 1, characterized in that:
the noble metal catalyst in the step (2) is at least one of platinum, palladium, rhodium and complex compounds thereof;
the acetoacetic ester in the step (2) is at least one of allyl acetoacetate, glycol acetoacetate methacrylate and glycol acetoacetate acrylate;
the organic solvent in the step (2) is at least one of toluene, cyclohexane and methylcyclohexane.
6. The method for preparing the silicone adhesion promoter for LED encapsulation according to claim 1, characterized in that:
the dosage of the noble metal catalyst in the step (2) is 0.01-0.3 percent of the mass of 1,3,5, 7-tetramethylcyclotetrasiloxane;
the amount of the organic solvent used in the step (2) is 1-2 times of the mass of 1,3,5, 7-tetramethylcyclotetrasiloxane.
7. The method for preparing the silicone adhesion promoter for LED encapsulation according to claim 1, characterized in that:
the amount of the reaction substances in the step (2) is 1,3,5, 7-tetramethylcyclotetrasiloxane: alkenyl acetoacetate: the molar ratio of the epoxy silane containing acrylate group is 1: 1: (1-2).
8. The method for preparing the silicone adhesion promoter for LED encapsulation according to claim 1, characterized in that:
the reaction time in the step (2) is 5-16 hours.
9. An organic silicon adhesion promoter for LED packaging is characterized in that: the preparation method of any one of claims 1 to 8.
10. The use of the silicone adhesion promoter for LED encapsulation according to claim 9 in addition silicone encapsulant.
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| JP2006241462A (en) * | 2002-04-04 | 2006-09-14 | Kaneka Corp | Composition for optical material, optical material, manufacturing method thereof, and liquid crystal display device using the same |
| CN101052671A (en) * | 2004-09-15 | 2007-10-10 | Ppg工业俄亥俄公司 | Fast-curing modified siloxane compositions |
| CN104650795A (en) * | 2015-03-05 | 2015-05-27 | 江西欧普特实业有限公司 | Preparation method and application of organosilicone pouring sealant adhesive |
| CN106279700A (en) * | 2016-08-08 | 2017-01-04 | 岳胜武 | Add-on type liquid silicon rubber viscosifier, preparation method and applications |
| CN108276948A (en) * | 2017-12-21 | 2018-07-13 | 宁波凯耀电器制造有限公司 | A kind of efficient UV solidification glues |
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