pH值对邻苯二亚胺纤维素的制备及荧光性能的影响

制备了席夫碱（Ｓｃｈｉｆｆ’ｓ ｂａｓｅ）邻苯二亚胺纤维素（ＰＤＩＭＣ），考查ｐＨ值对制备反应和产物荧光性能的影响。结果表明：氧化度为１００％的二醛纤维素在ｐＨ＝７￣１３、室温下、反应３０ｈ生成的邻苯二亚胺纤维素，具有强较的荧光性能，熔点４１０ｋ，分解温度为５７８Ｋ；ＰＤＩＭＣ水溶液在ＰＨ＝７．６，浓度为７．６×１０＾－４ｇ／ｍＬ，２０℃时，Ｅｘ＝４７０ｎｍ，Ｅｍ＝５５５ｎｍ处荧光最强。     

（Cu（C14H11O3）（C10H8N2）2NO3.C2H5OH的合成,晶体结构和红外光谱

合成了（Ｃｕ（Ｃ１４Ｈ１１ｏ３）（Ｃ１０Ｈ８Ｎ２）ＮＯ３．Ｃ２Ｈ５ＯＨ化合物并测定其晶体结构，晶体属Ｐ空间群，ａ＝１．１９１１（２）ｎｍ，ｂ＝１．５３２２（２）ｎｍ，ｃ＝１．０４９２（２）ｎｍ，ａ＝１０８．９８（１）°β＝１０７．０４（１）°，γ＝７０．２５（１）°Ｚ＝２．在（Ｃｕ（Ｃ１４Ｈ１１Ｏ３）（Ｃ１０Ｈ８Ｎ２）２）配合阳离子中，２个２．２’－联吡啶的４个氮原子和二苯羟乙酸的１个羟基氧原子位     

苯氧树脂增韧双酚A环氧树脂的研究

以双官能团环氧树脂和双酚Ａ为单体，制备高分子量苯氧树脂，通过ＦＴＩＲ对其分子结构进行分析后，将１０ｗｔ％苯氧树脂加入到Ｅ－４４环氧树脂中，用ＤＳＣ冲击仪和ＳＥＭ等对增韧效果的分析测定，固化反应活化能降低９％，冲击强度提高６３．２％，玻璃化温度提高了２８℃。     

N─苯基邻苯二甲酰亚胺和N─对甲苯基邻苯二甲酰亚胺的晶体和分子结构

报道一种新类型的有机电子晶体Ｎ－苯基邻苯二甲酰亚胺（１）（Ｃ＿（１４）Ｈ＿９ＮＯ＿２）和Ｎ－对甲苯基邻苯二甲酰亚胺（２）（Ｃ＿（１５）Ｈ＿（１１）ＮＯ＿２）的晶体和分子结构，（１）属正交晶系，空间群为Ｐｃａｂ，ａ＝７．６４９（４），ｂ＝１１．６５９（２），ｃ＝２３．７３９（３）Ａ，Ｖ＝２１１７．０Ａ￣３，Ｚ＝８，Ｄ＿ｃ＝１．４０１ｇ／ｃｍ￣３，Ｍ＿ｒ＝２２３．２３，μ＝０．８８５ｃｍ￣（－１），最终偏离因子Ｒ＝０．０５３，Ｒ＿ω＝０．０４８；（２）属正交晶系，空间群为Ｐｎａ２＿１，ａ＝７．６２４（２），ｂ＝１１．２３７（１），ｃ＝１３．８５６（２）Ａ，Ｖ＝１１８７．０　Ａ３，Ｚ＝４，Ｄ＿ｃ＝１．３２８ｇ／ｃｍ￣３，Ｍｒ＝２３７．２６，μ＝２．７６４ｃｍ－１，最终偏离因子Ｒ＝０．０３６，Ｒ＿ω＝０．０３２。晶体结构测定结果表明，邻苯二甲酰亚胺的内酰亚胺碳、氮、氧原子与其苯并环共平面。化合物（２）中的甲基碳原子与取代基苯环共平面，苯并酰亚胺平面与取代苯环平面间的夹角分别为５８．４°（化合物１）和５６．２°（化合物２）。     

N─苯基邻苯二甲酰亚胺和N─对甲苯基邻苯二甲酰亚胺的晶体和分子结构

报道一种新类型的有机电子晶体Ｎ－苯基邻苯二甲酰亚胺（１）（Ｃ＿（１４）Ｈ＿９ＮＯ＿２）和Ｎ－对甲苯基邻苯二甲酰亚胺（２）（Ｃ＿（１５）Ｈ＿（１１）ＮＯ＿２）的晶体和分子结构，（１）属正交晶系，空间群为Ｐｃａｂ，ａ＝７．６４９（４），ｂ＝１１．６５９（２），ｃ＝２３．７３９（３）Ａ，Ｖ＝２１１７．０Ａ￣３，Ｚ＝８，Ｄ＿ｃ＝１．４０１ｇ／ｃｍ￣３，Ｍ＿ｒ＝２２３．２３，μ＝０．８８５ｃｍ￣（－１），最终偏离因子Ｒ＝０．０５３，Ｒ＿ω＝０．０４８；（２）属正交晶系，空间群为Ｐｎａ２＿１，ａ＝７．６２４（２），ｂ＝１１．２３７（１），ｃ＝１３．８５６（２）Ａ，Ｖ＝１１８７．０　Ａ３，Ｚ＝４，Ｄ＿ｃ＝１．３２８ｇ／ｃｍ￣３，Ｍｒ＝２３７．２６，μ＝２．７６４ｃｍ－１，最终偏离因子Ｒ＝０．０３６，Ｒ＿ω＝０．０３２。晶体结构测定结果表明，邻苯二甲酰亚胺的内酰亚胺碳、氮、氧原子与其苯并环共平面。化合物（２）中的甲基碳原子与取代基苯环共平面，苯并酰亚胺平面与取代苯环平面间的夹角分别为５８．４°（化合物１）和５６．２°（化合物２）。     

新显色剂2－氯－5－羧基苯基重氮氨基偶氮苯的合成及与镉显色反应的研究

本文报道了新显色剂２－氯－５－羧基苯基重氮氨基偶氮苯（ＣＣＤＡＡ）的合成。研究了在ｐＨ９．８硼砂－氢氧化钠介质中、在ＴｒｉｔｏｎＸ－１００存在下镉（Ⅱ）与ＣＣＤＡＡ形成稳定的红色配合物，λ＿（ｍａｘ）＝４８５ｎｍ，ε＿（１８５）＝１．２４×１０￣５Ｌ．ｍｏｌ￣（－１）、ｃｍ￣（－１），镉量在０～１０μｇ／２５ｍＬ范围内遵守比尔定律。本法灵敏度高，选择性好，已用于测定工业废水中微量镐（Ⅱ），结果满意。     

聚芳醚酮膜的溶剂吸附与诱导结晶行为

研究了聚芳醚酮系列在１，２－二氯乙烷中的吸附，及溶剂与温度诱导结晶行为。得到６０℃时的最大吸附量Ｃ∞及假扩散系数Ｄ为：ＰＥＥＫ，Ｃ∞＝４６％，Ｄ＝３．１０×１０＾－１２ｍ＾２·ｓ＾－１；ＰＥＥＫＫ，Ｃ∞＝５０％，Ｄ＝６．５７×１０＾－１２ｍ＾２·ｓ＾－１；ＰＥＫＫ，Ｃ∞＝５５％，Ｄ＝９．４１×１０＾－１２ｍ＾２·ｓ＾－１。实验表明，吸附及脱附行为均与分子链刚性或羰基含量有关，膜的分子链受溶剂作用而     

1,5—苯并硫搂杂Zhou—α—苯基—β—内酰胺的合成及晶体结构

１，５－苯并硫氮杂Ｚｈｏｕ与苯乙酰氯反应生成１，５－苯并硫氮杂Ｚｈｏｕ－α－苯基－β－内酰胺。Ｘ－射线单晶衍射测定结果表明，该化合物分子式为Ｃ２９Ｈ２２ＣＩＮＯＳ，Ｍ＝４６７．５，晶体属单斜晶系，Ｐ２１／ｃ空间群，ａ＝１２．８６４（３），ｂ＝９．５１１（２），ｃ＝１９．４８９（４）Ａ，β９２．４１（３）°，Ｖ＝２３８２（１）Ａ＾３，Ｄｃ＝１．３０５ｇ／ｃｍ＾３，Ｚ＝４，Ｆ（０００）＝９７６，μ＝０     

多目标单纯形法在苯素红催化荧光测定痕量钒（V）中的应用

本建立了苯素红催化荧光测定痕量钒的新方法。在λｅｘ／λｅｍ＝３８１／４４５（ｎｍ）由多目标罚函数单纯形法获得最佳实验条件为：１％苯素红６ｍＬ，１ｍｏｌ／Ｌ盐酸２．１ｍＬ，饮和ＫＩＯ４１．８ｍＬ，反应温度８５℃，反应时间１５．３０ｍｉｎ，钒的检测下限为７×１０＾－１０ｇ／ｍＬ，反应对试剂及金属离子均为一极反应。方法用于水样和铬钒钢中钒的测定，结果满意。     

3－硝基邻苯二甲酸根桥联双核钴（Ⅱ）配合物的合成、磁性及抗癌活性

合成了两种以３－硝基邻苯二甲酸根为桥联配体的新型双核钴（Ⅱ）的配合物，即［Ｃｏ２（３ＰＴ）（Ｐｈｅｎ）４］·（ＣｌＯ４）２·４Ｈ２Ｏ（配合物１）和［Ｃｏ２（３ＰＴ）（ＮＰｈｅｎ）４］（ＣｌＯ４）２·５Ｈ２Ｏ（配合物２）（３ＰＴ＝３－硝基邻苯二甲酸根，Ｐｈｅｎ＝１，１０－菲口罗啉，ＮＰｈｅｎ＝５－硝基－１，１０－菲口罗啉）。使用元素分析，ＩＲ，ＵＶ－ｖｉｓ和电导测定方法对该两配合物进行了表征。测定了配合物的变温磁化率，并对所得数据进行了理论分析，求得了配合物１、２的磁交换积分均为２Ｊ＝－９．２ｃｍ－１。对配合物进行了体外抗人白血病癌细胞实验。发现该两配合物均具有较强的抑制人白血病癌细胞的活性。     

Modeling of Fischer-Tropsch Synthesis in a Slurry Reactor with Water Permeable Membrane

Fischer-Tropsch synthesis is an important chemical process for the production of liquid fuels and olefins. In recent years, the abundant availability of natural gas and the increasing demand of olefins, diesel, and waxes have led to a high interest to further develop this process. A mathematical model of a slurry membrane reactor used for syngas polymerization was developed to simulate and compare the maximum yields and operating conditions in the reactor with that in a conventional slurry reactor. The carbon polymerization was studied from a modeling point of view in a slurry reactor with a water permeable membrane and a conventional slurry reactor. Simulation results show that different parameters affect syngas conversion and carbon product distribution, such as the hydrogen to carbon monoxide ratio, and the membrane parameters such as membrane permeance.     

Conversion enhancement of tubular fixed-bed reactor for Fischer-Tropsch synthesis using static mixer

Recently,Fischer-Tropsch synthesis(FTS) has become an interesting technology because of its potential role in producing biofuels via Biomassto-Liquids(BTL) processes.In Fischer-Tropsch(FT) section,biomass-derived syngas,mainly composed of a mixture of carbon monoxide(CO) and hydrogen(H2),is converted into various forms of hydrocarbon products over a catalyst at specified temperature and pressure.Fixed-bed reactors are typically used for these processes as conventional FT reactors.The fixed-bed or packed-bed type reactor has its drawbacks,which are heat transfer limitation,i.e.a hot spot problem involved highly exothermic characteristics of FT reaction,and mass transfer limitation due to the condensation of liquid hydrocarbon products occurred on catalyst surface.This work is initiated to develop a new chemical reactor design in which a better distribution of gaseous reactants and hydrocarbon products could be achieved,and led to higher throughput and conversion.The main goal of the research is the enhancement of a fixed-bed reactor,focusing on the application of KenicsTM static mixer insertion in the tubular packed-bed reactor.Two FTS experiments were carried out using two reactors i.e.,with and without static mixer insertion within catalytic beds.The modeled syngas used was a mixed gas composed of H2/CO in 2:1 molar ratio that was fed at the rate of 30mL(STP)min1(GHSV≈136mL g1 cat h1) into the fixed Ru supported aluminum catalyst bed of weight 13.3g.The reaction was carried out at 180℃ and atmospheric pressure continuously for 36h for both experiments.Both transient and steady-state conversions(in terms of time on stream) were reported.The results revealed that the steady-state CO conversion for the case using the static mixer was approximately 3.5 times higher than that of the case without static mixer.In both cases,the values of chain growth probability of hydrocarbon products(α) for Fischer-Tropsch synthesis were 0.92 and 0.89 for the case with and without static mixer,respectively.     

Enzymes immobilized on montmorillonite: comparison of performance in batch and packed-bed reactors

Summary The enzymes a-amylase, invertase and glucoamylase were immobilized on acid activated montmorillonite using two techniques, viz. adsorption and covalent binding, and their activities were tested in a batch and packed-bed reactor and were compared. The packed-bed reactor showed an improved performance for all immobilized enzymes, which was attributed to lowering of diffusional restrictions to mass transfer. Lower activity in case of batch reactor for immobilized invertase was due to a combined effect of loss of native conformation of enzyme on account of immobilization and mass transfer resistances due to improper diffusion of substrate to the active site of enzyme. For immobilized glucoamylase, the packed-bed reactor demonstrated exceptionally high activity that was very close to the free enzyme. Covalently bound glucoamylase showed higher activity than the free enzyme.     

Design of a fluidized bed reactor for microencapsulated urease

A fluidized bed reactor was designed, constructed, and tested for handling microencapsulated urease. The working volume of the reactor was 10 mL, with a minimum fluidization velocity of 7.7×10⁻⁵ m/s. An even suspension of the microcapsules was obtained at fluid velocities between 1.5×10⁻⁴ and 6.0×10⁻⁴ m/s without breakage of the shear-sensitive microcapsules. The mixing behavior in the reactor was evaluated using pulse input tracer experiments and the hydrolysis rates of urea in continuous flow experiments were evaluated under various operating conditions.     

The use of an immobilized enzyme nylon tube reactor incorporating a four enzyme system for creatinine analysis

A single immobilized enzyme nylon tube reactor was produced incorporating a four enzyme system for the analysis of creatinine. The enzyme activity ratios in the coupling solution used to prepare the reactor were found to be of extreme importance in governing the activity of the latter. The reactor was incorporated into a continuous flow analysis system used to assay creatinine in urine samples and the results were correlated with a manual technique employing the same enzyme system in solution. The precision, correlation, high specificity, simplicity, and speed of the analysis were concluded to be factors in favor of the method's suitability for urine creatinine determinations.     

Successful application of microstructured continuous reactor in the palladium catalysed aromatic amination

Micro reactor technology was successfully applied in the palladium catalysed C-N cross-coupling reaction between 4-bromotoluene and piperidine. Excellent conversions and selectivities were obtained without any by-product formation in continuous reactor.     

The anaerobic treatment of soft drink wastewater in UASB and hybrid reactors

The anaerobic treatment of soft drink wastewater (SDW) was studied in two laboratory reactors—a 1.8-L UASB reactor and a 3-L hybrid reactor-sludge bed containing a layer of polyurethane in the upper part, at 35°C. The highest organic loading rates (OLR) achieved were 13 and 16.5 g COD/L · D for hybrid and UASB reactors, respectively, with the treatment efficiency of about 80% for both reactors. Despite the higher treatment productivity achieved for the UASB reactor, its lower ability to generate a sufficient level of alkalinity led to difficulties in maintaining a stable operation performance. Therefore, the hybrid reactor seems to be indicated for OLR higher than 10 g COD/L · d and HRT lower than 1 D, from the point of view of reliability of these two systems. Both reactors can treat the SDW with pH influent up to 11.0. The feeding of reactors with higher pH influent values led to their quick failure because of alkali shock. The duration of the recovery period after alkali shock was about 1.5-2 mo.     

The preparation and reaction of enolates within micro reactors

Over the past 5 years, interest in the miniaturisation of chemical synthesis has grown rapidly, however in order to facilitate transfer of the technology from its current position as a research tool to industrial applications, a core understanding of the challenges associated with transferring reactions from the macro to the micro domain is required. This paper therefore aims to broach this problem by investigating the application of micro reactors to a range of commonly employed synthetic reactions including acylation, aldol, alkylation, 1,4-conjugate addition (Michael addition) and the Knoevenagel condensation. Comparison of the results obtained with traditional batch techniques enable us to highlight some of the advantages associated with micro reaction technology.     

Design and Implementation of a Novel Quench Flow Reactor for the Study of Nascent Olefin Polymerisation

A novel stopped flow reactor system is described in the current work, along with the underlying design philosophy. While the concept of stopped flow technology is not recent, this system is the first to be designed with the objective of studying particle morphology, and to work at extremely short (40 ms) residence times. It is shown that traditional chemical engineering principles are required to properly design and operate this type of reactor, and that when correctly design, it is a very flexible tool for the study of nascent polymerisation of olefins.