树脂法分离纯化米洛培南

采用国产AAS大孔吸附树脂及D－280大孔脱色树脂对抗生素米洛培南制备母液进行分离纯化。实验表明，与日本Diaion公司生产的Diaion CHP20相比，AAS大孔吸附树脂对米洛培南具有更优良的吸附性能，使用D－280大孔脱色树脂对抗生素米洛培南制备母液进行脱色，未发现类似报道，分析结果证实，以上述方法制备的抗生素米洛培南收率高，纯度高，各项分析数据与文献报道相符。     

THE SEPARATION，PURIFICATION AND DECOLORIZATION OF NEW ANTIBIOTICS—MILUPEINAN USING ADSORPTION RESIN

Adsorption resin AAS was used for the separation and purification of milupeinan (M-13)from its mother liquor. The good adsorption property of AAS adsorption resin was found formilupeinan (M-13) compared with the Diaion CHP 20p. When acetone and water (2:1 in volume)were used as desorption reagents, it was found that 3 times of bed volume of the desorption reagentswould make the AAS resin which was saturately adsorpted M-13 desorption completely.Also a macroporous anion exchange resin (Poly-4-vinylpyridine type) D-280 was used for thedecolourization from M-13 solution. Good results was given when the sr=1～2.     

Study on Adsorption and Separation of Naringin with Macroporous Resin

X-5 resin, with higher adsorption and easier desorption of naringin, was selected from five kinds of macroporous resins through static adsorption and desorption experiments. Effects of concentration, pH value, and flow rate of naringin extract on the adsorption of naringin by X-5 resin were studied. Meanwhile, the effect of these factors on the desorption of naringin from X-5 resin was also investigated. The experimental results show that the adsorption isotherm of naringin by X-5 resin can be described by the Langmuir isotherm equation. The static maximum adsorption capacity of naringin is 32.6 mg/g with naringin concentration at 2.7 g/L, while the dynamic adsorption capacity of naringin is 23.8 mg/g with naringin extract flow rate at two times that of resin volume per hour. The optimal eluant is 60% (v/v) ethanol-water with pH value of 10. The desorption ratio will rise to more than 85% when the flow rate of this optimal eluant is one to two times that of resin volume per hour. Translated from Journal of Central South University (Science and Technology)     

大孔吸附树脂分离纯化异甘草素的研究

研究大孔吸附树脂分离纯化异甘草素的工艺条件及参数。通过研究HPD-600、D4020、D101、AB-8、NKA-II、AL-2和NKA-9树脂对异甘草素的吸附和解吸附能力,筛选最佳树脂为AB-8,并研究了其对异甘草素的吸附和解吸附性能,确定了最佳的吸附与解吸附工艺参数,吸附:pH=5,室温,流速1.5BV/h,溶液处理量为5BV;脱附:洗脱剂为70%的乙醇溶液,流速1BV/h,洗脱剂用量4.5BV。异甘草素样品溶液经AB-8树脂吸附与脱附后回收率为76.7%,纯度由2.02%提高到29.1%,提高了14.4倍。实验结果表明,AB-8树脂对异甘草素的吸附量大,脱附容易,可以应用于异甘草素的分离纯化。     

Separation and purification of flavonoid from Taxus remainder extracts free of taxoids using polystyrene and polyamide resin

An efficient separation process of flavonoid from Taxus wallichiana var. mairei remainder extracts free of taxoids was developed in this study. AB‐8 macroporous resin and polyamide resin offered the fine adsorption capacity, and its adsorption rate at 30°C fitted well to the Langmuir and Freundich isotherms. Resin dynamic adsorption and desorption experiments were conducted to optimize the separation process of total flavonoids from T. wallichiana var. mairei remainder extracts free of taxoids. The optimum parameters for adsorption by AB‐8 resin were as follows: (1) the concentration of flavonoids in a sample solution of 5.61 mg/mL with a processing volume of 2 bed volume (BV) (60 mL); (2) for desorption, ethanol–water (80:20, v/v), with 6 BV as an eluent at a flow rate of 2 BV/h. After a one‐run treatment with AB‐8 resin, the content of flavonoids was increased 5.10‐fold from 4.05 to 20.65%. The optimum parameters for adsorption by polyamide resin were as follows: processing volume of 2 BV (30 mL); for desorption, ethanol–water (70:30, v/v), with 8 BV as an eluent at a flow rate of 2 BV/h. After one‐run treatment with polyamide resin, the content of total flavonoids increased from 20.65 to 65.21%. The method will provide a potential approach for large‐scale separation and purification of flavonoid for its wide pharmaceutical use.     

大孔阳离子交换树脂对奈替米星的吸附研究

通过正交实验合成了9种大孔弱酸性阳离子交换树脂,筛选出具有最大动态饱和吸附量的FB-1树脂.采用红外光谱和热重分析的方法对其表征,并研究其对奈替米星的吸附及解吸性能,结果表明:该树脂对奈替米星的吸附符合Langrnuir吸附:用氨水做洗脱剂,0.3mol/L和0.4mol/L的氨水解吸率均达95%以上.FB-1与HD-2树脂比较:动态吸附量FB-1为398.0mg/mL湿树脂、HD-2为232.1mg/mL湿树脂;0.3mol/L氨水解吸,前者解吸率较后者高约15%.     

ADSORPTION AND DESORPTION OF DSD ACID MANUFACTURING WASTEWATER ON MACROPOROUS RESIN

4,4‘-diaminostilbene-2,2‘-disulfonic acid (DSD acid) manufacturing wastewater was treated by a macroporous resin in a fixed-bed column.The results showed that this method was suitable for removal of chemical oxygen demands(COD) and color,About 91% COD and 99.5% color removal were obtained under the optimum adsorption conditions.i.e.temperature 20℃,flow rate lbed volume/hour(BV/hr)and pH1-2.The resin was efficiently regenerated with aqueous sodium hydroxide and water.Furthermore,65.5% of 4,4‘-dinitrostilbene-2,2‘-disulfonic acid(DNS) could be recovered from wastewater for possible recycling to the manufactureing process.The adsorption capacity of resin remained constant during the repetition process of adsorption and desorption.     

Zn2＋型磺酸树脂对维生素B12的配位吸附及洗脱性能

原位吸附;分离;Zn2＋型磺酸树脂对维生素B12的配位吸附及洗脱性能     

大孔树脂-高速逆流色谱法分离纯化地黄中毛蕊花糖苷

该文建立了大孔树脂-高速逆流色谱分离中药材地黄中有效成分毛蕊花糖苷的方法。考察了4种大孔树脂对地黄粗提物中毛蕊花糖苷的静态吸附与解吸情况,其中D101大孔树脂对目标成分的吸附率与解吸率最理想,实验结果表明体积分数为10%的乙醇洗脱得到的毛蕊花糖苷含量最高,目标成分含量从4.9%提高到32.6%。最后,部分纯化的样品（165 mg）采用高速逆流色谱进一步纯化,两相溶剂系统由乙酸乙酯-正丁醇-水（1：4：5,v/v/v）组成,分离得到45 mg纯度为96%的毛蕊花糖苷。     

酚醛型吸附树脂对VB_(12)的吸附性能研究

研究了酚醛型吸附树脂JDW 1、JDW 2 (自制 )和DuoliteS 76 1对VB12 的静态和动态吸附 .结果表明 ,JDW 1对VB12 的吸附量达 84mg g ,明显优于DuoliteS 76 1;吸附VB12 的初始阶段 ,即达到 4 3%～6 9%平衡吸附时 ,吸附速率数据和半经验速率方程很吻合 ;酚醛型吸附树脂等温吸附VB12 的平衡吸附数据符合Langmuir方程 ,相关系数在 0 99以上 ,因此 ,酚醛型吸附树脂吸附VB12 属单分子层吸附 ;在动态条件下 ,用含甲醇 80 %溶液以 1 1BV h来洗脱吸附VB12 的JDW 2 ,在 4 2、6 4个床体积的洗脱率分别是 92 2 0 %、95 93% ,这表明酚醛型吸附树脂具有良好的洗脱性能 ,用含甲醇为 80 %溶液作洗脱剂从JDW 2洗脱VB12 ,效果很好     

Preparation of magnetic anion exchange resin and their adsorption kinetic behavior of reactive blue

Magnetic anion exchange resin(MD-1) was prepared from quaternization of magnetic copolymeric resin(glycidyl methacrylate -eo-divinylbenzene).For comparison,magnetic resin MD-0 without quaternization and non-magnetic resin(D-1) were also synthesized for the adsorption process.It was found that the adsorption was mainly contributed to the chemical interaction between quaternary ammonium groups and reactive blue RXHC.Due to the smaller size,MD-1 had faster adsorption and desorption kinetics than D-1.Coupled with the advantage of easy separation,the magnetic anion exchange resin was considered to be superior to common anion exchange resin in removal of reactive dye.     

SP700大孔树脂纯化酸枣仁中三萜总皂苷的研究

从7种极性不同的大孔树脂中筛选出一种对酸枣仁三萜总皂苷具有良好吸附和解吸性能的树脂—三菱SP700树脂。静态实验中,该树脂的最高吸附容量可达131.0mg皂苷/g树脂,皂苷在树脂表面的吸附符合Langmuir模型,用体积分数为90%的乙醇解吸得率最高可达97.8%;动态实验中,样液在膨胀床模式下上样,树脂的平均动态吸附容量为15mg皂苷/g树脂,上样后,用体积分数分别为50%和90%的乙醇溶液进行分段洗脱,洗脱得率最高可达到95.1%,经过纯化的皂苷提取物的含量提高了4倍。SP700大孔吸附树脂作为一种对酸枣仁中三萜总皂苷进行纯化的介质具有良好的性能和应用价值。     

树脂法提取茶多酚的研究

本文研究了用大孔吸附树脂由茶叶提取茶多酚的方法。通过对树脂的筛选，确定了NK-S3树脂对茶多酚吸附-解吸性能良好；选择由乙醇、乙酸乙酯和水组成的混合液为脱附剂；研究了流速对吸附、脱附性能的影响，并解决了茶水的前处理问题。     

茶碱印迹酚醛吸附树脂的研究

采用反相悬浮聚合技术,合成了茶碱模板酚醛吸附树脂和非模板酚醛吸附树脂,比较了两种树脂对茶碱的吸附状况.结果表明.对茶碱的吸附数据符合Langmuir方程,吸附属于单分子层吸附.在一定浓度范围内的吸附数据符合Freundlich方程,表明吸附是优惠吸附.Scatchard分析表明茶碱模板酚醛树脂具有特定的高亲和性吸附位点...     

The synthesis of new polymeric sorbent and its application in preconcentration of cadmium and lead in water samples

Metal determinations at low concentration levels (≤ng mL⁻¹) comprise one of most important targets in analytical chemistry. This interest also increases in different areas such as biology, medicine, environment and food samples. In spite of inherent high sensitivities obtained for electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma-mass spectrometry (ICP-MS), these techniques have some limitations depending on the concomitants. As a result, interest in preconcentration techniques still continues increasingly for trace metal determinations by flame atomic absorption spectrometry (FAAS) due to the high accuracy of this method.In this work, thioureasulfonamide resin was synthesized, characterized and applied as a new sorption material for determinations of cadmium and lead in water samples. The method is based on the sorption of Cd and Pb ions on the synthesized resin without using any complexing reagent. The optimization of experimental conditions was performed using factorial design including pH, amount of resin, contact time, first sample volume and final eluent volume. Using the experimental conditions defined in the optimization, the method was applied to the determination and preconcentration of Cd and Pb at ng mL⁻¹ level in natural water. Flame AAS was used for trace metal determinations. This method exhibits the superiority in compared to the other adsorption reagents because of the fact that there is no necessity of any complexing reagent and optimum pH of solution presents in acidic media. Consequently, 600- and 360-fold improvements in the sensitivity of FAAS were achieved by combining the slotted tube atom trap-atomic absorption spectrometry (STAT-FAAS) and the purposed enrichment method for Cd and Pb, respectively.     

Synthesis of the water-compatible p-acetaminophen resin and its adsorption performances for vanillin in aqueous solution

A novel p-acetaminophen resin(named as GQ-1) was synthesized with chloromethylated polystyrene and p-acetaminophen.It can be used without any wetting process.The objective of this work was to study the adsorption performances for vanillin onto GQ-1 with two kinds of the hydrogen bond site of acetamino group and hydroxyl group.The results showed that the adsorption property of vanillin onto GQ-1 was superior to XAD-4,H103,NDA150,and NDA88.The adsorption capacity of vanillin onto GQ-1 is not greatly discrepant until the solution pH is higher than 5.31.The saturated adsorption quantity of vanillin was up to 141.32 mg/mL(wet resin) according to the dynamic adsorption and desorption experiments at 293 K.The resin could be regenerated by 7 BV ethanol.     

新型酰乙基葡甲胺树脂的合成及吸硼性能

采用一步法, 用氯乙酰化聚苯乙烯树脂(PS-Acyl-Cl)与葡甲胺反应制得一种同时含有α-酰乙基胺和邻羟基双官能团的新型酰乙基葡甲胺树脂, 考察了溶液pH值、 温度、 初始浓度和吸附时间对酰乙基葡甲胺树脂吸附硼的影响. 结果表明, 在实验浓度范围内, 该树脂对硼的吸附符合Langmuir方程, 最大吸附量约为28.1 mg/g干树脂, 优于氯甲基树脂制得的硼特效树脂. 表明α-酰乙基胺和邻羟基双官能团对硼有双重或协同吸附作用. 该树脂在pH=6.0时对硼的吸附量最大; 温度对树脂吸附的影响不大; 树脂解吸率大于96%; 树脂重复使用5次后吸附量基本不变. 动力学研究结果表明, 吸附过程为液膜扩散控制过程.     

Separation and Purification of Glufosinate Through Combination of an Electrodialysis Membrane and a Macroporous Adsorption Resin

Glufosinate is a nonselective organophosphorus herbicide with low toxicity and high efficiency that is widely used in forestry, agriculture and other industries. In the process of manufacturing glufosinate, large amounts of ammonium chloride and coloured organic impurities are generated. Because of its high solubility in water, separation of glufosinate from inorganic salts is extremely difficult. Hence, a co-separation method combining an electrodialysis membrane and a macroporous adsorption resin was developed to obtain glufosinate with higlier purity. For the electrodialysis process, a glufosinate reaction solution was placed in a dilute chamber and desalinated. The concentration of inorganic salts in the resultant glufosinate aqueous solution was only 0.99 g/L under the optimal conditions of an operating voltage and a volume ratio of 9 V and 1:1, respectively. For the macroporous resin adsorption/desorption process, the sample solution treated by electrodialysis was pumped into the resin-filled column, which was eluted to obtain the eluent when the adsorption reached equilibrium. Consequently, nearly all the coloured organic impurities were removed under the optimal conditions, in which the resin type, pH value, flow rate, glufosinate concentration, temperature, ratio of ethanol and volume of eluent were LX-300C,3,0.5 mL·cm^2·min^-1,20 mg/mL,25℃, 50% and 400 mL, respectively. After the electrodialysis and adsorption/desorption process, the purity of the glufosinate was increased to 95.14%, and its recovery rate was as high as 98%. The advantages of this process included its ease of operation, environmental friendliness and low cost, which provided strong potential for its use in industrial applications.     

大孔树脂对白蜡种子鞣质的纯化工艺研究

选择6种大孔吸附树脂,比较其对大叶白蜡种子鞣质的吸附量和解吸率,筛选出较优的大叶白蜡种子鞣质吸附剂,并通过单因素实验和正交实验,对其静态吸附-解吸和动态吸附性能进行考察。实验结果表明,NKA-9树脂适合大叶白蜡种子鞣质的吸附分离,其最佳的吸附工艺参数为:上样浓度为3mg/mL、pH值为4、上样量为7BV、上样流速为1BV/h。     

Efficient adsorption and desorption of Cu2+ by a novel acid-resistant magnetic weak acid resin

A novel magnetic weak acid resin NDMC-1 was prepared in the presence of methyl acrylate（MA）,divinylbenzene（DVB） and titanate coupling agent（TCA） coated 7-Fe₂O₃ particles.To evaluate the adsorption of Cu²⁺ on the obtained resin NDMC-1,another two magnetic resins NDMC-0（the precursor of NDMC-1 without hydrolyzation） and NDMO-l（the synthesized weak acid resin using oleic acid coatedγ-Fe₂O₃） were chosen for comparison.The results showed that the carboxyl groups were formed after hydrolyzation,and NDMC-1 exhibited a greater adsorption capacity to Cu²⁺.The desorption experiment demonstrated that the desorption ratio at pH 2（95.14%） was greatly higher than pH 3（25.97%）.Moreover,the magnetic resin NDMC-1 was proved to be stable at pH 2,extending the application of magnetic materials which were always considered to be acid-nonresistant.