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Study On The Synthesis Of Chlorodimethyl-3,3,3-trifluoropropylsilane

Posted on:2019-06-20Degree:MasterType:Thesis
Country:ChinaCandidate:D P MaFull Text:PDF
GTID:2321330548462361Subject:Chemical engineering
Abstract/Summary:PDF Full Text Request
Fluororubber is widely used in many fields due to its excellent properties of oil resistance,solvent resistance,high temperature resistance,and chemical resistance.However,the traditional low-temperature performance of fluorine rubber is poor,the temperature is too low to be vulnerable to embrittlement,in the synthesis process of fluorine rubber,the addition of a fluorine silicon monomer,can improve the low temperature performance of fluorine rubber.In this thesis,the synthesis of Cl(CH3)2SiH(CH2)2CF3,a novel fluorosilicone rubber monomer,was studied using the hydrosilylation method,catalyzed by homogeneous catalysts and supported catalysts.Firstly,investigate the catalytic reaction under homogeneous conditions to obtain the best process conditions:the platinum amount was 1.02×10-5 mol g-1,and the molar ratio of CH2=CHCF3 to HSi(CH3)2Cl was 1.2:1.0,the reaction temperature is 120?.The addition of auxiliaries in H2PtCl6 solution can improve the catalytic performance,the effect of amine ligands is better than that of phosphine ligands.Among them,NEt3 has the best effect,he optimal molar ratio of H2PtCl6 to NEt3 was 1:0.9.Secondly,the preparation process of H2PtCl6 supported by ?-Al2O3 and the process conditions of heterogeneous system were optimized to obtain the best preparation conditions:preparation of catalyst by impregnation-liquid phase impregnation and reduction;added competitive adsorbent C2H2O4 in an amount of n(C2H2O4):n(H2PtCl6)=20:1,and immersion time 4h;add HCHO as reducing agent,n(HCHO):n(H2PtCl6)=70:1;reduction reaction pH=8?9,platinum loading 3.0%,calcination temperature 550?,calcination time 4h;catalyst dosage 0.817×10-Smol·g-1,CH2=CHCF3 and HSi(CH3)2Cl molar ratio of 1.3:1.0,reaction temperature 120?.Compared with the homogeneous catalytic system,the target product under the heterogeneous system has better effect.Finally,on the basis of the kinetic parameters,using Aspen Plus to simulate the relationship between different working conditions and reactor volume under the specified production capacity.The results show that when the molar flow rate of HSi(CH3)2Cl is 132mol/hr,the molar ratio of CH2=CHCF3 to HSi(CH3)2Cl is 1.0:1.0,and the reaction temperature is 398.15K,the volume of the reactor is the most economical.
Keywords/Search Tags:Fluorosilicone rubber, Chlorodimethyl-3,3,3-trifluoropropylsilane, Hydrosilylation reaction, Platinum catalyst
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