聚芳醚砜醚酮酮树脂的合成工艺研究
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摘要
1.采用“一锅法”通过亲电取代反应合成了单体4,4’-二苯氧基二苯砜,利用FT-IR、1H-NMR等技术对其进行表征。结果表明:合成DPODPS可重复性好,平均粗产率在90.0%以上,平均产率在80.0%以上,单体重结晶后的熔程为1℃,纯度较高。
2.以DPODPS为单体与对苯二甲酰氯(TPC)或间苯二甲酰氯(IPC)在亲电反应条件下共缩聚制得了二种聚芳醚砜醚酮酮树脂。用FT-IR、DSC、TG、WAXD等对其结构和性能进行了表征。结果表明:合成的两种PESEKK树脂都有较高的玻璃化转变温度(Tg)和热分解温度(Td),具有耐高温性能,i-PESEKK树脂属于非结晶聚合物,而p-PESEKK属部分结晶聚合物。
3.以4, 4'-二苯氧基二苯飒(DPODPS)为第三单体,与二苯醚和对苯二甲酞氯进行共缩聚制备了三种比例的聚醚酮酮/聚醚砜醚酮酮(PEKK/PESEKK)无规共聚物,并对其结构和性能进行了表征。结果表明:四面体结构的砜基的引入在一定程度上破坏了分子链的规整性,使得共聚物的结晶度有所下降。同时降低了聚合物的熔融温度(Tm),提高了玻璃化转变温度(Tg)使得共聚物的熔融加工性能大大改善。
4.以FeCl3为催化剂采用亲电路线合成了m-EKKE和p-EKKE两种PEKK的小分子模型化合物,并用其与TPC或IPC缩聚,合成了全对位聚芳醚酮酮(p-PEKK)和全间位聚芳醚酮酮(m-PEKK)。用FT-IR、DSC、TG、WAXD等对其结构和性能进行了表征。
5.以30% p-EKKE、70%DPODPS与TPC为单体,通过低温溶液缩聚,合成了三元无规共聚物,并用FT-IR、DSC、TG、WAXD等对其结构和性能进行了表征。结果表明:四面体结构型的砜基的引入,减弱分子链的相互作用降低了共聚物的Tm而Tg有所提高。合成的树脂在WAXD曲线中只出现一个弥散的衍射峰仍是非晶聚集态。
1. 4, 4'-bis(Phenoxy)diphenyl sulfone (DPODPS) was synthesized by electrophilic substitution in one pot. Its structure was characterized by FT-IR, 1H NMR, etc. The results show that the Synthesis of DPODPS is good repeatability, the average crude yield above 90.0% and total yield above 80.0%. After crystallization, the melting range in 1℃, higher purity.
2.Two kind of high molecular Poly (aryl ether sulfone ether ketone ketone) copolymers were synthesized by low-temperature solution polycondensation, with 4,4’-bis(Phenoxy)diphenyl sulfone (DPODPS) and terephthaloyl chloride (TPC) or isophthaloyl chloride (IPC) respectively. Its structure was characterized by FT-IR, TG, WAXD and DSC etc. The results show that the two kind of copolymers have a higher glass transition temperature(Tg)and thermal decomposition temperature(Td),high for performance. i-PESEKK is non-crystalline polymer, p-PESEKK is crystalline polymer.
3. 4, 4'-bis(Phenoxy)diphenyl sulfone (DPODPS) for the third monomer, with the diphenyl ether and terephthaloyl chloride prepared to co-condensation ratio of three PEKK / PESEKK random copolymer, and its structure and properties were characterized by FT-IR, TG, WAXD and DSC etc. The results show that the introduction of sulfonyl tetrahedral structure to some extent undermine the regularity of molecular chain, the crystallinity of the copolymer decreased. At the same time reduce the polymer melting temperature (Tm), to increase the glass transition temperature (Tg) of the molten copolymer allows greatly improved processing performance.
4. Two kind of PEKK small molecule model compounds was synthesized by electrophilic substitution with m-EKKE or p-EKKE and TPC or IPC ,FeCl3 as a catalyst . its structure and properties were characterized by FT-IR, TG, WAXD and DSC etc.
5. Take 30% p-EKKE, 70%DPODPS and TPC as monomers,by the low temperature solution condensation, synthesized three Yuan random copolymer. its structure and properties were characterized by FT-IR, TG, WAXD and DSC etc. The result indicated that, with the tetrahedron structure sulphone base introduction, weakened the molecular chain the mutual function to reduce copolymer Tm, but Tg to have the enhancement. The synthesis resin appeared a dissemination in the WAXD curve the diffraction peak was still only the crystalless state of aggregation.
2.以DPODPS为单体与对苯二甲酰氯(TPC)或间苯二甲酰氯(IPC)在亲电反应条件下共缩聚制得了二种聚芳醚砜醚酮酮树脂。用FT-IR、DSC、TG、WAXD等对其结构和性能进行了表征。结果表明:合成的两种PESEKK树脂都有较高的玻璃化转变温度(Tg)和热分解温度(Td),具有耐高温性能,i-PESEKK树脂属于非结晶聚合物,而p-PESEKK属部分结晶聚合物。
3.以4, 4'-二苯氧基二苯飒(DPODPS)为第三单体,与二苯醚和对苯二甲酞氯进行共缩聚制备了三种比例的聚醚酮酮/聚醚砜醚酮酮(PEKK/PESEKK)无规共聚物,并对其结构和性能进行了表征。结果表明:四面体结构的砜基的引入在一定程度上破坏了分子链的规整性,使得共聚物的结晶度有所下降。同时降低了聚合物的熔融温度(Tm),提高了玻璃化转变温度(Tg)使得共聚物的熔融加工性能大大改善。
4.以FeCl3为催化剂采用亲电路线合成了m-EKKE和p-EKKE两种PEKK的小分子模型化合物,并用其与TPC或IPC缩聚,合成了全对位聚芳醚酮酮(p-PEKK)和全间位聚芳醚酮酮(m-PEKK)。用FT-IR、DSC、TG、WAXD等对其结构和性能进行了表征。
5.以30% p-EKKE、70%DPODPS与TPC为单体,通过低温溶液缩聚,合成了三元无规共聚物,并用FT-IR、DSC、TG、WAXD等对其结构和性能进行了表征。结果表明:四面体结构型的砜基的引入,减弱分子链的相互作用降低了共聚物的Tm而Tg有所提高。合成的树脂在WAXD曲线中只出现一个弥散的衍射峰仍是非晶聚集态。
1. 4, 4'-bis(Phenoxy)diphenyl sulfone (DPODPS) was synthesized by electrophilic substitution in one pot. Its structure was characterized by FT-IR, 1H NMR, etc. The results show that the Synthesis of DPODPS is good repeatability, the average crude yield above 90.0% and total yield above 80.0%. After crystallization, the melting range in 1℃, higher purity.
2.Two kind of high molecular Poly (aryl ether sulfone ether ketone ketone) copolymers were synthesized by low-temperature solution polycondensation, with 4,4’-bis(Phenoxy)diphenyl sulfone (DPODPS) and terephthaloyl chloride (TPC) or isophthaloyl chloride (IPC) respectively. Its structure was characterized by FT-IR, TG, WAXD and DSC etc. The results show that the two kind of copolymers have a higher glass transition temperature(Tg)and thermal decomposition temperature(Td),high for performance. i-PESEKK is non-crystalline polymer, p-PESEKK is crystalline polymer.
3. 4, 4'-bis(Phenoxy)diphenyl sulfone (DPODPS) for the third monomer, with the diphenyl ether and terephthaloyl chloride prepared to co-condensation ratio of three PEKK / PESEKK random copolymer, and its structure and properties were characterized by FT-IR, TG, WAXD and DSC etc. The results show that the introduction of sulfonyl tetrahedral structure to some extent undermine the regularity of molecular chain, the crystallinity of the copolymer decreased. At the same time reduce the polymer melting temperature (Tm), to increase the glass transition temperature (Tg) of the molten copolymer allows greatly improved processing performance.
4. Two kind of PEKK small molecule model compounds was synthesized by electrophilic substitution with m-EKKE or p-EKKE and TPC or IPC ,FeCl3 as a catalyst . its structure and properties were characterized by FT-IR, TG, WAXD and DSC etc.
5. Take 30% p-EKKE, 70%DPODPS and TPC as monomers,by the low temperature solution condensation, synthesized three Yuan random copolymer. its structure and properties were characterized by FT-IR, TG, WAXD and DSC etc. The result indicated that, with the tetrahedron structure sulphone base introduction, weakened the molecular chain the mutual function to reduce copolymer Tm, but Tg to have the enhancement. The synthesis resin appeared a dissemination in the WAXD curve the diffraction peak was still only the crystalless state of aggregation.
引文
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