Preparation Of Epoxy-polyether Modified Silicone Oil And Its Emulsion Blended With Amino Modified Silicone Oil

Silicone oil with the excellent characteristics of polymer and inorganic materials is a class of linear silicone polymer. Silicone oil has special properties such as non-toxic, high flexibility and low surface tension, but its applications are limited by some default properties due to the poor intermiscibility with some organic solvents and water, poor reactivity with other substances. So more and more people are interested in modified silicone oil with various groups. Epoxy modified silicone oil has been applied in fabric finishing as spinning oil agent and increases the thermostability of fabric. Polyether modified silicone oil has been widely used as self-emulsifying defoamer and fabric hydrophilic antistatic agent, it improves polyether silicone oil itself hydrophilicity. So modified silicone oil with epoxy and polyether group is prepared by the bulk polymerization. Amino modified silicone oil with excellent softness and film-forming ability is a class of better softener and can be interacted with hydroxy and carboxyl group of fibers. For obtaining the special properties of emulsion with amino, epoxy and polyether group, we will reach the following content: epoxy-polyether group modified silicone oil and amino modified silicone oil are emulsified by compound emulsifier to prepare blue-white stabilized emulsion of 20% silicone. Then the preliminary experiment of finishing the PAN based carbon fiber precursor is carried out.(1)The capping agent-disiloxane with epoxy group and allyl polyether are synthesized by hydrosilylation reaction, this reaction is carried out with allyl polyether, epoxy chloropropane and 1,1,3,3-tetramethyldisiloxane as main raw material. The chemical structure is characterized by IR and 1H NMR. The effects of material feeding ratio, the amount of catalyst, the reaction temperature and time on capping agent are discussed. The optimum process parameters are 10 ppm of catalyst, 1: 1.8 of material feeding ratio(Si-H:C=C), 65℃ and 4h. The epoxide number, viscosity and yield of the capping agent produced under optimum condition are 0.1292mol/100 g, 280 cp and 84%, respectively.(2)The epoxy-polyether group modified silicone oil is prepared by the reaction of D4 and disiloxane with epoxy group and allyl polyether under the condition of tetramethyl ammonium hydroxide as catalyst.1H NMR confirms the synthesized product, and its thermal stability and hydrophilic are also investigated. The effects of material feeding ratio,reaction temperature and time, amount of catalyst on the properties of product are discussed. The optimum process parameters are 1:1 of the molar ratio of the disiloxane with epoxy group and allyl polyether to D4, 0.7wt% of catalyst with the respect to monomer, 60℃ and 3h, and the epoxide number, viscosity and yield of the target productobtained under the optimum conditions are 0.0930mol/100 g, 436-445 cp, 78%,respectively.(3)Epoxy-polyether group modified silicone oil and amino modified silicone oil are emulsified to prepare the emulsion. The effects of the ratio of silicone oil, the kind and amount of emulsifier, the ratio of compound emulsifier on the properties of emulsion are discussed. The optimum process routes are 3:2 of amino: epoxy-polyether, AEO-3 and AEO-9 compound emulsifier as emulsifier, 20wt% of emulsifier amount, 1:1of AEO-3:AEO-9. The size and surface topography of the compound emulsion are tested, and the results of surface tension and viscosity show that the paintability of emulsion reaches the standard of on the surface of carbon fiber precursor.(4) The pre-oxidation process is carried out after finishing by the maceration method.To better investigate the finished effects of the compound emulsion, the surface topography of pre-oxidated PAN based carbon fiber precursor is tested. The thermodynamic performance of finished and unfinished pre-oxidated yarn is tested for explaining the decomposition of pre-oxidated yarn for 320℃.