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Synthesis of Organosilicon Modified Phenolic Resin

May 26, 2023

There are two methods for synthesizing thermosetting organosilicon modified phenolic resin: one is to prepare thermosetting organosilicon modified phenolic resin by hydrolyzing oligomers with chlorosilane and phenolic resin. The resin prepared by this method is mainly used in the manufacturing of copper coated pins due to its low molecular halo, relatively poor toughness and heat resistance.

Another preparation method for organosilicon modified phenolic resin is to first prepare linear phenolic resin, then add oligomeric silicone resin to synthesize organosilicon modified phenolic resin, and then add formaldehyde to prepare thermosetting organosilicon modified phenolic resin.

Classic Preparation Method of Organosilicon Modified Phenolic Resin

(1) Organic chlorosilane reacts with sodium acetate to form organic acetoxy group silane,
(2) Phenol and methyl condensation polymerize to form linear phenol casein resin with low molar mass
(3) Silicone modified phenolic resin is obtained by co condensation of organic acetoxy group silane and phenolic resin oligomer:

The specific process is as follows:

Preparation of RSi (OAc) 3: First, toluene is added to a reaction flask, and AcONa is slowly added under stirring to form a paste. Then, MeSiCb and PhSiCb with a molar ratio of 1:1 are added, and heated and refluxed for several hours. Excess AcONa and by-product NaCl are removed by freezing and filtering. The filtrate is evaporated at 80 ° C and reduced pressure to remove the solvent, resulting in MeSi (OAc) and PhSi (OAc) 3.

Preparation of phenolic resin oligomers: Heat and melt warm water into a 1:1 molar ratio of 0-OH and HCHO [37% (mass fraction) aqueous solution] in a reactor. Slowly add a certain amount of ammonia [26% (mass fraction) ammonia aqueous solution] under stirring, heat and reflux for 9 hours, and let it stand for stratification. After removing the water layer, remove residual water at 80 ° C and reduced pressure. When the relative viscosity of the 10% (mass fraction) resin ethanol solution reaches 2 2 2. 4, the reaction can be stopped, and the product obtained is a condensate containing triphenol nucleus. The gel time at 100℃ is 20 30 min.

Silane phenolic resin co condensation: the ratio of acetoxy group silane to phenolic oligomer should be determined according to the use of the modified resin. When used as an electrical insulation material, the content of silicone resin in the copolymer ranges from 20% to 40%.

(Quality score) is appropriate. The specific process is to slowly add MeSiCOAc and PhSi (OAc) into the reactor filled with excess water, keep the temperature no more than 20 ° C ', and then add the phenolic resin ethanol solution. After heating and refluxing, once the reaction is completed, the solvent and water are evaporated under reduced pressure. When the product gel time reaches 20-30min/100 ° C, the reaction can be stopped to obtain silicone resin modified phenolic resin.

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