1, in order to terephthalic acid (PTA) and thionyl chloride (SOCl_2) as raw material, by phase transfer catalytic synthesis of benzaldehyde two benzoyl chloride (TPC). FTIR shows that the successful synthesis of the target product; DSC knows its melting point is 83 ℃, the boiling point is 259 ℃; XRD indicates that the target product is crystal. Study of material ratio and phase transfer catalyst content on the yield were investigated, results showed that n (PTA): n (SOCl_2) 1:3, a phase transfer catalyst content is 2%, the product yield the highest, up to 98%.
In 2, in TPC and ethanol amine (MEA) as raw material, the preparation of N~1, N~4- two (2- hydroxyethyl) - benzene two formamide (BAET). Analysis of FTIR and ~1H-NMR, prove the composition as the target product; DSC indicated that the melting of Shuangfeng BAET melting process, analysis of formation reason is the imperfect crystallization induced; TG showed that the thermal decomposition temperature of BAET is 299 ℃; XRD indicates that the target product is crystal. Effect of ratio of raw materials on the yield and hydroxyl value, results show that the TPC:MEA is 1:3, BAET yield the highest, reaching 96.60%, the hydroxyl value of approximately 54mgKOH/g.
In 3, TPC and two in ethanol amine (DEA) as raw materials for preparation of N~1, N~1, N~4, N~4- four (2- hydroxyethyl) - benzene two formamide (TAET). FTIR showed that generate the target product; DSC knows its melting point is 178 ℃; XRD indicates that the target product is crystal. Effect of ratio of raw materials on the yield and hydroxyl value, results show that the TPC:DEA=1:4, product yield the highest, reaching 83.72%, the hydroxyl value of approximately 141mgKOH/g. And respectively with two kinds of curing agent on the terminal carboxyl polyester resin curing film coating experiment, to investigate the performance of the.
In 4, TPC and BAET in the monomer, solution polycondensation of polyester amide (PEA) alternate. FTIR showed the reaction of chloride group and hydroxyl, hydroxyl and carbonyl peak disappeared, ester and amide groups, further shows that successful synthesis of the target product; DSC and TG show that the polymer has no melting occurred at 295 ℃ decomposition, probably due to PEA more benzene ring structure of molecular chain to increase rigidity and hydrogen bonds between molecular chains induced; XRD shows that the product is a polymer, with a certain degree of crystallization.
In 5, PTA/ in adipic acid (AA) and BAET as monomer, solution polycondensation synthesis two kinds of PEA. FTIR showed that the synthesized polyester amide two chain structure; using DSC and TG thermal properties of the two were compared, PTA/BAET polycondensation product not melt that decomposition, AA/BAET condensation product of melting at 174 ℃, which may be due to flexible chain component monomer AA conformation of polymer chain segment to get more easy to change caused by.
In 6, TPC and TAET in the monomer, high-temperature solution polycondensation synthesis of polyester amide, FTIR evidence of the occurrence of the expected response; DSC shows that the product is at 378 ℃ decomposition; XRD shows that the product is a polymer, with a certain degree of crystallization. In the whole reaction process produces no gel, results show that the low temperature synthesis of monomer, synthesis route after high temperature synthesis of polyester amide is feasible.