裂解气相色谱质谱法研究增塑剂邻苯二甲酸二甲酯的热降解机理

用裂解气相色谱-质谱联用方法研究了橡胶产品中使用的增塑剂邻苯二甲酸二甲酯(DMP)在不同温度条件下的热裂解行为.对不同温度条件下裂解产物的分析表明,在初始阶段DMP的裂解产物主要为二氧化碳、苯、甲苯和苯甲酸甲酯.随着温度的升高苯甲酸甲酯进一步裂解成为分子质量更小的自由基,并发生稠环化反应形成更稳定的菲、蒽、间-联三苯、三亚苯等芳香族多环化合物.根据分析实验提供的裂解产物信息和有机物热裂解化学反应的原理对DMP的热裂解反应机理作了探讨,表明在废旧合成橡胶热裂解回收过程中,增塑剂DMP的高温裂解会产生多环芳烃污染物.应选择合适裂解工艺和裂解温度,以减少对环境的污染.     

Mesoporous material as catalyst for the production of fine chemical: Synthesis of dimethyl phthalate assisted by hydrophobic nature MCM-41

Aluminum, iron and zinc containing MCM-41 molecular sieves were prepared by the hydrothermal method. The catalyst was characterized by the XRD, BET (surface area), FT–IR and ²⁹Si, ²⁷Al MAS–NMR techniques. The catalytic activity of these molecular sieves was tested with esterification reaction used with phthalic anhydride (PAH) and methanol (MeOH) in the autoclave at 135 °C, 150 °C and 175 °C. Conversion increases with an increase in temperature and mole ratio. The activity of these catalysts followed the order: Al-MCM-41 (112) > Fe-MCM-41 (115) > Al-MCM-41 (70) > Al-MCM-41 (52) > Fe-MCM-41 (61) > Al, Zn-MCM-41 (104) > Al-MCM-41 (30). The reaction yielded both monomethyl phthalate (MMP) and dimethyl phthalate (DMP). The nature of the catalyst sites has been proposed using with water as an impurity. The selectivity of the dimethyl phthalate increases with increase in temperature and mole ratio. The weight of the catalyst was optimized at 0.07 g. The hydrophilic and hydrophobic nature of the catalyst has been explained by the influence of water and the external surface acidity also facilitates the reaction and this has been confirmed by the supporting reaction.     

SO_4~(2-)/TiO_2固体超强酸新制备方法及其对形成邻苯二甲酸二丁酯的催化活性

建立了用钛白粉制备固体超强酸SO42-/TiO2的新方法.考察了超强酸SO42-/TiO2的制备条件对催化邻苯二甲酸酐和正丁醇酯化反应的催化活性的影响.实验表明,以合成的超强酸为催化剂,在160℃反应4h,邻苯二甲酸二丁酯的产率大于99%.     

相转移催化合成增塑剂BBP和水杨醛的研究

相转移催化合成增塑剂ＢＢＰ和水杨醛的研究郭锡坤，高文华，曾东宇（汕头大学化学系，汕头５１５０６３）关键词相转移催化，季铵盐，聚乙二醇，邻苯二甲酸丁苄酯，水杨醛，增塑剂邻苯二甲酸丁苄酯（增塑剂ＢＢＰ）是一种优良的增塑剂．邻羟基苯甲醛（水杨醛）不仅是重要...     

Convenient and High-Yielding Preparations of Mono(5-carboxy-2-ethylpentyl) Phthalate and its Ring-Deuterated Isomer – The “Third” Major Metabolite of Bis(2-ethylhexyl) Phthalate

Summary. The synthesis of an oxidative major metabolite of bis(2-ethylhexyl) phthalate is described. The target molecule and its ring-deuterated isomer were obtained via acylation of the appropriate -hydroxy benzyl ester or the corresponding carboxylate with phthalic anhydride or phthalic anhydride-d₄. All transformation steps proceed with high yields.     

Synthesis and structure of tetraphenylantimony hydrogen phthalate

Tetraphenylantimony hydrogen phthalate, Ph4SbOC(O)C6H4000H-o, was prepared by the reaction of pentaphenylantimony with phthalic acid. According to the data of X-ray structural analysis, the resulting compound is a trigonal-bipyramidal complex of antimony with three phenyl groups in equatorial positions; the fourth phenyl group and the carboxyl fragment are in axial positions. The CSbO angle is 177.5(1)° the Sb-C(Ph)_eq and Sb-C(Ph)ax distances are 2.099(4)-2.177(4) A and 2.129(4) A, respectively. The H atom of the free carboxyl group and the carbonyl O atom of another carboxylate group form an intramolecular hydrogen bond.DeceasedTranslated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 8, pp. 2082–2085, August, 1996.     

聚酯-聚酯多嵌段共聚物的合成及其动态力学性能

聚酯-聚醚多嵌段共聚物的动态力学性能谱上有两个T_8,不宜做阻尼材料。本文报道聚对苯二甲酸乙二醇酯(PET)-端羟基聚己二酸乙二醇酯(PEA)共聚物(简称嵌段共聚酯),比聚醚-聚酯多嵌段共聚物有更好的相容性。我们研究了PEA的分子量,间苯二甲酸的用量对嵌段共聚酯的结晶度,以及结晶度对嵌段共聚酯的动态力学性能的影响。     

固相萃取-液质联用法同时测定饮用水中双酚A和邻苯二甲酸二丁酯

建立了饮用水中痕量双酚A和邻苯二甲酸二丁酯同时测定的LC/MS-MS快速分析方法.水样中双酚A和邻苯二甲酸二丁酯经HLB固相萃取小柱富集,以V(乙腈)∶V(水)＝90∶10为流动相,选择双酚A m/z 227/212、邻苯二甲酸二丁酯m/z 301/228为检测离子对,利用多反应监测(MRM)和扫描时间分段检测技术实现正、负离子不同扫描模式一次完成.该方法对水样体积为250 mL时双酚A和邻苯二甲酸二丁酯的线性范围为0.4～40 ng/L,检出限分别为0.16和0.10 ng/L,低中高3个不同水平的加标平均回收率均在90%以上.应用于5种不同来源的饮用水及原水中双酚A和邻苯二甲酸二丁酯的测定.     

光电催化降解邻苯二甲酸二乙酯的研究

采用sol-gel法制备TiO2薄膜光电极，以该电极为工作电极，铂丝作对电极，饱和甘汞电极为参比电极，对邻苯二甲酸乙酯的光电催化降解进行了研究。结果表明：该电极具有n型半导体的特征行为，在外加偏压为＋0．7v、pH=2、50mg／L的H2O2中对初始浓度为50mg／L的DEP溶液光照180min降解率达67．85％，讨论了氧的存在、外加偏压等因素对光电催化反应的影响。     

双亲性希土-邻苯二甲酸正十四醇单酯-邻菲咯啉三元配合物的合成、表征、荧光特性及成膜性能

合成了双亲性的铕、铽-邻苯二甲酸正十四醇单酯-邻菲咯啉三元混配配合物，用红外光谱及差热-热重谱进行了表征。考察了发光性能。研究了它们在空气-水界面上的单分子膜行为，结果表明均具有良好的成膜行为。