m,m′-二氨基二苯酮与均苯四酸二酐的微波辐射聚合

研究 m,m′-二氨基二苯酮 (m,m′- DABP)与均苯四酸二酐 (PMDA)的缩聚及亚酰化 ,并运用微波辐射和常规加热两种方式对反应进行了比较。考察了微波辐射时间 (功率 )、单体浓度、单体配比和温度等因素对缩聚物的特性粘数、转化率的影响。用红外光谱对亚酰化度进行了表征 ,并用简并四波混频技术首次测量了该缩聚物的三阶光学非线性极化率系数及其响应时间。实验结果表明 ,微波辐射对提高聚合物的特性粘数和转化率都有显著作用 ;合成的缩聚物具有较大的三阶光学非线性极化率系数 (聚酰亚胺的 χ(3) =1.642× 10 -13 esu)和较快的时间响应 (19ps     

Synthesis and characterization of fluorine and nitrile containing polyimides

A series of polyimides were synthesized from new diamine, Bis [4,4′‐amino‐5,5′ trifluoromethyl phenoxy‐(hexafluoro isopropylidine) phenoxy phenyl] benzonitrile [BATFB] and various aromatic tetracarboxylic anhydrides by thermal and chemical imidization routes. The BATFB was synthesized in two steps by nucleophilic displacement reaction of 2,6‐dichloro benzonitrile, 4,4′‐(hexafluoro isopropylidine) diphenol and 2‐amino‐5‐fluoro benzotrifluoride in the presence of anhydrous potassium carbonate in N,N′‐dimethyl acetamide (DMAc) and the structure was confirmed by FTIR spectroscopy and CHNSO analyzer. The polymers were characterized by FTIR spectroscopy and thermal analysis were performed by differential scanning calorimetry and thermogravimetric analysis methods. The prepared polyimides had glass transition temperatures between 230 and 290°C and their 10% weight loss were recorded in the range 550–590°C in N₂ atmosphere. Majority of polymers are found to be soluble in most of the organic solvents such as DMSO, DMF, DMAc, m‐cresol, and THF even at room temperature and few becomes soluble on heating. The prepared polyimides showed water uptake values 0.34–0.54 wt % at room temperature. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 3455–3461, 2006     

聚酰亚胺的制备及其性能表征

以均苯四酸二酐(PMDA)为二酐单体,对苯二胺(PDA)为二胺单体,通过低温缩聚合成一系列聚酰胺酸(PAA)和聚酰亚胺(PI)薄膜,对其结构和力学性能进行表征。结果表明,聚酰胺酸的酰亚胺化较完全,PMDA-PDA聚酰亚胺薄膜的拉伸强度达到290 MPa。     

Preparation and properties of polyimide solvent‐resistant nanofiltration membrane obtained by a two‐step method

This study investigated the preparation of polyimide solvent‐resistant nanofiltration membranes by a two‐step method (casting the membrane first and then crosslinking by the thermal imidization method). The influences of polymer concentration, thickness of membranes, temperature of the imidization, phase inversion time and thermal imidization procedure were studied. The membranes with the highest rejection rate of Fast Green FCF (molecular weight 808.86 g mol^?1) were prepared in the following conditions: polymer concentration 13 wt%, phase inversion time 1 h, membrane thickness 150 µm and thermal imidization procedure 200 °C for 2.5 h, 250 °C for 2 h and 300 °C for 2 h in a vacuum environment; the heating rate was 5 °C min^?1. The membrane was stable in most of the solvents tested and the fluxes of some common solvents were equal to or higher than a number of commercial solvent‐resistant nanofiltration membranes. A much higher rejection of dyes in water than in methanol was observed in the filtration experiments and a new way to explain it was developed. Copyright © 2011 Society of Chemical Industry     

亚胺化工艺对聚酰亚胺性能影响的研究

以4,4’-二氨基二苯醚ODA和均苯四甲酸二酐PMDA为原料分别采用溶液-固相亚胺化和化学亚胺化法制备了2种聚酰亚胺(PI)树脂。通过FT-IR、DSC、TGA、溶解性能等对PI树脂进行测试与表征。FT-IR表明,2种方法均形成了酰亚胺结构,DSC和TGA分析表明化学亚胺化法得到的PI的热性能优于溶液-固相亚胺化PI。溶解性测试表明溶液-固相亚胺化PI要优于化学亚胺化PI。()()     

聚酰亚胺薄膜及纤维的探索研究

利用均苯四甲酸二酐(PMDA)、4,4'-二氨基二苯醚(4,4'-ODA)和自制三单体在强极性非质子有机溶剂N,N-二甲基乙酰胺(DMAc)中进行共缩聚反应,制得高粘度的聚酰胺酸(PAA)溶液,经涂膜、热亚胺化,得到坚韧透明的聚酰亚胺(PI)薄膜,其具有较好的拉伸断裂强度和合适的伸长率;同时将得到的PAA溶液进行湿法纺丝,制成PAA纤维,采用热亚胺化和高温拉伸的方法制得PI纤维,其断裂强度能达到3.67cN/dtex。     

Simulation of dry‐spinning process of polyimide fibers

As one type of high‐performance fibers, the polyimide fibers can be prepared from the precursor polyamic acid via dry‐spinning technology. Unlike the dry‐spinning process of cellulose acetate fiber or polyurethane fiber, thermal cyclization reaction of the precursor in spinline with high temperature results in the relative complex in the dry‐spinning process. However, the spinning process is considered as a steady state due to a slight degree of the imidization reaction from polyamic acid to polyimide, and therefore a one‐dimensional model based on White‐Metzer viscoelastic constitutive equation is adopted to simulate the formation of the fibers. The changes of solvent mass fraction, temperature, axial velocity, tensile stress, imidization degree, and glass transition temperature of the filament along the spinline were predicted. The effects of spinning parameters on glass transition temperature and imidization degree were thus discussed. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

二层法双面挠性覆铜板用热塑性聚酰亚胺的合成与应用研究

选用合适的单体芳香二酐二苯甲酮四酸二酐（BTDA）、2,2’-双[4-（3,4-二羧基苯氧基）苯基]丙烷四羧酸二酐（BPADA）和芳香二胺3,3′,5,5′-四甲基-4,4′-二氨基二苯甲烷（AMD）、4,4′-二氨基二苯甲烷（MDA）、4,4′-二氨基二苯醚（ODA）,3,4＇-二氨基二苯醚（3,4＇-ODA）根据不同配比反应得到聚酰胺酸,用乙酸酐／三乙胺经化学亚胺化得到热塑性聚酰亚胺（TPI）,将其用N-甲基吡咯烷酮（NMP）溶解配成一定固含量的胶液,涂覆铜箔烘干溶剂得到二层挠性覆铜板（2L—FCCL）,然后将2L—FCCL高温压合制备双面挠性覆铜板,其剥离强度较高。     

Synthesis of some novel silicone-imide hybrid inorganic–organic polymer and their properties

Synthesis and properties of poly(imide-siloxane) hybrid polymers (PIS), having alternate diimide and disiloxane units, based on 1,3-bis(succinyl anhydride)1,1,3,3-tetraorganodisiloxane (I or II) have been described. Polymers have been synthesized by the precursor synthesis i.e., poly(amic acid), using siloxanes (I or II) and 4,4′-diaminodiphenylmethane (DDM) or 4,4′-diaminodiphenylsulphone (DDS) in N,N-dimethylacetamide (DMAc) followed by thermal imidization. FT-IR, thermal (TGA and TMA), solvent resistant and dielectric properties of the compounds have also been studied. The glass transition, thermal stability and char yields of these hybrid polymers increased appreciably. These materials also showed very good solvent resistant properties in protic and aprotic solvents.