The Modification Of Phenolphthalein Polyetherketone (Sulfone) Resin

Phenolphthalein polyetherketone(sulfone) has been regarded as a kind of high performance resin and functional material due to its excellent thermal expansivity, mechanical behaviour, superior chemical resistance and thermal stability et al. It has been used in engineering plastic, composite material and function material aspect. Modification of such materials, you can maintain its heat resistance and mechanical properties based on the effective improvement of their processability and solubility in organic solvents, and give it a range of specific functions. Material modification including physics modification, such as blending, chemical constitution has been not changed, but property of it has been changed; and chemical modification, such as sulfnation, chloromethylation and quaternary ammonium reaction et al. Based on the actual needs of the application and the proposed modification of chloromethylated important in the functional value of material. In this thesis, a series of modification have been taken on phenolphthalein polyetherketone(sulfone).(1). Preparation by a unique post-processing of low bulk density of the PEK-C powder, heat treatment/grinding method to increase its bulk density, and be achieved under different treatment conditions in the bulk density of the control, in adapting to different composite materials preparation of demand results show that:PEK-C after the initial 80 mesh powder 260～280℃under the heat,30～120 min of treatment led to partially melt the resin present state, and then by mechanical grinding bulk density can be increased by about 8%.200 mesh of the resin powder 10% yield increased, the optimum conditions for the optimized heat treatment under 260℃and 30min.(2).Chloromethylation modification of phenolphthalein polyetherketone (PEK-C), using 96～98% of concentrated sulfuric acid as solvent and catalyst,1,4 dichloro-methoxy butane (BCMB) as chloromethylation reagent, in a homogeneous reaction system on the implementation of PEK-C modified chloromethylated, in mild reaction conditions (10～30℃/2～10 h) had been prepared high degree and linear chloromethylation phenolphthalein polyetherketone.The results show that CMPEK-C of chloromethylation degree (χCH2Cl-) is 2.0～3.4 can be easily producted under the mild reaction conditions. Chloromethylation degree of PEK-C can be controled by the reaction temperature and reaction time. This work shows more valuable results of chloromethylation degree of CMPEK-C compared to reported in the similar literatures.The chloromethylated PEK-C (CMPEK-C) resin were characterized By the FT-IR,1H NMR analysis. The solubility of chloromethylated PEK-C remained unchanged, The results of the DSC show the glass transition temperature (Tg) of CMPEK-C increace linear with chloromethylation degree (χcH2cl-).The results show that the linear polymer nature of CMPEK-C products. Initial decomposition temperature of CMPEK-C decreased with the increasing ofχCH2Cl-,whenχCH2Cl-as 3.4 the 5% weight loss temperature is 200℃,GPC data show that the average molecular weight of low chloromethylation degree CMPEK-C decreased slightly, Molecular weight distribution broadened, average molecular weight change greater under high chloromethylation degree.(3).The study of chloromethylation modification of phenolphthalein polyethersulfone (PES-C) with non-toxic, new chloromethylation reagents including preparation chloromethylation reagent 1,4-bis(chloromethoxyl)butane (BCMB), using of 1,4-butanediol, formaldehyde solution and phosphorus trichloride in the ratio of 30:75:50, at the temperature of 10～20℃BCMB can be producted, after vacuum distillation high purity of the BCMB can be get.The structure of product confirmed by 1H NMR spectrum. The BCMB is used as chloromethlation reagent in this paper.Chloromethylation modified PES-C were using homemade BCMB as chloromethylation reagents. Whicn replaced the traditional chloromethylation modified PES-C with chlorine ether/alkyl halides, Lewis acid as catalyst in the system. Firstly, we using concentrated sulfuric acid as the solvent and catalyst chloromethyled modified PES-C, but the reaction occurs in a very short period of time beginning gelation. When halogenated hydrocarbons as solvent, Lewis acid as catalyst, in the 30～80℃chloromethyled PES-C can be carried out well.Experimental results show that under the above conditions can be chloromethylated PES-C easily and effectively, and the chloromethylation degree ((χCH2Cl-) between the 0.2 to 0.7, chloromethylation degree is controled by reaction temperature and reaction time. This paper explores a kind of new method chloromethylated modified phenolphthalein polyethersulfon which convenient and effective with non-toxic and harmless.By the 1H NMR analysis CMPES-C were characterized. The solubility of chloromethylated PES-C remained unchanged, the TGA result shows that 5% of the thermal decomposition temperature of CMPES-C still above 200℃.