对叔丁基苄胺的合成研究

摘要选择Delepine反应法的路线合成对叔丁基苄胺，并对反应投料比、反应温度及酸化后的反应时间进行了优化试验，得到了较好的反应条件：反应温度为40℃，对叔丁基苄氯与乌洛托品投料比为1：1；加入酸和醇后的保温时间为2h，从而使反应收率稳定在90％以上，含量达到95％。     

强化两相混合的超临界技术制备聚乳酸微粒

针对商品化聚乳酸微球粒径分布较宽难于适用气溶胶给药要求的不足,采用水力空化混合强化超临界流体辅助雾化技术(SAA-HCM)制备聚乳酸(PLA)超细微粒.该技术主要特点是通过在超临界流体和液相进料处引入水力空化混合器,强化两相间的混合.考察SAA-HCM过程混合器压力、温度、沉淀器温度、进料中CO2与液体溶液质量流量比和溶液质量浓度等操作参数对微粒形态和粒径分布的影响,成功制备出球形度较好,粒径分布较窄(1～3μm)的PLA微球.经X射线衍射(XRD)分析和差示扫描量热(DSC)分析显示,与原料PLA相比,微球晶型及热曲线变化不大,但结晶度下降.同时把操作参数与相行为进行关联,探讨了影响颗粒形貌的机理.对比超临界流体辅助雾化法(SAA)的实验结果表明:水力空化的引入能有效强化混合器内的两相传质,混合更好,能制备出适用于气溶胶给药要求的超细微粒.     

Research on the friction and wear mechanism of Poly(vinyl alcohol)/hydroxylapatite composite hydrogel

Poly(vinyl alcohol)/Hydroxylapatite (PVA/HA) composite hydrogel was prepared with poly(vinyl alcohol) and hydroxylapatite as raw materials, using the method of repeated freezing and thawing. The morphologies of PVA/HA composite hydrogel were observed by means of high-accuracy 3D profiler and scanning electron microscope (SEM). The compressive elastic modulus and the stress relaxation characteristics of PVA/HA composite hydrogel were measured using the flat-head cylinder indenter. The friction and wear tests between PVA/HA composite hydrogel and bovine knee articular cartilage were performed on the micro-tribometer. The worn morphologies of PVA/HA composite hydrogel were observed with environmental scanning electron microscope (ESEM). The results showed that PVA/HA composite hydrogel has the cross-link network microstructure which is similar to that of the natural bovine knee articular cartilages. With the increase of freezing-thawing cycles and the HA content, the degree of cross-link and the crystallization of PVA/HA composite hydrogel both increase, the elastic modulus increases evidently, the rate of stress relaxation is improved and the value of balance stress decreases. The friction coefficient decreases with the increase of the freezing-thawing cycles and the HA content. The more the freezing-thawing cycles are, the earlier the friction coefficient reaches the stable balance value. The friction deformation depth between PVA/HA composite hydrogel and bovine knee articular cartilage is inversely proportional to freezing-thawing cycles and the HA content. The main wear mechanisms of PVA/HA composite hydrogel are plastic flowing and adhesive flaking. The wear severity degree decreases with the increase of freezing-thawing cycles and the HA content. Supported by Key Program of the National Natural Science Foundation of China (Grant No. 50535050), Program for New Century Excellent Talents in University (Grant No. NCET-06-0479) and Natural Science Foundation of Jiangsu Province (Grant No. BK2005403)     

Characterization of konjac glucomannan–quaternized poly(4‐vinyl‐N‐butyl) pyridine blend films and their preservation effect

Novel polymer blends were prepared from a mixture of 2 wt % konjac glucomannan and 4 wt % quaternized poly(4‐vinyl‐N‐butyl) pyridine (QPVP) in aqueous solution and dried at room temperature for 72 h. Their structure and properties were studied by infrared, wide‐angle X‐ray diffraction, scanning electron microscopy, thermogravimetric analysis, and differential scanning calorimetry. Thermal stability in the dry state was reduced with increasing content of QPVP. Compared with QPVP film, the tensile strength of the films was improved in the dry state. The maximum value of 12.74% tensile break elongation was reached when the content of QPVP was 30%. Structural analysis indicated that clear phase separation was observed when the content of QPVP was only 50%. Results from the filmcoating preservation experiments with lychee showed that this blend film had water‐holding ability. The fruit weight loss rate and rot rate both decreased in various degrees. The potential uses of these novel polymer films could be as preservative films. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 93: 1868–1875, 2004     

Melt‐processable rubber: Chlorinated waste tire rubber‐filled polyvinyl chloride

Chlorinated ground rubber tire (Cl‐GRT) particles were used as filler in a plasticized polyvinylchloride (PVC) to develop a melt‐processable rubber composition. Physical properties of the Cl‐GRT‐filled PVC compound showed improvement compared to the nonchlorinated counterpart. Interaction between Cl‐GRT and PVC was examined on the basis of results of stress relaxation, dynamic mechanical thermal analysis, and solvent swelling studies. The Cl‐GRT could be loaded upto 40 parts per hundred parts of PVC, and the composition still retains the elastomeric characteristics. The Cl‐GRT‐filled composite was found to be reprocessable like the unfilled PVC compound. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 622–631, 2002; DOI 10.1002/app.10352     

Effects of coagulation bath temperature on structure and performance of poly （vinyl butyral） hollow fiber membranes via thermally induced phase separation

Poly （vinyl butyral） （PVB） hollow fiber membranes were fabricated via thermally induced phase separation （TIPS）. The effects of coagulation bath temperature （CBT） on the structure and performance of membranes were investigated in detail. The morphologies of the membranes were studied by scanning electron microscopy （SEM）, the performances of water permeability, rejection, breaking strength and elongation were measured, respectively. The results indicate that all the membranes have the asymmetric morphology and the thickness of the skin layer decreases and the pore size of the outer layer increases with the increase of CBT. The permeability of membranes prepared at air gap 1.0 cm and take-up speed 0.253 m/s increases from 1.047×10-7 to 5.909×10-7 m3/（m2·s-kPa） with the CBT increasing from 20 ℃ to 40℃, and sharply increases to 35.226×10 7 m3/（m2.s.kPa）once the CBT arrives at 50 ℃. While the carbonic ink rejections have no significant decrease, totally exceed 98%, but that of acid-maleic acid copolymer greatly decreases with the increase of CBT. Both the breaking strength and elongation decrease with the increase of CBT.     

合成介质对PEDOT催化染料敏化太阳电池光阴极性能的影响

采用聚3,4-乙烯二氧噻吩(PEDOT)/FTO为对电极,研究了合成介质对循环伏安法电聚合制备的PEDOT/FTO对电极性能的影响。通过SEM、CV、EIS、Tafel曲线,并首次采用SECM方法对所制备的对电极的电催化性能进行了表征。结果表明:在LiClO4水溶液和1-丁基-3-甲基四氟硼酸盐离子液体(IL)中制备的光阴极具有良好的电催化性能。J-V测试曲线表明,在LiClO4水溶液和IL中制备的光阴极所组装的DSSC器件的光电转化效率分别达6.4%和6.6%,接近于同等条件下以Pt对电极构建的DSSC器件的光电转化效率。     

煤矿井下抗静电阻燃塑料管接件

介绍煤矿井下用塑料管接件的实验研究，通过调整材料比及工艺，使材料性能达到了煤炭工业部ＭＴ１８１－８８标准。     

仲丁醇含量对正丁烯直接水合法制仲丁醇的影响

研究了正丁烯直接水合法制仲丁醇工艺中原料水中仲丁醇含量对反应的影响.当原料水中含有少量仲丁醇时(约0.9%时),其对水合反应过程的转化率影响不大;原料水中含有少量仲丁醇时,反应过程的稳定性比较好.当水合反应的原料水中仲丁醇浓度增大时(原料水中仲丁醇浓度为2.0%左右时),反应过程的转化率明显下降.当水合反应的原料水中仲丁醇含量进一步增大时,反应过程的转化率下降明显,但呈非线性变化.     

用超临界二氧化碳法制备超强吸水剂

以N，N’-亚甲基双丙烯酰胺(BIS)为交联剂，研究了疏水性单体丙烯酸十八酯(OA)与亲水性单体丙烯酸(AA)在超临界二氧化碳中的聚合反应，制备了超强吸水剂。结果表明，65℃、压力大于13MPa时，制备的产物都为白色固体粉末。用超临界二氧化碳萃取技术可以对产物进行纯化，50℃、20MPa下，产物经超临界二氧化碳萃取2次后纯度可大于95％，4次后单体残留率为0．28％。该超强吸水剂的吸水率有一定下降，然而保水率却得到提高。