Preparation Of Amino Silicon Oil Through Bulk Copolymerization

Amino silicon oil (amino-alkyl polysiloxane) as a kind of functional silicon oil, is one of the fastest-developing organo-silicon products. For it's excellent performance of softness, lubricity, hydrophobia, defoaming, film forming, glazing and innocuity, no polution of it's synthesis process, it has been wildly used in many industrial and public fields.Through bulk copolymerization of octamethylcyclotetra siloxane and aminosilan monomer named N-β-aminoethyl-γ-aminopropyl methyl dymethoxysilane, an amino silicon oil was prepared.The comparison of effect of KOH and tetramethyl ammonium hydroxide (TMAH) as catalyst of the reaction with different status filled in was carried through. It was appoved that the catalysis effect of KOH is greatly influenced by it's granularity and necessary to be made into suspension in D4. The catalysis effect was not satisfactory for it's liability to react with CO₂ and tenderness to trace of water in the air. TMAH turned out to be of no difference on it's granularity for it's physical character to melt under the reation temperature and dispersed by stirring.After that, under the catalysis of TMAH, the dynamic characters and yield polymer structure of copolymerization reaction under different process conditions was probed. As to reaction velocity and conversion rate, concerntration of catalyst was proved to be dominating, the reaction can't be triggered under 50 ug/g and more than 210 ug/g needed on 10:1 monomer ratio. Monmer ration turned out to have no impact on reaction velocity and higher for better for conversion rate. As to polymer molecular weight, concerntration of catalyst was proved of minority impact and monomer ratio dominating, While AN performed little difference.Atoms of water as a special factor was proved to be of notable impact on the reaction velocity and conversion rate.As to unbalanced fasculation reaction, according to analysis of mechanisms, there exist very slow homocondension between methoxyl of polymer chain and APAEDMS and faster hetreocondension between hydroxyl which comes from reaction of water with methoxyl and methoxyl of polymer chain and APAEDMS.The research on impact of vacuum with no water supply to reaction proved that vacuum from —55cmHg to —71cmHg was of no marked influence on molecular weight and couldn't deepen the reaction even with change of monomer ratio only for homocondension. Water supply was validated to improve molecular weight and constitution of polymer through making hetreocondension possibole. Thereon mild reaction conditions of balanced water supply was designed to achieve slow while lasting deepeness of reaction to yield very high molecualr weight and constitution.A method of preparing polymer of different molecular weight and constitution through changing catalyst & water concertration and monomer ratio on balanced ring opening and controlling of water supply and reaction time-span of the fasculation was advanced.