ω-腈基十一酸分离提纯工艺优化

以ω-腈基十一酸(11-CUA)的收率(或质量百分含量)及纯度为目标函数,采用液相色谱法与电位滴定法进行相应的分析检测,对自行设计的两种不同的分离提纯11-CUA的萃取与结晶工艺进行对比实验,确定了合理的分离提纯工艺,然后用单因素实验法对所选的合理工艺的部分单元操作进行工艺参数优化.优化工艺参数为:氨气氨化时溶液pH值8.0-10.0、温度25-35℃、搅拌速率120-240rpm,萃取溶剂为甲苯,酸化试剂用硫酸(或盐酸)、酸化剂试用量:H2SO4;HN3为0.6(摩尔分数)、溶液pH值1.5-2.0、温度55-60℃,采用环己烷作为结晶介质,结晶溶液溶质初始质量比为5.00g粗品11-CUA/100.00g环己烷,粗品11-CUA溶解温度50-55℃,粗品11-CUA溶解后结晶前的静置沉降时间20min、结晶温度10℃,结晶母液可以直接重复利用一次.     

11-氰基十一酸的甲酯化研究

11-氰基十一酸甲酯(MCU)可由11-氰基十一酸(CUA)与甲醇酯化合成.CUA的氰基酯化时易水解,需选择合适的催化剂并控制好酯化条件.通过实验确定98% H2SO4是酯化反应合适的催化剂(兼具吸水作用).用正交试验考察酯化条件,优化条件为:将0.03 mol的CUA和3.0g硅胶(吸水剂)加入到0.225 mol甲醇与0.015 mol的浓H2SO4混合液中,回流3 h,反应的产品收率可达65.8%,酸醇比对收率影响最大.合成产物用正己烷结晶精制后经质谱测得其相对分子量为225,红外光谱、质谱、核磁共振(1HNMR及13CNMR)结构表征证明酯化产物确为MCU;其熔点27.3～28.4 ℃,40℃时折光率1.440 3.     

活性炭联合陶瓷膜超滤纯化香菇多糖

为了改善香菇多糖精制工艺及降低生产成本,以45%香菇多糖粗品为原料,利用陶瓷膜超滤对其进行纯化精制。结果表明,4.5mg/mL的香菇多糖粗品溶液用1%活性炭作预处理,超滤温度为40℃,超滤压力为0.2MPa,膜面流速为4.5m/s时纯化效果最优。蛋白质的脱除率可达81%,多糖粗品脱色率达90.9%,精制得香菇多糖的纯度为89.7%,回收率77.6%。     

曲克芦丁新工艺合成研究

以甲醇钠作为催化剂,芦丁、环氧乙烷为原料在甲醇中制备曲克芦丁.研究了在不同温度、反应时间及压强条件下对产品纯度和收率的影响.经实验证明,在高压釜内压强0.2 MPa、温度75℃条件下经5h反应,无需精制即可得到外标纯度高达80%的曲克芦丁.     

栀子蓝色素的制备及其抗氧化活性研究

用米曲霉发酵产物水解栀子苷,水解产物与味精反应制备栀子蓝色素,采用DM-2大孔树脂对产品进行精制,通过DPPH·捕获分光光度法测定栀子蓝色素精制前后的抗氧化活性.栀子蓝制备的最佳条件为:10.64 g栀子苷和129.36 g水混合后,加入米曲霉发酵液9.8 m L,在50℃,160¹80 r/min下水解6 h后,与3.15 g味精反应40 h,80℃保温30 min.所获栀子蓝色素粗品的色价(E1%1cm)为90.56,经DM-2大孔树脂纯化后产品色价提高至180.01%,收率为90.96%.抗氧化实验表明栀子蓝色素粗品和精制品均能有效清除DPPH·,且精制后的栀子蓝色素产品清除DPPH·的能力增强.     

利用Abuzov反应合成(对氰基苄基)膦酸二甲酯的工艺研究

以对甲基苯甲腈和亚磷酸三乙酯为原料合成了(对氰基苄基)膦酸二甲酯,研究了反应温度对氰基氯苄及(对氰基苄基)膦酸二甲酯的收率的影响。实验结果表明对氰基氯苄的反应温度在145℃;(对氰基苄基)膦酸二甲酯的反应温度150℃收率较高。     

11-氰基-十一酸熔点与折光率测定

11—氰基—十一酸是尼龙— 12的合成中间体 ,其物性常数有待精确测定 .在校正仪器的基础上 ,对其熔点和折光率进行了测定 ,并对所得结果进行了准确度和 (或 )精密度分析 ,表明所得结果是可靠的 ,结果为 :11—氰基—十一酸的熔点为 5 6 .6℃ ,在 6 0℃时折光率为 1.44 2 8.     

黄柏黄连素的压液提取和纯化

研究了压液提取法提取黄柏中的黄连素,并与常规冷浸法进行比较.用0.3%稀硫酸水溶液在压液和冷浸条件下分别提取20 min和24 h,将提取液过滤,滤液先用石灰乳调pH至12,过滤,滤液再用盐酸调pH至2-3,滤液中加入10%的固体氯化钠搅拌溶解,得黄连素粗品,再将所得粗品放入20倍量沸水中,加热溶解,放置过夜,制得黄连素精品.结果表明:压液提取所获产品收率高,纯度较低,而冷浸法所获产品收率低,纯度较高,综合看来,压液法提取黄柏黄连素经济可行.     

H_4PMo_(11)VO_(40)催化氧化2-甲基萘制备甲萘醌

以磷钼钒杂多酸H4PMo11V1O40为催化剂、乙酸为溶剂,用双氧水氧化2-甲基萘制备2-甲基萘醌.实验表明:H4PMo11V1O40具有一定的催化活性.通过正交试验和单因素试验考察了催化剂用量、乙酸用量、双氧水用量、反应时间、反应温度等对收率的影响,获得较佳的合成条件:杂多酸∶2-MN(质量比)=7%,乙酸∶2-MN(质量比)=10.5∶1,双氧水∶2-甲基萘(摩尔比)=4.2∶1,较适宜的温度为40~50℃,反应时间为30 min.     

离子交换法制备高纯辣椒碱类化合物

以辣素为实验原料 ,将辣素溶于 1 %的氢氧化钠溶液中 ,以 2 %的硫酸酸化 ,正己烷萃取并浓缩得辣椒碱类化合物粗品 (纯度为 82 %～ 84% ) .粗品辣椒碱类化合物溶于氢氧化钠溶液中 ,经离子交换法 ,以乙醇 -乙酸乙酯洗脱、浓缩、结晶得辣椒碱类化合物晶体 ,得率为 2 .8% (相对于辣素 ) .按GB1 0 783 -96标准检验 ,辣椒碱类化合物的纯度为 98.5 % .     

Markedness and its Interpretation in Language Use

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.     

Features of Women's language

Language is a means of verbal communication. People use language to communicate with each other. In the society, no two speakers are exactly alike in the way of speaking. Some differences are due to age, gender, statue and personality. Above all, gender is one of the obvious reasons. The writer of this paper tries to describe the features of women＇s language from these perspectives： pronunciation, intonation, diction, subjects, grammar and discourse. From the discussion of the features of women＇s language, more attention should be paid to language use in social context. What＇s more, the linguistic phenomena in a speaking community can be understood more thoroughly.     

An Analysis of Catherine＇s Character——Wuthering Heights

Wuthering Heights, Emily Bronte＇s only novel, was published in December of 1847 under the pseudonym Ellis Bell. The book did not gain immediate success, but it is now thought one of the finest novels in the English language. Catherine is the key character of this masterpiece, because everybody and everything center on her though she had a short life. We can understand this masterpiece better if we know Catherine well.     

Lower Paleozoic oil relationships within Williston Basin, Canada

The Williston Basin is a significant petroleum province, containing oil production zones that include the Middle Cambrian to Lower Ordovician, Upper Ordovician, Middle Devonian, Upper Devonian and Mississippian and within the Jurassic and Cretaceous. The oils of the Williston Basin exhibit a wide range of geochemical characteristics defined as "oil families", although the geochemical signature of the Cambrian Deadwood Formation and Lower Ordovician Winnipeg reservoired oils does not match any "oil family". Despite their close stratigraphic proximity, it is evident that the oils of the Lower Palaeozoic within the Williston Basin are distinct. This suggests the presence of a new "oil family" within the Williston Basin. Diagnostic geochemical signatures occur in the gasoline range chromatograms, within saturate fraction gas chromatograms and biomarker fingerprints. However, some of the established criteria and cross-plots that are currently used to segregate oils into distinct genetic families within the basin do not always meet with success, particularly when applied to the Lower Palaeozoic oils of the Deadwood and Winnipeg Formation.     

低渗透非均质砂岩油藏启动压力梯度研究

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。     

On Tragic Consciousness In The Works By Ernest Hemingway

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.     

Design and analysis of generic LBS application developing platform

Location based services is promising due to its novel working style and contents.A software platform is proposed to provide application programs of typical location based services and support new applications developing efficiently. The analysis shows that this scheme is easy implemented, low cost and adapt to all kinds of mobile nework system.     

Achieving Unusual States of Matter Under High Pressure

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-     

Exchange-Correlation and Electronic Excitation Energies from Pairing Matrix Fluctuations

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-     

Density Functional Theory for the Response of Periodic Systems to Electric Fields Based on the Vector Potential Approach

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