硼矿制硼酸母液中硼含量的测定方法探讨

报道了笔者用水相直接显色型比色法测定硼酸母液中硼含量的实验和结果。     

水中"一锅"合成7,7-二甲基-4-(3-氯苯基)-5-氧代-3,4,5,6,7,8-六氢香豆素的洁净方法

研究了四丁基溴化铵(TBAB)催化下的水介质中,3-氯苯甲醛、丙二酸亚异丙酯和5,5-二甲基-1,3-环己二酮三组分缩合,一步合成系列7,7-二甲基-4-(3-氯苯基)-5-氧代-3,4,5,6,7,8-六氢香豆素。产物的结构经IR和1HNMR进行了表征确证。该方法具有反应条件温和、操作简便、环境友好的优点。     

低温烘烤型双组分水性聚氨酯涂料

采用溶液聚合法，合成了丙烯酸五元共聚物；将该共聚物中的羧基中和后制成丙烯酸多元醇分散体，将其作为B组分与一种低黏度的多异氰酸酯固化剂(A组分)组成双组分水性聚氨酯涂料。研究发现：引发剂含量、羟基含量、中和度以及A、B两组分混合搅拌方式都对双组分涂膜的性能产生重要影响。当引发剂含量为1％，羟基含量为2．7％，中和度为100％，A、B组分采用机械搅拌混合时所得的涂膜综合性能最好。水性涂料的适用期达到8h，超过相应的溶剂型涂料。     

醇酮装置废酸水中副产物的回收利用探讨

分析了醇田装置副产物的生成过程和借鉴国外辞酮装置废酸水和皂化废碱液的回收利用技术，提出了合并浓缩、脱过氧化氢生产混合二元酸及硝酸后氧化、结晶、真空间歇精馏相结合分高己二酸、戊二酸、丁二酸的两种回收利用的工艺方法，并提出了两个工业化装置的设想，对治理废酸水提出了建设性意见。     

In situ composite of nano SiO2-P(VDF-HFP) porous polymer electrolytes for Li-ion batteries

Nano SiO₂-P(VDF-HFP) composite porous membranes were prepared as the matrix of porous polymer electrolytes through in situ composite method based on hydrolysis of tetraethoxysilane and phase inversion. SEM, TEM, DSC and AC impedance analysis were carried out. It is found that the in situ prepared nano silica was homogeneously dispersed in the polymeric matrix, enhanced conductivity and electrochemical stability of porous polymer electrolytes, and improved the stability of the electrolytes against lithium metal electrodes. The in situ composite method was found to be much better than the direct composite method in lowering the interfacial resistance between electrolyte and lithium metal electrode. Moreover, cycle test of lithium batteries using lithium metal as anode and sulfur composite material as cathode showed that the electrolyte based on in situ composite of silica presented stable charge-discharge behavior and little capacity loss of battery.     

一种能够抑制锂枝晶的锂金属电池电解液润湿性添加剂

将氟代有机溶剂2,2,3,3-四氟丙基甲基丙烯酸酯(TFPMA)作为双功能添加剂引入碳酸酯电解液体系,考察了TFPMA质量分数对增大润湿性的影响.采用交流阻抗、恒流充放电等测试了添加TFPMA后的锂金属电池性能.采用SEM和XPS表征了循环后的锂金属电极表面.结果表明,1.0％(质量分数,下同)TFPMA的添加使电解液与隔膜间的接触角从54°降至44°,内阻从6.15Ω降至1.94Ω,Li-LiFePO4电池在5 C电流密度下的比容量从66 mA·h/g提升至80 mA·h/g,1 C电流密度下的恒电流循环在100圈时还保持99％以上的库仑效率.TFPMA还促进了Li+的均匀沉积和优良固体电解质界面膜的形成,抑制了锂枝晶,电解液添加了1.0％TFPMA后,Li-Cu电池可以循环100圈以上,而库仑效率没有发生较大下降.循环后电极的SEM图表明,添加了1.0％TFPMA电解液的锂金属负极表面沉积更加平整,有较少的锂枝晶生成.     

球形磷酸铁锂材料的制备及其18650电池的测试

采用高能球磨和喷雾干燥法制备了球形磷酸铁锂材料LFP-1,并制作18650实装电池,测试电极片的压实密度,同时选择一种商业化磷酸铁锂材料LFP-2作为对比。测试结果显示,2种LFP材料均由平均粒径为300~500 nm的一次颗粒组成,比表面积为13~15 m²/g,碳质量分数为1.5%左右。通过CR2032纽扣型电池充放电测试表明,在0.2C时,LFP-1的比放电容量约为165 mA·h/g,与商业化磷酸铁锂材料LFP-2相近。制备18650电池的结果表明,商业化磷酸铁锂LFP-2材料制备的电极片的最高压实密度可以达到2.52 g/cm³,显著高于实验室制得的磷酸铁锂材料LFP-1的最高压实密度2.25 g/cm³,这可能与材料的颗粒粒度分布不同有关。     

HZSM-5型分子筛催化乙醇溶液脱水制备乙烯的工艺

以稀乙醇溶液为原料、自制分子筛HZSM-5为催化剂,催化脱水制备乙烯.考察了硅铝比、反应温度、质量空速及乙醇的质量浓度对该反应的影响,得到了较优化的反应工艺条件为:催化剂为HZSM-5(硅铝比30)分子筛,ρ(乙醇)为100~200 g/L,质量空速为2~6 h-1,反应温度为300℃.乙醇的转化率可达99%,乙烯的选择性达99%以上.     

水性聚氨酯的合成与改性

以甲苯二异氰酸酯(TDI)、聚醚二元醇(N220)和二羟甲基丙酸(DMPA)为主要原料,采用三羟甲基丙烷(TMP)进行交联改性合成了水性聚氨酯(WPU),研究了n(-NCO)/n(-OH)、DMPA及TMP对WPU的耐水性、稳定性和力学性能的影响。研究发现,改性后的乳液常温贮存稳定性好,适度交联可提高胶膜的拉伸强度及耐水性。     

Study of operating variables in the transformation of aqueous ethanol into hydrocarbons on an HZSM‐5 zeolite

With the aim of determining the possibilities of directly upgrading the liquid obtained from carbohydrate fermentation, the effect of operating conditions (temperature, space time, water content in the feed) has been studied in the catalytic transformation of aqueous ethanol into hydrocarbons on an HZSM‐5 zeolite in an isothermal fixed bed reactor. Special attention has been paid to the effect of water content on the yield, product distribution and catalyst deactivation. Although deactivation by coke decreases as the water content is increased, this content must be limited at 450 °C and higher temperatures in order to avoid irreversible deactivation of the catalyst by dealumination. © 2002 Society of Chemical Industry