专利

正马来酰亚胺封端含二氮杂萘酮联苯结构聚芳醚腈及其制备方法本发明涉及了一种马来酰亚胺封端含二氮杂萘酮联苯结构聚芳醚腈及其制备方法。以自制的4-[4(-4-羧基苯氧基)苯基]-2(-4-羧基苯基)二氮杂萘-1-酮或其衍生物,以及2,6-二氯苯腈为缩聚单体,同时也可加入其它双酚和芳香双卤单体;以对氨基苯酚为封端剂,并加入溶剂、共沸脱水剂和催化     

MM-HPPZ/NDA/TPA聚芳酰胺的合成与性能

采用新型的含间甲基取代杂萘联苯结构的二胺2-(4-氨基苯基)-4-[2-甲基-4-(4-氨基苯氧基)卜2,3-二氮杂萘-1-酮为单体,与2,6-萘二甲酸(NDA)进行溶液缩聚制备了新型聚芳酰胺,以对苯二甲酸(17PA)为第三单体对聚芳酰胺进行了共缩聚改性,并研究了TPA的含量及结构对聚芳酰胺性能的影响。n(NDA)/n（TPA)为4：6时,共聚物特性黏数最大为1．70dL/g。合成的聚芳酰胺具有良好的溶解性,可溶于N-甲基吡咯烷酮、N,N-二甲基乙酰胺等非质子极性溶剂中,玻璃化转变温度大于320℃,5％热失重温度大于435℃。     

多氯芳香族或杂环一、二、三腈基化合物的制备

本专利制得的化合物可分为下列几类:1.氯化芳腈——尤其是五氯苯甲腈、有三个异构体的四氯苯二腈、三氯三间腈、七氯1-氰化萘,七氯2-氰化萘和八氯4,4′-二氰二苯。2.氯化杂环腈——如氯化腈基吡嗪、氯化腈基嘧啶、氯化腈基1,3,5三嗪、氯化氰基吡啶(美国专利3,325,503)、四氯4-氰基吡啶。     

2,3-二甲基-4-(2,2,2-三氟乙氧基)吡啶-N-氧化物的合成

以2,3-二甲基吡啶为原料,通过N-氧化、硝化反应制得2,3-二甲基-4-硝基吡啶-N-氧化物,收率69.3%、质量分数98.5%以上;在相转移催化剂的作用下,2,3-二甲基-4-硝基吡啶-N-氧化物与三氟乙醇反应制得2,3-二甲基-4-(2,2,2-三氟乙氧基)吡啶-N-氧化物,收率74%、质量分数98.7%。化合物结构经~1H-NMR、IR确证。结果表明,本方法具有工艺简单、成本低、适应工业化生产的特点。     

新型耐热双马来酰亚胺改性环氧树脂性能研究

以4-(4-羟基苯基)-2,3-二氮杂萘-1-酮(DHPZ)为原料,制得含二氮杂萘酮结构的聚芳醚砜预聚物(PPES),再与顺丁烯二酸酐反应得到不同聚合度的含二氮杂萘联苯结构的双马来酰亚胺(PPES-BMI)。采用FT-IR和1H-NMR对其分子链结构进行了表征,测试了聚合物分子质量和溶解性能。通过TGA分析和冲击性能测试研究了不同含量、不同聚合度的PPES-BMI对PPES-BMI/DGEBA复合体系热-力学性能的影响。结果表明,PPES-BMI含量增加,体系初始热分解温度和最大热失重温度上升;PPES-BMI质量分数为35%,DP=20的PPES-BMI/DGEBA共混体系的冲击强度最大,达到2.67 kJ/m2,增幅为75.8%。     

2-(1,6-二溴-2-萘氧甲基)-5-芳基-1,3,4-(口恶)二唑类化合物的合成与表征

以碳酸钠作缚酸剂,1,6-二溴-2-萘氧乙酰肼(2)与芳酰氯反应制得N,N′-二酰基肼,后者在POCl3作用下,脱水环化成2-(1,6-二溴-2-萘氧甲基)-5-芳基-1,3,4-(口恶)二唑类化合物.其结构经元素分析、IR、1HNMR和MS表征.     

1-(4-氯苯胺基)-4-(4-甲基吡啶基)-2,3-二氮杂萘的合成与应用

1-(4-氯苯胺基)-4-(4-甲基吡啶基)-2,3-二氮杂萘的合成方法与应用,属于血管生成抑制剂抗肿瘤药物合成技术领域。该化合物是以苯酞为原料,与甲醛吡啶反应得到中间体3-羟基-2-(4-吡啶基)1-茚,再在水合肼中经扩环反应得到另一中间体4-(4-吡啶基)甲基-2H-1-2,3-二氮杂萘,最后与对氯     

含磷阻燃剂在环氧树脂中的应用

采用两种含磷阻燃剂六苯氧基环三磷腈(HPCTP)与9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)分别制备了两组不同配比的阻燃型环氧树脂,并使用锥形量热仪进行测试分析,同时对比了两组材料的拉伸性能。结果表明:两种阻燃剂都能有效降低环氧树脂的热释放速率(HRR),当阻燃剂用量为15%时,HRR分别下降了48.3%和62.0%;HPCTP可使材料的拉伸强度提高30.7%,而DOPO使材料的拉伸性能下降了49.5%。     

含二氮杂萘联苯结构聚氨酯的合成与性能研究

以聚己内酯二醇(PCL)、4-(4'-羟基苯基)-2,3-二氮杂萘-1-酮(DHPZ)、4,4'-二苯基甲烷二异氰酸酯(MDI)及1,4-丁二醇为原料,采用一步法设计合成了含二氮杂萘联苯结构聚氨酯溶液。采用红外光谱仪、X射线衍射仪、热重分析仪以及万能力学试验机,考察了DHPZ含量对聚氨酯胶膜耐高温性能和力学性能的影响。结果表明,二氮杂萘联苯结构提升了聚氨酯膜的耐热性能,DHPZ质量分数从0到5%,初始热分解温度(T_d~(1%))可提高10～20℃;当DHPZ质量分数为2%时,聚氨酯膜力学性能较优,其拉伸强度达到67. 1 MPa,断裂伸长率为860%,弹性模量为4. 5 MPa。     

新刊导读

农 药杀虫剂伏虫隆的合成/刘长春//精细化工中间体.-2001,31(6).-28～29,33 以1,2,4-三氯苯为原料,经硝化、氯化、氟化和还原等步骤合成了5-二氯-2,4-二氟苯胺,产率为72％;以2,6-二氯苯腈为原料,经氟化和水解制得2,6-二氟苯甲酰胺,产率为92％;将2,6-二氟苯甲酰胺先用二(三氯甲基)碳酸酯酰化后制得2,6-二氟苯甲酰异氰酸酯,再与3,5-二氯-2,4-二氟苯胺加成得到苯甲酰脲类杀虫剂伏虫隆,产率为93％。水杨酸双嘧啶(钠)的合成新方法/杨伟等//江苏农药.-2001,(4).-7～8     

Synthesis of dysprosium/Mn–Cu ferrite binary nanocomposite: Analysis of structural,morphological, dielectric,and optomagnetic properties

Manganese–copper ferrite (MCFO) and dysprosium (Dy)-doped manganese–copper ferrite nanocomposites (Mn_0.5Cu_0.5Dy_xFe_2−xO₄) (x = 0, 0.05, 0.10, and 0.15) were synthesized by sonochemical method. Crystal structure and the structural parameters of the MCFO were analyzed based on the doping concentration of Dy ion. It was observed that the average crystalline size of the synthesized nanocomposite decreases when the concentration of Dy increases. The existing spherical surface morphology of the MCFO and Dy-doped MCFO nanocomposites were obtained through scanning electron microscopy. In the UV spectrum, the pristine MCFO sample showed an absorbance peak at 743 nm whereas the absorbance values of Dy-doped ferrite nanocomposite considerably shifted (blue) toward a lower wavelength (231–222 nm). The dielectric parameters of all ferrite nanocomposites were studied in the frequency range of 100 Hz to 5 MHz. The dielectric spectrum revealed that dielectric constant and loss tangent decreased with increased doping concentration of Dy ion. The saturation magnetization also changed with Dy doping in MCFO. The impact of Dy on manganese–copper ferrite changed the optical, dielectric and magnetic properties of the prepared binary ferrite nanocomposite, which can be used for microwave-absorbing material applications.     

Mechanical Properties of Compression Molded Banana Pseudo-stem Filled Unplasticized Polyvinyl Chloride (UPVC) Composites

Mechanical strengths of a banana pseudo-stem (BPS) fiber and unplasticized polyvinyl chloride (UPVC) composite were evaluated to assess the possibility of using it as a new material in engineering applications. Samples were fabricated by the compression molding process with reference to the effect of filler loading. The samples were submitted to mechanical tests to measure tensile, flexural, and impact properties of the composites. The nature of adhesion between the matrix and the reinforcement and information relating the structure of mechanical properties can be obtained by scanning electron microscopy (SEM) assessment of the composite fracture surface. The mechanical properties show that the composites did not have good adhesion between filler and matrix; on the other hand, the filler insertion improved the flexural modulus and the material rigidity.     

核壳型纳米粒子合成方法及其性能的研究进展

核壳纳米粒子作为复合纳米粒子一个重要的分支,由于其光、磁和催化等方面的优异性能,近年来引起了人们广泛的关注.本文主要介绍了核壳纳米粒子的制备方法及诸多性能,并对核壳纳米粒子的发展进行了展望.     

单向玻璃纤维-铝合金层板的几种力学性能研究

本文用实验方法研究了单向玻璃纤维-铝合金层板的拉伸性能、疲劳性能和冲击性能。利用金属体积分数理论验证了这类层板的拉伸性能。通过对其疲劳性能的实验研究，发现裂纹扩展速率的大小及刚度的下降与加载的最大循环应力密切相关的规律。实验发现该层板具有比铝合金好得多的冲击性能。     

TMPTMA在硅橡胶中的应用研究

研究了助交联剂三羟甲基丙烷三甲基丙烯酸酯(TMPTMA)对硅橡胶硫化性能、力学性能、低温性能和粘接性能的影响。结果表明,加入少量TMPTMA能改善硅橡胶的硫化特性和工艺性,提高硫化胶的硬度,降低硅橡胶的结晶温度,并有效提高硅橡胶与金属的粘接强度;但TMPTMA用量超过一定数值后,由于TMPTMA部分自聚合,在硅橡胶内形成一定的交联网络,造成两相界面粘接力变差,致使硅橡胶的拉伸强度降低。当TMPTMA用量为1份时,硅橡胶具有最佳的综合性能。     

聚氨酯种类对机械性能以及阻尼性能影响研究

分别以聚四氢呋喃醚二醇(PTMEG)、聚氧化丙烯二醇(PPG-1000)为软段,以二苯基甲烷二异氰酸酯(MDI-50、MDI-100LL),以及扩链剂1,4-丁二醇(BDO)、三羟甲基丙烷(TMP)为硬段,采用预聚体法制备了聚氨酯弹性体。并系统研究了聚氨酯体系中各组分的种类对材料机械性能和阻尼性能的影响。     

A new precursor to lightweight porous Si–Al–O–B ceramics with enhanced microwave transmissivity

Nowadays, complicated preparation processes and harsh sintering conditions wave transparent ceramics limit its further development. To solve this problem, we explore a promising precursor by adopting a polymerization-pyrolysis method to prepare porous Si–Al–O–B ceramics at a mild sintering condition (1000 °C). The porous Si–Al–O–B ceramics exhibits enhanced wave transparency at 10–16 GHz with a low dielectric constant (<3), a low loss angle tangent value (<0.01), and simultaneously, a relative high flexible strength of 82 MPa. According to the results of the XRD and FTIR analysis, porous Al₄B₂O₉ crystallization dispersed in the amorphous SiO₂ matrix constructs the main phases of the products. The changes of Al and B elements are confirmed to have an effect on the phase compositions and micro structure of the composite ceramics, which obviously affect the mechanical and dielectric properties of the derived ceramics. The as-prepared porous Si–Al–O–B ceramics could be a potential candidate for next generation electronic window materials due to its low dielectric constant and loss angle tangent value, as well as high flexible strength.     

Effects of support and additive on oxidation state and activity of Pt catalyst in propane combustion

The effects of support and additive on the oxidation state and catalytic activity of Pt catalyst in the low temperature propane combustion were systematically investigated on Pt/MgO, Pt/Al₂O₃ and Pt/SiO₂–Al₂O₃. The catalytic activity varied much with both support materials and additives. The catalyst on the more acidic support showed higher activity, and the catalytic activity on every support materials increased as the electronegativity of additives increased, while some additives decreased the activity. The oxidation state of platinum, estimated by white line intensity of Pt L_III-edge XANES spectrum, also varied with the support and additives, and additives with higher electronegativity greatly prevented the platinum from its oxidation under oxidising atmosphere. Among almost all the catalysts with various supports and various additives, a clear relationship was observed between the oxidation state of platinum and the catalytic activity; the more metallic platinum showed higher activity. Thus, it was concluded that the total electrophilic/electrophobic property derived from those of the support and additive controls the oxidation state of platinum, which intensively affects the catalytic activity; i.e. higher electrophilic property provides less oxidised platinum, resulting in high catalytic activity. The mechanism of this effect was also discussed on the basis of thermochemical data, and it was proposed that the electrophobic materials promote the noble metal oxidation since the noble metal oxo-anion such as PtO^δ− is more stabilised with electrophobic cation.     

聚丙烯基抗菌塑料的制备与性能研究

利用熔融挤出共混技术制备了聚丙烯(PP)基抗菌塑料。研究了抗菌母料Antim-PP对PP的抗菌性能和力学性能的影响。结果表明,当抗菌母料与PP的质量比为4:100时,抗菌PP塑料对大肠杆菌的抗菌率大于99%,抗菌母料的加入使共混物的冲击性能有明显改善,其他力学性能基本不受影响。