3,4-二甲氧基苯乙胺的合成

对芳香乙胺化合物进行了研究,以选取适合工业生产的合成方法.邻苯二酚经醚化得到1,2-二甲氧基苯,收率96.7%,再选用高选择性的溴化剂溴化,收率96.5%,经格氏反应和羟乙基化反应制备3,4-二甲氧基苯乙醇,醇与对甲苯磺酰氯反应得到酯,收率97.0%,最后经Gabriel法可以制备3,4-二甲氧基苯乙胺,此步反应收率68.5%.通过实验对各步反应条件进行优化,为相关产品的研究开发提供了有效的途径.     

Coloring effect of the organic hybrid of polyamide 6 and N,N′‐ethylene‐bis(tetrabromophthalimide)

Coloring study in organic hybrid of polyamide (PA6) and N,N′‐ethylene‐bis(tetrabromophthalimide) (EPT), where the chromophore was self‐assembled by hydrogen bonding formed between PA6 molecular chains and EPT compound, have been characterized by several techniques. CS930 double wavelength lamella scanner was employed to measure the change of color. The existence of hydrogen bonding in PA6/N‐N′‐ethylene‐bis (tetrabromophthalimide) (PA6EPT) was investigated with Fourier transform infrared (FTIR), the results of which were compared with that of PA6 with the same thermal history. FTIR spectra at room temperature revealed that there is essentially hydrogen bonding between PA6 and EPT. The crystallization behavior of PA6EPT affected by hydrogen bonding was studied by using FTIR. The temperature‐dependent behavior of both PA6 and PA6EPT was studied by temperature‐FTIR spectroscopy and differential scanning calorimetry (DSC). With temperature increasing, changes in sensitive, high‐resolution absorbance spectra are observed as dissolve‐volatilizing thin film. Temperature‐FTIR results showed that the hydrogen bonding in PA6EPT attenuated and dissociated considerably at a smaller rate than PA6, that is to say, hydrogen bonding in PA6EPT is more stable than that in PA6. DSC showed that the melting temperature of PA6EPT and PA6 are similar. However, the crystalline degree and crystalline temperature and melting enthalpy of PA6 and PA6EPT are different. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 594–600, 2007     

醋酸装置催化剂循环使用周期短的原因及对策

根据乙醛氧化反应催化剂的循环使用机理对湘维醋酸装置催化剂循环使用周期短的原因进行了分析，找出了反应温度偏高、氧醛比偏大、醋酸锰循环使用流程不合理、用工业水溶解醋酸锰等四项原因，并提出了改进措施，实施后使湘维醋酸装置催化剂循环使用周期达到了国内先进水平。     

Lower Bounds for Eigenvalues of Elliptic Operators: By Nonconforming Finite Element Methods

The paper is to introduce a new systematic method that can produce lower bounds for eigenvalues. The main idea is to use nonconforming finite element methods. The conclusion is that if local approximation properties of nonconforming finite element spaces are better than total errors (sums of global approximation errors and consistency errors) of nonconforming finite element methods, corresponding methods will produce lower bounds for eigenvalues. More precisely, under three conditions on continuity and approximation properties of nonconforming finite element spaces we analyze abstract error estimates of approximate eigenvalues and eigenfunctions. Subsequently, we propose one more condition and prove that it is sufficient to guarantee nonconforming finite element methods to produce lower bounds for eigenvalues of symmetric elliptic operators. We show that this condition hold for most low-order nonconforming finite elements in literature. In addition, this condition provides a guidance to modify known nonconforming elements in literature and to propose new nonconforming elements. In fact, we enrich locally the Crouzeix-Raviart element such that the new element satisfies the condition; we also propose a new nonconforming element for second order elliptic operators and prove that it will yield lower bounds for eigenvalues. Finally, we prove the saturation condition for most nonconforming elements.     

Au/TS-1的合成及其对环己烷氧化反应的影响

用不同的:实验方法制备得到了钛硅负载金催化剂(Au/TS-1).并用于催化环己烷液相选择氧化反应。发现以无机钛硅为原料水热合成得到的Au/TS-1催化剂具有良好的催化性能;在反应体系中以氧气作为氧化剂,考察了反应时间、温度、压力等因素对催化剂活性的影响。结果表明,当叔丁基过氧化氢用量为0.04 g时,在150℃,1.0 MPa的条件下反应2.5 h,环己烷的转化率达到了9.42%,目的产物(环己醇、环己酮和环己基过氧化氢)的选择性为89.38%。     

二苯基环己基甲醇的合成

以环己基苯甲酮和溴苯为原料,合成了二苯基环己基甲醇。探讨了影响反应的各种因素,并找到了较好的合成条件。     

1,2,4-三唑-3-磺酸-N,N-二乙基甲酰胺-2,4,6-三甲基酚酯的合成及应用研究

对1，2，4-三唑-3-磺酸-N，N-二乙基甲酰胺-2，4，6-三甲基酚酯高效除草剂原药合成的工艺条件进行了优化，得到了优化的工艺条件为：原料配比n(N，N-二乙基甲酰胺-3-氯磺酰-1，2，4-三唑)：n(三甲基苯酚)：n(三乙胺)=1：1．05：1．05，反应温度为30℃，反应时间为3h。并对其应用进行了初步研究：结果表明1，2，4-三唑-3-磺酸-N，N-二乙基甲酰胺-2，4，6-三甲基酚酯具有合成工艺条件简单、合成收率达到95％、生物活性高与产品易加工等特点。     

ZnCl2/C气固催化氯化吡啶制备2,3,5,6-四氯吡啶

以氯化锌为活性组分，活性炭为载体，通过气固催化氯化吡啶合成2，3，5，6-四氯吡啶。催化剂在低温下具有较高的收率，但易发生平行副反应而导致催化剂失活，高温下ZnCl2/C具有较好的稳定性，催化剂高温失活原因主要是活性组分的流失。在氯气与吡啶摩尔配比为7、空速为1400h^-1、温度为420℃下，催化剂连续运行实验表明，2,3，5，6-四氯吡啶的收率大于54％，多氯吡啶的总收率稳定在91％以上。     

基于动态射频指纹的调频定位方法

针对调频(FM)广播信号动态变化对定位性能产生较大影响的问题,提出了动态射频指纹的FM定位方法。该方法采用多元线性回归和神经网络方法,根据离线阶段各个参考点和部分较准点的调频广播信号强度的关系,使用在线阶段较准点的信号强度实时估计在线阶段参考点的信号强度。通过这两种方法建立具有自适应能力的动态射频地图,并使用贝叶斯估计方法对目标进行定位。实验结果表明,相对静态射频指纹模型：采用多元线性回归的射频指纹动态映射模型定位误差平均减少9.1%,采用神经网络的射频指纹动态映射模型定位误差平均减少36.3%,有效抑制了射频信号动态变化时变性对定位性能的影响。     

纸浆黑液制气化型煤黏结剂研究

利用正交设计法研究纸浆黑液经化学改性制气化型煤黏结剂的工艺技术条件,结果表明:1 000mL纸浆黑液(固体质量分数45%)与80mL有机试剂A在80℃下恒温反应2h,然后升温至95℃,加入30mL有机试剂B,恒温反应1h;最后加入50g无机试剂M,充分搅拌0.5h,得到性能优良的纸浆黑液气化型煤黏结剂。用该黏结剂生产型煤,其抗压强度、落下强度、热稳定性分别为96kg/球、96%、95%,并具有良好的防水性能,完全达到了气化型煤的质量要求。