光稳定剂间苯二酚单苯甲酸酯的合成

研究了以苯甲酰氯和间苯二酚为原料、液碱为除酸剂,酯化合成然后精制得间苯二酚单苯甲酸酯的工艺.研究了酯化反应中温度、物料配比、pH、间苯二酚水溶液的浓度和反应时间等条件对反应的影响,获得了较佳的酯化工艺条件:苯甲酰氯与间苯二酚的摩尔比为1.15∶1;pH值为7.5;反应温度为25℃;反应时间为1.5 h;间苯二酚溶液的质量分数为10%.酯化反应收率为88.6%.考察了结晶溶剂配比、温度对产品质量和收率的影响,经实验评估得到了较佳的结晶工艺条件:结晶溶剂甲苯的体积(/mL)与初产物的质量(/g)之比为2.5∶1,结晶温度为30℃,结晶收率为95.0%.优化工艺条件下产品的总收率为84.2%.     

Mineralization of flue gas CO2 with coproduction of valuable magnesium carbonate by means of magnesium chloride

CO2 mineralization and utilization is a new area for reducing the CO2 emissions. By reacting with natural mineral or industrial waste, CO2 can be transformed into valuable solid carbonate （such as calcium carbonate or magnesium carbonate） with recovery of some products simultaneously. In this paper, a novel method was proposed to mineralize CO2 by means of magnesium chloride with small energy consumption. In this method, magnesium chloride was firstly transformed into magnesium hydroxide by electrolysis. The formed magnesium hydroxide showed high reactivity to mineralize CO2. In our study, even at low concentration, CO2 can be effectively mineralized by this method, which makes it possible to directly mineralize flue gas CO2, avoiding the expensive process of CO2 capture and purification. Moreover, valuable products such as hydromagnesite and nesquehonite can be recovered by this method. Because of the wide distribution of magnesium chloride in nature, largescale CO2 mineralization is potential by means of magnesium chloride.     

Identification of proteinaceous binding media for the polychrome terracotta army of Emperor Qin Shihuang by MALDI-TOF-MS

A proteinaceous binding media for the polychrome terracotta army of Emperor Qin Shihuang has been identified using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry(MALDI-TOF-MS).Methods for the preparation of the model samples and the elimination of interferences have been evaluated,as well as ageing processes.A method involving the complexation of EDTA in combination with dialysis was used to eliminate any interference in the polychrome layers taken from the historical samples.The model samples were aged by being buried in loess to replicate the ageing process of the historical samples as closely as possible.The optimum conditions for the extraction and subsequent enzymatic hydrolysis of the extracted protein were investigated.Under the optimized conditions,the‘‘peptide mass fingerprints’’of the proteinaceous binding media from the historical and model samples were determined by MALDITOF-MS.The results revealed that animal glue was used as the binding media for the polychrome layers of Emperor Qin Shihuang’s terracotta army.It also shows that animal glue used as binding media has a long history in China.     

氯化氢催化氧化反应器材质研究

选取哈氏C-2000、哈氏C-4、Inconel600、Incoloy825、316 L、Ni-6及纯Ta等7种有代表性的金属材料,开展了耐腐蚀性评价实验。根据实验前后挂片失重率与厚度变化情况及挂片在催化氧化反应体系中的腐蚀速率,确定了不同金属材料在氯化氢催化氧化反应体系中的耐腐蚀性。实验表明,Ta耐腐蚀性能最好,耐腐蚀率为0.309 3 g/(dm2·月)、0.053 0 mm/年;其次为Inconel 600,耐腐蚀率为0.566 8 g/(dm2·月)、0.230 2 mm/年。     

Ga(Ⅲ)在罗丹明B和丙醇的水溶液中与Zn(Ⅱ)、Al(Ⅲ)、Ir(Ⅳ)、Rh(Ⅲ)、V(Ⅴ)和Ti(Ⅳ)的绿色萃取分离

丙醇水溶液在氯化钠的作用下可分成醇-水两相,在分相过程中,GaCl4-与罗丹明B(RhB)生成的[GaCl4-][RhB+]能被丙醇相完全萃取.当溶液中丙醇和罗丹明B的浓度分别为30%(v/v),0.3 g/L时,Ga(Ⅲ)的萃取率达到97.8%以上,而Zn(Ⅱ)、Al(Ⅲ)、Ir(Ⅳ)、Rh(Ⅲ)、V(Ⅴ)和Ti(Ⅳ)基本不被萃取,实现了Ga(Ⅲ)与上述金属离子的分离.     

功能化PVDC负载钯配合物在微波促进下催化Suzuki反应

聚偏二氯乙烯(PVDC)被二乙烯三胺(DETA)修饰后可以有效负载氯化钯,从而制得催化剂PVDC-DETA-Pd.利用IR、TG、XPS等测试手段对其结构进行了表征.热分析表明,催化剂在室温至200℃有很好的热稳定性.该催化剂在微波促进条件下有良好的催化性能,可以催化各种芳基卤化物和四苯硼钠间的Suzuki反应.并且催化剂回收再利用5次后,产率仍能达到75%.     

N,N-二甲基甲酰胺催化的吡唑亲电/亲核氯代反应

在N,N-二甲基甲酰胺(DMF)催化下,用氯化亚砜氯代1-苯基-5-(4-甲基苯基)-1H-3-羟基吡唑(1a),以83%的高产率获得了4-氯-1-苯基-5-(4-甲基苯基)-1H-3-羟基吡唑(2a),用高效液相色谱(HPLC)跟踪反应,得出最佳反应条件为:n(1a)∶n(DMF)=10∶1,在SOCl2中回流4 h,并分离得到单质硫,提出了DMF催化的吡唑亲电/亲核氯代机制。通过合成系列吡唑底物1b~1h,研究了氯代机制的普适性,其氯代产物2b~2h经核磁共振氢谱(1H NMR)、核磁共振碳谱(13C NMR)和元素分析表征,并用X线衍射法测定了2d的晶体结构。该氯代反应操作简单、官能团相容性好。     

超声雾化液体除湿系统对室内空气品质的影响

研究了超声雾化液体除湿空调系统对室内空气品质的影响,得到室内空气中氯化锂质量浓度的安全阈值为70μg/m~3.通过实验分析了入口溶液中氯化锂的质量分数(w_i)、除雾器孔隙率等对空气带液量的影响.当w_i由31.5%上升至38.8%时,空气带液量也随之上升,最高为26.93μg/m~3.除雾器的孔隙率显著影响空气带液量,应使用孔隙率低于93.5%的丝网除雾器.在最不利工况下,该系统空气带液量未超过安全阈值,表明对室内空气品质没有影响.研究成果对超声雾化液体除湿系统的推广有一定指导意义.     

既有混凝土码头的时变氯离子扩散过程

为了研究不同暴露环境(大气区、潮差区和浪溅区)对氯离子在混凝土中传输的影响,以及氯离子扩散过程的时变特性,对北部湾某码头的混凝土现场耐久性进行了检测,得到了不同深度混凝土试样的自由氯离子浓度.结果表明,在同一侵蚀深度,浪溅区的氯离子浓度最大,潮差区的次之,大气区的最小,拟合得到的表面氯离子浓度和表观氯离子扩散系数亦表现出了相同特性;浪溅区是影响临海钢筋混凝土结构耐久性的最不利暴露环境;氯离子扩散系数随侵蚀时间递减,时间参数为服从正态分布的随机变量,大气区、潮差区和浪溅区时间参数的均值分别为0.19,0.36和0.43;在钢筋混凝土结构的耐久性分析中应考虑氯离子扩散系数的时变特性.     

含均三嗪结构苯并噻唑类化合物的合成和晶体结构

以三聚氯氰等为原料合成了一种含均三嗪结构苯并噻唑类化合物（HY），并通过X射线单晶衍射对其结构进行了表征。结果表明：HY属于单斜晶体，空间群为P2（1）／”。晶胞参数为：Z=4，a=1．4278（17）nm，b=1．6690（2）nm，c=1．44842（17）nm，α=90°，β=102．707（2）°，），γ=90°，V=3．3655（7）nm^3；R1=0．0755；wR2=0．2161。