以CaCl2-NH3-CO2为反应体系,采用分散鼓泡碳化法制备出单分散纯球霰石型碳酸钙微球.用扫描电镜(SEM、FE-SEM)、透射电镜(TEM)、X射线衍射(XRD)等手段对样品进行了表征.考察了反应初始pH、反应终止pH、反应初始温度、二氧化碳气体流速等因素对产物颗粒形貌和粒径的影响,并探讨了球霰石微球的形成机理.实验结果表明,与直接鼓泡碳化法相比,分散鼓泡碳化法形成的二氧化碳气泡数量多、大小均匀,能增大溶液中二氧化碳的过饱和度,有利于制备高纯度的单分散球霰石微球;反应初始温度低、二氧化碳气体流速大,均有利于球霰石的生成.最佳反应条件:反应初始pH为10.0,反应终止pH为7.0,二氧化碳气体流速为1 L/min.

褐藻多糖是一种天然的硫酸杂多糖,是羊栖菜多糖中最具药理活性的成分,在抗肿瘤、抗氧化、增强免疫力、抗炎等多方面有着重要的作用.羊栖菜多糖的药理活性与其褐藻多糖的含量密切相关,褐藻多糖的硫酸化程度越高,发挥的作用越强.本文就褐藻多糖的提取工艺及其抗肿瘤活性进行讨论,希望能对进一步的深入研究提供参考.

剑麻皂素是合成甾体激素类药物的重要原料,目前市场供不应求.我国20世纪60年代就已经开发出酸水解醇提制备剑麻皂素工艺技术,之后众多研究者在此基础上进行大量的工艺改进和技术优化,并获得许多产业化的研究成果.为此,本文综述从剑麻渣中制备剑麻皂素工艺技术,结合笔者多年的工作经验,重点介绍目前产业技术进展及科研成果,指出产业中存在的问题并提出合理化建议,为该产业绿色、高效开发提供参考.

利用红外、凝胶色谱、气-质联用等技术研究皂素废水在强对流微电解-芬顿氧化耦合技术下有机物的变化,揭示皂素废水降解的化学本质.研究发现,强对流微电解-芬顿氧化耦合技术能显著降低皂素废水的COD值、色度、氨氮和硫酸根离子浓度,提高废水的可生化性.降解反应主要发生在不饱和化合物的不饱和键上,苯及其衍生物是一类难降解的有机物.

The solubility of tigogenin in methanol (293-338K)and ethanol (293-353K)were determined by equilibrium method at atmospheric pressure, and the solubility date was correlated.The results showed that the solubility of tigogenin in methanol and ethanol increased monotonically with increasing temperature.The solubility of tigogen in methanol was greater than in ethanol at 293-323K,and in methanol was less than in ethanol above 323K.The adjusted determination coefficient of fitting equation was respectively 0.9961 and 0.9976,the average relative errors of solubility in methanol was 2.12% at 318-338K,in ethanol was 2.56% at 328-353K, which indicates that fitting equation can meet the need of engineering design.Applications of two solvents in production of tigogenin were studied,which show that ethanol as extraction solvent was better than methanol.

Applied hydrolysate as materials and ethanol as solvent,the extraction technology of tigogenin was studied. Effects of ethanol concentration, tigogenin concentration in the ethanol, extraction time, tigogenin/activated ratio and decolorization time on the yield and quality of tigogenin were investigated. Through single factor experiments, orthogonal design experiments and HPLC detector, the optimum extraction process of tigogenin was determined: ethanol concentration 95%, the concentration of tigogenin in ethanol 7.8g/L, extraction time 1h, tigogenin to activated carbon ratio 1:1.8, decolorization time 1.5h. Under the conditions, the content of tigogenin was 92.14%, extraction rate was 81.16%, the ethanol solubility and color of product was qualified.

建立高效液相色谱测定剑麻皂素提取液中剑麻皂甙元含量的方法.色谱条件如下:采用RID-10A示差折光检测器,色谱柱填料为Hypersil ODS2 5 μm,柱温为30℃,流速为1.0 mL/min,以乙醇-水(3+1,v/v)为流动相.实验表明,剑麻皂甙元在0.1～10 g·L-1范围内呈现良好的线性关系,线性相关系数为0.9998,RSD为0.32％(n=6).在测定溶液中加入标准品傲回收实验,测得回收率为98.38％.该检测方法简便快捷、精确稳定、重现性好,可为剑麻皂素生产提供实时监控和优化改进.

In order to get the highly efficient way of extracting Zinc from Ostrea Rivularis Gould , the Zinc content and the total amino acid content were used as evaluating indicator to assess the products which were made by different power ultrasonic, different material usage ratio and homogenate or not. The result showed that ultrasonic cell disrupting (without homogenate) could extract Zinc and amino acid from Ostrea Rivularis Gould efficaciously, and the best extraction condition was ultrasonic power 80 W, material usage ratio 1 : 3(g/g), extraction duration 20 min. Under this condition, the Zinc content was 66.0 mg/L , while the total amino acid content was 206.13 mg/100 mL in the concentrated solution.

Tow known diosgenin components and a new saponin constituent hecogenin 4-ethylene glycol glucose were isolated from the ethanol extract of sisal residue. Their structures were identified by IR, MS, 1 H-NMR, 13 C-NMR, and the two dimensional spectrum method.

剑麻皂甙元是重要的激素类药物中间体,越来越引起人们的关注和重视.综述了剑麻皂甙元生产技术进展,并提出目前存在的问题和合理化建议,为进一步提高剑麻皂素收率,降低生产能耗提供参考.

Hydrolysis process of sisal paste catalyzed by concentrated sulfuric acid was studied. Hydrolysis time, sulfuric acid concentration, sisal paste and concentrated sulfuric acid ratio affected the hydrolysis yield and the saponin content of sisal hydrolysate were investigated. Through single factor experiments, orthogonal experiments and HPLC detector, the optimum preparation process was determined:hydrolysis time 8h, acid concentration 15%, sisal paste and concentrated sulfuric acid ratio 1:1. Under the conditions, the yield of sisal hydrolysate reached to 62%, and the saponin content of sisal hydrolysate was 13.26%.

A method for the determination of tigogenin in fermented residues of sisal leaf-juices, sisal hydrolysate and sisal saponin product by HPLC with RID was established. C18 column was used as stationary phase and ethanol-water(3+1, v/v) as mobile phase, the flow rate was 1.0mL/min and the column temperature was 40℃. The calibration curve was linear in the range of 0.002~0.04mg (R2=0.9998). The average recovery were 97.1%(RSD=0.81%), 97.8%( RSD=0.65%) and 98.9%( RSD=0.51%) for the three kind of samples. The method was convenient, stable and accurate, so it could provide the effective proof for raw material purchase and quality evaluation in sisal saponin production.

采用粉煤灰为吸附剂直接处理冶金工业中排放的蒸氨废水中的苯酚,通过两步法,即通过一次直接吸附苯酚后的粉煤灰进行煤油萃取,脱除表面吸附的苯酚后,在含酚蒸氨废水中进行二次吸附苯酚过程。研究表明:在室温以及吸附剂用量为66.7g/L的情况下,苯酚的一次、二次脱除效率分别为:38.13%和75.00%,非离心过滤情况下吸附剂的沉降时间为8min。

利用毛细管气相色谱法对乙醇胺混合液中二乙醇胺的含量进行测定,采用SE-54毛细管色谱柱,程序升温及氢火焰离子化检测器对样品进行检测。进样口温度为250℃,检测器温度为300℃,以N2为载气,邻苯二甲酸二甲酯(DMP)为内标物。该方法的相关系数为R=0.9994,变异系数为0.1184%,平均回归率为99.7%。方法可用于二乙醇胺含量的测定。

Ethylenediamine was synthesized from ethanolamine by reductive amination method using self-made Ni-Co bimetallic activated catalyst.The products were analyzed by capillary gas chromatography with ethylene glycol as internal standard,and the results showed that ethanolamine,ethylenediamine,piperazine,diethylene triamine and aminoethyl piperazine were in reaction solution.Through single factor experiments and orthogonal experiments,the optimum preparation process was determined: reaction temperature 180℃,ammonia-alcohol ratio 5:1,catalyst concentration 1.5%,reaction time 4h.The conversion of the ethanolamine reached 72.6%,and the selectivity of ehylendiamine reached 76.1%.

The thermal stabilities of 4 kinds of insecticides in 6 kinds of fertilizers are determined,the results show that the decomposition rate of terbufos in MAP is of 4.7%, thermal decomposition rates of pesticide both chlorpyrifos and cartap are qualified of less than 5% mixed in the compound fertilizer with m(urea) ∶ m(MAP) ∶ m(KCl) = 2 ∶ 1 ∶ 1 respectively,however,thermal stabilities of carbofuran in 6 kinds of fertilizers are bad.

In this paper,it was proposed the method of synthetic diethanolamine.Before the reaction of epoxy ethane and ammonia,monoethanolamine which was previously synthesized was put into reactor in the cycle.A set of reaction equipment,which was easy to control,the product had high purity,and the operating process was safety and healthy,was designed.The influence factors of synthesis were studied and the experiment result showed that the product had less impurity content,the molar ratio of MEA∶DEA∶TEA was 13.1∶60.4∶20.8,epoxy ethane conversion percent was 87.6% when the reaction temperature was 50℃,the reaction pressure was 0.5MPa,NH3/EO was 4∶1 and monoethanolamine was circulated 5 times.

A modified catalyst was prepared with porous materials as carrier and Ni-Co bimetal as base material.The application of the catalyst in synthesis of ethylenediamine from ethanolamine was studied with TiO2 as carrier,Cu and Re as additive.Through single factor experiments and orthogonal design,the optimum preparation process was determined:metal loading 10%,Ni/Co ratio 4∶1,additive content 2%,and impregnating solution pH=8.The crystalline structure,surface micro-morpholot and element content of the catalyst were characterized by XRD and SEM-EDS.The results showed that Ni existed in the form of metallic state and Co existed in the form of oxides.The catalyst had rough surface,larger specific surface area,appropriate metal content and better catalytic activity.

Select TiO2 as carrier,Cu and Re as additive,the Ni-Co bimetallic activated catalyst was prepared by impregnation method.It was studied the application of catalyst in synthesis of ethylenediamine from ethanolamine.Through single factor experiments and orthogonal experiments,the optimum preparation process was determined: metal loading 10%,Ni/Co ratio 4:1,additive content 2%,and impregnating solution pH=8.The crystalline structure,surface micro-topography and element content of catalyst were characterized by XRD and SEM-EDS.The results showed that Ni exists in form of metallic state and Co existed in the form of oxides.The catalyst had larger surface area,metal content appropriate and better catalytic activity.

This article summarizes the research status on the deep processing technology of ethylene oxide according to the rapid development and the domestic market demand of deep processing products from ethylene oxide.It was emphatically introduced on the technical progress including the catalyst research,as well as the process and equipment improvement of the representative products,such as ethylene glycol,ethanolamine,polyether surfactant and glycol ether.Finally,some existing problems and suggestions were proposed.