硬脂酸铝/苯凝胶流变行为的研究

The effect of temperature on the viscosity for aluminum stearate/benzene gels either with or without benzoic acid has been investigated. The experimental results show that the McAllister's equation can be used to describe the relation between the viscosity and temperature for these gels. The viscosity of these gels increase with elevation of the temperature and the activation Gibbs functions of the viscous flow are negative, this behavior is contrary to that of the most liquids.     

硬脂酸/异氰酸酯摩尔比对聚丙烯/木粉复合材料性能的影响

用甲苯-2,4-二异氰酸酯（TDI）和硬脂酸（SA）复合改性木粉,在双螺杆挤出机中制备了聚丙烯（PP）基的木塑复合材料（WPC）,研究了SA/TDI摩尔比对木粉表面性能、复合材料力学性能和加工性能的影响。 结果表明,随着SA/TDI摩尔比的增大,改性木粉的表面张力逐渐减小,与PP的界面张力先减小后增大;与未改性的WPC相比,SA/TDI复合改性剂对WPC的拉伸强度、弯曲强度、缺口冲击强度影响不明显,但对无缺口冲击强度提升较大;当SA/TDI摩尔比为1.07时,复合材料的无缺口冲击强度和熔体质量流动速率分别达到9.74 kJ/m2和13.12 g/10 min,分别比未改性WPC提高了77%和22%。     

掺希土离子Eu3+的BaTiO3超细微粉的制备及物性表征

近年来人们对材料及由材料制备的元件提出了高可靠性、多功能等要求。为了达到这种要求,人们从多种途径进行了探索,其中,对现有材料进行掺杂就是很有效的方法之一［１,２］。本文报道对ＢａＴｉＯ３超细微粉进行Ｅｕ３＋的有效掺杂并对其进行了物性表征。１实验部分１...     

硬脂酸法制备SO42-/Fe2O3-SiO2固体酸及其催化性能的初步探讨

首次用硬脂酸法制备了Fe2O3-SiO2混合氧化物,经浸渍H2SO4后再焙烧得SO2-4/Fe2O3-SiO2固体酸催化剂.用TEM,XRD,N2吸附/脱附和TG-DTA等手段对其进行了表征,结果显示制得的Fe2O3-SiO2混合氧化物具有多孔结构.且随着Si含量的增大,其比表面积明显增大,但孔径减小.用乙酸/丁醇酯化催化反应评估了该固体酸的催化性能.     

CaO对Pt/C催化硬脂酸脱羧反应性能的影响

以硬脂酸(C₁₇H₃₅COOH)脱羧为探针反应,研究了亚临界水中CaO对Pt/C催化脱羧反应性能的影响.实验表明,CaO可以促进脱羧反应,对十七烷选择性没有影响.CaO/硬脂酸物质的量比为0.5时,在330 ℃反应1 h,硬脂酸转化率由未添加CaO时的46.06%提高到66.99%.硬脂酸催化脱羧的最佳反应温度为350 ℃,高于这一温度时,烷基链上碳碳键断裂的副反应增加,导致十七烷选择性降低.亚临界水中硬脂酸脱羧反应符合一级动力学,建立的动力学方程可以较好地预测不同反应条件下十七烷的产率.根据实验结果推测,氧化钙与硬脂酸反应生成硬脂酸钙,催化剂表面的吸附态羧酸盐增加,从而提高了脱羧反应的速率.     

固相反应法制备微/纳米复合相变储能材料及其测试表征

采用低热固相化学反应法制备了表面包覆SiO2的不同硬脂酸含量的复合相变储能微纳米材料.XRD分析表明所制备的相变材料均呈晶相结构,红外图谱显示复合材料包覆层SiO2与相变主体材料硬脂酸C18H36O2(SA)存在键合作用,扫描电镜图片说明所合成复合材料呈较均匀颗粒状,而差热分析则表明所制得复合相变材料的相变温度分别为66.4、64.9 ℃,相变焓分别为148.97、111.54 J/g,具有良好的蓄热能力,可用于太阳能利用等方面的储能蓄热.     

硫酸铁铵催化合成硬脂酸正丁酯

在十二水合硫酸铁铵存在下，正丁醇和硬脂酸发生酯化反应，高收率地合成了硬脂酸正丁酯。研究了十二水合硫酸铁铵和正丁醇用量及反应时间对收率的影响，当硬酯酸用量为7．1g(28mmol)，硬酯酸、正丁醇和硫酸铁铵的摩尔比为1：8:0．124，回流分水2h，酯收率达98．8％。     

Determination of Specific Refractive Index Increment （dn/dc）_μ at a Constant Chemical Potential,for Solutions of Polymer in Mixed Solvents by the GPC Method

A new chromatographic method is described for the determination of specific refractive index increment(dn/dc)μ at a constant chemical potential,for polymer/mixed solvent systems.In this method the(dn/dc)is obtained by measuring the areas of solvated-polymer peaks when the mixed solvent is used as an eluent.Values of(dn/dc)μ for the poly(dimethylsiloxane)(PDMS)-benzene-methanol system,determined by the proposed method are in good agreement with those determined by the conventional dialysis method.The new approach has the advantages of simplicity,fast speed,and high reproducibility.The experimental results for stearic acid-chloroform-methanol system show that this method can also be applied to nonpolymer/mixed solvent systems for the determination of(dn/dc)μ.     

SDS/CTAB/H2O的双水相性质及萃取作用

正负离子表面活性混合物;牛血清蛋白质;色氨酸;SDS/CTAB/H2O的双水相性质及萃取作用     

Separation/Extraction/Detection of Chloramphenicol Using Binary Small Molecule Alcohol-Salt Aqueous Two-phase System Coupled with High-performance Liquid Chromatography

A green and sensitive sample separation and purification method coupled with high-perfomiance liquid chromatography(HPLC)was developed for the analysis of chioramphenicol(CAP).One element small molecule alcohol-salt aqueous two-phase system(ATPS)can't effectively adjust the polarity of the system,but binary small molecule alcohol-salt ATPS can adjust the polarity and improve the extraction efficiency of antibiotics.A binary aqueous two-phase system based on 1-propanol+2-propanol and NaH2PO4 system was formed and applied to the separation and purification of trace CAP in real samples.The influence factors on partition behaviors of CAP were discussed,including the types and mass of salts,the volume ratio of alcohol,the pH,temperature and the standing time.The optimal condition was found at pH=5.0,2.5 g of NaH2PO4,3.0 mL of 1-propanol and 2-propanol(volume ratio 1:1)and 30℃by using response surface methodology.Under this optimal condition,the extraction efficiency of CAP reached 98.91%,and partition coefficient of CAP was 17.31.     

Purification of plasmid DNA vectors by aqueous two-phase extraction and hydrophobic interaction chromatography

The current study explores the possibility of using a polyethyleneglycol(PEG)-ammonium sulphate aqueous two-phase system (ATPS) as an early step in a process for the purification of a model 6.1 kbp plasmid DNA (pDNA) vector. Neutralised alkaline lysates were fed directly to ATPS. Conditions were selected to direct pDNA towards the salt-rich bottom phase, so that this stream could be subsequently processed by hydrophobic interaction chromatography (HIC). Screening of the best conditions for ATPS extraction was performed using three PEG molecular weights (300, 400 and 600) and varying the tie-line length, phase volume ratio and lysate load. For a 20% (w/w) lysate load, the best results were obtained with PEG 600 using the shortest tie-line (38.16%, w/w). By further manipulating the system composition along this tie-line in order to obtain a top/bottom phase volume ratio of 9.3 (35%, w/w PEG 600, 6%, w/w NH4)2 SO4), it was possible to recover 100% of pDNA in the bottom phase with a three-fold increase in concentration. Further increase in the lysate load up to 40% (w/w) with this system resulted in a eight-fold increase in pDNA concentration, but with a yield loss of 15%. The ATPS extraction was integrated with HIC and the overall process compared with a previously defined process that uses sequential precipitations with iso-propanol and ammonium sulphate prior to HIC. Although the final yield is lower in the ATPS-based process the purity grade of the final pDNA product is higher. This shows that it is possible to substitute the time-consuming two-step precipitation procedure by a simple ATPS extraction.     

Effect of 1-hexanol on the phase behavior of SDS/CTAB/NaBr/H2O system

Abstract

The influence of 1-hexanol on the phase behavior of sodium dodecyl sulfate (SDS)/cetyltrimethyl ammonium bromide (CTAB)/NaBr/H₂O system has been systematically investigated in this paper. The results showed 1-hexanol effectively dissolved the precipitate formed by the CTAB and SDS surfactants, while liquid crystal (LC) and aqueous two phase system (ATPS) were formed in a wider range. When the molar ratio of 1-hexanol to surfactant is higher than 1, the precipitation in the system disappeared completely and was transformed into ATPS and LC, indicating that alcohol inserted at least evenly between every two surfactant molecules and hence effectively weakened the electrostatic interaction between the anionic and cationic surfactants and limited the formation of precipitation. Polarizing microscope (POM) with crossed polarizers was employed to investigate the textures of liquid crystals. It was shown that the existence of lamellar LC was confirmed by “Maltese crosses” textures. Additionally, we showed that the thermal stability of LC was promising. The ATPS and LC regions remained stable and changed slightly when the temperature was increased from 40 to 70?°C. The results indicated that ATPS and LC of the system were quiet resistant to temperature with the addition of 1-hexanol.     

System Establishment of ATPS for One-Step Purification of Glutamate Decarboxylase from <Emphasis Type="Italic">E. coli</Emphasis> After Cell Disruption

The partition of glutamate decarboxylase (GAD) from Escherichia coli in polyethylene glycol (PEG) and sodium sulfate aqueous two-phase systems (ATPS) has been explored with the purpose of establishing a phase system for the purification of GAD after cell disruption. The results showed that the partitioning of GAD was slightly influenced by PEG molecular weight (MW) but depended on the tie line length (TLL) and NaCl and loading sample concentrations. The optimum system obtained for GAD purification was composed of a PEG MW of 4,000, TLL of 63.5%, a volume ratio of 2.31, a loading sample concentration of 0.4 g/mL, which produced a GAD recovery of 90% with the purification fold of 73. Furthermore, the feasibility of directly purifying GAD from the cell disrupts using ATPS was evaluated. The established ATPS for GAD purification exhibited an efficient integrated purification process compared to the reported purification process in terms of purification efficiency and recovery.     

1-Hexyl-3-Methylimidazolium Chloride-Potassium Carbonate Aqueous Two Phase System: Equilibrium Characteristics and BSA Partitioning Behavior

The partitioning behavior of the model protein (bovine serum albumin) was investigated in ionic liquid (1-hexyl-3-methylimidazolium chloride) -salt (potassium carbonate) based aqueous two phase system (ATPS). The phase diagram with binodal curve and tie lines for the selected ATPS was developed at different temperatures and analyzed through effective excluded volume (EEV) and Othmer-Tobias and Bancroft equations, respectively. The influence of various process parameters like the ionic liquid and salt concentration, system temperature, tie line length, phase volume ratio, and neutral salt addition on partition coefficient/extraction efficiency of BSA protein was evaluated.     

pH及有机小分子物质对SDS/CTAB/H2O系统双水相性质的影响

正离子表面活性剂与负离子表面活性剂混合物能产生比单一表面活性剂更高的表面活性[1 ] 。在适当条件下 ,正负离子表面活性剂的水溶液能产生两个互不相溶的水相 ,即表面活性剂双水相系统[2 ] (ＡｑｕｅｏｕｓＴｗｏ -ＰｈａｓｅＳｙｓｔｅｍ -ＡＴＰＳ)。作者曾指出双水相上相为液晶 (ＬｉｑｕｉｄＣｒｙｓｔａｌ -ＬＣ)结构 ,下相为各向同性溶液 ,盐离子通过改变双水相中表面活性剂有序组合体的反离子层的状态而对双水相的组成、结构等产生重要的影响[3,4] 。本文进一步研究ｐＨ及有机小分子物质在十二烷基硫酸钠 /十六烷基三甲基溴化铵 /…     

新型sPS/PET/SsPS-Zn工程塑料合金的研究

熔融共混法制备了新型综合性能较好的间规聚苯乙烯 (sPS) 聚对苯二甲酸乙二醇酯 (PET) 磺化间规聚苯乙烯锌盐 (SsPS Zn)工程塑料合金 ,研究了合金结构与性能之间的关系 .加入SsPS Zn后 ,合金的力学性能先提高而后下降 ,当sPS PET SsPS Zn为 85 15 2 (质量比 )时 ,合金的综合力学性能较好 ,冲击强度达到 10 6kJ m2 ,为纯sPS的 2 5倍 ;加入SsPS Zn后 ,合金的耐热性提高 ;合金中sPS的熔点与纯sPS相同 ,而初始结晶温度和达到最大结晶速度时的温度均高于纯sPS ,且基本不受SsPS Zn用量的影响 .PET的熔点、初始结晶温度、达到最大结晶速率时的温度和结晶度均随SsPS Zn用量的增加而逐渐降低 ;DMA结果中所有合金均只呈现一个Tg,并且加入SsPS Zn后 ,Tg 和半峰宽都逐渐提高 ,常温下的储能模量在其用量为 2份时达到最大值 ;SEM观察到加入 2份SsPS Zn后 ,PET分散相的尺寸明显减小 ,继续增加其用量 ,PET分散相的尺寸反而有所增大和不均匀 ,并且合金的冲击断面由显著的层状结构转为相对平整     

A METHOD TO QUANTIFY CRAZING DEFORMATION BY TENSILE TESTS FOR POLYSTYRENE/POLYOLEFIN ELASTOMER IMMISCIBLE BLENDS

A method to quantify crazing deformations by tensile tests for polystyrene （PS） and polyolefin elastomer （POE） blends was investigated. The toughness of PS/POE blends, reflected by the Charpy impact strength, increased with the content of POE. SEM micrographs showed the poor compatibility between PS and POE. In simple tensile tests, it is very easy to achieve the ratio of crazing deformation, i.e. K by measuring the size changes of samples. The K values decreased with increasing the content of POE, and the deformations of PS/POE blends were dominated by crazing. The plots of the change of volume （△V） against longitudinal variation （△I） showed a linear relationship, and the slope of lines decreased with the content of POE. Measuring samples at the tensile velocities of 5 mm/min, 50 mm/min, and 500 mm/min respectively, the K values kept unchanged for each PS/POE blends.     

Rapid linear scale-up of a protein separation by centrifugal partition chromatography

The scaling up of the separation of two proteins with an aqueous two-phase system (ATPS) from 176 mg with a 500 ml laboratory scale centrifugal partition chromatography (CPC) column to 2.2g with a 6.25 litre pilot-scale column is presented. A model sample system of a mixture of lysozyme and myoglobin was chosen for this study using an ATPS system comprising 12.5% (w/w) PEG-1000:12.5% (w/w) K2HPO4. It was found that the maximum sample concentration possible without precipitation was 2.2mg/ml for each constituent. The optimisation of rotor speed, mobile phase flow rate and sample loading was performed on a laboratory-scale device. It was found that a centrifuge speed of 2000 rpm (224 'g'), 10 ml/min mobile phase flow rate with a 43 ml (10% of active column volume) sample volume gave optimum operating conditions. This was linearly scaled up to pilot scale by increasing mobile phase flow rate, fraction size and sample loading in the ratio of the system capacities (i.e. 12.5:1). Flow rate was therefore increased from 10 ml/min to 125 ml/min, fraction size from 10 ml to 125 ml and sample loading from 43 ml to 500 ml. Rotor speed however was reduced from 2000 rpm on the laboratory device to 1293 rpm on the pilot-scale device to maintain the same 224 'g' field in each chamber, as the pilot-scale CPC unit has a larger rotor radius than the laboratory one. Resolution increased from Rs=1.28 on the 500 ml rotor to Rs=1.88 on the 6.25 litre rotor, giving potential throughputs in batch mode of over 40 g/day.