N－氰基乙亚胺酸乙酯含量的气相色谱分析

采用GC-900气相色谱仪、3%PEG-12000/Chromosorb880AWDMCS填充柱和FID检测器,以水杨酸甲酯为内标物测定N-氰基乙亚胺酸乙酯含量,回收率在98.5%—101.8%之间,标准偏差为0.27%,变异系数为0.27%。     

盐酸小檗碱-环糊精包合物的体外溶出度研究

目的探讨包合技术对中药制剂体外溶出度以及缓释作用的影响。方法选用饱和溶液法生成包合物 ,用DSC证明包合物的生成 ;采用分光光度法 ,考察盐酸小檗碱包合物的体外溶出度和缓释作用。结果 β CD·BH、RM β CD·BH和BH的T50 、Td分别为 5 69.8,740 .2min ;73 .7,10 7.0min和 19.6,2 5 .5min ,包合物的释药数据与t作线性回归方程为 :Y =0 .0 63 9t -0 .473 8,Y =0 .5 5 64t+5 .65 8。结论RM β CD·BH和 β CD·BH的溶出速率明显慢于BH ,具有一定的缓释作用 ,同时RM β CD·BH较β CD·BH具有更好的生物利用度 ;β CD·BH和β CD·BH的体外溶出度与t为一相关性良好的线性方程 ,符合零级释药方程。     

水乳剂用壬基酚聚氧乙烯配磷酸酯的合成

以壬基酚聚氧乙烯醚(TX-10)、P2O5为原料,合成了水乳剂壬基酚聚氧乙烯醚磷酸酯。通过对还原剂用量等因素的讨论,确定最佳工艺条件为:次亚磷酸钠用量为TX-10的0.4%,n(TX-10)∶n(P2O5)∶n(H2O)=2∶1∶0.8,反应温度60℃,反应时间5h。在此条件下产品的酯化率为96.84%。     

对氨基苯甲脒盐酸盐的合成

介绍了以对硝基苯甲腈为原料,经加成、胺化和还原反应合成对氨基苯脒盐酸盐的方法,将加成、胺化与还原反应改用一锅法,产品总收率达到67%。     

Incorporation of different crystallizable amide blocks in segmented poly(ester amide)s

High molecular weight segmented poly(ester amide)s were prepared by melt polycondensation of dimethyl adipate, 1,4-butanediol and a symmetrical bisamide-diol based on ε-caprolactone and 1,2-diaminoethane or 1,4-diaminobutane. FT-IR and WAXD analysis revealed that segmented poly(ester amide)s based on the 1,4-diaminobutane (PEA(4)) give an α-type crystalline phase whereas polymers based on the 1,2-diaminoethane (PEA(2)) give a mixture of α- and γ-type crystalline phases with the latter being similar to γ-crystals present in odd-even nylons. PEA(2) and PEA(4) polymers with a hard segment content of 25 or 50 mol% have a micro-phase separated structure with an amide-rich hard phase and an ester-rich flexible soft phase. All polymers have a glass transition temperature below room temperature and melt transitions are present at 62-70 °C (T_m,1) and at 75-130 °C (T_m,2) with the latter being highest at higher hard segment content. The two melt transitions are ascribed to melting of crystals comprising single ester amide sequences and two or more ester amide sequences, respectively. These polymers have an elastic modulus in the range of 159-359 MPa, a stress at break in the range of 15-25 MPa combined with a high strain at break (590-810%). The thermal and mechanical properties are not influenced by the different crystalline structures of the polymers, only by the amount of crystallizable hard segment present.     

环丙烷甲酰氯的合成

环丙烷甲酸异丙酯因异丙基的位阻很大，所以其很难水解，即使加热回流12h，得率也只有68．6％，选用合适的相转移催化剂使得率超过了84％。由环丙烷甲酸制备环丙烷甲酰氯比较简单，文献报道得率为94．08％，通过对其合成条件的优化，使得率超过了97．2％。     

SO_4~(2-)/ZrO_2-Al_2O_3催化合成脂肪酸季戊四醇酯的研究

以脂肪酸和季戊四醇为原料,三甲苯为带水剂,SO42-/ZrO2-Al2O3固体超强酸催化,合成脂肪酸季戊四醇酯。实验结果表明,控制酯化温度(180～200)℃、醇酸物质的量比为1∶5.6、催化剂加入量为原料总量的0.9%和反应时间为4h时,可获得最佳反应结果,酯化率达99.88%。IR谱表明,产品中羟基吸收峰基本消失,证明酯化反应较充分和完全。     

Polymer pendant ligand chemistry, 4. Recovery of precious metal ions from strongly acidic solution with a polymer-supported o-phenylenediamine hydrochloride ligand

We report on the synthesis and reactivity of a polymer-supported o-phenylenediamine hydrochloride ligand, PS-PDHC, using macroporous 6% crosslinked polystyrene-divinylbenzene beads. The PS-PDHC ligand was found to be highly selective to AuCl₄⁻ ions in strongly acidic solutions in the presence of other precious metal ions, PdCl₄²⁻, PtCl₄²⁻, RhCl₆³⁻, and RuCl₅²⁻ (selectivity values: 2.5, Au/Pd; 7.5, Au/Pt; 7, Au/Rh; 2.2, Au/Ru) as well as other transition metal ions, Fe ³⁺, Cr³⁺, CU²⁺, Nit+, and Mn²⁺. The sorption capacity, selectivity, kinetics of removal and recovery, and solution isotherms have been determined for AuCl₄⁻ ions in competition with the above-mentioned metal ions. The relative ease of formation of the anionic complex in 0.5 M HCI, AuCl₄⁻ was thought to be the primary reason for its selective ability to bind to the PS-PDHC ligand by an anion-exchange mechanism. Therefore, the effect of the HCI concentration on the kinetics of AuCl₄⁻ ion removal from solution was also investigated to clearly show that raising the pH from 0 to 5 caused a dramatic decrease in rate. The AuCl₄⁻ ion can be recovered quantitatively from the PS-PDHC beads using a 5% thiourea solution in 0.1 M HCl, allowing the polymer-supported ligand to be reused.     

环氧乙烯基酯树脂 (Ⅱ)环氧乙烯基酯树脂在酸、碱、盐溶液中的稳定性

较为详细论述了影响环氧乙烯基酯树脂在酸、碱、盐溶液中稳定性的各种结构因素。     

Fuel properties and emissions of soybean oil esters as diesel fuel

The effects of using blends of methyl and isopropyl esters of soybean oil with No. 2 diesel fuel were studied at several steady-state operating conditions in a four-cylinder turbocharged diesel engine. Fuel blends that contained 20, 50, and 70% methyl soyate and 20 and 50% isopropyl soyate were tested. Fuel properties, such as cetane number, also were investigated. Both methyl and isopropyl esters provided significant reductions in particulate emissions compared with No. 2 diesel fuel. A blend of 50% methyl ester and 50% No. 2 diesel fuel provided a reduction of 37% in the carbon portion of the particulates and 25% in the total particulates. The 50% blend of isopropyl ester and 50% No. 2 diesel fuel gave a 55% reduction in carbon and a 28% reduction in total particulate emissions. Emissions of carbon monoxide and unburned hydrocarbons also were reduced significantly. Oxides of nitrogen increased by 12%.