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Production of Redix with siloxane structural unit

A structural unit, epoxy resin technology, applied in the field of epoxy resin preparation, can solve the problems of low silicone content of epoxy resin, difficult to achieve modification and toughening, affecting heat resistance, etc., and achieve good elasticity and flexibility. , Excellent bonding performance, the effect of eliminating internal stress

Inactive Publication Date: 2005-12-28
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The organosilicon content in the silicone-containing epoxy resin obtained by them is very small, it is difficult to achieve the purpose of modification and toughening, and the raw material preparation is also difficult and the cost is high
[0007] Hydrosilylation reaction of α, ω-dihydropolysiloxane with allyl glycidyl ether, etc., can also obtain silicone-modified epoxy resin, but there are The ether bond of the product affects the heat resistance of the product, and the price of α, ω-dihydropolysiloxane is relatively high

Method used

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  • Production of Redix with siloxane structural unit
  • Production of Redix with siloxane structural unit
  • Production of Redix with siloxane structural unit

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 11

[0032] Example 1.1,1,1,3,5,7,7,7-octamethyl-3,5-di(γ-chloropropyl)-tetrasiloxane (I) and 1,1,1,3 , 5,7,9,9,9-nonamethyl-3,5,7-tris(γ-chloropropyl)-pentasiloxane (II) synthesis

[0033] Add 366g of γ-chloropropylmethyldimethoxysilane and 200ml of ether to a 1000ml four-necked bottle, stir to dissolve, add a few drops of concentrated hydrochloric acid to the four-necked bottle, add 200ml dropwise through a separatory funnel while stirring water, and stirred the reaction at room temperature for 2h, then raised the temperature to 40°C and continued the reaction for 2.5h. After standing still, the organic layer was separated, and the aqueous layer was extracted twice with 20 ml of ether, and combined with the organic layer. The organic layer was washed with distilled water until neutral, and then washed with 20 g of anhydrous Na 2 SO 4 Dry and leave overnight. After filtration, the filtrate was transferred to a 500ml round-bottomed flask, and the ether was distilled off by heat...

Embodiment 2

[0036] Example 2. Synthesis of α, ω-dichloropropyl-terminated polydimethylsiloxane oligomers

[0037] In a 250ml four-neck flask equipped with a stirrer, a thermometer and a reflux condenser, add 28.7g 1,3-bis(3-chloropropyl)-1,1,3,3-tetramethyldisiloxane[ For the preparation method, refer to the literature: Jiang Hongqin, Zhang Dunming, Jiang Xiqun, etc., Fine Chemical Industry, 2004, 21 (3): 232], 29.6g octamethylcyclotetrasiloxane (D 4 ) and 1.2g of concentrated sulfuric acid were stirred and reacted at 50°C for 9h. After the reaction, add 60ml 30~60℃ petroleum ether and 10ml distilled water, mix well, separate the water layer with a separatory funnel, wash the organic phase with water until neutral, and then wash it with anhydrous Na 2 SO 4 Let dry overnight. Filter out Na 2 SO 4 , evaporate petroleum ether at normal pressure, and then distill under reduced pressure to steam out unreacted D 4 and other low boiling substances. The residue was a pale yellow liquid wei...

Embodiment 3

[0039] Example 3. Synthesis of α, ω-dichloropropyl-terminated polydimethylsiloxane oligomers

[0040] 59.2 g of octamethylcyclotetrasiloxane was used to replace 29.6 g of octamethylcyclotetrasiloxane in Example 2, and other conditions remained unchanged, Example 2 was repeated to obtain 78.1 g of the product.

[0041] use 1 The molecular weight of the product was measured by HNMR, and the average molecular weight was 933.

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Abstract

Production of epoxy resin with silicone structural unit is carried out by reacting chlorsilane or chlorsilicone with silicone or its ring from acid catalyst, obtaining silicone small molecule or oligomer containing at least two chlor-groups in molecular chain, reacting dimethyl-silicone small molecule containing dichlorpropyl with bisphenol A salt in non-protonic polar solution, adding epoxy chloropropane into reaction mixture, reacting at 60í½140íÒC, filtering reaction mixture, de-pressuring and distilling to remove excess epoxy chloropropane and solvent, and obtaining epoxy resin with silicone structural unit. It achieves clear molecular structure, easy synthesis and better flexibility.

Description

technical field [0001] The present invention relates to the preparation method of the epoxy resin containing organosilicon structural unit Background technique [0002] Epoxy resin and polysiloxane are two very important polymers in synthetic materials. Epoxy resin has the advantages of excellent mechanical strength, solvent resistance, adhesive performance, etc., but it is easy to become brittle, easy to degrade under high temperature, and easy to be affected by water and oil. Silicone has attracted much attention due to its low-temperature flexibility, low surface energy, heat resistance, water repellency, and high dielectric strength. However, its mechanical properties, solvent resistance, and adhesion are poor, and its production cost is high. Therefore, modifying epoxy resin with silicone is an effective way to modify epoxy resin developed in recent years. It can not only reduce the internal stress of epoxy resin, but also increase the toughness and high temperature re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/00
Inventor 张墩明蒋锡群姜红芹鲁广昊
Owner NANJING UNIV
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