Preparation And Properties Of Amino-modified Silicone Based Oil Agent For Carbon-fiber-precursor Acrylic Fiber

As a kind of high-performance composite material,carbon fiber has been used in aerospace,national defense security,transportation,military weapons,new energy and other fields due to its high strength and high modulus.However,the core preparation technology of this material is monopolized by Japan and the United States.Carbon fiber precursor acrylic fiber is an important raw material and oil agent is critical and essential auxiliary agent in the preparation of carbon fiber.In this article,octamethyl cyclotetrasiloxane(D4),N-?-(aminoethyl)-?-aminopropyl methyldimethoxy silane(KH-602),hexamethyldisiloxane(MM)and tetramethylammonium hydroxide(TMAH)solution were used as raw material to synthesize a kind of amino modified silicone emulsion(AMSE1).Fourier infrared spectrometer(FT-IR)and nuclear magnetic resonance(~1HNMR)were employed to characterize the synthesized product structure.Furthermore,the method of single factor analysis was exploited to analyze the amino modified silicone oil emulsion and the best synthetic conditions were figured out as:1.4%of MM,12.64%of KH-602,0.17%of TMAH and 85.96%of D4.Under the proportion of raw materials,the reaction kept at105?for 6 hours and received the yield of 82.1%.Secondly,octamethyl cyclotetrasiloxane,1,3-Bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane,tetramethylammonium hydroxide solution were used as raw material to synthesize second kind of amino modified silicone oil emulsion(AMSE2).Fourier infrared spectrometer(FT-IR)and nuclear magnetic resonance(~1HNMR)were employed to characterize the synthesized product structure.Furthermore,the method of single factor analysis was exploited to analyze the amino modified silicone oil emulsion and the best synthetic conditions were figured out as:1.4%of 1,3-Bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane,0.17%of TMAH and 98.6%of D4.Under the proportion of raw materials,the reaction kept at 105?for 6 hours and received the yield of 88.2%.In this article,amino-modified silicone oil(AMSE1)was emulsified with two methods.The first method was based on two kinds of external emulsifier and one auxiliary agent and the second method was based on the self-emulsifying of the product made from the epoxy modified silicone reacted with primary amine and polyether amine.After testing and analyzing the emulsified and compounded oil agent,it drew a conclusion that the smaller content of ammonia in the side chain of amino modified silicone oil can lead to the larger the particle size.When the ammonia content in the side chain was too low,the particle size became smaller because polymer chain tend to be tangled.The heat resistance enhanced with the decrease of ammonia content in the side chain.In order to ensure the stability of the emulsion,the coupling agent kept at12.5~33.3%(wt%)and used to synthesize the side chain amino modified silicone oil.When the proportion of amino modified silicone oil was used in same content,the compounding emulsion of amino modified epoxy silicone oil and amino modified silicone oil possessed smaller particle size and stronger heat resistance than the emulsion of amino modified silicone oil.In this article,amino modified silicone oil and domestic commercial amino silicone oil at different dosages on the strand integrity,wettability,antistatic and mechanical properties of carbon fibers.The following conclusions are drawn that the larger the amount of oil agent was used and the better the strand integrity,wettability,antistatic and mechanical properties of the treated carbon fibers within a certain range.At the same dosage,AMSE1 has better stand integrity,wetting,antistatic and mechanical properties to carbon fiber than common amino silicone oil in business situation.