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Synthesis And Characterization Of Novel Polymer Containing Xanthene Moieties Based On Multicomponent Polymerization

Posted on:2018-03-27Degree:MasterType:Thesis
Country:ChinaCandidate:Y J WangFull Text:PDF
GTID:2321330512992383Subject:Polymer Physics and Chemistry
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This paper mainly introduces the development of multi-component polymer and its application.The main content of the experiment is divided into three parts:1.The first experiment is based on xanthone,thionyl chloride,phenol as raw material,using a pot two-step reaction to produce 9,9-bis(4-hydroxyphenyl)xanthene(BHPX),Then 9,9-bis(4-hydroxyphenyl)xanthene(BHPX)was reacted with trifluoromethanesulfonic anhydride in the presence of ice bath to get9,9-bis[4-(trifluoromethylsulfonyloxy)phenyl]xanthene.Finally,it was reacted with trimethylsilylacetylene to form the final desired monomer 9,9-bis(4-ethynylphenyl)-xanthene(BEPX).The yield of monomer reached 80%.9,9-bis(4-ethynylphenyl)-xanthene(BEPX)as a stationary monomer with different diacid chloride and n-butyl mercaptan carried in one-pot mulicomponent polymerization reaction under the corresponding reaction conditions,the corresponding polymer was P1a-P1 d respectively.The polymers obtained by this method have good solvent properties in various solvents such as DMAc,DMF and THF,indicating that the polymer has good machinability;From the UV spectrum of the measured polymer,we can see that when ? = 500 nm,the optical transparency of polymer between 97.26%-99.31%,when ? = 600 nm,the optical transparency of polymer in the 97.95% and 99.54%,When ? = 700 nm,the optical transparency of the polymer is between 98.17% and 99.77%,When ? = 800 nm,the optical transparency of the polymer is between 98.18% and 99.78%,and the initial cutoff wavelength of the polymer is 320 nm to 347 nm.Through the analysis of WXRD curve can be found,the polymer is amorphous structure,it is non-crystalline.In addition,the thermal decomposition temperature of the polymer at 5% and 10% weight loss ranged from263-320 oC and 347-418 oC in nitrogen,respectively,these figures show that they have good thermal properties,and all the polymer left above 58% residual even at 750 oC in nitrogen.2.The second part of the experimental content is 9,9-bis(4-ethynylphenyl)xanthene(BEPX),terephthaloyl chloride and n-butylamine,cyclohexylamine,benzylamine through a pot method to synthesis the polymer Pa-Pc under the catalysis of Pd(PPh3)2Cl2,CuI,9,9-bis(4-oxo-ethynylphenyl)xanthene,terephthaloyl chloridewith n-butylamine,cyclohexylamine,benzylamine through a pot method to get the polymer Pd-Pf under the catalysis of Pd(PPh3)2Cl2,CuI.We have done a corresponding performance test of the polymer,a series of data show that the polymer not only has a high average molecular weight,but also has excellent solubility.Not only in strong polar solvents was dissolved such as NMP,DMAc,DMF,but also the weak polar solventsIn of pyridine,tetrahydrofuran also have completely dissolved,which shows that the polymer has a good solubility,but also shows a great dealability.Through the analysis of WXRD curve can be found,the polymer is amorphous structure,is non-crystalline.In addition,we can also get from the UV analysis,when?= 500 nm,the optical transparency of polymer between 97.05%-99.31%,when ?=600nm,the optical transparency of polymer between 98.40%-100.0%,When ?=700nm,the optical transparency of the polymer is between 98.63% and 100.0%,and when ?= 800 nm,the optical transparency of the polymer is between 98.63% and100.0%,and the initial cutoff wavelength of the polymer is 363 nm to 383 nm.When the weight loss is 5%,the thermal decomposition temperature of the polymer from193 to 308 oC.When the weight loss is 10%,the thermal decomposition temperature from 248 to 337 oC,which shows that it has good thermal performance.3.The experimental content of the third part is 9,9-bis(4-ethynylphenyl)xanthene(BEPX)with p-methylbenzaldehyde,p-bromobenzaldehyde,p-chlorobenzaldehyde,p-cyanobenzaldehyde in three Boron chloride to obtain polymer of Pa-Pd.The polymers obtained by this method have good solvent properties in various solvents such as DMAc,DMF and THF,indicating that the polymer has good machinability.Through the analysis of WXRD curve can be found,the polymer is amorphous structure,it is non-crystalline.We use GPC technology to measure the molecular weight of polymer,it is relatively high.From the UV spectrum of the measured polymer,we can see that when ? = 500 nm,the optical transparency of polymer between 97.95%-99.77%,when ? = 600 nm,the optical transparency polymer in the97.95% and 99.54%,When ? = 700 nm,the optical transparency of the polymer is between 98.63%-100.0%,When ? = 800 nm,the optical transparency of the polymer is between 98.63%-100.0%,and the initial cutoff wavelength of the polymer is261 nm to 290 nm.The thermal decomposition temperature of the polymer is174-193 oC when the weight loss is 5%,and the thermal decomposition temperature is245-298 oC when the weight loss is 10%,which shows that it has good thermal performance.
Keywords/Search Tags:xanthenes, 9,9-bis(4-hydroxyphenyl)xanthenes, 9,9-bis(4-(trifluoromethylsulfonyloxy)phenyl)xanthenes, 9,9-bis(4-(trimethylsilanylethynyl)phenyl)xanthenes, 9,9-bis(4-ethynylphenyl)xanthenes, a pot of multicomponent polymerization
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