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Organic boron silicon adhesion promoter with high refractive index as well as preparation method and application of organic boron silicon adhesion promoter

An adhesion promoter and high refractive index technology, applied in the direction of polymer adhesive additives, adhesives, adhesive additives, etc., can solve the problem of difficult control of reaction conditions, easy ring opening of epoxy groups, poor compatibility of silica gel, etc. Problems, to achieve the effect of cheap raw materials, good bonding performance, and good compatibility

Active Publication Date: 2016-04-27
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN104531003A has reported a kind of borate adhesion promoter containing C=C double bond that utilizes borate ester and containing C=C double bond and active hydroxyl compound to carry out transesterification reaction synthesis, and this adhesion promoter can improve Addition-type encapsulation silica gel has good adhesion performance to stainless steel and polyethylene terephthalate substrates, but has the disadvantages of low refractive index and poor compatibility with silica gel
However, the reaction conditions of the hydrolysis and condensation method are difficult to control, gels are easy to form, and the epoxy group is easy to open rings under strong acidic and strong alkaline conditions, so its practical application is limited.

Method used

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  • Organic boron silicon adhesion promoter with high refractive index as well as preparation method and application of organic boron silicon adhesion promoter
  • Organic boron silicon adhesion promoter with high refractive index as well as preparation method and application of organic boron silicon adhesion promoter

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 21.63g of diphenylsilanediol, 8.28g of 3-(2,3-epoxypropoxy)propyltrimethoxysilane, 8.13g of 3-methacryloxypropyltrimethoxysilane, 3.12g of boric acid trimethoxysilane Add methyl ester and 20g of toluene into a 250mL three-necked flask equipped with a thermometer, mechanical stirring, and a condensing reflux tube, stir well at room temperature, add 0.41g of tetraethyl titanate, control the reaction temperature at 30°C, react for 12h, and then control the vacuum The temperature is 0.06MPa, the temperature is 90°C, and the reaction is continued for 6h to obtain adhesion promoter 1 with a refractive index of 1.541.

[0024] 100 parts by mass of vinyl phenyl silicone resin with a vinyl content of 4 wt%, 15 parts by mass of vinyl phenyl silicone oil with a viscosity of 500mPa·s, 30 parts by mass of phenyl hydrogen-containing silicone oil with an active hydrogen content of 0.45 wt%, 3 parts by mass of adhesion promoter 1 and 0.02 parts by mass of 1-ethynyl-1-cyclohexanol were ...

Embodiment 2

[0026] 21.63g of diphenylsilanediol, 11.14g of 3-(2,3-epoxypropoxy)propyltriethoxysilane, 14.52g of 3-methacryloxypropyltriethoxysilane, 2.92g Add triethyl borate and 30g of xylene into a 250mL three-necked flask equipped with a thermometer, mechanical stirring and a condensing reflux tube, stir well at room temperature, add 0.25g of tetraisopropyl titanate, control the reaction temperature at 50°C, and react for 10h , and then control the vacuum degree to 0.08MPa, the temperature to 100°C, and continue the reaction for 4h to obtain adhesion promoter 2 with a refractive index of 1.537.

[0027] The adhesion promoter 1 in Example 1 was changed to the adhesion promoter 2, and the dosage was 4 parts by mass. The properties of the samples are shown in Table 1 and Table 2.

Embodiment 3

[0029] 21.63g of diphenylsilanediol, 4.93g of 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 18.58g of 3-methacryloxypropyltrimethoxysilane, 1.88g Add tri-n-propyl borate and 40g of acetone into a 250mL three-neck flask equipped with a thermometer, mechanical stirring and a condensing reflux tube, stir well at room temperature, add 0.94g of tetra-n-butyl titanate, control the reaction temperature at 40°C, and react for 8h , and then control the vacuum degree to 0.06MPa, the temperature to 110°C, and continue the reaction for 3h to obtain adhesion promoter 3 with a refractive index of 1.539.

[0030] The adhesion promoter 1 in Example 1 was changed to the adhesion promoter 3, and the dosage was 2 parts by mass. The properties of the samples are shown in Table 1 and Table 2.

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Abstract

The invention discloses an organic boron silicon adhesion promoter with a high refractive index as well as a preparation method and an application of the organic boron silicon adhesion promoter. The preparation method comprises steps as follows: diphenylsilanediol, epoxy silane, ester silane, borate and a solvent are uniformly stirred at the room temperature, a titanate catalyst is added, a mixture reacts for 4-14 h at the reaction temperature controlled in a range from 25 DEG C to 60 DEG C and continuously reacts for 2-6 h at the vacuum degree controlled in a range from 0.05 MPa to 0.098 MPa and at the temperature controlled in a range from 60 DEG C to 140 DEG C, and the organic boron silicon adhesion promoter with the high refractive index is prepared. The prepared adhesion promoter can not only remarkably improve the adhesion performance of high-refractive-index addition type silica gel for LED packaging, but also has the high refractive index and good compatibility with the silica gel, particularly has a remarkable function for improvement of the adhesion performance of plastic base materials such as polyphthalamide, polyethylene terephthalate, 1,4-cyclohexanedimethanol terephthalate, polycarbonate and the like and can be expected to be widely applied to the field of LED device packaging.

Description

technical field [0001] The invention relates to the technical field of silicone packaging materials, in particular to a high-refractive-index organic borosilicate adhesion promoter and a preparation method thereof. The invention also relates to the application of the adhesion accelerator in the addition type silica gel with high refractive index for LED packaging. Background technique [0002] Compared with traditional packaging materials such as epoxy resin, addition-type packaging silicone has no low-molecular by-products during the curing process, can be deeply cured, has extremely low shrinkage, good dimensional stability of the cured product, and excellent heat resistance and stability. In particular, the addition of high refractive index packaging silicone can also effectively improve the light extraction efficiency and become one of the high-performance packaging materials. However, most of the surface of the addition-type encapsulation silicone is non-polar organic ...

Claims

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Application Information

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IPC IPC(8): C08G77/56C09J11/08C09J183/07
CPCC09J11/08C09J183/04C08G77/56C08L2205/035C08L2205/025C08L2203/206C08L83/04C08L83/14
Inventor 曾幸荣潘科学赖学军陈中华李红强
Owner SOUTH CHINA UNIV OF TECH
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