盐效萃取法从制药废液中回收正丁醇

用盐效萃取法从制药废液中回收正丁醇,考察碳酸钾水溶液与该废液的质量比对脱水率的影响,测定正丁醇-水-碳酸钾体系在40℃时的液-液相平衡数据,用Pitzer理论和NRTL方程对液-液相平衡数据进行了理论计算。结果表明:当质量分数为60.00%的碳酸钾水溶液与废液的质量比为1.00时,脱水率高达84.50%;将有机相进行精馏可得到质量分数为99.50%的正丁醇;计算值与实测值接近,水相和有机相的绝对平均偏差分别为0.60%和0.20%。

精馏与盐效萃取偶合过程

设计了一种适用于从含水量较高的共沸液中分离有机溶剂的装置,该装置将精馏和盐效分相器结合起来,并带有中间储罐,其特点是:分相器可以将塔顶蒸出的共沸物中的大部分水除去,中间罐可以实现水从塔底除去。该装置上、下同时出水,有机溶剂浓缩在中间罐中。该装置大大缩短了操作时间,节约了能源。对该装置进行了数学模拟,与实验结果吻合较好。

盐效萃取法从电子产品清洗废液中回收异丙醇

用盐效萃取法从电子产品清洗废液中回收异丙醇,考察了碳酸钾水溶液与该清洗废液的质量比对脱水率的影响,测定了异丙醇-水-碳酸钾体系在40℃时的液液相平衡数据,用 Pitzer 理论和 NRTL 方程对液液相平衡数据进行了理论计算。结果表明:当质量分数为60.00%的碳酸钾水溶液与该废液的质量比为2.00时,脱水率高达90.00%;将有机相进行精馏可得到质量分数为99.50%的异丙醇;计算值与实测值接近,水相和有机相的绝对平均偏差分别为0.62%和0.46%。

盐效萃取法分离环己酮-水恒沸物的研究

针对现有恒沸精馏提纯环己酮工艺能耗大的缺点,选用盐效萃取法分离环己酮-水恒沸物.测定了40℃时环己酮-水-氟化钾体系的液-液相平衡数据,用Pitzer理论和NRTL方程对液-液相平衡数据进行了关联计算,计算值与实测值吻合较好;考察了质量分数为60.0%氟化钾水溶液与该恒沸物的质量比对脱水率的影响.结果表明:当氟化钾水溶液与恒沸物的质量比为1.2时,氟化钾的脱水率高达99.04%.

顶空固相微萃取-气相色谱-质谱法测定水中四乙基铅

四乙基铅为神经剧毒物且具有高脂溶性,可以通过吸入、饮入、皮吸等途径摄入,严重危害人体健康[1]。四乙基铅曾被广泛应用于汽油抗震添加剂中,通过机动车尾气排放,加油站无组织排放等方式对环境造成污染[2]。含铅汽油虽已被禁用多年,但近年来,在一些环境水体、土壤甚至人体血液中仍然能检出四乙基铅[2-4]。因此,我国对于环境中四乙基铅的监测还一直非常关注。

盐效萃取分离共沸蒸馏后的正丁醇-水混合物

本文利用盐效萃取方法,选择不同无机盐,对超细SiO2共沸蒸馏后产生的饱和正丁醇-水溶液进行分离,结果表明无机盐溶液可以萃取出正丁醇水溶液中的正丁醇,且萃取效果随无机盐浓度提高而增大,温度对确定质量分数的盐溶液萃取效果影响很小。萃取比小于1.5时,萃取效果随其增大而显著增大;萃取比大于1.5时,萃取效果随其变化明显变缓。常温下,萃取比R=1.5时,60%K2CO3溶液对饱和正丁醇的水溶液的萃取率可达95%以上。有机相通过二次萃取,无机盐质量分数可降至10-4以下,可回收继续用于共沸蒸馏。K2CO3溶液的蒸发浓缩次数对萃取效果没有显著影响,表明K2CO3溶液具有良好的稳定性,可以满足工业循环使用要求。

Determination of magnolol and honokiol in traditional Chinese medicine Magnolia officinalis and its preparations by liquid-phase microextraction-back extraction combined with high performance liquid chromatography

Liquid-phase microextraction with back extraction （LPME-BE） combined with high performance liquid chromatography （HPLC） was investigated for the extraction and determination of magnolol and honokiol in Magnolia officinalis, a traditional Chinese medicine （TCM）, and its pharmaceutical preparations, Huo Xiang Zheng Qi peroral liquid and Xiang Sha Yang Wei pellet. Organic solvent, donor and acceptor phases, stirring rate and extraction limes were all factors which can influence the efficiency of extraction and were all optimized during the course of this work. Linear calibration curves were obtained in concentration ranges of 1,56-156 μg/mL for magnolol and 1.10-110 μg/mL for honokiol. Detection limits （S/N = 3） were 0.10 and 0.07 μg/mL, respectively. The relative recoveries were both in the range of 98.3% - 105.1% and RSD was lower than 2.5% .

A new combination process of distillation with salt extraction for separating organic solvent-water azeotropes

A novel process which can purify the organic solvents from their azeotropes with water is proposed. In this process,water can be drained off both from bottom and overhead of tower at the same time,and the organic solvent is concentrated in the tower and accumulated in the middle vessel at last. So the progress is time-shortened and energy-saving. The product purity is 99. 8% and the product yield is more than 99.5%. Simulation of liquid-liquid equilibrium (LLE) and the equipment operation data agree well with the experiment.

Determination of Eleutheroside B and E in Acanthopanax Preparations by High-P erformance Liquid Chromatography with Solid-Phase Extraction

Aim An HPLC method for analyzing eleutheroside B (ELU B) and eleutheroside E(ELU E) , two of the main active substances of Acanthopanax preparations were studied. Methods Thesamples were analyzed on a kromasil ODS column with water-acetonitrile as a gradient mobile phase.The flow rate was 0.8 mL·min^(-1) and detecting wavelengths were 206 nm for ELU B, 220 nm for ELUE, solid phase extraction (SPE) and internal standard-salicin were selected. Results The recoveriesof Acanthopanax tablets and injection were 90.4% - 96.8% and 96.4% - 99.8% for ELU B, 87.7% -93.3%and 95.7% - 98.5% for ELU E, respectively. The linear ranges were 4.45 - 22.25 μg· mL^(-1) (r =0.999 8) and 5.11 - 25.55 μg·mL^(-1) ( r = 0.999 7) respectively. Conclusion This method can savethe time for cleaning the chromatographic system and improve sensitivity for Acanthopanaxpreparations , thus providing a way to evaluate the quality of Acanthopanax preparations.

利用氟化钾从制药废液中回收正丁醇

测定了正丁醇-水-氟化钾体系在25℃时的液-液相平衡数据,以Pitzer理论和Wilson方程对液-液相平衡数据进行了关联计算,计算值与实测值接近,水相和有机相的绝对平均偏差分别为0.72%和0.56%。考察了氟化钾水溶液与制药废液质量比对脱水率的影响,结果表明,当质量分数为60%的氟化钾水溶液与该废液的质量比为0.75时,脱水率高达91.38%,将有机相进行精馏可得到质量分数为99.50%的正丁醇,水相中氟化钾稀溶液经蒸发回收后循环使用不影响分离性能。

Extraction of Cadmium from Sewage Sludge Using Polyepoxysuccinic Acid

Polyepoxysuccinic acid （PESA）, as an environmental benign biodegradable chelant, was used to remove heavy metals from the sewage sludge of Shanghai Taopu Wastewater Treatment Plant. The extraction of cadmium （Cd） from sewage sludge using aqueous solution of PESA was studied. It was found that PESA was capable of extracting Cd from the sludge, and the extraction efficiency was dependent on both pH and the concentration of the chelating reagent. The extraction efficiency decreased gradually with increasing of pH, whereas the dependency on pH decreased as the concentration of PESA increased. In the case of the high PESA to total metal ratio, e.g., 10：1, the extraction efficiency reached above 70% within the pH range from 1 to 7. The highest extraction efficiency obtained in tbe experiment was 78%. By comparing the contents of the heavy metals in sewage sludge before and after the extraction, it was found that the extracted Cd came mainly from the four fractions： acid-soluble, reducible, oxidizable, and water-soluble fractions.

Comparison between sequential and single extraction procedures for metal speciation in fresh and dried Sedum Plumbizincicola

Sequential and single extraction procedures were applied to both fresh and dried Sedum Plumbizincicola leaves and stems.The extractants, different from those of soil, sediment or sewage sludge metal fractions, were water, 80%(v/v) ethanol, 1 mol/L Na Cl,2% HAc and 0.6 mol/L HCl. Zn, Cd and Cu in the extracts and samples were measured by flame atomic adsorption spectrometry. In sequential extraction procedures, water soluble form and ethanol soluble form are the main fractions for Zn, while water soluble form and Na Cl soluble form for Cd, and comparatively uniform distribution for Cu with the residue form most and HCl soluble form second. Single extraction procedures are used to compare the extraction efficiencies of the five reagents to screen appropriate extractants and operating conditions for liquid extraction to deal with large amount of harvested metal-contained biomass, which will pose a threat to the environment if treated improperly. The sequences of extraction efficiencies are HCl>Na Cl≈HAc>Water≈Ethanol for Zn and HCl≈Na Cl≈HAc>Water>Ethanol for Cd. As for Cu, all the five extractants cannot effectively extract Cu, but HCl achieves a higher efficiency(>70% in fresh samples, and 45%-60% in dried samples). Besides, extraction efficiencies for most extractants in fresh samples are higher than those in dried samples, and extraction efficiencies of stems and leaves for the five extractants are close. The two extraction procedures can obtain high degree of accuracy with the relative standard deviation(RSD)lower than 10%, and metal recoveries are controlled between 80%-120% with most of 90%-110%.

Magnetic Solid-Phase Extraction of Phthalate Esters from Environmental Water Samples using Fibrous Phenyl-functionalized Fe3O4@SiO2@KCC-1

A new kind of phenyl-functionalized magnetic fibrous mesoporous silica(Fe3 O4@Si O2@KCC-1-phenyl) was prepared by copolymerization as an efficient adsorbent for the magnetic extraction of phthalate esters from environmental water samples. The obtained Fe3 O4@Si O2@KCC-1-phenyl showed monodisperse fibrous spherical morphology, fairly strong magnetic response(29 emu/g), and an abundant π-electron system, which allowed rapid isolation of the Fe3 O4@Si O2@KCC-1-phenyl from solutions upon applying an appropriate magnetic field. Several variables that affect the extraction efficiency of the analytes,including the type of the elution solvent, amount of adsorbent, extraction time and reusability, were investigated and optimized. Under optimum conditions, the Fe3 O4@Si O2@KCC-1-phenyl was used for the extraction of four phthalate esters from environmental water samples followed by high-performance liquid chromatographic analysis. Validation experiments indicated that the developed method presented good linearity(0.1-20 ng/m L), low limit of detection(7.5-29 μg/L, S/N =3). The proposed method was applied to the determination of phthalate esters in different real water samples, with relative recoveries of 93%-103.4%and relative standard deviation of 0.8%-8.3%.

Microwave-assisted Extraction of Effective Compounds from Traditional Chinese Herbal Medicine Ciwujia

Microwave-assisted extraction (MAE) for active ingredients in Ciwujia was studied by using ethanol as the extractant. Comparing MAE with conventional methods, the former can save the extracting time and increase the content of the active ingredients in product. As to the operation in MAE, the continuous radiation process is more convenient for the extraction for traditional Chinese medicine than the intermittent radiation process. Optimized by uniform design, MAE was proved to be an effective and novel process for extracting active ingredients in Ciwujia. The optimized MAE conditions are as follows: the microwave power is 510W, the radiation time 30min, the alcohol concentration at 80%, the ratio of solvent to solid material being 5:1, the soaking time 0.5h, and the herbal particle size is (520±19)μm.

Prediction of dispersed phase holdup in pulsed disc and doughnut solvent extraction columns under different mass transfer conditions

Using experimental data from a number of pulsed disc and doughnut solvent extraction columns, a unified correla- tion for the prediction of dispersed phase holdup that considers the effects of mass transfer is presented. Pulsed disc and doughnut solvent extraction columns （PDDC） have been used for a range of important applications such as ura- nium extraction and nuclear fuel recycling. Although the dispersed phase holdup in a PDDC has been presented by some researchers, there is still the need to develop a robust correlation that can predict the experimental dispersed phase holdup over a range of operating conditions including the effects of mass transfer direction. In this study, dis- persed phase holdup data from different literature sources for a PDDC were used to refit constants for the correlation presented by Kumar and Hartland lind. Eng. Chem. Res.,27 （1988）,131-138] which did not consider the effect of col- umn geometry. In order to incorporate the characteristic length of the PDDC （i.e. the plate spacing）, the unified cor- relation for holdup proposed by Kumar and Hartland based on data from eight different types of columns [Ind. Eng. Chem. Res.,34 （1995） 3925-3940] was refitted to the PDDC data. New constants have been presented for each hold- up correlation for a PDDC based on regression analysis using published holdup data from PDDCs that cover a range of onerating conditions and nhwical nronerties and consider the direction of mass transfer.

Improved determination of salicylaldoxime in water samples by liquid-liquid extraction followed by high performance liquid chromatographic analysis

For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatography with ultraviolet detector.Parameters including extraction solvent,ionic strength,solution pH,and extraction pattern were discussed for the optimal quantification of salicylaldoxime-spiked water.When the described method was applied to four spiked water samples,the obtained average extraction recovery rate was found between 87%–107%and relative standard deviation was below 6%.At the same time,good linear relationships were observed for spiked water samples from 0.01 to 10μg/mL(R2=0.9993).In addition,the detection limit of salicylaldoxime was revealed between 0.003–0.008μg/mL,which is two orders of magnitude lower than previously reported results.Thus,the presented method may be advantageous for the high-efficiency determination of salicylaldoxime in water samples.

Liquid-Liquid-Liquid Three Phase Extraction Apparatus:Operation Strategy and Influences on Mass Transfer Efficiency

Abstract A new mixer-settler-mixer three chamber integrated extractor is proposed in this work for liquid-liquid- liquid three phase countercurrent and continuous extraction. Experiments revealed the influences of the structural design of the three-liquid-phase extractor and some key operational parameters on three-phase partition of two phenolic isomers, p-nitrophenol （p-NP） and o-nitrophenol （o-NP）. The model three-liquid-phase extraction system used here is nonane （organic top-plaase）-polyethylene glycol （PEG 20UU） （polymer mlddle-phase）-（NH4）2SO4 aqueous solution （aqueous bottom-phase）. It is indicated that agitating speed and retention time in three-phase mixer are key parameters to extraction fraction of nitrophenol. Dispersion band behavior is related to agitating intensity, and its occurrence does not affect the extraction fraction of target compounds. The present work highlights the possibility of a feasible approach of scaling up of the proposed three-phase extraction apparatus for future in- dustrial-aimed applications.

Association between polycyclic aromatic hydrocarbons and human rectal tumor or liver cancer

Objective: The aim of this study was to investigate the effect of polycyclic aromatic hydrocarbons (PAHs) in rectal carcinoma and hepatocarcinoma genesis. Methods: The PAHs in the human rectal cancer and liver cancer tissues, the adjacent tissues and homologous tissues without rectal cancer or liver cancer were extracted by ultrasonic wave. The extracts were then cleaned up and enriched by solid phase extraction, analyzed by high performance liquid chromatography (HPLC) with fluorescence spectroscopy. Results: Four kinds of PAHs were detected in human rectal and hepatic tissues. The contents of pyrene, 2-methylanthracene and benzo (a) pyrene in both rectal cancer tissues and adjacent homologous tissues were higher than rectal tissues without rectal cancer, the differences were statistically significant (P < 0.05). The contents of phenanthrene in the three kind of tissue were not significant (P > 0.05). The differences of the content of each PAHs between rectal cancer and adjacent tissue were not significant (P > 0.05). The contents of the four PAHs in the three kinds of liver tissues were not statistically significant (P > 0.05). Conclusion: PAHs are found in human rectal tissues or hepatic tissues. The contents of PAHs in human rectal tissue may have an effect on the occurrence of human rectal cancer while the contents of PAHs in human hepatic tissues may have not ones.

Effect of water on extractive desulfurization of fuel oils using ionic liquids： A COSMO-RS and experimental study

When evaluating ionic liquids （ILs） for extractive desulfurization （EDS） of fuel oils, the inevitable presence of water in the system may have a significant and in many cases strongly negative effect. However, few studies have considered this particular issue and a promoted water effect on EDS is scarcely reported. In this work, COSMO-RS was firstly employed to calculate the capacity and selectivity for EDS of various IL/H20 mixtures, which cover different IL characters and a wide water concentration range. Experiments were then conducted with a representative IL [C4MIM]IH2P04], whose stable and even promoted extraction performance with a small amount of water was suggested by COSMO-RS. Through analyses of the desulfurization ratio, the cross- solubility and the water content in the desulfurized fuel, the promoted effect of water within a certain range （〈 10 wt%） was experimentally demonstrated. Moreover, such effect of water was explained combining the viscosity, the solvent-solute interactions and the COSMO-RS based analysis.

CS_2 extraction and FTIR & GC/MS analysis of a Chinese brown coal

The abundance of low-rank coals in China, such as bituminous and brown coals, makes studies of their composition and structure of great significance to both coal chemistry research and for efficient utilization of the coal. We describe how a Chinese brown coal was ultrasonically extracted with carbon disulfide （CS2） and the raw and extracted coals were characterized by Fourier Transform Infrared Spectroscopy （FTIR）. The corresponding extract was analyzed with a coupled gas chromatograph mass spectrometer （GC/MS）. The FTIR analysis shows a great abundance of amidocyanogen, carbonyl, aromatic and hetero aromatic rings and single carbon-beteroatom bonds. This suggests the possible occurrence of compounds like alcohols, phenols, amines, esters, carboxylic acids, ethers, aromatics or heteroaromatics. The GC/MS analysis of the CS2 extract detected 62 compounds, among which the non-polar ones were of lower abundance while the polar ones were in higher abundance and were structurally diverse. This demonstrates the compositional and structural complexity of Shengli coal.