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Various Preparation Methods of Silicone Resin

Mar 24, 2023

The performance of the final processed silicone product depends on the amount of organic groups contained (i.e., the ratio of R to Si) and the ratio of different organic groups (e.g., methyl/phenyl). Therefore, when manufacturing silicone resin, the first step is to choose which monomer and how to determine their ratio. The choice of monomer type and its dosage depend on the product's use object and specific requirements. The general rule is that the smaller the R/Si value, the more capable the silicone resin obtained can harden at lower temperatures; The higher the R/Si value, the hardening of the obtained silicone resin requires long-term baking at high temperatures (such as 200 to 250 ° C), but the thermal elasticity of the obtained silicone resin film is much better than the former.

(1)MeSiCb is directly hydrolyzed and condensed to produce methyl silicone resin. In an acid resistant reaction with an agitator with a rotating speed of 200~240r/min, add 13 parts of ice water mixture by mass, maintain at 0 ° C, and stir. Add 1 part of MeSiCb within 0.5h, and maintain stirring for 1min. The product can be transferred to a settling tab. Maintain at 0 ° C for 4~5h, allowing the condensation reaction to be further completed, and allowing the generated methyl silicone resin to settle. Remove the flocculent from the liquid surface, discharge the acid water, slowly add deionized water at 70 ° C with stirring, and the silicone resin will condense into a white solid. Filter off the water layer and continue washing with deionized water at 70 ° C several times until neutral. Then air dried or vacuum dried to obtain a white solid silicone resin that is easily crushed. It is completely soluble in ethanol and neutral. The softening point is 40~47 ° C. The gel time at 150 ° C is about 9 min. The applicable period is 2 to 7 days. The product is suitable for preparing high temperature and arc resistant molding materials.


(2) MeSi is hydrolyzed and condensed in the presence of organic solvents to produce methyl silicone resin. In industrial production, MeS Biduo conducts hydrolysis condensation reaction in the presence of organic solvents (such as toluene, xylene, isopropanol, n-butanol, methyl ethyl ketone, acetone, methyl isobutyl ketone, dioxane, ethyl acetate, butyl acetate, etc.) to obtain soluble and fusible methyl silicone resin with low gel content. For example, slowly add 600 parts by mass of MeS to a reaction pad containing 540 parts by weight of toluene, 118 parts by weight of water, and 27 parts by weight of fumed silica. After hydrolysis, filter, and neutralize to obtain 135 parts by weight of methylsilicone resin with a viscosity (25 ° C) of 600 mPa • s. After being placed at room temperature for 3 hours, it is solidified into an insoluble product. If stored at low temperature or formulated as a solution, the storage period can be extended to 6-12 months.

(3) A transparent methyl silicone resin is prepared from MeSi (OR). The hydrolysis rate of the SiOR bond in MeSl (OR) 3 (R is Me, Et) is much slower than that of the Si-Cl bond, so that it requires the aid of a catalyst to successfully hydrolyze. This method is easier to obtain prepolymers with predetermined properties and containing SiOH and SiOR. After curing, it has high transparency and good wear resistance, and is suitable for use as a hardening coating and waterproof agent for transparent plastics. For example, when MeSi (OEt) is hydrolyzed under the catalysis of excess water and a trace amount of hydrochloric acid, the initial reactant is divided into two phases, and as the reaction proceeds and the amount of by-product EtOH increases, it is converted into a homogeneous phase. Finally, a colorless transparent methyl silicone resin containing SiOEt and soluble in thousands of EtOH is obtained. The specific process is as follows: adding an industrial grade MeSi (OEt) and saturated Na2C03 aqueous solution at a volume ratio of 100: (1-2) to a column bar for heating, steaming, and refining, After removing the low boiling substance from the tower top, collect the refined MeSi (OEt) 3, which has a boiling range of 140~145 ° C and a CHCI content of as low as 2 µ L/L. Take out 180 parts by mass, add them to a porcelain binding reaction stick with stirring, add another 60 parts of dilute hydrochloric acid containing 153 µ L/L HCI, and fry for 3 hours at 80 ° C 'at 80 ° C, then add 0.025 parts of Me core NHSiMe3 to neutralize HCI, heat up to 90 ° C, evaporate most of EtOH and water, and heat up to ll0 ° C within 0.5 h to complete the silicone resin pre curing process. After cooling, add 110 parts of anhydrous ethanol, 200 parts of methyl silicone resin ethanol solution with a concentration of about 40% (mass fraction) were obtained by filtration.

SILIBASE SILICONE currently including below silicone resins: Methyl Silicone Resin IntermediateMethyl, MQ Silicone Resin Powder, MQ Silicone Resin,Liquid MQ Silicone Resin,Silicone Resin for Motor, Amino Phenyl Silicone Resin,Vinyl MQ Silicone Resin, Silicone Adhesive.

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