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Chemical method for preparing organic silicon modified epoxy resin

A technology of epoxy resin and chemical method, which is applied in the direction of adhesives, etc., can solve the problems of low reaction efficiency, difficulty in compatibility, and phase separation, and achieve the effects of simple preparation process, high modification efficiency, and improved compatibility

Inactive Publication Date: 2012-07-04
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In previous studies, most of the silicones used were polydimethylsiloxane, because the solubility parameters (SP) of epoxy resin and polydimethylsiloxane were very different, which were 10.9 and 7.4~ 7.8, when modified by chemical methods, it is difficult to dissolve in each other, and there is phase separation, resulting in low reaction efficiency

Method used

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  • Chemical method for preparing organic silicon modified epoxy resin
  • Chemical method for preparing organic silicon modified epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1. Add 25g of hydroxyl-terminated methylphenylpolysiloxane (the mass fraction of hydroxyl group is 9.4%), 100g of bisphenol A epoxy resin E-51, and 2.0g of triphenylphosphine into a 250mL three-necked flask. After stirring evenly, heat to 120°C and react for 4h. Continue at 125°C / 10mmHg for 0.5h, and remove low boiling point compounds in vacuum to obtain a homogeneous and non-layered silicone-modified epoxy resin. The yield was 98%. From figure 1 It can be seen that 915cm -1 The absorption peak at the place is the absorption peak of the epoxy group, at 1085-1122cm -1 There is an absorption peak of Si-O-C, which proves the formation of polymethylphenylsiloxane-epoxy resin graft copolymer.

[0019] Take 50g of the prepared silicone-modified epoxy resin, add 3g of tris-(dimethylaminomethyl)phenol, mix evenly, and bond the aluminum alloy at 180°C for 2h, and the measured shear strength is 125kg / cm 2 ;After aging for 12 hours at 300℃, the measured shear stren...

Embodiment 2

[0020] Example 2. Add 40g of hydroxyl-terminated methylphenyl polysiloxane (the mass fraction of hydroxyl group is 5.6%), 100g of bisphenol F epoxy resin DER-354, and 5.0g of dibutyltin dilaurate into a 250mL three-necked flask. After stirring evenly, heat to 80°C and react for 6h. Continue at 125°C / 8mmHg for 0.5h, and remove low boiling point compounds in vacuum to obtain a homogeneous and non-separated silicone-modified epoxy resin. The yield was 97%.

[0021] Take 50g of the prepared silicone-modified epoxy resin, add 3g of tris-(dimethylaminomethyl)phenol, mix evenly, and bond the aluminum alloy at 180°C for 2h, and the measured shear strength is 143kg / cm 2 ;After aging at 300℃ for 12h, the measured shear strength is 85kg / cm 2 .

Embodiment 3

[0022] Example 3. Add 35g of hydroxyl-terminated methylphenylpolysiloxane (0.6% of the hydroxyl mass fraction), 100g of bisphenol A epoxy resin E-44, and 7.0g of tetramethylammonium hydroxide into a 250mL three-necked flask. Heated to 110°C and reacted for 5h. Continue at 125°C / 8mmHg for 0.5h, and remove low boiling point compounds in vacuum to obtain a homogeneous and non-separated silicone-modified epoxy resin. The yield was 95%.

[0023] Take 50g of the prepared silicone-modified epoxy resin, add 3g of tris-(dimethylaminomethyl)phenol, mix evenly, and bond the aluminum alloy at 180°C for 2h, and the measured shear strength is 106kg / cm 2 ;After aging at 300℃ for 12h, the measured shear strength is 59kg / cm 2 .

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Abstract

The invention relates to a chemical method for preparing organic silicon modified epoxy resin, aiming to solve the technical problems that the compatibility is not good and the efficiency is low in a modification process of organic silicon epoxy resin. The chemical method comprises the following steps of: adding epoxy resin (one of bisphenol A epoxy resin and bisphenol F epoxy resin), hydroxyl-terminated methyl phenyl polysiloxane (with the use amount of 20-50% of the mass of the epoxy resin) and a catalyst (which is 1-5% of the total mass of two components including the epoxy resin and the hydroxyl-terminated methyl phenyl polysiloxane) into a reactor; uniformly agitating and gradually raising the temperature to 60-140 DEG C, and reacting for 4-6 hours; after the reaction, lasting under the condition of 120-130 DEG C / 5-10 mmHg for 0.5 hours; and desorbing low-boiling-point compounds, which are generated in the reaction, in vacuum to obtain the organic silicon modified epoxy resin.

Description

[0001] technical field [0002] The invention relates to the technical field of chemical industry, in particular to a chemical method for preparing organosilicon-modified epoxy resin. Background technique [0003] Epoxy resin has excellent chemical stability, electrical insulation and good bonding performance, and has been widely used in adhesives, coatings, electronic appliances, aerospace and other fields. However, the highly cross-linked structure of epoxy resin limits its application in some high-tech fields. The chemical modification of epoxy resin with silicone not only maintains the excellent physical and mechanical properties of epoxy resin, but also increases the performance of oxidation resistance and heat and humidity resistance, while reducing its internal stress. It has important application prospects and is especially suitable for use as High temperature resistant adhesive. [0004] The chemical modification of epoxy resin with linear structure silicone has a...

Claims

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Application Information

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IPC IPC(8): C08G81/00C09J187/00
Inventor 来国桥李美江胡自强蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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