Equilibrium and kinetic data of adsorption and separation for zirconium and hafnium onto MIBK extraction resin

The equilibrium and kinetics of methyl isobutyl ketone(MIBK) extraction resin for adsorption and separation of zirconium and hafnium were studied under the different conditions of acidity,initial total concentrations of zirconium and hafnium and temperature.The equilibrium data of both zirconium and hafnium are found to follow the Freundlich adsorption isotherm,and the Freundlich isotherm constants(KF) are 3.53 and 0.64 mg/g,respectively.The equilibrium data of zirconium also fit the Langmuir adsorption isotherm,and the saturation adsorption capacity(Qmax) and the Langmuir isotherm constant(KL)are 75.93 mg/g and-0.012 7 L/g,respectively.The obtained kinetic data of both zirconium and hafnium are found to fit the HO pseudo-second-order kinetic model,and the rate constants of pseudo-second-order equation(k2) are-0.019 and 0.41 g/(mg·min),respectively.Column tests show that the MIBK extraction resin could be used as efficient adsorbent material for separating hafnium from zirconium.

Extraction of cerium(Ⅳ) using tributyl phosphate impregnated resin from nitric acid medium

Tributyl phosphate （TBP） solvent was used for impregnation into Amberlite XAD-16 nonionic polymeric resin beads using the wet method to prepare solvent impregnated resin （SIR）. Undiluted TBP in a ratio to the resin support （volume to mass） of 6.0 at room temperature （RT） in 24 h was impregnated the resin with a mass ratio of 1.944, while the prepared gross sample of SIR at the ratio of solvent to resin of 3.0 was impregnated with a mass ratio of 1.88. Cerium（Ⅳ） oxide concentrate, prepared from crude Egyptian monazite sand, containing 37% cerium, 1.6% thorium and about 40% the other trivalent rare earth oxides, was used to prepare cerium（Ⅳ） nitrate solution for extraction using the prepared SIR. The impregnated resin was satisfactory for Ce（Ⅳ） extraction from nitric acid medium at room temperature. Cerium loading capacity of the impregnated resin reached 95.6% of the calculated theoretical capacity （173 g/kg （Ce/SIR）） under the conditions of 51.57 g/L cerium and 2.48 g/L thorium, 5.0 mol/L free nitric acid, solution to resin ratio of 10.0 and contacting the phases for 5.0 min. The loading capacity reached 98.75% when cerium concentration was increased to 91.43 g/L under the same conditions.

Progress in Solid-Liquid Extraction Resin for Separation of Rare Earth Elements

The latest development in solid-liquid extraction resin for the separation of REE was reviewed. The chemistry of inorganic supports based on diatomite, silica gel or alumina as well as organic supports based on cellulose, chitosan natural macromolecular support and poly(styrene-divinylbenzene), polyacrylate, aldehyde polymer, polyurethane, polyacrylonitrile synthetic macromolecular supports was covered, low molecular weight extractants such as acidic, organophosphorus, amine, macrocyclic compounds as well as macromolecular extractants were outlined. The different approaches involving ion exchange, ion-pair and chelating separation mechanisms were discussed. Physical adsorption, enclosing and chemical bonding mechanisms about extractants immobilized on solid supports were presented. The relation between resin shape and the property of packed columns was highlighted. Modern synthetic techniques such as molecular assembly, ionic imprinting, chemical modification for the preparation of resins were described. Basic fundamentals, advantages and synthetic methods of novel solid-liquid extraction resins as well as possibilities to improve resins performance were introduced.

Preparation and decolorization of sapindus mukurossi extract and its application in sebum-control shampoos

Background:Sapindus mukurossi extract(SME)is a kind of natural surface active ingredient with potential applications in cleansing products.However,the polyphenols and pigments contained in the extract may cause color browning of the products during storage especially at elevated temperatures,affecting its high level addition in the products.Objective:To explore a decolorization process suitable for industrialization realize the high level addition of SME and explore the potential of SME in the field of controlling sebum esters.Materials and Methods:SME was prepared by adsorbing polyphenols on the D301 resin and oxidation decoloring oxidation.Investigated its sebum-control efficacy by SZ95 model and clinical study.Results:The results demonstrate that the D301 resin displays the best adsorption selectivity for polyphenols in SME,and the polyphenol adsorption ratio of D301 resin(5 wt%)can reach 83.6%;The optimal decolorization conditions are pH=7.8,temperature 73℃and decolorization time 5.7 h when H2O2 content is 6%,The prepared SME shows no obvious changes in color and retain stable during the high temperature(50℃)test period of 28 days.4μg/mL of SME decreases the lipid synthesis of SZ95 cells by 24.8%.The clinic efficacy of the shampoo containing 10%SME(by dry extract weigh)is further evaluated.No significant changes in the skin moisture content and transepidermal water loss(TEWL)are observed within four weeks after using the product,while the scalp sebum level is significantly reduced.Conclusion:In this study,we prepared a light-colored,highly stable SME,enabled its high-level addition in cleansing and care products and found its sebum-control efficacy.

Evaluation study on properties of a macroporous silica-based CMPO extraction resin to be used forminor actinides separation from high level liquid waste

Basic properties of a silica-based octyl(phenyl)-N,N-diisobutylcarbamoyl-methylphosphine oxide (CMPO) extraction resin (CMPO/SiO2-P) was investigated.Adsorption behavior for some rare earth elements (RE) which are constituents of high level liquid waste (HLLW) and the long-term stability of the extraction resin in nitric acid solution were examined.The CMPO extraction resin was significantly stable in 3 mol·L?1 HNO3 solution at 50oC.Furthermore,the RE(III) were efficiently separated from non-adsorptive fission product (FP) elements such as Sr(II) in a column experiment using a highly nitric acid solution.The separation behaviors of the elements are considered to result from the difference in their adsorption and elution selectivity based on the complex formation with CMPO.There was no strong dependency of RE(III) separation efficiency on feed solution flow rate.Only from the perspectives of the acid-resistant behavior of CMPO extraction resin and the elution kinetics for the metal ions with the extraction resin,the CMPO extraction resin can be used in the modified MAREC process for HLLW partitioning.

The Extraction and Purification of Stevioside from Stevia

tevioside is a natural sweetener extracted from stevia,which is widely used in the food industry and the pharmacy.Centre on the extraction and purification of stevioside,using ADS-7 resin to extract stevioside through one single step,greatly shorten the process and solve the problems of lower yield and higher raw materials cost existed in the general process.

Solid-liquid extraction for yttrium recovery using porous polymeric resin(XAD-7) functionalized with D_(2)EHPA

The recovery of yttrium is proposed by applying a solid-liquid extraction process using di-2-ethyl hexylphosphoric acid(D2EHPA) as extracting agent.The extracting agents were supported on a macro porous polymeric resin XAD-7(solid phase).Yttrium ions extraction and discharge tests were performed,firstly from a synthetic aqueous solution of 100 mg/L Y(liquid phase) at 25℃ with stirring.The effects of pH of aqueous solutions bearing yttrium,volume fraction of extracting agents and the solid/liquid(S/L)ratio on the yttrium recovery were studied.The most favorable conditions for yttrium ions extraction are;20 vol% D_(2)EHPA functionalized resin,pH=1.5 and an S/L ratio of 10 mg/mL The discharge of yttrium ions was done under the same conditions of extraction stage,using a 2 mol/L [H_(2)SO_(4)] as stripping solution.Up to 80% yttrium is extracted,while 75% yttrium is recovered in the striping solution.In all experiments,the reaction equilibrium is reached after 20 min,and the kinetics for the extraction stage was determined as a second-order model.Also,experiments were carried out to discharge the yttriumloaded resins,and it has been determined that the best pH value to strip the Y ions is 1.5.Cyclic tests of extraction and discharge for yttrium ions show that the functionalized resin can work at least five cycles without decreasing its efficiency.Finally,the proposed process was tested in a real solution with Y ions fro m a waste fluorescent la mp powder leached in H_(2)SO_(4),demonstrating the ability to effectively recover yttrium,separating it from various metals from the studied residue.

Synthesis of condensed polynuclear aromatic resin from furfural extract oil of reduced-pressure route Ⅱ

As an industrial byproduct of oil refining,furfural extract oil from reduced-pressure route Ⅱ with high aromatic content was used to prepare heat-resistant condensed polynuclear aromatic（COPNA） resin for the first time.The basic properties of furfural extract oil and the resultant COPNA resin were characterized by infrared spectroscopy（FT-IR）,nuclear magnetic resonance spectroscopy（1H-NMR）,thermogravimetric analysis（TGA） and elemental analysis（EA）.The result showed that heat treated furfural extract oil was successfully used for the synthesis of heat-resistant COPNA resin.The average structural parameters of raw materials and prepared resin were calculated by the improved Brown-Ladner method,and the averaged molecular structure of the resin was obtained.The reaction mechanism for the synthesis of COPNA resin was suggested as an acid-catalyzed positive ion type polymerization.

1Assessing Soil Available Potassium by Cation Exchange Membrane and Conventional Chemical Extractions

Four testing methods using canon exchange membrane (CEM), ammonium acetate, ASI (0.25 mol L-1 NaHCO3+0.01 mol L-1 EDTA +0.01 mol L-1 NH4P) and 1.0 mol L-1 boiling nitric acid, respectively, were used to evaluate soil available K. The soil K tested by CEM was significantly correlated with that by the other (conventional) methods (r2=0.43**~0.95***). The soil K tested by CEM saturated with NH4HCO3 (15 min extraction) was most closely correlated with that by the other methods (2 =0. 60***~0.95***). Potassium availability, as predicted by soil test, was comparable to actual K uptake by canola and wheat grown on the soils in growth chamber. Regression analyses showed that plant K uptake was more closely correlated with K extracted by CEM (r2=0.56***~0.81***) than that by the conventional methods (r2=0.46***~;0.81***), most closely correlsted with that by NH4HCO3-saturated CEM for 15 min (r2=0.81***), and worst correlated with that by HNO3 (r2=0.45**~0.72***).

ADSORPTION OF GOLD ON TBP EXTRACTING RESIN FROM HCI SOLUTION

Adsorption of gold on TBP extracting resin from HCI solution was researched. All the effects of factors, such as solution acidity, TBP content,tempo)uture, etc. , on adsorption equilibrium were discussed and the equilibrium equation was formulated. The breakthough time of adsorption process withfixed bed uns studied through experiment.

锌冶炼过程中提取镓的技术研究及其进展

针对镓从锌冶炼过程中回收占比低的问题,总结分析了锌冶炼过程中镓回收技术研究进展.在鼓风炉炼锌(ISP)工艺中,镓主要富集在鼓风炉炉渣里,其质量分数通常在0.025%~0.031%,从鼓风炉炉渣中回收镓主要有还原蒸发法、高温氯化挥发法、硫酸浸出法、碱熔–浸出法、还原熔炼–电解法和还原熔炼–熔融造渣法等方法,但这些工艺普遍流程长,回收率低,加工成本偏高,部分工艺环境污染大,难以工业化应用.传统的湿法炼锌工艺中,大于93.5%的镓富集在浸出渣中,浸出渣处理以火法还原挥发工艺为主,在回转窑挥发浸出渣工艺中90%的镓保留在窑渣中,导致镓的回收流程长且回收率低,湿法处理浸出渣存在镓和铁分离的难题,至今未得到有效解决.氧压浸出炼锌工艺中,镓主要富集在锌粉置换渣里,锌粉置换渣采用酸性浸出和萃取工艺分离富集镓,最终制备金属镓,镓的综合回收率达到71%.通过对火法和湿法炼锌中镓回收工艺进行分析,对镓回收工艺中存在的关键问题和分离技术进行了总结,提出萃取分离、乳状液膜和树脂吸附有望成为锌冶炼过程中回收镓的绿色高效短流程关键技术.

Solvent impregnated resin prepared using ionic liquid Cyphos IL 104 for Cr(VI) removal

Ionic liquid (IL) trihexyl (tetradecyl) phosphonium bis 2,4,4-trimethylpentylphosphinate (Cyphos IL 104) was impregnated on XAD-7 resin. The solvent impreganated resin (SIR) was prepared and applied in Cr(VI) removal. The morphology and the thermal stability of the resins were explored. The effects of equilibrium time and initial pH value on Cr(VI) adsorption were investigated. Adsorption isotherm, separation and desorption of the SIR, and selectivity of SIR were also explored. The results show that Cyphos IL 104 exists in the inner XAD-7 resin, and the optimum pH value range of the SIR for Cr(VI) extraction is 0 to 2. When NaOH used as desorption solution, the Cr(VI) can be effectively desorbed from the SIR.

白术多糖提取分离工艺研究

目的优选白术多糖的提取分离工艺。方法比较氯仿-正丁醇Sevage法去蛋白与不去蛋白白术多糖含量。以吸附率和解吸率为考察指标,优选AB-8型、D101型、LX-38型3种大孔吸附树脂。通过吸附时间、解吸时间、上样流速、上样浓度、洗脱剂用量、洗脱剂浓度和洗脱流速研究AB-8型大孔树脂纯化白术多糖工艺。结果未去蛋白的多糖含量为(5.582±1.4480)%、(5.407±0.7668)%、(5.155±0.7214)%,Sevage法去蛋白后的多糖含量为(4.658±0.1558)%、(4.247±0.0742)%、(4.610±0.1734)%。AB-8型大孔树脂较其他两种树脂,其吸附率及解吸率可达(18.40±0.0300)%,(91.73±0.0781)%,纯化工艺为吸附时间3 h、解吸时间3 h、上样流速1 BV/h、上样浓度0.75 mg/mL、洗脱剂用量4 BV、洗脱剂浓度15%乙醇、洗脱流速3 BV/h。结论本试验为白术多糖的提取分离提供了试验依据,为白术多糖的工业化生产提供了参考。

超声浸提-电感耦合等离子体发射光谱法测定石灰性土壤中的有效磷

采用超声浸提-电感耦合等离子体发射光谱法(ICP-AES)实现了石灰性土壤中有效磷的快速、准确、批量化分析要求.将水土混合液在400 W超声功率下于25℃浸提10 min,用3.50 g苯乙烯阳离子交换树脂降低基体干扰.分析谱线P 214.914 nm,射频功率1150 W,载气流量0.6 L/min,采用ICP-AES测定有效磷.结果显示:磷在0~5.00 mg/L范围内校准曲线线性良好(相关系数0.9996),检出限为0.072 mg/kg.方法用于4种不同碱性土壤有效态标准物质的分析,测定值相对误差小于±7%,相对标准偏差小于10%,且和标准方法(NY/T 1121.7—2014)测定值接近.

两面针粗生物碱的富集

目的探索两面针对体外人红系白血病细胞(HEL细胞)增殖活性有抑制作用的粗生物碱富集方法,为两面针药材抗肿瘤活性研究提供参考。方法以不同浓度(60%、70%、80%、90%、100%)乙醇对两面针药材的干燥根进行提取,以最高提取率确定最佳提取条件;通过静态、动态吸附实验考察不同类型(HPD 100、XDA-5、D101、HPD 722、HPD 400)大孔树脂对两面针药材的吸附量确定上样量,富集两面针粗生物碱;采用噻唑蓝(MTT)法研究各组粗生物碱对HEL细胞增殖活性的影响。结果两面针药材经5种浓度乙醇提取,其中60%乙醇提取浸膏的得率最高[(11.937±0.002)%];静态、动态吸附实验表明,5种大孔树脂对两面针药材吸附量为1:500(两面针浸膏:大孔树脂);不同型号大孔树脂富集得到的粗生物碱对HEL细胞的增殖活性影响不同,两面针粗生物碱样品浓度为80μg·mL-1时,抑制率分别为(59.62±3.46)%(XDA-5)、(55.81±5.16)%(HPD 100)、(59.33±1.33)%(D101)、(79.63±1.02)%(HPD 722)、(83.97±0.38)%(HPD 400),HPD 400型大孔树脂富集的两面针粗生物碱抑制HEL细胞增殖作用最显著(P<0.01)。结论大孔树脂富集两面针粗生物碱工艺简单、可行,HPD 400型大孔树脂富集的两面针粗生物碱对HEL细胞抑制作用显著。

马蓝叶吲哚苷提取纯化工艺优化及其抑菌活性评价

采用超声波低温提取结合大孔树脂吸附分离技术从马蓝叶中提取富集吲哚苷,在单因素试验基础上通过响应面法优化超声波提取工艺,从6种大孔树脂中筛选最适类型并确定大孔树脂纯化吲哚苷的吸附/解吸最佳工艺条件,制备高纯度吲哚苷提取物;采用96孔板微量法测定了高纯度吲哚苷对金黄色葡萄球菌和大肠杆菌的抑菌活性。研究结果表明:超声波提取的最佳工艺条件为5 g干燥马蓝叶粉末、超声波功率458 W、提取时间29 min、温度32℃、料液比1∶10(g∶mL)、提取2次,在此条件下马蓝叶吲哚苷提取率为(93.15±0.26)%。X-5型大孔树脂对吲哚苷吸附/解吸效果最好,大孔树脂纯化最优条件为:大孔树脂100 g、提取液上样量500 mL、洗脱液乙醇体积分数为40%、洗脱液体积400 mL,该条件下吲哚苷回收率为(82.97±0.30)%,纯度由(18.32±0.18)%提升至(86.43±0.31)%;吲哚苷粗提物对金黄色葡萄球菌和大肠杆菌的最小抑菌质量浓度(MIC)值均为350 mg/L,经纯化后的高纯度吲哚苷提取物对金黄色葡萄球菌和大肠杆菌的MIC值分别为21.88和43.75 mg/L,显示出比阳性对照硫酸庆大霉素(MIC值分别为43.75和87.50 mg/L)更好的抑菌效果。

超声辅助酶提取、双水相萃取及大孔树脂纯化天麻素的工艺研究

目的:优化超声辅助酶提取天麻中天麻素工艺并通过双水相萃取和大孔树脂进一步纯化,为精制天麻素提供工艺参考。方法:通过单因素试验考察和正交优化试验得到最佳超声辅助酶提取条件。通过双水相工艺考察得到最佳双水相萃取条件。通过大孔树脂工艺考察对大孔树脂型号进行筛选,对上样条件、洗脱条件进行优化。结果:超声辅助酶提取选择α-淀粉酶,最佳提取条件设定为料液比为1∶30,加酶量为0.8%,酶解时间为80 min,酶解温度为60℃,酶解pH值为5.5。最佳双水相萃取条件设定为乙醇体积分数为47.5%,硫酸铵质量分数为15.0%,萃取液浓度为0.2 g/mL,大孔树脂筛选型号为HPD100,最佳上样浓度为0.2 g/mL,径高比为1∶5,上样流速为3 BV/h,上样量为100 mL,最佳洗脱液体积分数为30.0%,洗脱流速为4 BV/h,洗脱液用量为230 mL。结论:本研究对超声辅助酶提取工艺优化结果较好,采用双水相体系和大孔树脂纯化,使天麻素纯度明显提高。且这一系列工艺稳定可靠,可为后续制剂及新药研发奠定基础。

顶空-气相色谱法测定到手香提取物11种溶剂残留量

目的建立顶空-气相色谱法测定中药到手香提取物中苯、丙烯腈、甲基丙烯酸甲酯、甲苯、1,2-二氯乙烷、对二甲苯、间二甲苯、邻二甲苯、氯苯、苯乙烯和二乙烯苯11种溶剂残留的分析方法。方法供试品经顶空进样器85℃平衡45 min,分流比10∶1(V∶V),采用DB-WAX聚乙二醇为固定相的弹性石英毛细管柱(长30 m,内径0.32 mm,膜厚0.5μm),FID氢火焰离子化检测器进行分析。结果11种挥发性有机物分离效果较好,在0.22~23.86μg·mL^(-1)的浓度范围内线性关系良好(r≥0.99);方法定量限为0.0084μg·mL^(-1)≤LOQ≤0.5432μg·mL^(-1);低、中、高水平下各成分的平均回收率为84%~103%之间;相对标准偏差≤10%(n=6),经方法学验证后该方法符合实验要求。3批样品中甲苯、间二甲苯、邻二甲苯及二乙烯基苯有检出,低于定量限,均未超标。结论该方法易于操作,结果可靠,可用于中药到手香提取物中的残留溶剂检测,亦为其他中药提取物中残留溶剂分析提供方法参考,确保用药安全。

一种适用于梅花鹿源性产品鉴定的微量组织DNA提取方法的建立

为建立一种适宜梅花鹿源性产品分子鉴定的高效、便捷微量组织基因组DNA提取的方法。本研究分别以鲜品梅花鹿茸、风干梅花鹿茸、烘干梅花鹿茸、鲜品梅花鹿鞭、烘干梅花鹿鞭、风干梅花鹿鞭、鲜品梅花鹿肉、干品梅花鹿尾、梅花鹿血为样本,采用Chelex-100树脂溶液和蛋白酶K结合的方法提取基因组DNA,并检测其浓度与纯度;以此DNA为模板,扩增梅花鹿线粒体DNA的Dloop区特异性基因,并对PCR扩增产物进行琼脂糖核酸电泳及测序。结果表明,基于Chelex-100树脂提取法获得的基因组DNA模板浓度为52.57~63.39 ng/μL,A260/A280比值为1.75~1.96;梅花鹿线粒体特异性基因扩增产物电泳条带清晰,且长度准确;扩增产物测序,相似性大于95%。Chelex-100树脂提取法能够提取微量梅花鹿组织样本基因组DNA,且此方法低价、简便,适用于梅花鹿源性产品的真伪鉴定。

苦荞酒糟黄酮富集生产苦荞蒸馏酒的研究

苦荞富含生物类黄酮,但由于其沸点较高,作为原料酿造白酒时会残留在酒糟中。该研究通过苦荞和大米发酵制备苦荞蒸馏酒,采用单因素及正交试验优化了苦荞酒糟中黄酮类物质的提取工艺与纯化工艺,添加纯化的黄酮提取物到蒸馏酒中,并通过感官评价确定了富含黄酮的苦荞蒸馏酒配制方案。结果表明,超声提取苦荞酒糟黄酮最佳工艺为超声功率600 W、乙醇体积分数90%、料液比1∶30(g∶mL)、超声时间50 min,此工艺条件下总黄酮得率为0.9%,纯度为38.3%;大孔树脂纯化苦荞酒糟黄酮工艺条件为:pH=4,上样流速2 mL/min,上样质量浓度0.2 mg/mL,50 mL体积分数70%乙醇洗脱,洗脱流速11 mL/min,经此工艺制得苦荞酒糟黄酮提取物纯度为85.36%;苦荞蒸馏酒的最佳配制方案为:添加纯化的黄酮提取物至蒸馏酒中,使得总黄酮提取物含量为400~600 mg/L时,复配型苦荞蒸馏酒评分最佳。该研究优化工艺下可得较高纯度黄酮提取物,复配可得苦荞香明显、口感柔和、风味协调富含黄酮类物质的苦荞蒸馏酒。