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1.
在乙醛酸等化合物存在下乙二醛测定方法研究   总被引:4,自引:0,他引:4  
本文介绍了对含有乙醛酸等羰基化合物的乙二醛水溶液,用分光尤度计测定乙二醛含量的方法。所用试剂为对硝基苯肼,显色剂为氫氧化四甲铵,加碱后3分钟内即可进行测定。乙二醛和乙醛酸浓度分别在10~(-6)—10~(-5)和0—10~(-4)mol/L之内,所测相对误差低于5.0%。本方法具有简便、快速和专一性较高的优点,可用于乙二醛制备乙醛酸工艺中,测定原料转化率之用。  相似文献   

2.
大孔树脂负载金属离子催化合成尿囊素   总被引:3,自引:0,他引:3  
以乙二醛和尿素为原料,用FeSO4-H2O2催化氧化合成乙醛酸.将所得乙醛酸溶液在不经分离及大孔树脂负载的Ce(SO4)2固体酸催化剂存在的情况下,与尿素缩合制备尿囊素,实验考察了催化剂用量、反应温度、反应时间、原料配比、催化剂重复使用次数等因素对收率的影响.确定了最佳工艺条件,乙二醛氧化制乙醛酸的最佳工艺条件为反应温度15~20℃,n(乙二醛):n(H2O2)=1:1.1,乙醛酸收率达82%.缩合反应的最佳工艺条件为Ce(SO。)2/大孔树脂催化剂用量为投料量的2%(质量比),原料配比n(乙二醛):n(尿素)=1:2.5,反应温度80℃,反应时间4h,产品尿囊素的收率可达54%,催化剂可重复使用11次以上。  相似文献   

3.
超临界CO2萃取-高速逆流色谱分离纯化丹皮中丹皮酚   总被引:2,自引:0,他引:2  
采用超临界CO2提取中药丹皮中总丹皮酚,选择萃取温度、萃取压力、物料粒度为因素进行正交实验优选出超临界CO2萃取的最佳工艺条件:即物料粒度40~60目,萃取温度40℃,萃取压力20MPa,提取率可达90%以上。将萃取后的总丹皮酚应用高速逆流色谱进行分离纯化,两相溶剂系统为石油醚-乙酸乙酯-甲醇-水(1:0.4:1:0.4),进样量为330mg,得180mg纯度为99.0%的丹皮酚。  相似文献   

4.
溶剂萃取法提取氨基酸   总被引:6,自引:1,他引:6  
以二(2-乙基己基)磷酸(P204)为萃取剂,从沉淀胱氨酸后的毛发水解母液中提取复合氨基权。萃取过程的最佳工艺条件为:萃取剂组成P204(0.75)-磺化煤油(0.15)-乙基己醇(0.10),室温,初始水相的pH值为2.5;用去离子水反萃取,萃取及反萃取的理论级数分别为8级和9级。  相似文献   

5.
微波辐射促进阔叶十大功劳叶萃取过程的研究   总被引:5,自引:0,他引:5  
研究了在间歇式微波辅助萃取装置中提取阔叶十大功劳叶中的药用有效成分小檗碱。确定了萃取液中盐酸小檗碱的分析方法--Al2O3柱层析-紫外分光光度法;分别选取了甲醇、乙醇、乙醇-水(V/V=9:1)为溶剂;微波辐射时间为2min、4min、6min;处理比(g原料/mL溶剂)为1:40、1:60、1:80;利用正交实验设计考察了不同湿分原料的微波辅助萃取效率,得出了最优工艺条件;拍摄了典型萃取条件下萃取基本的透射电镜照片;探讨了微波辐射在植物原料萃取过程中对细胞结构破坏的机理。  相似文献   

6.
百合中秋水仙碱的分离及结构表征   总被引:2,自引:0,他引:2  
采用超临界二氧化碳流体萃取百合中秋水仙碱, 用高效液相色谱法对萃取物中秋水仙碱的含量进行测定, 用重结晶、薄层色谱法对萃取物中秋水仙碱进行分离纯化, 纯化后的目标物用核磁共振和红外光谱进行表征. 研究结果表明: 采用高效液相色谱法测得萃取物中秋水仙碱的质量分数为6.4%, 纯化后分离收率为88%, 核磁共振和红外光谱表征的结果与标准物的图谱一致, 可见超临界流体萃取-测定-分离百合中秋水仙碱的方法具有较好的选择性.  相似文献   

7.
以萃取压力、萃取温度、分离温度与萃取时间为参数,对紫穗槐精油超临界CO2萃取的最佳工艺条件进行了分析,并用气相色谱-质谱联用技术(GC-MS)对精油成分进行了鉴定.结果表明:萃取温度40 ℃、萃取压力25 MPa、分离温度38 ℃、萃取时间1.5 h为最佳工艺条件;精油含26种成分,占总萃取物含量的89.96%,主要包括α-蒎烯,月桂烯,α-雪松烯,β-桉叶油醇,反式-石竹烯,β-荜澄茄油烯等.  相似文献   

8.
针对传统硝酸氧化乙二醛制备乙醛酸存在周期长、选择性低等问题,本文提出了一种在微反应器中高选择性合成乙醛酸的方法。先将35%硝酸与40%乙二醛按照一定摩尔比输送到T形微混合器,在微通道和降膜微反应器中反应一段时间,将得到的乙醛酸反应液再和硝酸以一定摩尔比输送到T形微混合器、微通道以及降膜微反应器中,循环几次后得到最终反应液。结果表明:当硝酸(流速0.13 mL/min)与乙二醛(流速0.24 mL/min)初次混合的摩尔比为0.42∶1、硝酸(流速0.02 mL/min)与收集的乙醛酸反应液(流速0.24 mL/min)混合反应6次、T形微混合器与微通道的温度和停留时间分别为60℃和2 min、降膜微反应器反应温度为90℃时,乙二醛转化率为82%,乙醛酸选择性可达95%。  相似文献   

9.
在氧气辅助下,硝酸选择性氧化乙二醛制备了乙醛酸。在单因素试验基础上,通过高效液相色谱法,考察了通氧速率、保温反应温度、硝酸用量等因素对乙二醛转化率和乙醛酸收率的影响。研究结果表明:制备乙醛酸的最佳反应条件为通氧速率50 m L/min,保温反应温度60℃,硝酸与乙二醛物质的量比0. 59。在此条件下,乙二醛转化率为99. 00%,乙醛酸收率为84. 00%。与传统的硝酸氧化生产工艺相比,硝酸物质的量降低近10%,乙醛酸收率提高了5%以上。  相似文献   

10.
建立基于悬浮固化液相微萃取预处理的高效液相色谱-荧光检测法(SFODME-HPLC-FLD)用于两种植物生长素(吲哚丙酸和吲哚丁酸)的分析. 实验考察各因素对萃取过程的影响,确定最佳条件:50 μL十二醇(纯)为萃取剂,20.0 mL样品溶液(pH 3.0)、0.25 g·mL-1 NaCl、26 ℃、1 800 r·min-1条件下萃取10 min. 结果表明,SFODME技术重现性好、灵敏度高,相对标准偏差小于8.66%,检测限为0.01 ng·mL-1,线性范围为0.02~60 ng·mL-1,加标回收率大于84.3%. 方法快速、稳定、环境友好,适用于实际样品的检测.  相似文献   

11.
Language markedness is a common phenomenon in languages, and is reflected from hearing, vision and sense, i.e. the variation in the three aspects such as phonology, morphology and semantics. This paper focuses on the interpretation of markedness in language use following the three perspectives, i.e. pragmatic interpretation, psychological interpretation and cognitive interpretation, with an aim to define the function of markedness.  相似文献   

12.
理论推导与室内实验相结合,建立了低渗透非均质砂岩油藏启动压力梯度确定方法。首先借助油藏流场与电场相似的原理,推导了非均质砂岩油藏启动压力梯度计算公式。其次基于稳定流实验方法,建立了非均质砂岩油藏启动压力梯度测试方法。结果表明:低渗透非均质砂岩油藏的启动压力梯度确定遵循两个等效原则。平面非均质油藏的启动压力梯度等于各级渗透率段的启动压力梯度关于长度的加权平均;纵向非均质油藏的启动压力梯度等于各渗透率层的启动压力梯度关于渗透率与渗流面积乘积的加权平均。研究成果可用于有效指导低渗透非均质砂岩油藏的合理井距确定,促进该类油藏的高效开发。  相似文献   

13.
As an American modern novelist who were famous in the literary world, Hemingway was not a person who always followed the trend but a sharp observer. At the same time, he was a tragedy maestro, he paid great attention on existence, fate and end-result. The dramatis personae's tragedy of his works was an extreme limit by all means tragedy on the meaning of fearless challenge that failed. The beauty of tragedy was not produced on the destruction of life, but now this kind of value was in the impact activity. They performed for the reader about the tragedy on challenging for the limit and the death.  相似文献   

14.
正The periodicity of the elements and the non-reactivity of the inner-shell electrons are two related principles of chemistry,rooted in the atomic shell structure.Within compounds,Group I elements,for example,invariably assume the+1 oxidation state,and their chemical properties differ completely from those of the p-block elements.These general rules govern our understanding of chemical structures and reactions.Using first principles calcula-  相似文献   

15.
We have developed an adiabatic connection to formulate the ground-state exchange-correlation energy in terms of pairing matrix linear fluctuations.This formulation of the exchange-correlation energy opens a new channel for density functional approximations based on the many-body perturbation theory.We illustrate the potential of such approaches with an approximation based on the particle-particle Random Phase Approximation(pp-RPA).This re-  相似文献   

16.
正The electronic and nuclear(structural/vibrational)response of 1D-3D nanoscale systems to electric fields gives rise to a host of optical,mechanical,spectral,etc.properties that are of high theoretical and applied interest.Due to the computational difficulty of treating such large systems it is convenient to model them as infinite and periodic(at least,in first approximation).The fundamental theoretical/computational problem in doing so is that  相似文献   

17.
For molecular systems,the quantum-mechanical treatment of their responses to static electromagnetic fields usually employs a scalar-potential treatment of the electric field and a vector-potential treatment of the magnetic field.Although the potential for each field separately is associated with the choice of an(unphysical)origin,the precise choice of the origin for the electrostatic field has little consequences for the results.This is different for the  相似文献   

18.
Franck-Condon factors bridge the gap between theoretical modeling and experimental observations for molecular electronic spectroscopy and electron transfer.Under the displaced harmonic oscillator approximation,multidimensional Franck-Condon factors are decomposed into a product of many one-dimensional(1D)Franck-Condon(FC)factors,and each 1D-FC factor is associated with one Huang-Rhys factor that determines the leading contribution of  相似文献   

19.
<正>"The Journal of Shanghai Normal University:Mathematics"is published by Shanghai Normal University as regular issues of The Journal of Shanghai Normal University each year from 2014 in English.The editors-in-chief of the issues are professors Yuhao Cong and Maoan Han.The Journal of Shanghai Normal University was started in 1958 with  相似文献   

20.
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