Application of phosphorus-containing compound in one-step synthesis of flame-retardant epoxy resin, flame-retardant epoxy resin and preparation method and application thereof
An epoxy resin and compound technology, applied in the field of flame retardant epoxy resin and its preparation, can solve the problem that the flame retardant epoxy resin cannot meet the high-frequency and high-speed use requirements of electronic products, the flame retardant epoxy resin has poor heat resistance, and the processing It is difficult to solve problems such as great difficulty, so as to achieve the effect of favorable industrialization promotion, excellent flame retardant performance, and easy control.
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[0062] According to a third aspect of the present invention, the present invention provides a method for preparing the above-mentioned flame retardant epoxy resin, comprising the following steps: uniformly mixing phosphorus-containing compounds, epichlorohydrin and optional hydroxyl-containing phenolic compounds in a solvent , One-step polymerization reaction under alkaline conditions, that is, the preparation of flame retardant epoxy resin.
[0063] The flame-retardant epoxy resin provided by the invention is prepared from two or three kinds of raw materials through a one-step method, and the process is simple and easy to control, which is beneficial to industrialization promotion.
[0064] In a preferred embodiment of the present invention, the temperature of the polymerization reaction is controlled to be 50-100°C, so as to facilitate the polymerization reaction between epichlorohydrin and the hydroxyl group in the phosphorus-containing compound and the optional hydroxyl gro...
Embodiment 1
[0074] This embodiment provides a flame retardant epoxy resin, which is prepared according to the following steps:
[0075] 1mol of the phosphorus-containing compound (DOPO-NQ) (374g) as described in formula 1 and 6mol of epichlorohydrin (ECH) (555g) are used as co-reaction solvents in isopropanol (IPA) and propylene glycol monomethyl ether (PM) (The mass ratio of IPA to PM is 150:75), at 50 DEG C, use liquid caustic soda as a catalyst, carry out polymerization reaction, then stand for liquid separation, heat up to 150 DEG C to remove remaining epichlorohydrin, and then Add toluene, and drop dilute liquid alkali (concentration: 3%) to refine at 80°C, finally remove toluene under reduced pressure, add propylene glycol monomethyl ether (PM) (322.67g) as a dissolving solvent, and obtain a 60wt% flame-retardant ring oxygen resin. Wherein the structural formula of the phosphorus-containing compound described in formula 1 is as follows:
[0076]
[0077] The flame retardant epo...
Embodiment 2
[0079] This embodiment provides a flame retardant epoxy resin, which is prepared according to the following steps:
[0080] With 1mol DOPO-NQ (374g) and 1.88mol epichlorohydrin (ECH) (174g) as described in formula 1 in embodiment 1, in Virahol (IPA) and propylene glycol monomethyl ether (PM) do co-reaction solvent ( Under the condition that the mass ratio of IPA to PM is 150:75), at 50°C, using liquid caustic soda as a catalyst, carry out a polymerization reaction, then stand for liquid separation, raise the temperature to 150°C to remove the remaining epichlorohydrin, and then add Toluene, and dropwise adding dilute liquid alkali (concentration is 3%) is refined at 80 ℃, removes toluene under reduced pressure at last, adds propylene glycol monomethyl ether (PM) (318.19g) as dissolving solvent, obtains 60wt% flame-retardant epoxy resin.
[0081] After testing, the flame retardant epoxy resin prepared in this example has an epoxy equivalent of 300 g / mol and a phosphorus conten...
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Abstract
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