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Study On Synthesis And Properties Of Bisphenol-A Polyarylester/Semi-aromatic Polyamide Random Copolymers

Posted on:2012-09-06Degree:MasterType:Thesis
Country:ChinaCandidate:L WangFull Text:PDF
GTID:2211330338468344Subject:Materials Physics and Chemistry
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1. A series of bisphenol-A Polyarylester (PAR-A) and semi-aromatic plyamide random copolymers (PAR-co-PA6I) were synthesized by interfacial polycodensation f rom bisphenol-A(BPA),1,6-hexamethylenediamine and isophthaloyl chloride(IPC). Th e reaction was catalyzed by phase transfer catalyst. The resulting copolymers were white or pale yellow granules. The amount segments of PA6I in the copolymers'm ain chain was controlled by alerting the molar ratio of 1,6-hexamethylenediamine to BPA. The chemical structures of copolymers were confirmed by fourier transform infrared spectrophotometer (FT-IR) and hydrogen nuclear magnetic resonance (1H-N MR). The decomposition temperature (Td) at 5% weight loss of the resulting copoly mers was obtained by thermal gravimetric analyst (TGA) which is more than 325℃. Differential scanning calorimetry (DSC) results showed that the glass transition temp erature (Tg) of the copolymers are in the range of 161~183℃. The Tg of the rando m copolymers was increasing by increasing the mole ratio of the PA6I, which was decreasing when the mole ratio is more than 20%. The copolymers were easily sol uble in concentrated sulfuric acid, chloroacetic acid and 1,1,2,2-tetrachloroethane/phe nol(v/v=1:1) at room temperature. The copolymers'crystallization were characterized by X-ray diffraction and the results show that the crystallinity increased by increas ed the mole ratio of PA6I in the copolymers.2. Novel white or pale yellow granules quaternary Polyarylester-polyamide copo lymers were prepared by phase transfer catalyst interfacial polycodensation from bis phenol-A(BPA), 1,6-hexamethylene-diamine(HMDA), terephthaloyl chloride(TPC) and isophthaloyl chloride(IPC). Two series of quaternary copolymers were synthesized. Firstly E series changed the mole ratio of BPA and the HMDA, while the mole rat io of TPC and IPC was settled at 1:1. Secondly I series were by changed the mol e ratio of TPC and IPC, while it was the BPA and HMDA settled at 1:9. The title d copolymers were characterized by FT-IR, 1H-NMR, WAXD, TGA and DSC. The results show that the copolymers were expected and had excellent thermal properti es. The solubility of the copolymers was also investigated. It proved that the proper ties of I series were better than the E series'. 3. Polyarylester and semi-aromatic polyamide copolymers (PAR-A-co-PA4T/4I) were synthesized by the former mentioned methods from 1,4-butanediamine, BPA, TPC and IPC. The glass transition temperature (Tg) of PAR-A-co-PA4T/4I conducted by differential scanning calorimetry (DSC) and were in the rang of 182.8~200.6℃. The copolymers also showed high thermal stability with 5% weight-loss temperatures between 318.5℃and 377.1℃in nitrogen according to thermogravimetric analysis (TGA). The chemical structures of the copolymers were characterized by FT-IR and 1H-NMR. The thermal properties of PAR-A-co-PA4T/4I were better than the corresponding of PAR-A-co-PA6T/6I.4. Determined the intrinsic viscosity ([η]) of bisphenol-A polyarylester (PAR-A) by the viscometric method, in pure dichloromethane (CH2Cl2) solution at room temperature (25℃). Then set the Mark-Houwink equation parameters by the gel permeation chromatography (GPC). Based on the Mark-Houwink equation lg [η]=lgK+algM, the lg [η] for the vertical axis, lgM(lgMn, lgMw and lgMη) as abscissa, made a series of analysis charts, respectively. The slope and intercept from the straight line obtained the Mark-Houwink equation parameters:K1=1.630×10-4,α1=0.7639; K2=4.245×10-6,α2=1.0525 and K3=8.634×10-7,α3=1.1776. The corresponding data can be obtained from these kinds of equation, such as the corresponding number-average molecular weight (Mn), weight-average molecular weight (Mw) and viscosity-average molecular mass (Mη) and molecular weight polydispersity index. And the specific equations were...
Keywords/Search Tags:Bisphenol-A polyarylester, Semi-Aromatic Polyamide, Random copolymer, Viscometric method, molecular weight
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