尾式吡啶基金属卟啉配合物的合成与表征

合成了一种新的尾式卟啉５－邻［４－（３－吡啶氧基）丁氧基］苯基－１０,１５,２０－三苯基卟吩（简称ｏ－ＰｙＴＰＰ）,并以ｏ－ＰｙＴＰＰ为配体合成了金属铁卟啉ｏ－ＰｙＴＰＰＦｅ（Ⅲ）Ｃｌ和金属锰卟啉ｏ－ＰｙＴＰＰＭｎ（Ⅲ）Ｃｌ。通过元素分析、质谱、紫外可见光谱、红外光谱、核磁共振氢谱、顺磁共振波谱等手段进行了表征,结果表明,三价金属卟啉处于高自旋状态。     

三元乙丙橡胶-g-2-丙烯酰胺-2-甲基丙磺酸的制备与表征

采用反相乳液聚合法制备了三元乙丙橡胶-g-2-丙烯酰胺-2-甲基丙磺酸(EPDM-g-AMPS),考察了反应条件对接枝共聚物接枝率的影响,并用傅里叶变换红外光谱对EPDM-g-AMPS进行了表征。结果表明,在反应温度为55℃、反应时间为4 h、引发剂质量分数为0.8%、EPDM/AMPS(质量比)为1以及AMPS中和度为110%的条件下,所得共聚物为EPDM-g-AMPS,其接枝率最大为19%,且乳液的综合性能较好。     

Preparation and characterization of carbon-sulfur surface compounds

Carbon-sulfur surface compounds (C_χS), in which sulfur is chemically bound, have been prepared with a sulfur content greater than 30 wt.%. X-Ray diffractometry and electron microscopy show that the structure of the material is similar to that of disordered carbons. C_χS compounds are chemically stable in base and after an initial loss of several per cent of sulfur, they are stable in strong acids such as HCl and HNO₃. In inert atmosphere, no measurable loss of sulfur was detected after being heated to 700°C. The XPS spectra (C_1s,: 284.3 eV; S2p3/2: 163.7 eV) and the Fourier transform IR absorption spectra (1180,1550 cm^?1) of CχS materials indicate no significant charge separation in carbon-sulfur bonds. Furthermore, these results suggest that, on CχS, carbon-sulfur surface groups exist in the form of thiocarbonyls,

C and thiolactones,

C, analogous to carbonyls and lactones existing on activated carbons.     

纳米铜-镁-铝类水滑石的制备与表征

采用恒定pH低过饱和共沉淀法制备纳米铜-镁-铝类水滑石,采用单因素试验得出最佳反应工艺条件。在超声波反应器中反应,恒定pH=7.5~9.0,n(铜+镁)/n(铝)=2.0~4.0,n(铜)/n(镁)=0.25~1.0的条件下,采用冷冻干燥法可得到晶相单一的铜-镁-铝类水滑石,且制得的产物晶面生长的有序程度高,结晶度好。采用X射线衍射(XRD)、红外光谱(FT-IR)和扫描电镜(SEM)对其进行表征,大多数分子粒度为纳米级尺寸,粒径为50 nm左右。     

Preparation and characterization of carbon based acid catalysts for the dehydration of 2-propanol

The catalytic conversion of 2-propanol on carbon based acid catalysts obtained by chemical activation of lignocellulosic waste with H₃PO₄ was investigated. The carbon acid catalysts were prepared in a single step, without the need for incorporating acid surface groups in a complementary step by chemical oxidation of the carbon surface. The porous structure was characterized by N₂ and CO₂ adsorption, showing a strong dependence on the impregnation ratio. The surface chemistry was studied by XPS and TPD. A significant amount of phosphorus remains on the catalysts surface, as phosphate and/or polyphosphate esters, stable at relatively high temperature (<700 °C), despite the washing process carried out during the preparation of the catalysts. The total acidity and acid strength distribution were determined by NH₃-TPD. The conversion of 2-propanol yielded only dehydration products, mainly propylene with very low amounts of di-isopropyl ether, confirming the acidic nature of the catalyst sites. The amount and strength of acid sites affected the catalytic activity but did not change significantly the apparent activation energy of the dehydration reaction. The catalysts were stable at the operation conditions. The presence of water vapor did not affect significantly the conversion and the product distribution.     

纳米TiO_2的制备、表征及光催化降解酸性品红

以钛酸四正丁酯为原料,采用溶胶-凝胶法制备了纳米TiO2粒子,对其进行了TG-DTA,XRD,TEM和BET分析,并分别在紫外光和可见光下考察了其光催化降解酸性品红性能。结果表明,自制的纳米TiO2对酸性品红具有很好的光催化降解脱色能力,500℃的样品在紫外光下,20 min内即可将200 mg/L的酸性品红溶液完全降解脱色,在可见光下,210 min内酸性品红的脱色率达80%。     

Preparation and characterization of the poly(2-hydroxyethyl methacrylate)–salicylic acid conjugate

A new polymeric system containing hydrolysable ester bond linked to salicylic acid to be used for controlled drug release was synthesized. Poly(2-hydroxyethyl methacrylate) (PHEMA) functionalized with chloroacetate groups was obtained by the reaction between PHEMA and chloroacetyl chloride using the N,N-dimethylacetamide/5% lithium chloride system as a solvent and pyridine as a catalyst. The degree of substitution was calculated from the chlorine content and ranged from 32.2 to 98.1 mol.% depending on the ratio of chloroacetyl chloride to PHEMA. The coupling of salicylic acid to PHEMA functionalized with chloroacetate groups was carried out by the reaction between PHEMA and the sodium salt of salicylic acid. The structures of chloroacetylated PHEMA and PHEMA–salicylic acid conjugates were determined by means of FTIR, ¹H-NMR and ¹³C-NMR spectra. The hydrolysis in the heterogeneous system of PHEMA–salicylic acid conjugates were performed in buffer solutions (pH 7.6 and 8.5) at 37 °C and showed that the release of the drug (sodium salicylate) from tablets was dependent on the hydrophilic character of conjugate as well as on the pH value of the medium.     

聚乳酸共混膜的制备与表征

以聚乳酸(PLA)为膜基材、动物油或植物油为添加剂、二氯甲烷为溶剂,通过流延法制备聚乳酸共混膜。考察添加剂种类、添加剂与PLA的质量比对膜的表面结构与相关性能的影响。结果表明:制备的聚乳酸共混膜具有"海岛"结构;随着添加剂与PLA质量比值的增大,共混膜的"岛径"、接触角、弹性模量、渗析系数和铵根离子的累积渗透量均呈现有规律性的变化,具有良好的可调节性,在包膜缓控释肥料领域具有发展潜力。     

透明质酸自组装聚合物胶束的制备及表征

为了增强抗肿瘤药物的靶向性与抗肿瘤活性,本文制备了透明质酸-十八烷聚合物,用其对阿霉素进行包载,考察其理化性质及体外细胞毒性。合成两亲性透明质酸-十八烷聚合物,利用核磁对其结构进行确证。选择超声法制备载阿霉素的聚合物胶束,考察胶束的粒径、电位、包封率、载药量以及体外释放行为。选择乳腺癌细胞MCF-7为肿瘤细胞模型,考察载药胶束的体外抗肿瘤活性。成功合成了透明质酸-十八烷聚合物。制备的空白胶束和载药的胶束的粒径分别为（180.7±1.25）nm和（178.3±2.24）nm,Zeta电位分别为（-21.3±0.25）mV和（-18.1±0.31）mV。载阿霉素聚合物胶束的包封率为（96.1%±0.72%）,载药量为16.1%±1.18%,体外释放行为表明在72h的累计药物释放率仅为40%左右,具有明显的缓释行为。体外细胞毒性结果表明,空白聚合物胶束对肿瘤细胞几乎没有毒性,而载阿霉素的聚合物胶束具有较好的抗肿瘤活性。结论：透明质酸-十八烷聚合物胶束可以有效地包载抗肿瘤药物阿霉素,具有良好的缓释特性和抗肿瘤活性。     

硫酸改性高岭土的制备及表征

为了对比高岭土改性前后的结构变化,将鄂尔多斯高岭土分别用10%、20%、30%、40%、50%的硫酸进行改性,得到酸改性高岭土样品。采用IR、XRD、SEM、BET、EDS等对样品进行表征分析。结果表明,由于硫酸的吸水性,随着酸浓度的增加,脱除高岭土中吸附水的能力越强;酸改性浓度的变化对高岭土的结构影响不大;改性后的高岭土比表面积减小,表面粗糙度增加,密集堆积,凝结成块状,有堆积孔道出现;硫酸改性会使高岭土中大量的铝被浸出。     

Polylactic acid/epoxidized palm oil/fatty nitrogen compounds modified clay nanocomposites: Preparation and characterization

Clay modification was carried out by treatment of fatty nitrogen compounds (FNCs); fatty hydrazide (FH), hydroxy methyl fattyamide (HMFA), and difatty acyl thiourea (DFAT) were synthesized from vegetable oils with a sodium montmorillonite (MMT) as natural clay. This process was accomplished by stirring the clay particles in an aqueous solution of FH, HMFA, and DFAT, by which the clay layer thickness increased from 1.23 to 2.69, 2.89 and 3.21 nm, respectively. The modified clay was then used in the preparation of the polylactic acid/epoxidized palm oil (PLA/ EPO) blend nanocomposites. The interaction of the modifier in the clay layer was characterized by X-ray diffraction (XRD) and Fourier transform infrared (FTIR). Elemental analysis was used to estimate the presence of FNCs in the clay. The nanocomposites were synthesized by solution casting of the modified clay and a PLA/EPO blend at the weight ratio of 80/20, which has the highest elongation at break. The nanocomposites were then characterized using XRD, transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and tensile properties measurements. Improvement in mechanical properties of the FH-MMT, HMFA-MMT, and DFAT-MMT nanocomposites was obtained when 2% of the DFAT-MMT and 3% of both FH-MMT and HMFA-MMT loadings were used. PLA/EPO modified clay nanocomposites show higher thermal stability in comparison with those of the PLA/EPO blend. The XRD and TEM results confirmed the production of nanocomposites.     

Preparation and characterization of a novel series of amphiphilic phospholipids compounds

For application of phospholipids compounds in drug permeation field, a novel series of amphiphilic phospholipids compounds containing different aliphatic chains as the hydrophobic tail groups and phosphorylcholine as the hydrophilic head groups were synthesized in three steps: preparation of hydroxyalkyl methacrylate by the reaction of various aliphatic chain diols with α‐methacryloyl chloride; preparation of 2‐(2‐oxo‐1,3,2‐dioxaphospholoyloxy)alkyl methacrylate by the reaction of hydroxyalkyl methacrylate with 2‐chloro‐2‐oxo‐1,3,2‐dioxaphospholane; preparation of the amphiphilic phospholipids compounds by the ring‐opening reaction of 2‐(2‐oxo‐1,3,2‐dioxaphospholoyloxy)alkyl methacrylate in the presence of trimethylamine. The chemical structure of the amphiphilic phospholipids compounds were supported by Fourier transform infrared spectroscopy and ¹H NMR. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

新型钆石墨层间化合物复合材料的制备及表征

通过Hummers法制备氧化石墨,并以化学吸附法将氯化钆（GdCl3）饱和溶液中的钆离子引入氧化石墨（GO）,合成新型水合碳酸氧钆-氧化石墨层间化合物复合材料。采用XRD、FT-IR和TG-DTA对产物进行分析表征。表明,制备水合碳酸氧钆-氧化石墨层间化合物的最佳质量配比为m（Gd2O3）∶m（EG）=5∶1。通过TG-DTA分析确认,水合碳酸氧钆-氧化石墨层间化合物的还原温度为480℃。     

Synthesis, structure characterization and photocatalytic properties of two new uranyl naphthalene-dicarboxylate coordination polymer compounds

Two new uranyl-organic coordination compounds, UO₂(NDC)[(CH₃)₂SO)]₂ (1) and [UO₂(NDC)(CH₂OH)₂] (2) (H₂NDC = 1,4-naphthalene dicarboxylate), have been synthesized from the solutions of dimethyl sulfoxide (DMSO) and ethylene glycol (EG), respectively, through a volatilization method. Single-crystal X-ray diffraction analyses show that compound 1 consists of novel straight chains modified by pairs of DMSO molecules, whereas compound 2 features one-dimensional zigzag chains which are cross-linked by non-coordinating solvent molecules through hydrogen bonding interactions, forming a two-dimensional network. Both 1 and 2 decompose rhodamine B (RhB) molecules efficiently under the irradiation of UV and visible light.     

十二烯基琥珀酸环糊精酯的制备及其性能测定

为制备一种绿色乳化剂产品，采用湿法工艺以十二烯基琥珀酸酐（DDSA）和β-环糊精（β-CD）为原料成功制备十二烯基琥珀酸环糊精酯（DDS-β-CD）。通过傅里叶变换红外光谱（FT-IR）对DDS-β-CD结构进行了表征；热重分析（TGA）发现DDS-β-CD的热稳定性与β-CD相比有所降低，但是起始分解温度仍高达225 ℃，满足其在食品、日化、微胶囊等领域的应用；当DDS-β-CD的取代度大于0.198时，所测样品质量分数为6%的水溶液透光率仍可达97%以上。取代度为0.295的DDS-β-CD的亲水亲油平衡值（HLB）为16.520，说明其具有一定的起泡能力和乳化能力：泡沫稳定性较好为79.08%；对植物油和液体石蜡的乳化性能分别为991 s和545 s；DDS-β-CD质量分数为0.5%时的水包植物油乳液的起始平均粒径为4.42 μm，并具有良好的稳定性。     

葡萄糖炭基固体酸催化剂的制备与表征

利用固体葡萄糖进行炭化、磺化制备炭基固体酸催化剂,将其应用于甲醇与油酸的反应中。结果表明,在200℃下炭化2 h,130℃磺化2 h,油酸的转化率高达95.79%。有着良好的催化效果,并对催化剂进行了XRD、SEM、BET表征,结果表明,该催化剂为表面不规则以大孔为主的不定型炭。     

葡萄糖炭基固体酸催化剂的制备与表征

利用固体葡萄糖进行炭化、磺化制备炭基固体酸催化剂,将其应用于甲醇与油酸的反应中。结果表明,在200℃下炭化2 h,130℃磺化2 h,油酸的转化率高达95.79%。有着良好的催化效果,并对催化剂进行了XRD、SEM、BET表征,结果表明,该催化剂为表面不规则以大孔为主的不定型炭。     

十二烯基琥珀酸环糊精酯的制备及其性能测定

为制备一种绿色乳化剂产品,采用湿法工艺以十二烯基琥珀酸酐（DDSA）和β-环糊精（β-CD）为原料成功制备十二烯基琥珀酸环糊精酯（DDS-β-CD）。通过傅里叶变换红外光谱（FT-IR）对DDS-β-CD结构进行了表征;热重分析（TGA）发现DDS-β-CD的热稳定性与β-CD相比有所降低,但是起始分解温度仍高达225 ℃,满足其在食品、日化、微胶囊等领域的应用;当DDS-β-CD的取代度大于0.198时,所测样品质量分数为6%的水溶液透光率仍可达97%以上。取代度为0.295的DDS-β-CD的亲水亲油平衡值（HLB）为16.520,说明其具有一定的起泡能力和乳化能力：泡沫稳定性较好为79.08%;对植物油和液体石蜡的乳化性能分别为991 s和545 s;DDS-β-CD质量分数为0.5%时的水包植物油乳液的起始平均粒径为4.42 μm,并具有良好的稳定性。     

Preparation and characterization of surface active erucic acid derivatives

Nonionic, cationic and anionic surfactants, derivatives ofcis-13-docosenoic acid (erucic acid), have been prepared and characterized, and their performance has been evaluated and compared with the corresponding derivatives of fatty acids with shorter alkyl chain length. Nonionic erucic acid ethoxylates give a solution behavior anticipated from the hydrophilic-lipophilic balance of the molecule; however, the increased molecular size as compared to ordinary surfactants results, e.g., in higher temperature stability of the surfactant aggregates. Anomalous solution behavior was found and investigated for anionic surfactants, triethanolammonium salts of erucic acid, and some shorter homologues. The effects are discussed in terms of the acid-base equilibria of the alkanolammonium counterion and the acid, together with effects due to the molecular size of the counterion.     

Preparation and characterization of 2-cyanoacrylate copolymers

Butyl and ethoxyethyl 2-cyanoacrylate and mixtures thereof in different molar ratios were subjected to polymerization at pH 2.0, 3.0, 4.0, 5.5, and 6.9 and characterized by X-ray diffraction, hot-stage microscopy, and NMR analysis. The polymers were in an X-ray amorphous state. Their softening temperatures increased with ascending pH during polymerization. In all cases, the temperatures of the ethoxyethyl polymers were below those of the butyl polymers. Softening temperatures between those of the pure polymers could by achieved by copolymerization. The molar composition of the polymers was checked by NMR analysis. © 1992 John Wiley & Sons, Inc.