Low-hygroscopicity epoxy resin and preparation method thereof

A technology of epoxy resin and low hygroscopicity, applied in the field of low hygroscopicity epoxy resin and its preparation, can solve the problem that epoxy resin crosslinking density, mechanical properties and heat resistance are not improved at the same time, and the performance of matrix resin is degraded , easy to migrate to the surface and other problems, to achieve good nano-enhancing effect, improve heat resistance and barrier properties, and improve the effect of barrier properties

Active Publication Date: 2016-07-20
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cross-link density, mechanical properties and heat resistance of epoxy resins have not been improved at the same time.
Li Qifang etc. (a kind of preparation method of cyanate ester-epoxy resin-POSS hybrid resin, Chinese patent, publication number CN101565545A) use cyanate ester, POSS to modify epoxy resin, prepared a kind of heat resistance, A hybrid material with excellent dielectric properties and moisture absorption resistance. Although the added silsesquioxane can be well dispersed in the resin matrix, this modification belongs to physical mixing, and it is easy to migrate to the surface after a long period of storage, thus affecting Appearance and lead to a decrease in the performance of the matrix resin

Method used

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  • Low-hygroscopicity epoxy resin and preparation method thereof
  • Low-hygroscopicity epoxy resin and preparation method thereof
  • Low-hygroscopicity epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Synthesis of organic titanium hybrid silsesquioxane

[0029] Dissolve 4g of heptaisobutylsilsesquioxane trisilanol in 100mL of chloroform, stir for 20min under nitrogen flow, then add 1.73mL of n-butyl titanate (molar ratio, heptaisobutylsilsesquioxane Trisilanol: n-butyl titanate = 1:1), stirred for 20 minutes and then heated to 60°C for reflux reaction for 4 hours. After the reaction was completed, the solution was concentrated by rotary evaporation, and finally organic titanium hybrid silsesquioxane was precipitated with acetonitrile .

[0030] The infrared spectrogram characterization of the organic titanium hybrid silsesquioxane is shown in figure 1 shown. 920cm -1 The spectral peak is the characteristic absorption peak of -Si-O-Ti- group.

[0031] (2) Preparation of low hygroscopicity epoxy resin

[0032] Weigh 20g of epoxy resin E-51, heat up to 100°C, add 1g of organic titanium hybrid silsesquioxane (according to mass percentage, organic titanium hybrid...

Embodiment 2～3

[0041] With embodiment 1 process, change the addition amount of organic titanium hybrid silsesquioxane in step (2), be respectively 2.0g and 3.0g (by mass percentage, organic titanium hybrid silsesquioxane is respectively epoxy 10%, 15% of the resin). Measure the water absorption according to the method described in step (4). The measurement results are shown in Table 2.

[0042] Table 2

[0043] Example

Embodiment 4～6

[0045] The same process as in Example 1, changing the feeding amount of n-butyl titanate in step (1) to 3.46 mL (molar ratio, heptaisobutylsilsesquioxane trisilanol: n-butyl titanate=1:2) , change the amount of organic titanium hybrid silsesquioxane added in step (2), respectively 1.0g, 2.0g, 3.0g (by mass percentage, organic titanium hybrid silsesquioxane is 5% of epoxy resin respectively %, 10%, 15%). Measure the water absorption according to the method described in step (4). The measurement results are shown in Table 2.

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Abstract

The invention discloses low-hygroscopicity epoxy resin and a preparation method thereof and relates to epoxy resin. The low-hygroscopicity epoxy resin consists of epoxy resin, a curing agent and organic titanium hybrid silsesquioxane, wherein the dosage of the organic titanium hybrid silsesquioxane is 1-20% of that of the epoxy resin by mass; and the dosage of the curing agent is in a stoichiometric ratio to the epoxide equivalent of the epoxy resin. The preparation method comprises the following steps: putting the epoxy resin into a container and heating and stirring; adding organic titanium hybrid silsesquioxane for reacting while performing vacuum suction of small molecules; adding the curing agent; stirring uniformly and pouring into a preheated mould; curing for 4h at 120-130 DEG C; preserving heat for 2h at 130-150 DEG C; and finally, preserving heat for 2h at 150-170 DEG C, and molding to obtain the low-hygroscopicity epoxy resin. The water absorption of the epoxy resin is reduced, and the crosslinking density of the resin is increased; and meanwhile, the mechanical property and heat resistance of the epoxy resin are improved, and the barrier performance of the epoxy resin is enhanced.

Description

technical field [0001] The invention relates to epoxy resins, in particular to a low-hygroscopic epoxy resin and a preparation method thereof. Background technique [0002] Due to its good acid and alkali resistance, solvent resistance, dielectric insulation and high adhesion, epoxy resin has been widely used in electronic sealing materials, adhesives, coatings and other fields. However, the hygroscopicity of epoxy resin is relatively large, which affects the reliability and service life of electronic components to a certain extent, and limits its application in the direction of high performance. [0003] In the research work on the hygroscopicity of epoxy resins, Zhang Shuyong et al. (Zhang Shuyong, Luo Xiaowen, etc. Chemical Bulletin, 1998, 08:31-35) reviewed the influencing factors and mechanisms of water absorption and diffusion in epoxy resins, pointing out The water absorption rate and equilibrium water absorption of epoxy resin are mainly determined by the free volum...

Claims

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Application Information

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IPC IPC(8): C08L63/02C08L83/04C08G59/50C08G77/398
CPCC08G59/50C08G77/398C08L63/00C08L2201/08C08L2203/20C08L83/04
Inventor 曾碧榕刘永洲杨丽朱继红戴李宗陈国荣李忠裕
Owner XIAMEN UNIV
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