新型金刚烷基杂双子表面活性剂的合成及其表面活性

以1-金刚烷甲酸为原料,经酰化,取代和还原反应制得N,N-二甲基-1-金刚烷基甲胺(1);1与双子季铵盐(2)在无水乙醇中反应合成了一种新型的金刚烷基杂双子表面活性剂——1-(N,N-二甲基-1-金刚烷甲基溴化铵)-6-(N,N-二甲基-十二烷基溴化铵)-己烷(3),总收率30.9%,其结构经1H NMR和元素分析表征。采用表面张力法研究了3的表面活性。结果表明:3具有较强的聚集能力和界面吸附能力,其cmc,γcmc,p C20,Γmax,Amin分别为1.18 mmol·L-1,35.5 m N·m-1,0.48,2.63μmol·m-2和0.63 nm2。     

新型季铵盐氟碳表面活性剂的合成及其表面活性

以六氟环氧丙烷多聚体为原料,与N-甲基哌嗪经酰胺化反应制得含氟化合物(3);3与碘代烷经季铵化反应合成了4个新型的季铵盐型氟碳表面活性剂(5a~5d),其结构经1H NMR,19F NMR,IR和HR-ESI-MS表征。表面性能测试结果表明,5a~5d具有较高的表面活性,水溶液的临界胶束浓度(CMC)分别为1.38×10-4g·mL-1,1×10-4g·mL-1,1.40×10-4g·mL-1和3.72×10-4g·mL-1,对应CMC的表面张力分别为19.47mN·m-1,17.20 mN·m-1,17.98 mN·m-1和19.79 mN·m-1。     

N-[γ-(二烷基氨基)烷基]全氟丁基酰胺类表面活性剂的合成及其表面活性

以全氟丁酸为原料,通过酰化与酰胺化反应合成了新型中间体[C4F7ONH(CH2)n N(CH3)2(n=2或3)](3和4);3或4分别与四种不同碳链长度的溴代烷烃经季铵化反应合成了两类共8个新型的N-[γ-(二烷基氨基)烷基]全氟丁基酰胺类阳离子含氟表面活性剂(6a~6d和7a~7d),其结构经1H NMR表征。表面活性测定结果表明,6和7水溶液的表面张力在22.251 mN·m-1~33.301 mN·m-1,CMC在37.8 mmol·L-1~49.5 mmol·L-1,最小截面积在0.607 nm2~0.626 nm2。     

粉状白钨酸的研究——Ⅲ.从粉状白钨酸制备偏钨酸铵和偏钨酸有机铵盐以及它们的性质研究

本文继活性粉状白钨酸的制得,用其制备偏钨酸钠后,进一步报道了以粉状白钨酸为出发点的偏钨酸铵(NH_4)_6[H_2(W_3O_(10))_4]·nH_2O、偏钨酸乙基铵、二乙基铵、三乙基铵和四乙基铵盐的合成及部分性质研究。同法还制得偏钨酸三正丁基铵,经化学分析其组成接近[(n-C_4H_9)_3NH]_6·[H_2(W_3O_(10))_4],与文献报道的“酸式盐”[(n-C_4H_9)_3NH]_5H[H_2(W_3O_(10))_4]不同。     

一种酯类双季铵盐Gemini表面活性剂的合成研究

酯类双季铵盐Gemini表面活性剂含有正电荷性和酯类官能团,具有cmc低、高界面活性、易生物降解的特点。本研究先用三乙胺(TEA)和环氧氯丙烷(EPIC)合成新型季铵盐阳离子表面活性剂失水甘油基三乙基氯化铵(GTA)中间体,最后用GTA和己二酸反应合成得到一种新型酯类双季铵盐Gemini表面活性剂——双季铵盐己二酸酯表面活性剂(BQAA)。超声条件下得出BQAA合成的最佳条件为:超声频率:60KHz,反应体系pH=8,反应温度:50℃,n(GTA)∶n(己二酸)=2. 5∶1. 0,反应时间:6. 5h,BQAA为白色晶体,产率为88. 79%,通过元素分析和IR对产品BQAA进行了表征,对产物BQAA的表面活性、泡沫性能和乳化性能进行了研究,实验结果表明:BQAA的cmc=1. 3×10~(-4)mol·L~(-1),γ_(cmc)=27. 96 mN·m~(-1),泡沫形成稳定性高,起泡能力强,乳化能力好。     

新试剂4,4'-二[3-(4-苯基-2-噻唑基)三氮烯基]联苯与阳离子表面活性剂显色反应的研究

本文研究了新试剂4,4'-二[3-(4-苯基-2-噻唑基)三氮烯基]联苯(BPTTBP)与阳离子表面活性剂溴化十六烷基吡啶(CPB)和溴化十六烷基三甲基铵(CTMAB)的显色反应.结果表明,在NaOH碱性介质中,试剂BPTTBP分别与CPB和CTMAB形成紫色离子缔合物,最大吸收波长为607 nm.试剂BPTTBP与CPB和CTMAB的缔合比均为1:1,其表观摩尔吸光系数分别为2.46×10 4 L·mol-1·cm-1和1.82×10 4 L·mol-1·cm-1,CPB和CTMAB含量在0～1.0×10-5 mol·L-1范围内符合比耳定律.方法直接用于废水中微量CPB和CTMAB的测定,结果满意.     

新型含双长链和苄基的有机硅季铵盐的合成

以双十二胺(1)为原料,与氯化苄经取代反应制得中间体苄基双十二胺(2);2与γ-氯丙基三甲氧基硅烷(3)经季铵化反应合成了一种新型的含双长链和苄基的有机硅季铵盐(4),其结构经UV-Vis和FT-IR表征。通过正交实验L9(34)优化了2和4的反应条件。合成2的最佳工艺条件为:以乙腈为溶剂,1 5 mmol,n(1)∶n(Bn Cl)=1.0∶1.2,回流反应20 h,收率80.4%。合成4的最佳工艺条件为:以乙二醇为溶剂,2 5mmol,n(2)∶n(3)=1.0∶1.6,于110℃密闭反应80 h,收率57.8%。     

新型硫酮基哌嗪荧光探针的合成及其对铜(Ⅱ)的识别性能

以苯胺和三氟乙酰乙酸乙酯为原料,经环合反应制得4-三氟甲基-2(1H)喹啉酮(1);1与劳森试剂反应生成4-(三氟甲基)喹啉-2(1H)-硫酮(2);2与间隔基反应合成中间体2-[(3-氯丙基)硫基]-4-(三氟甲基)喹啉(3);将3连接到识别基团哌嗪上合成了一个新型的双荧光侧臂的探针化合物——1,4-二【3-{2-[4-(三氟甲基)喹啉]硫基}丙基】哌嗪(4),其结构经1H NMR和LC-MS表征。UV-Vis和FL研究结果表明,4的发射波长在396 nm;对Cu2+具有良好的识别作用,在1.0×10-7mol·L-1~1.0×10-4mol·L-1内可定量检测Cu2+含量。     

一种新型表面活性剂的表面活性的研究

采用表面张力法确定了新型表面活性剂3-对壬基苯氧基-2-羟丙基三甲基溴化 铵的临界胶束浓度(cmc)，并考察了盐度、温度和pH值对其cmc的影响。结果表明， 此种表面活性剂的表面活性较高，盐度对其cmc影响最大，其次是pH值，温度对其 cmc的影响较为复杂。理论计算结果表明，采用热力学函数可较好地解释试验结果 。     

新型N-(3-醛基-4-羟基苄基)型季铵盐的合成及其抗菌活性

5-氯甲基水杨醛和季铵(1a~1e)或吡啶(1f)在乙酸乙酯存在下经取代反应合成了一系列新型的N-(3-醛基-4-羟基苄基)型季铵盐(2a~2f),其结构经1H NMR,IR和MS表征。初步的抗菌活性测试结果表明,2a~2f对迟钝爱德华菌、嗜水气单胞菌、哈氏弧菌和鳗弧菌的MIC分别为0.18 mg·mL-1,0.09 mg·mL-1,0.18mg·mL-1和0.09 mg·mL-1。     

生物质与废轮胎共热解催化热解油蒸发过程及其动力学研究

采用热重微商(TG-DTG)法考察生物质稻壳与废轮胎共热解经催化与非催化热解油的热失重行为，并同0#柴油的热失重行为进行了比较；同时采用Achar微分法和Coats-Redfern积分法对热解油热失重蒸发过程的蒸发热进行了计算，并结合Satava和Bagchi法确定了热失重蒸发过程的机理函数， 建立了0#柴油和在催化与非催化条件下得到的热解油蒸发过程的动力学方程，得出了在催化与非催化条件下热解油热失重过程的机理函数，其动力学方程为dα/dt=Ae-△vapH/RT(1-TBX〗α)2；而0#柴油的热失重蒸发过程动力学方程为dα/dt=1.5Ae-△vapH/RT(1-α)2/3\[1-(1-α)1/3\]-1。蒸发热的顺序由大到小依次为,柴油＞非催化热解油＞SBA-15热解油＞MCM-41热解油。结果表明，通过建立的模型函数得到的蒸发热与实验值非常接近。催化剂SBA-15和MCM-41的存在对降低高沸点馏分的物质具有一定作用，而SBA-15催化作用强于MCM-41。     

柴油溶剂中脂肪酶催化高酸值废油脂酯化制备生物柴油

采用0＃柴油作为反应溶剂,利用固定化脂肪酶催化高酸值废油脂与甲醇酯化反应制备生物柴油。来源于Candida antarctica的固定化脂肪酶Novozym435在0＃柴油溶剂中具有极高的催化活性。以酸价高达157×10-3的废油脂为原料,废油脂质量比10%的Novozym435,甲醇与废油脂初始摩尔比2∶1,0＃柴油与废油脂质量比5∶1,摇床摇速170r/min,50℃下反应2h甲酯化率可达95.10%。0＃柴油作为反应溶剂有效地溶解了高酸值废油脂和甲醇,降低了反应体系的黏度和消除了甲醇对Novozym435的负面影响,提高了Novozym435的稳定性。同时,0＃柴油溶剂对未脱胶废油脂中残留的对脂肪酶有害的磷脂等胶类物质具有一定的稀释作用。该工艺省却了溶剂蒸馏的繁琐工序,直接得到脂肪酸甲酯和石化柴油的混合燃料。     

Utilization of waste seashells and Camelina sativa oil for biodiesel synthesis

The seafood industry produces over 100 million pounds of seashell waste every year. With landfill space diminishing quickly, ways to recycle waste materials are becoming more sought for. Herein, we utilized waste mussel, clam and oyster shells as heterogeneous catalysts for the transesterification of Camelina sativa oil as a feedstock into biodiesel. Camelina sativa oil provides a reliable solution for biodiesel production because it has high tolerance of cold weather, drought, low-fertility soils and contains approximately 40% oil content. The catalysts from waste seashells were characterized by X-ray powder diffraction and Fourier transform infrared (FTIR) spectroscopy. High biodiesel yields were achieved at a 12:1 (alcohol:oil) molar ratio with 1?wt.% waste seashell catalysts in 2?h at 65°C. Biodiesel was analyzed by ¹H NMR and FTIR spectroscopy and the fuel properties of the biodiesel produced from Camelina sativa oil and waste seashells were compared with American Society for Testing and Materials standards.     

Impact of elevated carbon dioxide on primary, secondary metabolites and antioxidant responses of Eleais guineensis Jacq. (oil palm) seedlings

A split plot 3 by 3 experiment was designed to investigate the relationships among production of primary metabolites (soluble sugar and starch), secondary metabolites (total flavonoids, TF; total phenolics, TP), phenylalanine lyase (PAL) activity (EC 4.3.1.5), protein and antioxidant activity (FRAP) of three progenies of oil palm seedlings, namely Deli AVROS, Deli Yangambi and Deli URT, under three levels of CO? enrichment (400, 800 and 1,200 μmol·mol?1) for 15 weeks of exposure. During the study, the treatment effects were solely contributed by CO? enrichment levels; no progenies and interaction effects were observed. As CO? levels increased from 400 to 1,200 μmol·mol?1, the production of carbohydrate increased steadily, especially for starch more than soluble sugar. The production of total flavonoids and phenolics contents, were the highest under 1,200 and lowest at 400 μmol·mol?1. It was found that PAL activity was peaked under 1,200 μmol·mol?1 followed by 800 μmol·mol?1 and 400 μmol·mol?1. However, soluble protein was highest under 400 μmol·mol?1 and lowest under 1,200 μmol·mol?1. The sucrose/starch ratio, i.e., the indication of sucrose phosphate synthase actvity (EC 2.4.1.14) was found to be lowest as CO? concentration increased from 400 > 800 > 1,200 μmol·mol?1. The antioxidant activity, as determined by the ferric reducing/antioxidant potential (FRAP) activity, increased with increasing CO? levels, and was significantly lower than vitamin C and α-tocopherol but higher than butylated hydroxytoluene (BHT). Correlation analysis revealed that nitrogen has a significant negative correlation with carbohydrate, secondary metabolites and FRAP activity indicating up-regulation of production of carbohydrate, secondary metabolites and antioxidant activity of oil palm seedling under elevated CO? was due to reduction in nitrogen content in oil palm seedling expose to high CO? levels.     

4-(邻甲基苯氨基重氮基)-4'-硝基偶氮苯的合成及其与汞(Ⅱ)的显色反应

合成了一种新三氮烯试剂4-(邻甲基苯氨基重氮基)-4'-硝基偶氮苯(OMADNA), 并研究了其物化性质及与Hg(Ⅱ) 的显色反应. 结果表明, 在乳化剂OP存在下, 在pH 10.2的Na2B4O7-NaOH缓冲介质中, Hg(Ⅱ)与该试剂形成稳定的桔红色络合物, 最大吸收波长位于570 nm, 表观摩尔吸光系数为1.42×105 L·mol-1·cm-1, Hg(Ⅱ)的质量浓度在0～0.9 μg/mL范围内服从比耳定律. 所拟方法用于环境水样中微量Hg(Ⅱ)的直接测定, 结果与双硫腙法一致.     

The concentration of oleocanthal in olive oil waste

The aim of this study was to determine the concentration of oleocanthal in olive pomace waste and compare this to its concentration in extra-virgin olive oil (EVOO). The concentration of oleocanthal in freshly pressed EVOO and its subsequent waste was analysed at early, mid and late season harvests. Oleocanthal concentrations were quantified using high-performance liquid chromatography-mass spectrometry. In oil, oleocanthal concentration was as follows: 123.24 ± 6.48 mg kg(-1) in early harvest, 114.20 ± 17.42 mg kg(-1) in mid harvest and 152.22 ± 10.54 mg kg(-1) in late harvest. Its concentration in waste was determined to be: 128.25 ± 11.33 mg kg(-1) in early harvest, 112.15 ± 1.51 mg kg(-1) in mid harvest and 62.35 ± 8.00 mg kg(-1) in late harvest. Overall, olive pomace waste is a valuable source of oleocanthal.     

脂肪醇聚氧乙烯醚磺酸钠的性能研究

对合成的不同碳链脂肪醇聚氧乙烯醚磺酸钠(AnESO,EO=3,n=14,16,18)的应用性能及与重烷基苯磺酸钠(HABS)的复配进行了研究.结果表明:(1)AnESO的γcmc分别为36.16 mN·m-1,35.47 mN·m-1和34.85 mN·m-1,A14ESO发泡性较好,A18ESO稳泡性较强,耐钙稳定性分别达到了8700mg/L,9500mg/L和10000mg/L,耐盐性为A18ESO ＞ A16ESO ＞A14ESO;(2)AnESO与HABS复配可以改善HABS的耐盐性,AnESO/HABS体系与大庆原油间的界面张力在ω(AnESO):ω(HABS)约为3:7时最低,达到了3.9×10-2mN·m-1,1.4×10-2mN·m-1和4.3×10-3mN·m-1,A18ESO/HABS体系油水界面张力在NaCl含量为0～15000mg·L-1下均达到10-3mN·m-1数量级.     

GC-MS analysis of the PCB substitute Ugilec 141 and its occurrence in waste mineral oils

After the restrictions on production and use of PCBs, Ugilec 141, a technical mixture of dichlorobenzyldichlorotoluenes (DBDTs), has been used as a PCB substitute in hydraulic systems. In the Netherlands, the production, import and use of Ugilec 141 has been forbidden since 1988. A method has been developed for the analysis of Ugilec 141 in waste mineral oils to control waste oil import and processing. The method development was based on modification of procedures for the analysis of PCBs in oil and dioxins in fatty matrices and analysis was performed with gas chromatography with mass spectrometry. For sample clean-up, several combinations of column chromatography with activated carbon, alumina, and silica gel have been tested to obtain extracts free from matrix interferences. An internal standard of ¹³C-labeled DBDT was examined to check recoveries from the clean-up procedures. Quantification was performed by comparison with the six most abundant peaks of an external Ugilec 141 standard mixture. Validation experiments showed a linear range from 0.25 to 60 mg Ugilec 141 kg^?1 oil, a reproducibility of 3% and a limit of determination of 0.25 mg Ugilec 141 kg^?1 waste oil. The method was applied in a survey of 70 samples of waste mineral oils from producers all over the Netherlands; this revealed levels below the limit of determination and one positive sample with a concentration of 5.7±0.1 mg Ugilec 141 kg^?1 oil. In an inspection inquiry, one contaminated oil was found containing 116 ± 9 g Ugilec 141 kg^?1 oil.     

吸收液采样-顶空-气相色谱法测定废气中吡啶

用吸收液采集废气样品,顶空进样,采用气相色谱法测定进样气体中吡啶的含量。用DB-FFAP毛细管色谱柱分离,氢火焰离子化检测器测定。优化的试验条件如下:①采用多孔玻板吸收瓶采集样品;②吸收液的体积为45mL;③采样流量为0.5L·min^-1;④样品在4℃下,7d内完成分析;⑤吸收液的pH大于12;⑥加入3g氯化钠调节吸收液离子强度;⑦顶空温度为80℃,顶空平衡时间为30min。吡啶的质量浓度在100mg·L^-1以内与其对应的峰面积呈线性关系,检出限为0.05 mg·m^-3。对3个不同浓度水平的吡啶标准气体进行测定,相对误差为-8.0%^-4.7%,测定值的相对标准偏差(n=6)为1.3%~7.8%。     

Rapid—In—situ Determination of Chromium （VI） in Water Using Modified Diphenylcarbazine with Citrate

In recent years, the determination of Cr (VI) has attracted great attention because of its toxicity to human, plants and animals1-5. Usually, in the industrial waste water, the concentration of Cr (VI) is relatively high and should be determined frequently. So, an accurate, quick, and convenient method for the measurement of Cr (VI) in environmental water, as well as in river, lake, sea and tap water, is of great importance. The method for determination of Cr (VI) by diphenylcarbazine …