Synthesis and characterization of arsenate antimonic acid AAAc(1 : 1)

The AAAc(1 : 1) was synthesized in water by As2O3 and Sb2O3 with molar ratio of 1 : 1: AAAc(1 : 1)was characterized by Raman, IR, TG/DTG, DSC, XPS and XRD. The results show that there are four peaks to vsof As-OH, As-O-Sb, Sb-OH and Sb-O-Sb in Raman spectra of AAAc(1 : 1) at 100 - 1 000 cm-1. The solution of AAAc(1 : 1) was also titrated with KOH solution. The titration results show that AAAc(1 : 1) is a hexabasic acid with dissociation constants of k1 = 3.62 × 10-2 , k2 = 3.05 × 10-3 , k3 = 6. 43 × 10-6 , k4 = 9. 78 × 10-8 ,k5 = 1.32 × 10-11 , k6 =3.87 × 10-12. AAAc(1 : 1) has a good solubility and stability in water, its solid obtained by free volatilizing water from its solution under air at ambient temperature is amorphous. Chemical and thermal analyture of AsO ( OH )2-OH-Sb ( OH )4-O-Sb ( OH )4-OH-AsO ( OH )2 or As ( OH )3-O-Sb(OH)4-O-Sb(OH)4-O-As(OH)3 (isomerism) through experimental determination and geometry optimization.     

植酸铜配合物的合成与表征

以植酸为配体合成了两种植酸铜配合物,利用原子吸收法、配位滴定法、元素分析、IR、固体紫外漫反射光谱、热重-差热等分析测试手段,对配合物的组成和结构进行了表征,推测了配合物可能的结构式.植酸分子通过环上的磷羟基氧原子与Cu2+配位,同时Cu2+又与邻近植酸分子中羟基氧原子发生配位,未参加配位的羟基和水或氨可能通过氢键相连,从而形成了结构复杂的难溶性聚合物.     

3（5）-取代-1H-吡唑甲酸及其铜配合物合成与表征

以四种不同的酮类化合物及草酸二乙酯为原料,设计合成了四种3（5）-取代-1H-吡唑甲酸化合物,通过IR及^1H NMR对所合成的化合物结构进行了表征．化合物3a与金属铜离子配位,得到一个双核铜配合物晶体,该晶体属三斜晶系,空间群为P-1,晶胞参数为a=7．082（8）A,b=9．156（10）A,c=25．86（3）A,a=97．088（19）°,β=92．024（18）°,γ=112．649（13）°,V=1529（3）A3,Z=4,Dc=1．597g/cm^3,配合物的晶体结构进一步确证了所合成化合物结构的准确性．     

Synthesis and characterization of polyamides based on dimer acid

A series of dimer acid-based polyamides were synthesized by melt-polycondensation of dimer acid and various aromatic diamines, and were characterized by Fourier transform infrared spectrum (FT-IR) and nuclear magnetic resonance (¹H NMR). The physical properties of the polyamides, such as glass transition temperature, melting temperature, decomposition temperature and mechanical properties were also investigated. The polyamides’ intrinsic viscosity ranges from 1.8 dL·g⁻¹ to 2.2 dL·g⁻¹, and the melting temperature ranges from 140 °C to 181 °C. The glass transition temperatures, observed from dynamic mechanical analysis, fall in the range of 34.8–48.2 °C. The physical and mechanical properties of the resultant polyamides are similar to those of the PA1212. The heat resistance and mechanical properties of poly (4, 4′-diphenylsulfone dimeramide) (PSD) and poly(4, 4′-diphenyl dimeramide) (PPDI) are comparable to those of PA1212.     

Synthesis and Characterization of a Proton-transfer Complex of 1,2,4,5-benzenetetracarboxylic Acid with 1,10-phenanthroline

1Introduction Uptonow,manyproton transfercomplexesofaro maticcarboxylicacidsandLewisbaseshavebeen reported[19].Theproton transferfromorganicacidsto aminesmaytakeplacereadilywithaverylowactivation energyincontrastwiththeattackoftheaminetothecar bonylcarbon…     

偏苯三酸酐酰氯的合成及其结构表征

以偏苯三酸酐(TMA)为反应原料、过量氯化亚砜作溶剂,二甲基甲酰胺(DMF)作催化剂制备了偏苯三酸酐酰氯(TMAC).利用三因素三水平正交实验研究了反应温度、反应时间、氯化亚砜用量3个因素对TMAC合成效率的影响并得到了优化工艺参数:反应温度70℃,反应时间7h,氯化亚砜用量为TMA质量的5倍时,TMAC的产率可高达96.47%.用红外图谱对化合物结构进行了确证:羧基特征峰完全消失,生成了相应的酰氯基团.该合成工艺可操作性强,提高了产物产率、纯度,反应速率,无副产物生成,可直接投入下步反应,对同类有机中间体获得更广泛的应用起到一定的作用.     

新型聚芳酰胺酰亚胺的合成与表征

基于新型邻二苯基取代偏三酸酐合成了粘度在0．39－1．43系列聚芳酰胺酰亚胺，新型无定型聚合物在极性非质子溶剂DMAC，NMP，DMF，DMSO等中有良好的溶解性，其玻璃化转变温度在284－336℃．5%热失重温度大于468℃。     

新型聚芳酰胺酰亚胺的合成与表征

基于新型邻二苯基取代偏苯三酸酐合成了粘度在0.39～1.43系列聚芳酰胺酰亚胺,新型无定型聚合物在极性非质子溶剂DMAC,NMP,DMF,DMSO等中有良好的溶解性. 其玻璃化转变温度在284～336℃. 5 %热失重温度大于468℃.     

含羧酸稀土配合物的合成与表征

采用不同pH条件下,利用邻苯二甲酸氢钾做缓冲溶液,将邻苯二甲酸氢钾和氯化铈稀土溶液在一定条件下进行合成,得到一系列以邻苯二甲酸氢钾为配体的铈一邻苯二甲酸配合物.并通过X射线衍射、红外光谱、紫外光谱、热失重等分析测试方法,对所合成的羧酸稀土助剂(RECar3)的紫外光吸收效果进行表征.结果表明:配合物中的邻苯二甲酸根与Ce(Ⅲ)离子发生了配位,pH为6～7存在着配合物配位方式的转折点,且pH为6时配合物的紫外吸收最强,具有较好的紫外光吸收效果,可用作降解高分子材料助剂使用.     

过渡金属谷氨酸希夫碱配合物的合成及表征

利用模拟酶催化氧化的方法合成了五种谷氨酸希夫碱过渡金属配合物Mn(Glu -Sal)、Fe(Glu-Sal)、Co(Glu -Sal)、Ni(Glu -Sal)、Cu(Glu -Sal) ,对配合物进行了热重———差热分析、红外光谱分析、XPS分析 ,用ICP法测定了配合物的金属含量 ,配合物的结构分析与目标基本吻合。     

Poly（styrene-co-divinylbenzene）-PAMAM-IDA chelating resin： Synthesis,characterization and application for Ni（II） removal in aqueous

PS-PAMAM-IDA chelating resins were prepared by low-generations of polyamidoamine（PAMAM） and then chloroacetic acid functionalizing commercially available ammoniated polystyrene matrix, to preconcentrate Ni2＋ from synthetic aqueous samples. Different generations of PAMAM were used to obtain different chelating resins, PS-IDA, PS-1.0G PAMAM-IDA and PS-2.0G PAMAM-IDA. The synthesized resins were characterized by FTIR and elemental analysis. The effect of solution pH, kinetic studies, resin loading capacity, matrix effects etc., on metal ion adsorption to adsorbent phase, were studied by batch method. The PS-1.0G PAMAM-IDA resin was the most excellent adsorbents, with a maximum adsorption capacity of（24.09±1.79） mg/g for Ni2＋ ion at pH=7. The interpretation of the equilibrium data was given by Langmuir isotherms model, and the correlation coefficient values for PS-IDA, PS-1.0G PAMAM-IDA and PS-2.0G PAMAM-IDA resins were 0.992, 0.994 and 0.987, respectively.     

聚乳酸纤维的合成加工与应用

阐述了聚乳酸的合成方法、聚乳酸纤维的纺丝成型方法、聚乳酸纤维的结构性能及主要应用范围.合成高分子量聚乳酸的主要方法有开环聚合、扩链聚合、溶液聚合及熔融固相聚合等.采用适当高分子量的聚乳酸树脂经干法纺丝或熔融纺丝可以制备聚乳酸纤维,聚乳酸具有高结晶和取向性,除具有特有的生物降解性外,聚乳酸纤维在强度、模量、断裂伸长率等方面可以与聚酯、尼龙等合成纤维相媲美.聚乳酸纤维广泛应用于纺织、卫生医疗、建筑、农林等行业.     

3-溴-1-(3-氯-2-吡啶基)-1H-吡唑-5-甲酸的合成

3-溴-1-(3-氯-2-吡啶基)-1H-吡唑-5-甲酸(V)是合成新型杀虫剂氯虫苯甲酰胺的重要中间体.以2,3-二氯吡啶为起始原料,与水合肼亲核取代制得3-氯-2-肼基吡啶(Ⅰ),Ⅰ与马来酸二乙酯环合制得2-(3-氯-2-吡啶基)-5-氧-3-吡唑烷甲酸乙酯(Ⅱ),Ⅱ经三溴氧磷溴代制得3-溴-1-(3-氯-2-吡啶基...     

(R)-3,3’-二羧酸-1,1’-联萘酚的合成

手性联萘酚及其衍生物是一类重要的有机化合物,广泛应用于不对称合成中。本文以手性联萘酚为原料,三步合成了(R)-3,3’-二羧酸-1,1’-联萘酚,三步总收率达到了68%。最后用红外、紫外和元素分析对中间体和最终产物的结构进行了表征。     

水热法镧-对苯二甲酸二元配合物的合成与表征

利用元素分析（EA）、红外光谱（FTIR）、热分析（DSC-TGA）和扫描电镜（SEM）等分析手段对配合物的组成、尺寸和形貌进行分析与表征.采用水热法合成了树叶状的镧（La）-对苯二甲酸（1,4-bdc）二元配合物.结果表明,对苯二甲酸的羧基氧与La3＋配位,树叶状配合物的组成为La2（1,4-bdc）2.3H2O,树叶状叶片厚度范围约为1～3μm.     

表面羧基可控的单分散P（St-co-AA）亚微球的制备与表征

用无皂乳液聚合法制备了具有不同表面羧基含量的单分散聚（苯乙烯-共-丙烯酸）亚微球,通过扫描电镜和透射电镜测试发现,制得的聚合物微球粒径均一,具有良好的单分散性.结果表明：通过改变聚合过程丙烯酸用量,可以在一定范围内调控共聚物微球的直径;经红外光谱和X射线光电子能谱分析发现,得到的聚合物亚微球表面存在大量羧基;通过X射线光电子能谱可计算出聚合物微球的表面羧基含量,并且该值可以通过在聚合过程中改变丙烯酸用量进行调控.     

Synthesis and fluorescence properties of Tb(Ⅲ) complexes with pyridine-2,6-dicarboxylic acid derivatives

Two novel ligands named 4-styrylpyridine-2,6-dicarboxylic acid (4-SPDA) and 4-(4-(2-(2, 6-dicarboxypyridin-4-yl)-vinyl)styryl)pyridine-2,6-dicarboxylic acid(DSPDA) and their complexes with Tb(Ⅲ) were synthesized and characterized by infrared spectrometry, 1H nuclear magnetic resonance, elemental analysis and gas chromatograph-mass spectrometry. The ligand synthetic route was optimized. The fluorescence properties of the complex in solid state, in different kind of solvents and in solutions with different pH values were investigated in detail. The results show that the yields of DSPDA and 4-SPDA reach over 78% by Wittig-Horner reaction and other eight pyridine-2, 6-dicarboxylic acid derivatives with different substituents on pyridine ring, and their complexes with Tb(Ⅲ) are also obtained. The fluorescence intensities of the complexes with electron-donating groups are more intense than those of the complexes with electron-withdrawing groups on pyridine ring; fluorescence intensities of the complexes are the strongest in neutral solution (pH=7), and the less the dipole moment of solvent molecule is, the stronger the fluorescence intensity is. It is found that the two ligands (4-APDA and DSPDA) are the good sensitizers for Tb(Ⅲ) ion.     

[N(CH_2CH_2CH_2CH_3)_4]_3[AsMo_(12)O_(40)]的合成、晶体结构及磁性研究

合成了有机无机杂化化合物[N(CH2CH2CH2CH3)4]3[AsMo12O40],用X-射线单晶衍射、元素分析、红外光谱和变温磁化率对晶体结构进行了表征.该晶体属于单斜晶系,Pc空间群,a=1.416 48(14)nm,b=1.753 25(17)nm,c=2.280 7(2)nm,β=101.626(2)°,V=5 547.9(9)nm3,Z=2,R1=0.076 5,wR2=0.240 9.在该晶体结构中,带相反电荷的Keggin结构多阴离子[AsMo12 O40]3-簇和四丁基胺阳离子以静电引力结合,并交错排列.     

以乙酰丙酸为原料合成5-羟基乙酰丙酸的研究

对新型聚酯单体5 羟基乙酰丙酸（5-HLA）的合成工艺进行了改进和优化.以来源于生物质资源的乙酰丙酸(LA)为原料，通过改进的溴化和水解反应合成了5-HLA.优化溴化反应温度、液溴滴加速率、反应介质用量等溴化反应条件；同时利用3 溴乙酰丙酸甲酯等溴化物的分子内重排和歧化反应，对溴化反应生成的副产物回收再利用，将中间产物5 溴乙酰丙酸甲酯的产率从文献值30%提高到45%.5-溴乙酰丙酸甲酯经一步水解、乙醚连续萃取和重结晶得到5-HLA.改进后的工艺基于乙酰丙酸的产率为30%，与二步法相比，操作时间短，产率大大提高.     

二对甲苯磺酸乙二醇酯的合成与表征

以对甲苯磺酰氯和乙二醇为原料合成了二对甲苯磺酸乙二醇酯,采用红外光谱和元素分析对其进行了表征,并用X-射线晶体衍射的方法测定了其晶体结构.该晶体属于单斜晶系,C2/c空间群,晶胞参数a=1.071 38（17）nm,b=1.036 80（16）nm,c=1.570 3（2）nm;每个晶胞中所含分子数Z=4,晶体密度计算值Dcalc=1.411 g/cm^3.整个分子结构呈“蝙蝠”状,分子间存在C-H…O弱相互作用.红外光谱和元素分析与实验结果一致.