酶解产物人参皂苷Rh_2、Rh_3的二氯甲烷层析分离

人参皂苷Rh2、Rh3具有一定的抗癌作用,而这些稀有皂苷在传统红参中的含量甚微。为了获得纯度较高的人参皂苷单体,将人参二醇类皂苷经酶转化等方法处理,得到以人参皂苷Rh2和Rh3为主的混合物。常压下,用二氯甲烷-甲醇作为洗脱液变换梯度进行硅胶柱分离,分别采用流动相V(二氯甲烷)∶V(甲醇)=7∶0.10、7∶0.13、7∶0.15、7∶0.18、7∶0.2、7∶0.3渐变梯度进行洗脱,当流动相V(二氯甲烷)∶V(甲醇)=7∶0.3时,成功分离出人参皂苷Rh2和Rh3。经高效液相色谱检测,为反式的二十、二十二碳烯Rh3和顺式的二十、二十二碳烯Rh3(即Rk2)混合物,纯度达到95%以上;也得到较纯的Rh2,经高效液相色谱检测为20(S)-Rh2和20(R)-Rh2异构体的混合物,纯度达到85%以上。     

人参皂苷Re的分离提纯

采用硅胶柱层析法分离人参叶三醇皂苷,以氯仿-甲醇为流动相洗脱,得到了纯度较高的人参皂苷Re。结果表明,利用硅胶柱层析柱从35 g叶三醇皂苷中分离得到人参皂苷Re7.36 g,得率为21.03%。采用重结晶法对经硅胶柱分离制备的5 g Re进行提纯,将结晶产品分开收集,第2次结晶效果最好,得产品2.43 g,得率为48.68%,纯度为98.89%。     

早强剂对掺硅灰的水泥砂浆强度与结构影响的研究

探讨了不同早强剂对掺硅灰的水泥砂浆强度及微观结构的影响.结果表明：掺入不同的早强剂均可提高掺硅灰的水泥砂浆早期强度,且对其1 d抗压强度的增强效果优于3 d.其中掺入适量的硫酸钠可迅速生成大量的钙矾石晶体,提高水泥砂浆的密实度,同时促进了硅灰的火山灰反应,明显提高了掺硅灰的水泥砂浆的早期强度,但早强剂对掺硅灰的水泥砂浆后期强度影响不大.3种早强剂对掺硅灰的水泥砂浆早期强度增强作用从大到小的顺序依次为硫酸钠、氯化钙、三乙醇胺,其中硫酸钠掺量为3%时增强作用最佳.     

AB8大孔树脂吸附与硅胶层析法分离姜酚的对比研究

采用硅胶柱层析和AB8大孔树脂吸脱附两种方法分离姜油树脂中的姜酚,采用气相色谱-质谱(gas chromatography-mass spectrometry,GC-MS)对分离样品进行表征,用峰面积归一化法对测试样品的气相色谱-质谱结果进行分析,确定了分离样品中各组分的相对峰面积百分比。以姜酚标准样品为参比,确定了姜油树脂所含姜酚在分离样品中的富集率。结果表明硅胶柱层析法的分离样品中姜酚集中在第3、4段,其中第4段含量最高,共鉴定出19种成分,姜酚峰面积百分数为14.34%,富集率为59.01%;采用AB8大孔树脂分离时姜酚集中在洗脱液前5号样,其中2号样含量较高,鉴定出11种成分,姜酚峰面积百分数为55.68%,富集率为70.88%。     

杂化介孔二氧化硅溶胶的制备及表征

在室温、不同pH值条件下合成出纳米球形介孔二氧化硅溶胶。通过研究得出当pH=4时为最佳生产工艺,在pH=4条件下以十六烷基三甲基溴化铵为模板剂,利用正硅酸乙酯和硅烷偶联剂共水解制备了杂化介孔二氧化硅溶胶。运用激光纳米粒度仪、透射电镜、X射线衍射等测试方法对材料进行表征。结果表明:通过共水解溶胶-凝胶法成功合成了改性介孔二氧化硅溶胶,其粒径约为25 nm,具有规则的介孔结构和良好的分散性。     

Hybrids perfluorosulfonic acid ionomer and silicon oxide membrane for application in ion-exchange polymer-metal composite actuators

This paper reports a new technique to fabricate an ion-exchange polymer-metal composite (IPMC) actuator. This technique is based on a hybrid organic-inorganic composite membrane. In the fabrication course, silica oxide particles, prepared from hydrolysis of tetraethyl orthosilicate in situ with sol-gel reaction, co-crystallize with perfluorosulfonate acid (PFSA) ionomer. Attenuated total reflectance fourier transform infrared spectroscopy (ATR-FTIR) analyses demonstrate that a highly water-saving hybrid mem...     

Role and distribution of different Ba-containing phases in supported Pt–Ba NSR catalysts

Pt–Ba/MeO (where MeO = Al₂O₃, CeO₂, SiO₂ and ZrO₂) NO _x storage-reduction catalysts with Ba-loading varying from 0 wt.% to 28 wt.% were investigated concerning stability of Ba phases and NO _x storage-reduction efficiency. For Pt–Ba/Al₂O₃ three different Ba-containing phases with different thermal stability are distinguished based on their interaction with the support. The relative concentration of these phases varies with the Ba-loading and NO _x storage tests indicated that the BaCO₃ phase decomposing between 400 °C and 800 °C (LT-BaCO₃) is the most efficient Ba containing phase for NO _x storage. Similar investigations of Pt–Ba catalysts supported on CeO₂, SiO₂ and ZrO₂ showed that the relative amount of LT-BaCO₃ phase depends also on the support material. NO _x storage measurements confirmed a correlation between the concentration of LT-BaCO₃ and NO _x storage efficiency. Basicity and textural properties of the support are identified as crucial parameters for efficient NO _x storage catalysts.     

用1，10－二氮杂菲分光光度法测定沉淀法白炭黑中的铁含量

提出并研究了使用１，１０－二氮杂菲分光光度法测定沉淀法白炭黑中铁含量的分析方法。其具体步骤为：首先用氢氟酸处理试样，使沉淀法白炭黑（二氧化硅）转化成四氟化硅气体逸出。而后在ｐＨ为４～５条件下，用盐酸羟胺处理剂将残留液中的三价铁离子还原成二价铁离子，加入１，１０－二氮杂菲显色剂（与二价铁离子反应可生成橙红色络合物），再用分光光度法测定其中的铁含量。实验表明，本方法原理可靠，分析步骤简便，抗铜、锰离子干扰性强，精密度与准确度较高。     

Phase Separation in Gelling Silica–Organic Polymer Solution: Systems Containing Poly(sodium styrenesulfonate)

Phase separation which occurs in parallel to the hydrolysis and gelation of alkoxysilane solution containing poly(sodium styrenesulfonate) (NaPSS) has been investigated. Depending on the reaction conditions, gel morphologies such as isolated pores, particle aggregates, and interconnected continuous pores from 0.1 to 100 μm long have been observed. Time-resolved light scattering of gelling solution suggested the occurrence of spinodal phase separation through the polymerization of silica and the subsequent freezing of the developing structure by sol-gel transition. The effects of reaction parameters on the periodic size are explained mainly in terms of their influence on the "chemical cooling" rate which is determined by the polymerizatica rate of silica and the solubility of NaPSS in the reacting solution.     

UV固化蓖麻油基聚氨酯丙烯酸酯/SiO2杂化材料的制备与性能Q

以异佛尔酮二异氰酸酯（IPDI）、蓖麻油（CO）和丙烯酸羟乙酯（HEA）合成了蓖麻油基聚氨酯丙烯酸酯（COPUA），以正硅酸乙酯（TEOS）和3-(异丁烯酰氧)丙基三甲氧基硅烷（MEMO）通过溶胶-凝胶法制备了改性硅溶胶，作为无机相与COPUA有机相复合得到了UV固化COPUA/SiO2杂化材料。调节MEMO与TEOS的配比得到一系列改性硅溶胶，通过测试确定了MEMO与TEOS的最佳配比为1：1（MT-1）。在此基础上，改变MT-1的添加量得到UV固化COPUA/SiO2杂化材料。用FT-IR、TEM、SEM、TGA等对杂化材料和涂层进行结构表征，测试复合涂层的力学性能和表面性能。当MT-1添加量为COPUA树脂质量的15%时，涂层内部SiO2粒子分布均匀，涂层表面光滑平整，光透过率达到100.2%，硬度为5H，附着力0级，柔韧性1mm；涂膜拉伸强度达到13.52MPa，断裂伸长率为7.49%。