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1.
Two series of polynaphthalimides (PNIs), II and III , were prepared from 1,4,5,8‐naphthalene tetracarboxylic dianhydride with the usual aromatic diamines ( Ia – Ih ) or Ia , which was used as a soluble modifying agent, and Ib – Ih via a one‐stage process with high‐temperature condensation. Series II and III had inherent viscosities of 0.57–1.34 and 1.15–1.63 dL/g, respectively. IIa and most of the III series were soluble in 1‐methy‐2‐pyrrolidone and m‐cresol at 5–10 wt % and afforded transparent and tough films by m‐cresol solvent casting with a tensile strength in the range of 75–99 MPa. The glass‐transition temperature and softening temperature of these PNIs were in the ranges of 360–404 and 188–241 °C, respectively, and the 10% weight loss temperatures were above 495 °C, with more than a 44% char yield at 800 °C in nitrogen. These PNI films had dielectric constants of 4.14–6.46 (1 MHz), with moisture absorption in the range of 0.87–1.91 wt %. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 940–948, 2006  相似文献   

2.
2,2,′3,3′‐Biphenyltetracarboxylic dianhydride (2,2,′3,3′‐BPDA) was prepared by a coupling reaction of dimethyl 3‐iodophthalate. The X‐ray single‐crystal structure determination showed that this dianhydride had a bent and noncopolanar structure, presenting a striking contrast to its isomer, 3,3,′4,4′‐BPDA. This dianhydride was reacted with aromatic diamines in a polar aprotic solvent such as N,N‐dimethylacetamide (DMAc) to form polyamic acid intermediates, which imidized chemically to polyimides with inherent viscosities of 0.34–0.55 dL/g, depending on the diamine used. The polyimides from 2,2,′3,3′‐BPDA exhibited a good solubility and were dissolved in polar aprotic solvents and polychlorocarbons. These polyimides have high glass transition temperatures above 283°C. Thermogravimetric analyses indicated that these polyimides were fairly stable up to 500°C, and the 5% weight loss temperatures were recorded in the range of 534–583°C in nitrogen atmosphere and 537–561°C in air atmosphere. All polyimides were amorphous according to X‐ray determination. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 1425–1433, 1999  相似文献   

3.
A high‐yield synthesis toward 5,5′‐bis(silyl)‐functionalized 3,3′‐dibromo‐2,2′‐dithiophenes with very efficient work‐up procedure is presented. The molecular structures of two silyl functionalized dibromo‐dithiophenes in the solid state have been determined to investigate the structural influences of different functional groups on the degree of π‐conjugation within the dithiophene moieties, as well as their packing properties. The planar alignment of the tert‐butyldimethylsilyl‐functionalized dibromo‐dithiophene shows a significantly higher degree of conjugation of the π‐system with a more favorable molecular packing than the skewed arrangement of the triisopropylsilyl‐substituted species. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

4.
Reaction of Ti(OCH2CH2OR)4 (R?CH3 and C2H5) with 8‐hydroxyquinoline in benzene at room temperature resulted in the formation of Ti(C9H6NO)2(OCH2CH2OR)2, characterized by IR, 1H‐NMR, UV and mass spectroscopies. The molecular structure of Ti(C9H6NO)2(OCH2CH2OCH3)2 has been determined by single‐crystal X‐ray structure analysis. The geometry at titanium is a distorted octahedron, with the nitrogen atoms of quinolinate occupying the trans position with respect to oxygens of the 2‐methoxyethoxy groups. The prepared quinolinate derivatives of titanium alkoxides are very stable towards hydrolysis and harsh conditions are required for hydrolytic cleavage. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

5.
To check the previously proposed crystal structure of poly(p‐phenylene benzobisoxazole) [PBO], we performed an X‐ray structure analysis for single crystals of low molecular weight model compounds with the following chemical formulas: Both of these two model compounds show essentially the same molecular and subcell structures as those of PBO: the molecular chains take an almost perfect planar conformation and are packed together with a relative height between the adjacent chains of about 3 Å along the chain axis, although for the polymer the chains are shifted by the same value but in a disordered mode with respect to the direction of the shift (upward or downward), different from the regular packing in model compounds. These structural features are reproduced well with energy calculations. Structural ordering in PBO fibers caused by heat treatment at high temperatures, as clarified by X‐ray diffraction measurement, are interpreted on the basis of the energy calculations. © 2001 John Wiley & Sons, Inc. J Polym Sci Part B: Polym Phys 39: 1296–1311, 2001  相似文献   

6.
Fiber‐structure‐development in the poly(ethylene terephthalate) fiber drawing process was investigated with online measurements of wide‐angle and small‐angle X‐ray scattering with both a high‐luminance X‐ray source and a CO2‐laser‐heated drawing system. The intensity profile of the transmitted X‐ray confirmed the location of the neck‐drawing point. The diffraction images had a time resolution of several milliseconds, and this still left much room for improvement. Crystal diffraction appeared in the wide‐angle X‐ray images almost instantaneously about 20 ms after necking, whereas a four‐point small‐angle X‐ray scattering pattern appeared immediately after necking. With the elapse of time after necking, the four‐point scattering pattern changed into a meridional two‐point shape. © 2005 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 1090–1099, 2005  相似文献   

7.
To address a need for highly X‐ray opaque biodegradable materials, a series of poly(ε‐caprolactone) derivatives were prepared using oxime post‐polymerization modification to conjugate two different iodinated hydroxylamines. These materials were synthesized with up to 32 wt. % iodine content and demonstrated improved X‐ray contrast relative to both the ketone precursors and previously reported monoiodinated materials. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55, 787–793  相似文献   

8.
A class of extended 2,5‐disubstituted‐1,3,4‐oxadiazoles R1‐C6H4‐{OC2N2}‐C6H4‐R2 (R1=R2=C10H21O 1 a , p‐C10H21O‐C6H4‐C?C 3 a , p‐CH3O‐C6H4‐C?C 3 b ; R1=C10H21O, R2=CH3O 1 b , (CH3)2N 1 c ; F 1 d ; R1=C10H21O‐C6H4‐C?C, R2=C10H21O 2 a , CH3O 2 b , (CH3)2N 2 c , F 2 d ) were prepared, and their liquid‐crystalline properties were examined. In CH2Cl2 solution, these compounds displayed a room‐temperature emission with λmax at 340471 nm and quantum yields of 0.730.97. Compounds 1 d , 2 a – 2 d , and 3 a exhibited various thermotropic mesophases (monotropic, enantiotropic nematic/smectic), which were examined by polarized‐light optical microscopy and differential scanning calorimetry. Structure determination by a direct‐space approach using simulated annealing or parallel tempering of the powder X‐ray diffraction data revealed distinctive crystal‐packing arrangements for mesogenic molecules 2 b and 3 a , leading to different nematic mesophase behavior, with 2 b being monotropic and 3 a enantiotropic in the narrow temperature range of 200210 °C. The structural transitions associated with these crystalline solids and their mesophases were studied by variable‐temperature X‐ray diffractometry. Nondestructive phase transitions (crystal‐to‐crystal, crystal‐to‐mesophase, mesophase‐to‐liquid) were observed in the diffractograms of 1 b, 1 d , 2 b, 2 d , and 3 a measured at 25200 °C. Powder X‐ray diffraction and small‐angle X‐ray scattering data revealed that the structure of the annealed solid residue 2 b reverted to its original crystal/molecular packing when the isotropic liquid was cooled to room temperature. Structure–property relationships within these mesomorphic solids are discussed in the context of their molecular structures and intermolecular interactions.  相似文献   

9.
The reaction of acetylferrocene [Fe(η‐C5H5)(η‐C5H4COCH3)] (1) with (2‐isopropyl‐5‐methylphenoxy) acetic acid hydrazide [CH3C6H3CH(CH3)2OCH2CONHNH2] (2) in refluxing ethanol gives the stable light‐orange–brown Schiff base 1‐[(2‐isopropyl‐5‐methylphenoxy)hydrazono] ethyl ferrocene, [CH3C6H3CH(CH3)2OCH2CONHN?C(CH3)Fe(η‐C5H5)(η‐C5H4)] (3). Complex 3 has been characterized by elemental analysis, IR, 1H NMR and single crystal X‐ray diffraction study. It crystallizes in the monoclinic space group P21/n, with a = 9.6965(15), b = 7.4991(12), c = 29.698(7) Å, β = 99.010(13) °, V = 2132.8(7) Å3, Dcalc = 1.346 Mg m?3; absorption coefficient, 0.729 mm?1. The crystal structure clearly shows the characteristic [N? H···O] hydrogen bonding between the two adjacent molecules of 3. This acts as a bidentale ligand, which, on treatment with [Ru(CO)2Cl2] n, gives a stable bimetallic yellow–orange complex (4). Copyright © 2002 John Wiley & Sons, Ltd.  相似文献   

10.
Cations derived by protonation of the ligand title compound (L1) have been structurally characterized in their di‐ and tetra‐ protonated forms in the salts [H2L1][ClO4]2·2H2O and [H4L1][ZnCl4]2·4H2O. In both structures, one half of the formula unit comprises the asymmetric unit of the structure, the macrocycle being centrosymmetric, with the two macrocycles adopting similar conformations. In both salts, a pair of diagonally opposed macrocyclic secondary amine groups are protonated; in the [H4L1]4+ salt, the additional pair of protons are accommodated on the exocyclic pendant amine groups. The dispositions of the pendent amines differ between the two structures, being ‘equatorial’ with respect to the macrocyclic ring in the [H2L1]2+ salt, and ‘axial’ in the [H4L1]4+ salt. In other structurally characterized compounds containing [H4L1]4+ the equatorial disposition was found in the ferricyanide adduct, while in the tetraperchlorate salt the axial disposition was identified. The differences in disposition of the exocyclic groups are ascribed to the extensive H‐bonding in the lattices.  相似文献   

11.
Collection of the single crystal X‐ray refraction data of the Bisphenol‐A‐type Macrocyclic oligocarbonate trimer (c‐3mer) at room temperature was carried out. The single crystal of the cyclic trimer that is recrystallized from ethyl acetate showed solvent molecule in the center of macro ring. Similarly, cyclic tetramer (c‐4mer) contained two p‐xylene molecules. Smaller dimer (c‐2mer) did not afford co‐crystal with solvent. Conformation of the carbonate in c‐3mer was s‐cis and s‐cis as in c‐4mer. A relationship between the conformation of carbonate and noncatalyst polymerization activity was not found. Copyright © 2000 John Wiley & Sons, Ltd.  相似文献   

12.
Poly(octamethylene terephthalate) (POT), a semicrystalline aromatic polyester, is synthesized by melt‐condensation reaction, and its thermal property and crystal structure are investigated by using differential scanning calorimetry, X‐ray diffraction, and molecular modeling methods, respectively. It is revealed that the synthesized POT sample has comparably low melting temperature of 131 °C and forms one crystalline phase. Based on two‐dimensional X‐ray fiber diagram and molecular modeling analyses, the crystal structure of POT is identified to be triclinic with dimensions of a = 4.560 Å, b = 5.597 Å, c = 18.703 Å, α = 104.87°, β = 119.45°, and γ = 100.32°, in which one chemical repeating unit of POT with all‐trans conformation of octamethylene group is packed according to the space group of . © 2008 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 47: 276–283, 2009  相似文献   

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16.
Structural studies and morphological features of a new family of linear, aliphatic even–even, X 34‐nylons, with X = 2, 4, 6, 8, 10, and 12, are investigated with X‐ray diffraction and electron microscopy. Solution‐grown crystals were obtained by isothermal crystallization from N,N‐dimethylformamide solutions. The thickness of lamellar‐like crystals was orders of magnitude less than the chain lengths of the polymer samples used, implying that the chains fold to form chain‐folded lamellae. The results bear a close resemblance, with the noticeable exception of 2 34‐nylon, to those reported for nylon 6 6 and other even–even nylon chain‐folded lamellar crystals. The basic structure of the straight‐stem lamellar core is similar to that of the classic nylon 6 6 triclinic α structure, and the chains tilt ≈42° relative to the lamellar normal. In the case of 2 34‐nylon, the structure resembles the 2 Y nylon series, and the chain tilt angle reduces to 36.6°. These combined results suggest that, even with a relatively low frequency of amide units along the backbone of these molecules, hydrogen bonding is still the dominant element in controlling the behavior, structure, and properties of these polymers. In addition, gels were prepared in concentrated sulfuric acid, and gel‐spun fibers were studied using X‐ray diffraction. The data are interpreted in terms of a modified nylon triclinic α structure that bears a resemblance to the structure of even–even nylons at elevated temperatures. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 40: 2685–2692, 2002  相似文献   

17.
A low‐coordinate aryloxo erbium complex, [(ArO)3Er(THF)](MePh), has been synthesized by the reaction of anhydrous ErCl3 with three equivalents of NaOAr in tetrahydrofuran. The central erbium atom is coordinated by three oxygen atoms of the aryloxo ligands and one oxygen atom of the tetrahydrofuran molecule, resulting in a distorted tetrahedron. Copyright © 2004 John Wiley & Sons, Ltd.  相似文献   

18.
The phosphetidine 2,4‐Di‐tert‐butyl‐3‐chloro‐1λ6‐thia‐2,4‐diaza‐3‐phosphetidine‐1,1‐dioxide, O2S (tBuN)2PCl, reacts with tetrasulfur tetranitride, S4N4, in benzene under reflux to afford the novel 4,6‐spirocycle in moderate yield. The deep‐blue crystals of the spirocycle are airstable and high melting in nature. The spiro phosphorus atom subtends a four‐membered PVSVIN2 ring which is saturated, and a six‐membered PVS N3 ring which is unsaturated. The single‐crystal X‐ray structure of this first example of the spirocycle reveals a planar PSN2 ring and a puckered PS2N3 ring and the molecule is symmetric in nature. Copyright © 2006 John Wiley & Sons, Ltd.  相似文献   

19.
o‐Formylphenylboronic acid reacts with morpholine to form 1,3‐dihydro‐1‐hydroxy‐3‐morpholin‐4‐yl‐2,1‐benzoxaborole. The typical hydrogen‐bonded dimer motif with a planar benzoxaborole fragment has been obtained in the solid state. Copyright © 2005 John Wiley & Sons, Ltd.  相似文献   

20.
New regioregular head‐to‐tail type poly(6‐alkylpyridine‐2,5‐diyl)s (P6RPys; R = nonyl, dodecyl, and pentadecyl) were prepared by organometallic polycondensation. The head‐to‐tail (HT) content in the polymers was higher than 95%, as revealed by 1H NMR spectroscopy. Powder X‐ray diffraction data of HT‐P6RPys indicated that P6RPys formed a new type of structure composed of an alternating end‐to‐end packed unit and an interdigitation packed unit. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 43: 215–222, 2005  相似文献   

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