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Polyether type hyperbranched epoxy resin and preparation method thereof

An epoxy resin and polyether-based technology, which is applied in the field of polyether-type hyperbranched epoxy resin and its preparation, can solve the problems of popularization and application limitations, difficult product purification, cumbersome preparation and purification process, etc.

Active Publication Date: 2009-11-04
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chang and Frechet (Hang-Ting Chang; Jean M.J.Frechet.Journal of Chemical Society, 1999, 121, 2313) used proton transfer method to use 3,5-dimethylol diglycidyl ether phenol as AB 2 Monomer synthesized polyether type hyperbranched epoxy resin, then Caiguo Gong; JeanM.J.Frechet. (Macromolecules, 2000, 33, 4997) used bisphenol acid diglycidyl ether as AB 2 Monomer synthesized polyester type hyperbranched epoxy resin, but AB 2 The cumbersome preparation and purification process of the monomer limits the promotion and application of this method
Frechet and his colleagues extended the proton transfer method to commercial multifunctional monomers (Todd Emrick; Hang-Ting Chang; Jean M.J.Frechet.acromolecules, 1999, 32, 6380) (Todd Emrick; Hang-Ting Chang; JeanM. J.Frechet.Journal of Polymer Science: Part A: Polymer Chemistry, 2000, 38, 4850), with A 2 +B 3 The aliphatic polyether type hyperbranched epoxy resin was synthesized in the form of monomer, but the similar solubility of monomer, polymer and catalyst in this system makes the purification of the product very difficult, and the presence of the catalyst makes the storage stability of the resin greatly affected

Method used

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  • Polyether type hyperbranched epoxy resin and preparation method thereof
  • Polyether type hyperbranched epoxy resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: 4.56g (0.02mol) of bisphenol A, 6.62g (0.02mol) of trimethylolpropane triglycidyl ether, 0.6g of tetrabutylammonium chloride, and 40ml of N,N-dimethylformamide were added In the reaction kettle, react at 60°C for 15 hours under the protection of nitrogen, precipitate in ethanol after cooling, and dry to obtain a nearly colorless hyperbranched epoxy resin. The weight-average molecular weight of the product is 8452 and the molecular weight polydispersity index is 1.66 as measured by GPC.

[0020] figure 2 It is the nuclear magnetic hydrogen spectrogram of the hyperbranched epoxy resin that embodiment 1 obtains 1 HNMR (DMSO), δ: 0.765 (-CH 2 CH 3 ), 1.28 (-CH 2 CH 3 ), 1.541(-Φ-C(CH 3 ) 2 -Φ), 2.512 (epoxy, -CH 2 )2.625 (epoxy, -CH), 3.000 (epoxy, -OCH 2 ), 3.262-3.899 (-OCH 2 , -CH(OH)), 4.960, 5.029 (-OH), 6.631-7.068 (aromatic-H). From this spectrum, the polymer has both the structures of bisphenol A and trimethylolpropane triglycidyl ether. In ad...

Embodiment 2

[0021] Embodiment 2: Bisphenol F 6g (0.03mol), pentaerythritol triglycidyl ether 6.36g (0.02mol), tetrabutylammonium hydroxide 1.5g, N, N-dimethyl sulfoxide 40ml add in the reactor, nitrogen Under protection, react at 120°C for 96 hours, after cooling, precipitate in a mixture of methanol and water (volume ratio 1:1), and dry to obtain a nearly colorless hyperbranched epoxy resin. The weight-average molecular weight of the product measured by GPC is 87452, which is more The dispersion index was 2.15.

Embodiment 3

[0022] Example 3: Add 1 g (0.01 mol) of hydroquinone, 14.4 g (0.05 mol) of trimethylolethane triglycidyl ether, 0.725 g of potassium tert-butoxide, and 40 ml of tetrahydrofuran into the reactor, and react for 40 After reacting at ℃ for 80 hours, after cooling, it was precipitated in methanol and dried to obtain a nearly colorless hyperbranched epoxy resin. The weight-average molecular weight of the product was 50915 as measured by GPC, and the molecular weight polydispersity index was 1.96.

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Abstract

The invention relates to polyether type hyperbranched epoxy resin and a preparation method thereof. The preparation method is as follows: the polyether type hyperbranched epoxy resin is synthesized by taking commercial dihydric phenol and polylol glycidyl ether as raw materials through a proton translocation reaction under the protection of nitrogen. All reactants are added to a reaction unit once during reaction, and in the reaction process, the hyperbranched epoxy resin is obtained according to the following steps in sequence: catalyst catalyzes the epoxy groups of a plurality of epoxy monomers to open epoxy rings, a phenolic hydroxyl group and secondary oxygen anion are processed by proton transfer and phenoxy oxygen anion is processed by electrophilic substitution. The hyperbranched epoxy polymer can be used in the fields of modification of environment-friendly bond with less solvent or no solvent, painting, traditional epoxy resin, and the like.

Description

Technical field: [0001] The invention relates to a polyether hyperbranched epoxy resin and a preparation method thereof. Background technique: [0002] Hyperbranched polymers have a highly branched three-dimensional ellipsoidal structure and a large number of terminal groups. Compared with traditional linear polymers, hyperbranched polymers have the characteristics of good solubility, lower melt and solution viscosity, easy film formation, and a large number of terminal groups, and are one of the research hotspots in polymer science. [0003] Epoxy resin is an important thermosetting resin variety. Due to its excellent physical and mechanical properties, electrical insulation properties, chemical resistance, heat resistance and adhesive properties, it is widely used in chemical industry, light industry, water conservancy, transportation, machinery, electronics, home appliances, automobiles and aerospace industries. . New varieties of epoxy resins are also being introduced...

Claims

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Application Information

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IPC IPC(8): C08G59/02
Inventor 李效玉马丽杰王海侨何立凡
Owner BEIJING UNIV OF CHEM TECH
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