Method for preparing thermoplastic boron phenolic resin by solid-phase synthesis method

Abstract

The invention relates to a method for preparing thermoplastic boron phenolic resin through a solid-phase synthesis method, and belongs to the technical field of high polymer material preparation. According to the invention, a phenolic compound, the boride, an acidic catalyst, a water-carrying agent and a solid aldehyde compound are used as raw materials, and thermoplastic boron phenolic resin is prepared by adopting a solid-phase synthesis method, so that the blocking rate of phenolic hydroxyl groups can be improved, the heat resistance of the resin is improved, the reaction process is stable,and the manufacturability of the synthesis process is improved; and popularization and application of industrial production and application are facilitated.

Description

technical field [0001] The invention relates to a method for preparing thermoplastic boron phenolic resin through a solid-phase synthesis method, and belongs to the technical field of polymer material preparation. Background technique [0002] Introducing boron, silicon, phosphorus and other inorganic elements into the structure of phenolic resin is an effective way to improve its heat resistance, among which boron modified phenolic resin is one of the most successful methods. Due to the advantages of low raw material prices, high initial decomposition temperature, and high carbon residue rate, the related research on boron phenolic resin has received more and more attention in recent years. [0003] There are three main synthesis methods of boron phenolic resin, namely blending method, salicyl alcohol method and solid-phase synthesis method. The three methods have their own advantages and disadvantages, but the core idea is to block the easily oxidized by introducing B-O-C ...

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Problems solved by technology

Chinese patent CN 103289033 A discloses a method for introducing boron into phenolic resin by adding aryl boronic acid and its derivatives, but since aryl boronic acid and its derivatives are difunctional monomers, although the boric acid modified The lack of poor processability of phenolic resin reduces the crosslinking density of the resin, so that the heat resistance cannot be maximized

Chinese patent CN 109467662 A discloses a method for preparing low-viscosity boron phenolic resin without a catalyst. By adding a small amount of boric acid, the reaction is sufficient to obtain a liquid boron phenolic resin that is not easy to hydrolyze, has low viscosity, and can be stored stably. It is suitable as a wetting agent or impregnating The use of resin, such as a large amount of main binder for thermoforming, is prone to problems such as flow and high porosity

Chinese patent CN 104371083 discloses a process for synthesizing boron-containing thermoplastic phenolic resin by hot solvent method. The thermoplastic phenolic resin and boron-containing compound are dissolved in a solvent and heated for reaction, and finally the solvent is removed to obtain thermoplastic boron-containing phenolic resin. This method is relatively Simple, low equipment requirements, essentially belongs to the category of blending method, and the modification effect is not good

[0004] To sum up, there are many synthesis methods of boron phenolic resin, but the boron element introduced to block the phenolic hydroxyl group indirectly increases the crosslinking degree of the resin, It makes the preparation process difficult to control, and problems such as gel and sudden polymerization are easy to occur, which limits the large-scale production and application of boron phenolic resin

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