Modification of sulfonated poly(ether ether ketone) with phenolic resin

Soluble phenol formaldehyde resin containing hydroxymethyl groups has been used to modify sulfonated poly(ether ether ketone) (SPEEK). Modification has been carried out with films containing both the polymers and using dimethyl formamide (DMF) as casting solvent at various temperatures under reduced pressure. Associated solvent and the hydrogen‐bonded by‐product dimethyl amine (DMA) were removed through mild alkali–acid–water treatment. Cured and treated films show good and consistent mechanical properties, water uptake (22–25%), ion‐exchange capacity (1.1–1.5 meq/g) and proton conductivity (125–150 mS/cm) at 30°C and hold promise for application in fuel cells, as indicated by a polarization study in a fuel cell test station. Copyright © 2007 John Wiley & Sons, Ltd.     

Structural characteristics of phenol formaldehyde novolak resin depending on polycondensation type using molecular simulation

Phenol formaldehyde novolak resins have various structures depending on the polycondensation types. Their structures were characterized using molecular mechanics and molecular dynamics. Dimer, tetramer, hexamer, octamer, and decamer of the resins with the ortho–ortho, ortho–para, and para–para sequences were calculated. The ortho–ortho resins have the structural characteristics of intramolecular hydrogen bonds between hydroxyl groups of the adjacent phenolic units. For the ortho–para and para–para resins, the intramolecular hydrogen bonds are formed mainly between hydroxyl groups of the backbone phenolic units. The para–para resins also have intramolecular hydrogen bonds between hydroxyl groups of the branched phenolic units. A factor determining the structural characteristics of the resins was found to be the geometry of the basic unit (dimer). The order of the end‐to‐end distances between hydrogen atoms on the para‐position of the basic units of the resins is ortho–ortho resin < ortho–para resin < para–para resin. The calculational results were found to be consistent with the gel permeation chromatography (GPC) analysis. Copyright © 2001 John Wiley & Sons, Ltd.     

Preparation of phenol formaldehyde resins containing pendant isoimides and their isomerization to stable resins

Aminophenols were allowed to react with maleic and phthalic anhydrides, producing high yields of the corresponding N‐(hydroxyphenyl) maleamic and phthalamic acids, respectively. The amic acids were dehydrated to the corresponding maleisoimides and phthalisoimides with N,N‐dicyclohexylcarbodiimide or ethyl chloroformate as the dehydrating agent. Formaldehyde was allowed to react with the products in the presence of an acid catalyst, and novel phenol formaldehyde resins (Novolac‐like) were produced. The resins on treatment with a sodium carbonate solution or on prolonged heating at 50 °C suffered rearrangement to corresponding phenol formaldehyde resins with pendant imides. This rearrangement was accompanied by an increase in the softening point and thermal stability. © 2000 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 38: 3244–3252, 2000     

Preparation and characterization of microencapsulated LDHs with melamine‐formaldehyde resin and its flame retardant application in epoxy resin

Layered double hydroxides (LDHs) are emerging as a new and green high‐efficient flame retardant. But LDHs aggregate seriously because of their hydrophilicity, which affect deeply the mechanical and flame retardant properties of their composites. For the first time in this paper, microencapsulated LDHs (MCLDHs) with melamine‐formaldehyde (MF) resin were prepared by microencapsulation technology to enhance their compatibility and dispersion within epoxy resin (EP). The mechanical and flame retardant performances of EP/MCLDH composite were studied by comparing with EP/LDH composite. Results showed that the water contact angle of MCLDHs increased from 8.9° to 122.1°, which indicated good compatibility. The particle size of MCLDHs decreased sharply, and more than one‐third were up to submicron scale, which can be conducive to dispersion. Moreover, the tensile strength and elongation at break of EP/MCLDHs with different flame retardant contents were higher than those of EP/LDHs. And the addition of MCLDHs increased the glass transition temperature (Tg) of EP/MCLDHs, which meant a strong interfacial interaction. Besides, compared with EP/LDHs, the limiting oxygen index values of EP/MCLDHs were higher, and its peak of heat release rate and total heat release decreased by 16.3% and 5.5% respectively. EP/MCLDHs achieved from V‐1 to V‐0 rate with the increasing content of MCLDHs from 20% to 30%, while LDHs/EP never passed tests. In the process of heating, H₂O, CO₂, and NH₃ released from MCLDHs formed gaseous phase, and the remaining dense char layers and oxides produced condensed phase, which played an important role in inhibiting combustion.     

Preparation and characterization of hexadecane microcapsule with polyurea--melamine formaldehyde resin shell materials

<正>This paper gives a brief report of the preparation of hexadecane microcapsule with polyurea-melamine formaldehyde resin shell materials(HMPM).The sealing performance and thermal stability of HMPM was enhanced much more effectively than that of microcapsule with polyurea shell material(HPM).The results of microscopical imaging analysis system,DSC,TG,and laser particle analyzer were briefly introduced.     

Polymer structure of cured alkaline phenol–formaldehyde resol resins with respect to resin synthesis mole ratio and oxidative side reactions

A wood adhesive-type phenol–formaldehyde (PF) resol resin synthesized with a typical formaldehyde to phenol mol ratio of 2.10 was thoroughly cured and studied by the solid-state crosspolarization/magic angle spinning ¹³C nuclear magnetic resonance (CP/MAS NMR) spectroscopy. The methylene group/phenol mol ratio values found were between 1.35 and 1.46, close to the value of a completely cured PF polymer structure. The amount of formaldehyde emitted during resin curing was very small. Other formaldehyde-derived groups determined from CP/MAS NMR spectra and relatively high levels of oxidation products of formaldehyde determined from water extracts of cured resin raised the total formaldehyde-derived groups/phenol mol ratio value to close to that of the synthesis mol ratio. Technological implications of these findings are discussed. © 1997 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 35: 3275–3285, 1997     

Investigation of a resorcinol–formaldehyde resin by 13C-NMR spectroscopy and intrinsic viscosity measurement

Various molecular weight fractions and oligomers isolated from a novolac type resorcinol–formaldehyde (RF) wood adhesive resin were studied by ¹³C-NMR, gel permeation chromatography (GPC), and intrinsic viscosity measurements. The ¹³C-NMR results indicate that methylene groups occur mostly between C₄–C′₄ and C₂–C′₄ carbons and in minor amounts between C₂–C′₂ carbons of resorcinol rings. By suppressing the nuclear Overhauser effect (nOe) and using a long delay time for ¹³C-NMR measurements, reasonable methylene/aromatic carbon ratios were obtained from the aromatic C₁ carbon patterns that have resulted from different numbers of methylene groups bonded on the aromatic ring. This analysis results indicate that the RF resin has an appreciable amount of branch structures and compare favorably with the gel permeation chromatography and intrinsic viscosity measurement results. © 1993 John Wiley & Sons, Inc.     

Cure kinetics of biphenyl epoxy‐phenol novolac resin system using triphenylphosphine as catalyst

The effects of the concentration of triphenylphosphine as a catalyst on the cure reaction of the biphenyl epoxy/phenol novolac resin system were studied. The kinetic study was carried out by means of the analysis of isothermal experiments using a differential scanning calorimeter. All kinetic parameters including the reaction orders, activation energy and kinetic rate constants were evaluated. To describe the cure reaction with the catalyst concentration, the normalized kinetic model was developed. The suggested kinetic model with a diffusion term was successfully able to describe and predict the cure reaction of epoxy resin compositions as functions of the catalyst content and temperature. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 713–720, 1999     

气相色谱法同时测定树脂中氯化苄、苄醇和苯酚

对于通用型酚醛树脂和专用型酚醛树脂,其游离酚的分析方法通常采用容量法。但对碳素材料专用酚醛树脂,由于在生产时添加氯化苄对酚醛树脂进行改性,使树脂能浸润碳素材料的中心。这种树脂的生产过程控制和产品质量检验时,涉及游离酚、氯化苄和苄醇的分析测定,如果采用分别测定,其操作相当繁琐,准确性也不高。在常规方法蒸馏苯酚的过程中,氯化苄和苄醇也会被蒸馏出来,蒸馏出来的氯化苄和苄醇对苯酚的容量分析有干扰。在此基础之上,对氯化苄、苄醇和苯酚的蒸馏进行回收率测定,结果表明回收率满足要求。因此,本文建立了气相色谱法同时测定碳素材料专用树脂中的氯化苄、苄醇和苯酚的分析方法。即采用与容量分析方法一样的样品前期处理（酒精溶解样品、水浴蒸馏）,使游离酚、氯化苄和苄醇同时与树脂分离后,采用气相色谱法测定。本方法使测定步骤简化,可用于氯化苄改性的专用酚醛树脂的科研和生产控制。     

Synthesis of a novel epoxy resin containing naphthalene moiety and properties of its cured polymer with phenol novolac

A new epoxy resin (Bis-ENA) containing naphthalene structure linked with a 1,4-bis(isopropylidene)phenylene was synthesized and was confirmed by elemental analysis, infrared spectroscopy, and ¹H nuclear magnetic resonance spectroscopy. To estimate the effect of naphthalene moiety on the cured polymer, an epoxy resin (Bis-EP) having phenyl moiety was synthesized, and curing behaviors of Bis-ENA and Bis-EP with phenol novolac were evaluated by differential scanning calorimetry. The incorporation of naphthalene structure into the resin backbone increased the curing temperature and reduced the curing reactivity. Thermal properties of the cured polymers obtained from Bis-ENA and Bis-EP with phenol novolac were examined by thermomechanical analysis and dynamic mechanical analysis. Mechanical properties and moisture resistance were evaluated by flexural strength, flexural modulus, and moisture absorption measurements. The cured polymer obtained from Bis-ENA showed higher glass transition temperature, higher flexural modulus, lower thermal expansion, and lower moisture absorption than that from Bis-EP. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 3063–3069, 1999     

硼酸与甲阶酚醛树脂的配位反应及配合物的结构

本文通过对溶液pH值的测定和外光谱分析，研究了硼酸与甲阶酚醛树脂的配位反应。结果表明：在室温下硼酸能与甲阶酚醛树脂中的羟基发生配位反应，并产生H^ 使溶液的pH值降低；溶液的酸性强弱与甲阶酚醛树脂中的羟甲基含量和硼酸的用量有关；硼酸以硼酸根离子的形式与树脂中的酚羟基和邻位羟甲基发生配位反应，形成了一个含有两个氧原子和一个硼原子的六元环，使甲阶酚醛树脂发生交联。     

Aggregation behavior of star-like PEO-PPO-PEO block copolymer in aqueous solution

The aggregation behavior of a star-like amphiphilic block copolymer (denoted as AP432, which was synthesized via anionic polymerization), in aqueous solutions was investigated by surface tension, steady-state fluorescence, dynamic light scattering (DLS) and transmission electron microscopy (TEM). For comparison, a commercially available linear amphiphilic PEO-PPO-PEO block copolymer, Pluronics L64, which has a similar PEO fraction to AP432, was also studied. It is found that the different molecular structure of AP432 and L64 leads to a significant difference on their behavior both at the air/water interface and in bulk aqueous solutions. The results of surface tension measurements indicate that the surface activity of AP432 is much more pronounced than that of L64. The formation of AP432 and L64 aggregates are identified by DLS, fluorescence and TEM measurement.     

Aggregation behavior of block polyethers with branched structure at air/water surface

The block polyethers with various branch structure, such as TEPA[(PO)₃₆(EO)₁₀₀]₇, TEPA[(PO)₃₆(EO)₁₀₀(PO)₃₆]₇, and TEPA[(PO)₃₆(EO)₁₀₀(PO)₅₆]₇ were synthesized. Moreover, the aggregation behavior was investigated via the measurements of equilibrium surface tension, dynamic surface tension, and surface dilational viscoelasticity, in order to probe the effect of the block structure on the property of the branched block polyethers. The surface tension results show that the efficiency and effectiveness of the block polyethers to lower surface tension increase with the increase of the PO group numbers. The maximum surface excess concentration (Γ_max) values and the minimum occupied area per molecule at the air/water interface (A_min) values of the branched block polyethers obtained from Gibbs adsorption equations increase and decrease with the increases of the PO group numbers, respectively. The dynamic parameters n and t^* representing the diffusion speed of the polyether molecules from bulky solution to the subsurface and from the subsurface to the air/water surface are obtained according to the equation proposed by Rosen. The results show that the n values firstly increase and then decrease and t^* values decrease with the increase of the polyether concentrations. The results of surface dilational viscoelasticity show that the dilational modulus of TEPA[(PO)₃₆(EO)₁₀₀(PO)₅₆]₇ is the largest among the three block copolymers at the low concentration (<1 mg L⁻¹) but that of TEPA[(PO)₃₆(EO)₁₀₀]₇ is the largest at the high concentration (>1 mg L⁻¹).     

Synthesis of a novel epoxy resin containing diphenylether moiety and thermal properties of its cured polymer with phenol novolac

A new type of epoxy resin containing 4,4′-diphenylether moiety in the backbone (2) was synthesized, and was confirmed by gel permeation chromatography, infrared spectroscopy, and ¹H nuclear magnetic resonance spectroscopy. In addition, in order to evaluate the influence of 4,4′-diphenylether moiety in the structure, epoxy resins having 4,4′-biphenylene moiety (4) and having 1,4-phenylene moiety (6) in place of 4,4′-diphenylether moiety were synthesized. The cured polymer obtained through the curing reaction between the new diphenylether-containing epoxy resin and phenol novolac was used for making a comparison of its thermal and physical properties with those obtained from 4, 6, and bisphenol-A (4,4′-isopropylidenediphenol) type epoxy resin. The cured polymer obtained from 2 showed markedly higher anaerobic char yield at 700°C of 44.0 wt %, higher fracture toughness, and higher mechanical strength and modulus. © 1999 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 37: 3687–3693, 1999     

DH-2树脂对镝的吸附及机理

研究了镝离子在HD-2树脂上的吸附行为。在HAc-NaAc体系pH=6.20时吸附最佳,测得静态饱和吸附容量为356mg/g(树脂),用0.1~2.0 mol/L HC l可定量洗脱,表观速率常数k198=1.16×105s-1,表观活化能Ea=16.1kJ/mol。等温吸附服从Freun ilich经验式,吸附热力学参数△H=16.5kJ/mol,△S=58.2 J/(mol.K),△G298=-0.859kJ/mol。用化学和红外光谱等方法讨论了吸附机理。     

可反应性纳米二氧化硅填充聚氯乙烯树脂在空气中的热分解行为

利用热重分析和差热重量分析(TG/DTG)技术研究了可反应性纳米二氧化硅填充聚氯乙烯(PVC/n-SiO2)树脂在空气气氛中的热分解行为,利用Ozawa-Flynn-Wall (OFW)方程和Friedman方程对其热分解进行了动力学分析.结果表明,可反应性纳米SiO2对PVC树脂热分解的第一阶段影响比较明显,当纳米S...     

Mechanical properties of phenol/formaldehyde resin composites reinforced by cellulose microcrystal with different aspect ratio extracted from sisal fiber

Sisal cellulose fiber (SCF) and sisal fiber cellulose microcrystal (SFCM), produced with sulfate pulping method and ball‐milling approach separately, were in‐situ polymerized and dispersed into phenol/formaldehyde (PF) resin, to manufacture SCF/PF and SFCM/PF composites via rolling and molding method and investigate the effect of SCF and SFCM on the impact, flexural, and dynamic mechanical properties of the SCF/PF and SFCM/PF composites. As a result, under the condition of same content, SFCM could preferably enhance these properties maybe resulting from the better dispersion in resin matrix than SCF. In particular, when SFCM content was 7%, the impact strength and equilibrium relaxation modulus of the SFCM/PF composite were increased by 26.5% and 37.7%, while the creep deformation was decreased by 26.5%. In addition, when SFCM content was 5%, the flexural strength, initial storage modulus and glass transition temperature of SFCM/PF composite were increased by 8.5%, 22.6%, and 13°C. Copyright © 2016 John Wiley & Sons, Ltd.     

Melamine–formaldehyde resin supported H a mild and inexpensive reagent for synthesis of coumarins under mild conditions

Melamine-formaldehyde resin supported H~+ is used as an efficient catalyst in the Pechmann condensation reaction of phenols withβ-ketoesters,in solvent-free media leading to the formation of coumarin derivatives using conventional heating and microwave irradiation in excellent yields with good purity.     

Design and preparation of magnetic mesoporous melamine–formaldehyde resin: A novel material for pre‐concentration and determination of silver

Using commercially available melamine and formaldehyde as the starting materials, a magnetic mesoporous melamine–formaldehyde resin (MMF@Fe₃O₄) possessing large surface area was prepared via a simple method and could be used as an efficient adsorbent for magnetic solid‐phase extraction. Compared with the traditional synthetic methods of MMF@Fe₃O₄, this approach is easily operated under mild conditions, is time‐saving and environmentally friendly, and can produce the material in high yields. The as‐prepared MMF@Fe₃O₄ possesses good adsorption capacity and selectivity for silver ions. The affecting factors such as pH, amount of MMF@Fe₃O₄, extraction time, desorption solvent, eluent concentration and sample volume were systematically investigated and optimized. Under the optimized conditions, the material exhibited a good response to silver ions at concentrations in the range 2.0–200 μg l^?1 with good linearity (r² = 0.9982), while the limit of detection was found to be 0.12 μg l^?1. The material was successfully applied to the determination of silver in a variety of water samples.