Synthesis and characterization of quaternized poly(phthalazinone ether sulfone ketone)for anion-exchange membrane

Chloromethylated poly（phthalazinone ether sulfone ketone） （CMPPESK） was prepared from poly（phthalazinone ether sulfone ketone） （PPESK） using chloromethyl octyl ethers （CMOE） with lower toxicity as chloromethylated regent. CMPPESK was soluble in N-methyl-2-pyrrolidone （NMP）, N,N-dimethylacetamide （DMAc） and chloroform. Quaternized poly（phthalazinone ether sulfone ketone） （QAPPESK） was prepared from CMPPESK by quaternization. QAPPESK had excellent solvent resistance, which was only partly soluble in sulfuric acid （98%） and swollen in N,N-dimethylformamide （DMF）. The vanadium redox flow battery （V-RFB） using QAPPESK anion-exchange membrane had better performance with 88.3% of overall energy efficiency.

Synthesis and characterization of novel poly(aryl ether sulfone ketone)s containing phthalazinone and biphenyl moieties

A novel series of poly（aryl ether sulfone ketone）s （PPESKs） containing phthalazinone and biphenyl moieties were prepared by two-step nucleophilic polycondensation reaction. The ^-Mw values of these copolymers were between 38,330 and 67,900. The glass transition temperatures （Tg） and 5% decomposition temperatures were ranged in 253-269 ℃ and 488-500 ℃, respectively, The structures of these copolymers were confirmed by FT-IR and ^1H NMR. Moreover, all the resultant copolymers were amorphous determined by wide angle X-ray diffraction （WAXD）.

Synthesis of Poly(phthalazinone ether ketone) Containing Sodium Sulfonate Groups via Direct Polymerization

1, 2-Diliydro-4-(4-hydroxyphenyl)(2H)phthalazin-1-one(DHPZ) was sulfonated in concentrated Sulfuric acid. Poly(phthalazinone ether ketone) containing pendant sodium sulfonate group was synthesized from sulfonated and pure 1,2-dihydro-4-(4-hydroxyphenyl)(2H)phthalazin-1-one, and 4,4'-difluorodiphenylketone. The sulfonated monomer and sulfonated polymer were characterized with FT-IR and H-1-NMR.

Characterization and tribological investigation of self-assembled trimethoxysilyl-functionalized poly(phthalazinone ether ketone)thin films on glass substrates

Trimethoxysilyl-functionalized PPEK（PKGS） films had been designed to serve as wear resistant coatings for silicon surfaces. These surface films were formed by a dip-coating technique applied to self-assembled monolayers（SAMs）.The formation and wetting behavior of PKGS films were characterized by means of contact angle measurement.The friction coefficient of the film prepared is very low（about 0.1）,and the anti-wear behavior is good,with a lack of failure after sliding over 1800 s.

Synthesis and characterization of trimethoxysilyl-functionalized poly(phthalazinone ether ketone)

A novel alkoxysilyl-functionalized poly(phthalazinone ether ketone) (PPEK) was prepared for the boundary lubricant application in micro-electro-mechanical system (MEMS). The synthesis of functionalized PPEK was started from the hydroxylation of PPEK, then following with the corresponding ring-opening reaction of 3-glycidoxypropyltrimethoxysilane (GPTMS). The structures of the functional PPEK were confirmed by FTIR, 1H NMR, 29Si NMR, and UV–vis spectrum.

SYNTHESIS AND PROPERTIES OF SULFONATED POLY(ETHER KETONE)S CONTAINING 3,5-DIMETHYL PHTHALAZINONE MOIETIES AS PROTON EXCHANGE MEMBRANE MATERIALS

Sulfonated poly（ether ketone）s containing 3,5-dimethyl phthalazinone moieties （SPPEK-DMs） with different degrees of sulfonation （DS） were synthesized via direct polycondensation from 4-（3,5-dimethyl-4-hydroxyphenyl）-2,3- phthalazinone, 4,4＇-difluorobenzophenone and 3,3＇-disulfonate-4,4＇-difluorobenzophenone. The chemical structure of SPPEK-DMs was characterized by FTIR and 1H-NMR. Thermal stability of SPPEK-DMs was characterized by the thermogravimetric analysis. The membranes prepared from SPPEK-DMs exhibited ion exchange capacities （IEC） ranging from 0.93 mmol.g-1 to 1.86 mmol.g-1. Water uptake, swelling, oxidative stability and methanol permeability of SPPEK- DMs membranes were investigated. SPPEK-DMs membranes exhibited high oxidative stability. The methanol permeability values of SPPEK-DMs membranes were in the range 5.15× 10^-8-6.61×10^-7 cm^2.s-1, which was much lower than those of Nafion117. The proton conductivity of SPPEK-DM40 membranes was 1.1 ×10^-2 S.cm^-1 at 70℃.

成型温度对CF/PPEK复合材料的缺陷和力学性能影响

分别采用溶液浸渍法及真空热压成型法制备了连续碳纤维增强含杂萘联苯结构聚芳醚酮(CF/PPEK)预浸料和复合材料,对不同成型温度制备的复合材料进行了超声相控阵和三维X射线显微镜(XRM)无损检测,利用旋转流变仪、电子万能试验机、动态力学分析仪(DMA)、红外光谱仪(FT-IR)、扫描电镜(SEM)、金相显微镜对CF/PPEK复合材料进行了表征,系统研究了成型温度对纤维的浸润质量以及复合材料孔隙率、弯曲行为和层间剪切性能的影响,通过力学性能分析和断口形貌表征研究了断裂机理及缺陷对其性能产生的影响。试验结果表明:成型温度为350℃时,CF/PPEK复合材料的弯曲模量和层间剪切强度分别为125 GPa和64 MPa;成型温度为360℃时,CF/PPEK复合材料的缺陷最少,弯曲强度可达1376 MPa;而370℃高温下,复合材料出现明显缺陷,各方面性能急剧下降。

杂萘联苯聚芳醚酮表面水凝胶涂层的制备及其抗菌性能

在杂萘联苯聚芳醚酮(PPEK)与银粉掺杂制备的复合材料表面造孔后,采用银离子催化表面自由基聚合法制备聚丙烯酸/丙烯酰胺水凝胶涂层。通过傅里叶变换红外光谱仪、钨灯丝扫描电子显微镜、X射线光电子能谱仪等对水凝胶涂层的结构与性能进行表征,并研究水凝胶涂层改性PPEK的抑菌作用及其细胞相容性。结果表明:PPEK表面造孔后,涂层与基体材料的结合能从185.83 J/m^(2)提高到926.26 J/m^(2);该水凝胶涂层对大肠杆菌和金黄色葡萄球菌的抑菌率达到95%以上,且无细胞毒性,扩大了PPEK在医疗卫生领域的应用。

HYDROPHILIC MODIFICATION OF PPESK POROUS MEMBRANES VIA AQUEOUS SURFACE-INITIATED ATOM TRANSFER RADICAL POLYMERIZATION

Hydrophilic surface modification of poly(phthalazinone ether sulfone ketone)(PPESK) porous membranes was achieved via surface-initiated atom transfer radical polymerization(ATRP) in aqueous medium.Prior to ATRP.chloromethyl groups were introduced onto PPESK main chains by chloromethylation.Chloromethvlated PPESK(CMPPESK) was fabricated into porous membrane through phase inversion technique.Hydrophilic poly(poly(ethylene glycol) methyl ether methacrylate)(P(PEGMA)) brushes were grafted from CMPPESK membrane ...

Synthesis of polypiperazine-amide thin-film membrane on PPESK hollow fiber UF membrane

A new interfacial polymerization （IP） procedure is developed in order to synthesize polypiperazine-amide thin-film membrane on the inner surface of poly（phthalazinone ether sulfone ketone） （PPESK） hollow fiber ultrafiltration （UF） membrane. A hollow fiber composite membrane with good performance was prepared and studied by PT-IR and scanning electron microscopy.

SYNTHESIS OF AN AMPHIPHILIC PPESK-g-P(PEGMA)GRAFT COPOLYMER VIA ATRP AND ITS USE IN BLEND MODIFICATION OF PPESK MEMBRANES

Preparation of an amphiphilic graft copolymer having poly(phthalazinone ether sulfone ketone)(PPESK) as main chains was carried out by atom transfer radical polymerization(ATRP).The precursor,chloromethylated PPESK (CMPPESK),was prepared by using chioromethylether as chloromethylation agent.Then,poly(ethylene glycol) methyl ether methacrylate(PEGMA) was used as monomer to synthesize PPESK-g-P(PEGMA) by ATRP method under the catalysis of a cuprous chloride/2,2'-bipyridyl system.PPESK/PPESK-g-P(PEGMA) blend m...

氯甲基化杂萘联苯聚芳醚酮的热交联及性能

对杂萘联苯聚芳醚酮(PPEK)进行氯甲基化改性,得到一系列不同氯甲基化程度(DCM)的氯甲基化杂萘联苯聚芳醚酮(CMPPEK),以三氯化铝为催化剂,采用热交联的方式制备得到TMPPEK耐溶剂膜,考察了热处理温度和DCM对TMPPEK膜结构和性能的影响。结果表明,随着热处理温度和DCM的增加,膜交联程度增加,耐溶剂性能逐渐增强,同时热稳定性也有所提高;当热处理温度为120℃时,膜在N-甲基吡咯烷酮、乙醇和四氢呋喃等有机溶剂中的凝胶含量介于90%~99%;当DCM在2.34 mmol/g以上时,膜在N,N-二甲基乙酰胺等有机溶剂中的凝胶含量高于90%,表明TMPPEK膜具有优异的耐溶剂性。

高耐热聚芳醚酮固化邻苯二甲腈树脂

以4-(4-羟基苯基)-2,3-二氮杂萘-1-酮、4,4’-二氟二苯甲酮和4-氨基苯酚为原料,通过两步一锅法合成了一种新型的氨基封端杂萘联苯聚芳醚酮(A-PPEK),采用差示扫描量热法(DSC)探究了其对间苯二酚基邻苯二甲腈(DPPH)的固化性能。相比于常用的芳香二胺固化剂4,4’-二氨基二苯砜(DDS),A-PPEK的5%热失重温度(T_(d5%))提高了69.3℃。另外,与DDS在400℃时快速升华不同,A-PPEK在相同温度下的质量保留率仍>95%,说明A-PPEK可以有效解决小分子固化剂高温下分解,容易在邻苯二甲腈树脂中形成缺陷的问题。一系列实验表明,以A-PPEK固化DPPH,体系具有优异的耐热性和加工流动性,当A-PPEK含量为DPPH质量的10%时,固化树脂的T_(d5%)可达553.2℃,玻璃化转变温度高于实验测试范围380℃,最低黏度可达0.167 Pa·s。

含烯丙基杂萘联苯聚芳醚砜酮的合成

以4-(4-羟基苯基)-2,3-二氮杂萘-1-酮、2,2′-二烯丙基双酚A(DABPA)、4,4′-二氟二苯砜及4,4′-二氟二苯酮为单体,通过溶液缩聚法合成一系列烯丙基功能化杂萘联苯聚芳醚砜酮(APPBAESK),探讨了溶剂、单体配比对APPBAESK相对分子质量、溶解性、结晶性能及热性能的影响。结果表明:APPBAESK的相对分子质量随DABPA单体用量的增加而降低,呈现无定形结构,玻璃化转变温度在200℃左右,N2氛围下质量损失5%时的温度在450℃以上,具有较好耐热性,同时实现了烯丙基功能化。

PPBES基膜厚度对复合膜水蒸气渗透性能的影响

使用非溶剂致相分离(NIPS)法,以杂萘联苯共聚醚砜(PPBES)制备不同厚度的PPBES超滤基膜.随着基膜厚度从53μm增加到260μm,基膜接触角、平均孔径、孔隙率和截留率增大,水通量降低.随后,以磺化含侧苯基杂萘联苯聚醚酮(SPPEK-P)为选择层,采用涂覆法制备SPPEK-P/PPBES复合膜.研究基膜厚度对复合膜水蒸气渗透选择性的影响,并对复合膜进行扫描电子显微镜和红外光谱表征.结果表明,随着基膜厚度增大,复合膜水蒸气渗透速率从2244GPU降低到1033GPU,水蒸气/氮气的选择性从445降低到288.

羟基化PPESK复合膜的制备及性能研究

采用NaBH4对杂萘联苯聚芳醚砜酮(PPESK)支撑膜进行羟基化亲水改性,通过间苯二胺和均苯三甲酰氯的界面聚合反应制备复合膜。利用傅里叶变换红外光谱仪(FT-IR)、水接触角仪、扫描电子显微镜(SEM)和X射线光电子能谱仪(XPS)研究羟基化改性对膜表面的形貌结构、原子组成的影响,并测定复合膜对2000 mg·L^(-1)Na_(2)SO_(4)水溶液的分离性能。结果表明:羟基化改性的PPESK-OH支撑膜的亲水性增强;PPESK-OH复合膜的聚酰胺层的交联度较高;PPESK-OH复合膜和PPESK复合膜的脱盐率接近,PPESK-OH复合膜的水通量较PPESK复合膜增大了约38%。

二氮杂萘酮结构对医用聚芳醚酮表面蛋白吸附性能的影响

采用溶液缩聚的方法,合成含二氮杂萘酮结构的杂萘联苯聚芳醚酮(PPEK)、含萘环结构的聚芳醚酮(Nap-PAEK)和含二氮杂萘酮与萘环结构的聚芳醚酮(Nap-PPEK55) 3种不同结构的聚芳醚酮材料。通过核磁共振氢谱、红外光谱、元素分析及X射线光电子能谱证明了所合成聚合物的分子结构和元素组成。原子力显微镜及接触角分析结果表明,3种材料的表面粗糙度及润湿性基本相同。力学性能测试显示3种材料具有与骨组织相匹配的适宜模量。采用耗散型石英晶体微天平(QCM-D)和BCA法分别测试材料动态及静态蛋白质的吸附量,相比于Nap-PAEK和Nap-PPEK55,二氮杂萘酮结构含量较多的PPEK所吸附的蛋白质量明显提高。采用MC3T3-E1成骨细胞评价3种聚芳醚酮材料的生物相容性,结果表明3种材料细胞相容性良好。

一种杂环磺化聚芳醚腈酮质子交换膜材料的合成及表征

用含二氮杂萘酮结构类双酚DHPZ，3，3＇-二磺酸钠基-4，4’-二氟二苯酮，2，6-二氯苯腈以及4，4’-二氟二苯酮，通过缩合共聚合反应合成了一系列不同磺化度、高分子量的磺化聚芳醚腈酮．聚合物特性粘数为0．58～2．0dL／g．用红外光谱（FT-IR），核磁共振谱（^1H-NMR）表征了聚合物结构．用差示扫描量热仪（DSC）和热重分析仪（TGA）研究了聚合物的耐热性能，研究表明其玻璃化温度（Tg）可达352℃，5％热失重温度大于500℃．以N-甲基吡咯烷酮为溶剂，溶液浇铸法制备了聚合物膜，并测定了膜的溶胀率以及质子交换能力．结果表明，与Nation膜相比，磺化聚芳醚腈酮膜在相同的质子交换能力条件下，溶胀率显著降低．

短碳纤维增强PPEK复合材料的性能研究

采用熔融共混的方式制备了不同短碳纤维含量增强含二氮杂萘酮聚芳醚酮(PPEK)基复合材料,对复合材料的加工性能、力学性能、摩擦性能、耐热性进行了研究。结果表明:短碳纤维增强复合材料均可以注塑成型;短碳纤维对PPEK的增强作用明显,拉伸强度和弯曲强度均有大幅提高;复合材料中短碳纤维起到了明显的自润滑作用,复合材料的摩擦系数和磨损率均随碳纤维含量的增加而明显降低;短碳纤维的加入进一步提高了复合材料的耐热性。