磺化三聚氰胺甲醛树脂合成的磺化工艺及磺化结构分析

研究了羟甲基三聚氰胺磺化阶段的pH值、温度和时间对磺化反应的影响,并采用13C-NMR分析了磺化的化学结构.研究表明,在pH>11 5,温度为80～90℃和合适的时间内可以获得高磺化程度的三聚氰胺磺酸盐;在摩尔比F/M=4 0和S/M=1 0的反应体系中,磺化可同时发生在仲氮和叔氮原子上,两种结构之比约为2∶1.     

汽车罩光清漆的固化和降解机理研究(Ⅲ)——核磁共振研究罩光清漆的固化和降解

利用13C交叉极化（CP）和门控高功率去偶（GHPD）二个脉冲序列的魔角旋转核磁共振（MASNMR）技术表征了汽车罩光清漆的固化和降解过程,研究结果表明涂料在固化后形成的丙烯烯酯－三聚氰胺交联,经较长时间的紫外线曝晒,逐步降解,生成少量的三聚氰胺－三聚氰胺交联和丙烯酸酯－丙烯酸酯交联。     

Synthesis of a new schiff base oxovanadium complex with melamine and 2‐hydroxynaphtaldehyde on modified magnetic nanoparticles as catalyst for allyl alcohols and olefins epoxidation

A new magnetically recoverable nanocatalyst designated as Fe₃O₄@SiO₂@PTMS@Mel‐Naph‐VOcomplex was synthesize by covalent binding of a Schiff base ligand derived from melamine and 2‐hydroxy1naphtaldehyde on the surface of silica coated iron oxide magnetic nanoparticles followed by complexation with VO (acac)₂. Characterization of the prepared nanocatalyst was accomplished with FT‐IR, XRD, SEM, HRTEM, VSM and atomic absorption techniques. It was found that the epoxidation of geraniol, trans‐2‐hexen‐1‐ol, 1‐octen‐3‐ol, norbornene, and cyclooctene is highly selective, affording quantitative yields of the corresponding epoxides with tert‐butyl hydroperoxide (TBHP) using Fe₃O₄@SiO₂@Mel‐Naph‐VOcomplex as catalyst. High reaction yields, short reaction times, simple experimental and work up procedure, catalyst stability and excellent reusability even after five‐cycles of usage in the case of geraniol are some advantages of this research.     

Preparation of Microporous Melamine‐based Polymer Networks in an Anhydrous High‐Temperature Miniemulsion

We report the first example of a successful preparation of a microporous organic polymer within the droplet phase of an inverse non‐aqueous miniemulsion. Stable nanoparticles with enhanced specific surface area could be obtained despite the harsh conditions regarding reaction temperature (180 °C) and time (72 h) needed for building melamine‐based Schiff base networks. Our new flexible method can in principle be applied to other water‐sensitive protocols suitable for the bulk synthesis of MOPs that are based on Friedel‐Crafts, Sonogashira‐Hagihara or Yamamoto chemistry.     

新型阻燃剂季戊四醇双磷酸二氢酯三聚氰胺盐的合成与应用

以季戊四醇、氧氯化磷和三聚氰胺为原料，成功地合成了季戊四醇双磷酸二氢酯三聚氰胺盐，经元素分析，ＩＲ和＾３１ＰＮＭＲ证实了结构，测定了该化合物对聚丙烯的阻燃性能。     

Effects of melamine polyphosphate and halloysite nanotubes on the flammability and thermal behavior of polyamide 6

Melamine polyphosphate (MPP) and halloysite nanotubes (HNT) were introduced to polyamide 6 (PA6) by melt blending in order to improve the fire resistance. PA6 composite containing 12% flame retardants with good spinnability was obtained. The flammability of PA6 composite was characterized by limiting oxygen index (LOI), UL‐94 vertical burning and cone calorimeter (CONE) tests. The results indicated that the LOI value could reach 24.0 vol.% and UL‐94 rating could achieve V2 level at the presence of 12% flame retardants. CONE data demonstrated that peak heat release rate was significantly reduced from 554 kW/m² of neat PA6 to 368 kW/m² of the sample containing flame retardants. Thermal analysis indicated that the thermal stability and char formation were improved by the presence of flame retardants. The morphology of residue char was characterized by scanning electron microscopy; and it suggested that a network‐structured protective char layer had been formed. The possible synergism between MPP/HNT and their flame retardant mechanism was also analyzed and discussed. Copyright © 2014 John Wiley & Sons, Ltd.     

新型多功能三溴三聚氰胺催化剂催化醇甲酰化和乙酰化反应MaryamHajjami,ArashGhorbani-Choghamarani,ZahraKaramshahi,MasoomehNorouzi简

Tribromo melamine has been found to be an efficient and green organocatalyst for the acetylation and formylation reactions of alcohols with acetic anhydride and ethyl formate at room temperature and under mild reaction conditions.     

Hydrogen-bonding recognition-induced aggregation of gold nanoparticles for the determination of the migration of melamine monomers using dynamic light scattering

The migration of melamine monomers from food contact materials has aroused particular attention since the 2008 melamine-tainted milk scandal in China. However, the determination of melamine monomer’s migratory quantity (MMMQ) has remained an open question because of the complex sample pretreatment and the low sensitivity. Based on the hydrogen bonding interaction between DNA thymine and melamine, this paper described a simple and rapid method focusing on the measurement of MMMQ from melamine tableware by gold nanoparticles (GNPs) and dynamic light scattering (DLS). With the presence of probe DNA (p-DNA), the GNPs were stable in NaCl solution (0.06 M), whereas they became aggregated when the p-DNA hybridized with melamine. The change in the hydrodynamic diameter of GNPs could be detected by DLS technology. Under the optimal conditions, the average diameter increased linearly with the concentration of melamine over the range from 5.0 to 320.0 μg L⁻¹, and showed a detection limit of 2.0 μg  L⁻¹ (3σ/slope). The MMMQ was investigated within a range from 6.00 × 10⁻⁴ to 2.58 × 10⁻¹ mg dm⁻² (n ≥ 3) in four different food simulants at different temperatures and time points. The results suggest that the DLS method has great potential in the analysis of the migration of melamine monomers.     

Synthesis and Characterization of S-Triazine Cored Tripodal Keto-oxime and Its Trinuclear Complexes

2,4,6-Tris(4-hydroxybenzimino)-1,3,5-triazine (II) has been synthesized by the reaction of 1 equiv. melamine (I) and 3 equiv. 4-hydroxybenzaldehyde and characterized by means of elemental analysis, ¹H NMR, Fourier transform–infrared spectroscopy, and liquid chromatography–mass spectrometry (LC-MS). 2,4,6-tris(4-(2-phenyl-2-keto-hydroxyiminoyloxy)benzimino)-1,3,5-triazine L (III) has been synthesized by the reaction of 1 equiv. II and 3 equiv. chloroisonitrozoacetophenone and characterized by means of the same methods. Four novel trinuclear Fe(III) and Cr(III) complexes involving tetradentate Schiff bases N,N′-bis(salicylidene)ethylenediamine-(salenH₂) or bis(salicylidene)-o-phenylenediamine-(salophen H₂) with L (III) have been synthesized and characterized by means of elemental analysis, Fourier transform–infrared spectroscopy, LC-MS (ESI⁺), and thermal analyses. The metal ratios of the prepared complexes have been determined using atomic absorption spectroscopy. The aim of the present study is to synthesize novel tridirectional-trinuclear systems and to present their effects on magnetic behavior of [salen or salophenFe(III)/Cr(III)] capped complexes. The complexes have also been characterized as low-spin distorted octahedral Fe(III) and as distorted octahedral Cr(III) bridged by keton-oxime group.     

Chemically Crosslinked pH- and Temperature-Sensitive (N-isopropylacrylamide-co-1-vinyl-2-pyrrolidone) Based on New Crosslinker: I. Swelling Behavior

Novel pH- and temperature-sensitive polymer matrices based on N-isopropylacrylamide have been developed. The hydrogels were prepared by bulk radical polymerization of N-isopropylacrylamide and 1-vinyl-2-pyrrolidinone in appropriate amounts of distilled water using different mol% of traditional N,N-methylene bisacrylamide (MBA) and the new synthesized N,N,N-tris acryloyl melamine (MAAm) crosslinkers. Lower critical solution transition temperatures (LCST) were measured by differential scanning calorimetry. The synthesized hydrogels have LCST lower than 40°C. The influence of environmental conditions such as temperature and pH on the swelling behavior of these polymeric gels was investigated. The swelling behaviors of the resulting gels show pH sensitivity. The crosslinked NIPAAm/VP with MAAm hydrogels exhibited more rapid deswelling rate than NIPAAm/VP hydrogels crosslinked with MBA in pure water in response to abrupt temperature changes from 20°C to 50°C.