新型防霉剂富马酸二甲酯的合成及抑菌试验研究

本文讨论了以马来酸酐为原料，在复合催化剂存在下，一步合成食品及饲料新型防霉剂富马酸二甲酯的最佳反应条件，结果证明本法具有原料价廉易得，工艺流程简单、反应时间短，产率高，纯度高，甲醇损失少，易于实现工业化等优点，通过对富马酸二甲酯与苯甲酸钠，山梨酸钾，丙酸钙，尼泊金乙酯及内酯及丙酯等的抑菌效果比较，结果表明富马酸二甲酯对多种霉菌、酵母菌及细菌有较强的抑制作用。     

Ti(SO4)2/C催化合成邻苯二甲酸二异戊酯(DIAP)

研究了Ti(SO4 ) 2 /C在邻苯二甲酸酐和异戊醇酯化中的催化性能 ,结果表明 ,Ti(SO4 ) 2 /C在该反应中具有较高的催化活性 ,并得到了合成邻苯二甲酸二异戊酯的新工艺条件是 :催化剂用量 (邻苯二甲酸酐质量分数 )为 5 % ;异戊醇 0 5mol,邻苯二甲酸酐 0 2mol,反应温度 185℃ ,反应时间 180min ,在此条件下收率可达 95 %。     

One Novel Red-luminescent Coordination Polymer of Eu-p-benzenedicarboxylate with Nitrogen-donor-containing Lewis Base

The crystal structure of novel coordination polymer with excellent characteristic luminescence of Eu^3 ,the three-dimentional network of {Eu2(p-BDC)3(Phen)2(H2O)2}n is presented.     

气相色谱／质谱联用法测定皮革中的富马酸二甲酯

本文研究了用气相色谱一质谱法测定皮革中富马酸二甲酯（DimethylFumamte）含量的方法。探讨了样品测定过程中有关条件的变化对测定的影响．优化了部分条件。结果表明：方法线性范围在0．05—1．Oppm,相关系数为0．999,方法的检测下限为0．1mg／kg,回收率在85％-95％。所建方法能很好地应用于皮革中富马酸二甲酯的检测。     

TiO2/N可见光光催化降解邻苯二甲酸二甲酯

采用氮掺杂的二氧化钛为催化剂,探索了可见光催化氧化降解邻苯二甲酸二甲酯(DMP)的研究.系统地考察了光催化降解反应中DMP的初始浓度、光照时间、催化剂的量、pH值等因素对邻苯二甲酸二甲酯(DMP)的降解效率及速率的影响;同时对其光降解动力学及光降解过程中的矿化程度进行了一定的分析.结果表明,只有在催化剂和光源同时存在的情况下,DMP才有比较好的降解效果.当DMP的初始浓度为10 mg/L时,在优化条件下,即光催化剂为量1 g/L,pH值为6.20时,在以500W氙灯下进行光照8h,其降解率可达到90%以上.此光催化降解反应过程符合一级反应动力学.     

气相色谱-质谱法快速测定食品塑料包装材料中的邻苯二甲酸二(2-乙基己)酯

建立了气相色谱–质谱法检测食品塑料包装材料中邻苯二甲酸二(2-乙基己)酯含量的分析方法。比较了水浴振荡提取法、超声提取法、索氏提取法和微波辅助萃取法对测定结果的影响。实验结果表明,在微波辅助萃取条件下,样品中邻苯二甲酸二(2-乙基己)酯的检出限为0.02 mg/kg,测定结果的相对标准偏差为1.58%～1.74%(n=5),加标回收率为89.0%～98.4%。该方法具有操作快速简便、精密度好、检出限低和准确度高等优点,适用于食品塑料包装材料中邻苯二甲酸二(2-乙基己)酯含量的测定。     

一种2,5–取代的吡啶类药物中间体的合成

吡啶衍生物因其独特的化学结构,已被作为一类合成子广泛地应用于药物中间体的构建。以2,5–吡啶二甲酸二甲酯为原料,通过水解、酰化和还原等反应合成了一种新的2,5–取代的吡啶类药物中间体。     

3,4-二芳基吡咯的合成

卟啉化合物及其金属配合物是一类极具潜力、环境友好的光电转换材料而成为国际上人们研究的热点,3,4-二芳基吡咯作为构建该卟啉类化合物的中心体,其合成方法的研究很少。本文以亚氨基二乙酸为原料,经酯化和酰基化2步反应得到N-乙酰基-亚胺基二乙酸二甲酯,再将得到反应物在甲醇钠溶液中与二芳基乙二酮发生缩合反应得到3,4-二芳基吡咯-2,5-二甲酸,最后将3,4-二芳基吡咯-2,5-二甲酸在乙醇胺中回流脱羧制得3,4-二芳基吡咯,其结构经1H NMR、13C NMR和元素分析得以确证。该合成方法具有反应条件温和、反应速度快、产率较高、操作简单等优点。     

CoMn@NC催化5-羟甲基糠醛常压氧化为2, 5-呋喃二甲酸二甲酯

Dimethyl furan-2, 5-dicarboxylate (DMFDCA) is a valuable biomass-derived chemical that is an ideal alternative to fossil-derived terephthalic acid as a monomer for polymers. The one-step oxidation of 5-hydroxymethylfurfural (HMF) to DMFDCA is of practical significance. It not only shortens the reaction pathway but also avoids the separation process of intermediates; thus, reducing cost. In this work, non-noble bimetallic catalysts supported on N-doped porous carbon (CoMn@NC) were synthesized via a one-step co-pyrolysis procedure using different pyrolysis temperatures and proportions of metal precursors and additives. We employed the prepared CoMn@NC catalysts in the aerobic oxidation of HMF under mild reaction conditions to obtain DMFDCA. High-yield DMFDCA was obtained by screening the prepared catalysts and optimizing the reaction conditions, including the strength and amount of the base, as well as the reaction temperature. The optimized yield of DMFDCA was 85% over the Co₃Mn₂@NC-800 catalyst after 12 h at 50 ℃ using ambient-pressure oxygen. The physicochemical properties of the catalysts were determined using a variety of characterization techniques, the factors affecting the performance of each catalyst were investigated, and the relationship between the physicochemical properties and performance of the prepared catalysts was elucidated. A porous structure with a high surface area had a positive effect on mass transfer efficiency. Cobalt nanoparticles (NPs) and atomically dispersed Mn were coordinated to N-doped carbon to form M―N_x (where M = Co or Mn). Based on the Mott-Schottky effect, there was significant electron transfer between each metal and the N-doped carbon, additionally, the metal NPs supplied electrons to the carbon atoms. The electron-deficient metal site in the pyridinic N-rich carbon was beneficial for the activation of HMF and oxygen. The activation of oxygen produced reactive oxygen species (such as superoxide radical anions) to ensure high selectivity to DMFDCA through dehydrogenative oxidation of the hemiacetal intermediate and hydroxymethyl group of 5-hydroxymethyl-2-methyl-furoate. The existence of disordered and defective carbons increased the number of active sites. Subsequently, we performed a series of control experiments. Based on our current experimental results and previous studies, we propose a simple mechanism for the aerobic oxidation of HMF to DMFDCA. The catalyst was stable, its performance decreased slightly after two cycles, and it was tolerant to SCN⁻ ions and resistant against N or S poisoning. Furthermore, the use of this catalytic system can be expanded to various substituted aromatic alcohols, such as benzyl alcohols with different substituents, furfuryl alcohol, and heterocyclic alcohols. Simultaneously, the product type was further extended from methyl esters to ethyl esters with a high yield when the substrate reacted with ethanol. In conclusion, this catalytic system can be applied in the production of carboxylic esters for polymers.     

酯交换法合成2,6-萘二甲酸乙二醇酯动力学研究

2,6-萘二甲酸二甲酯和乙二醇酯交换反应为探针反应,研究了催化剂种类及其用量、乙二醇/2,6-萘二甲酸二甲酯摩尔比对探针反应动力学影响。实验结果表明,2,6-萘二甲酸二甲酯和乙二醇酯交换反应不是单纯地遵循二级反应动力学。催化剂种类、用量以及乙二醇/2,6-萘二甲酸二甲酯摩尔比均对探针反应动力学方程有影响。