CoO—NiO／Al2O3催化剂中Ni含量测定方法

应用分光光度法测定了CoO-NiO／Al2O3催化剂中Ni含量,试样溶于硫磷混酸中,溶液中的二价镍离子在碱性溶液中有氧化剂（过硫酸铵）存在时与丁二酮肟生成可溶性红色络合物。用3cm比色皿,在波长460nm处测定,方法最小检出限质量分数为0.025%。考核了方法的精密度和准确度,样品测定8次,求得测定结果的相对标准偏差为0.86%,标准加入回收率在85.7%-102.3%。     

ZL50活性炭吸附脱除二氧化硫的吸附动力学模型(英文)

A semi-empirical adsorption kinetic model was proposed with the time compensation method to describe the chemisorption of SO2 in flue gas by carbon adsorbents for flue gas purification. The change in adsorption capacity and adsorption rate with time at different water vapor concentrations and different SO2 concentrations was studied. The model was in good agreement with experimental data. The surface reaction was probably the rate controlling step in the early stage for SO2 adsorption by ZL50 activated carbon. The parameters m and n in the nth order adsorption kinetic model were related to the magnitude of the time compensation and adsorption driving force, respectively. The change of parameter n with water vapor concentrations and sulfur dioxide concentrations was studied and some physical implications were given. The sum of square errors was less than 1.0 and the average absolute percentage deviations ranged from 0.5 to 3.2. The kinetic model was compared with other models in the literature.     

陕西某地泥炭腐植酸提取工艺的实验研究

本实验与陕西某地合作,就当地泥炭进行了分析,并在腐植酸的提取的实验研究中对腐植酸提取的传统工艺做了改进,采取先用NaOH水溶液浸泡泥炭,再在球磨机中进行水磨(同样的仪器干磨粒度只能到60～80目,而水磨可以到100～150目).再絮凝,提取时间缩短到了1 h(传统的方法需要1.5 h)<'[1] >,腐植酸的提取率提高...     

双烯树脂废水处理的研究

对双烯树脂生产中的含高浓度有机废水的分步处理方法作了介绍：第一步静置、絮凝、沉降;第二步精馏;第三步活性炭-H2O2催化氧化。3种方法结合在工业实践中收到良好的效果,COD去除率达99％以上。     

纳米钛酸锶钡粉体制备及其对水中Cd2+吸附行为

采用草酸盐化学共沉淀法制备了草酸氧钛锶钡前驱体,通过905℃高温煅烧,制得了高纯纳米钛酸锶钡,并利用SEM、TEM、FT-IR和XRD对其进行了表征;并将该粉体应用于水中重金属镉离子的吸附.结果表明：该法合成的钛酸锶钡粉体为球形,钙钛矿结构,平均粒径为36 nm.对水中的镉离子具有较强的吸附能力,其吸附量与介质的pH值有密切关系,吸附动力学符合Langmuir和Bangham速率方程所描述的规律;吸附等温线较好地符合Langmuir和Freundlich等温方程,吸附行为是自发的、放热的物理吸附过程.     

鸢尾酮的合成研究

采用山苍子油提取得到的柠檬醛和丙酮等为主要原料合成鸢尾酮。合成分三步完成。先用柠檬醛与丙酮在碱的催化下生成假紫罗兰酮 ,收率为 93 .2 %。假紫罗兰酮甲基化生成假鸢尾酮 ,收率为 52 .3 %。假鸢尾酮环化得到鸢尾酮 ,收率为 98.3 %。合成的总收率较高达到 4 7.9%。并对合成的鸢尾酮进行了理化性质、光谱、色 -质和评香等的确证     

茶皂甙纯化工艺研究

对茶皂甙的提取纯化工艺进行了研究。以含量为70%的粗茶皂甙为原料,经N,N-二甲基甲酰胺溶解、乙酸乙酯沉析、胆甾醇复合吸附、苯解吸工艺得到含量大于99%的茶皂甙,提取率大于80%。结果表明,该工艺为高纯度茶皂甙的制备提供了参考。     

杀菌剂噻菌灵在香菇上残留量测定

以丙酮作提取剂，经二氯甲烷萃取，用丙酮定容，然后用ＳＩＧＭＡ－３００型带ＮＰＤ检测器的气相色谱仪测定。其测定结果的准确度和精密均符合残留量测定的要求。     

三氯蔗糖-6-乙酸酯脱乙酰基制三氯蔗糖的工艺研究

研究了三氯蔗糖-6-乙酸酯(TGS-6-A)醇解为三氯蔗糖的工艺。重结晶的三氯蔗糖-6-乙酸酯于CH3ONa/CH3OH体系中醇解,用H+型阳离子交换树脂中和,蒸去甲醇、乙酸甲酯等,在水相中用活性炭脱色,水溶液经浓缩,在38℃以上结晶数小时,分离得三氯蔗糖。用乙酸乙酯和水对三氯蔗糖进行重结晶,可得质量分数在98%以上的三氯蔗糖产品。对产物三氯蔗糖,经熔点测定、元素分析I、R及1H NMR确认了结构。三氯蔗糖-6-乙酸酯醇解为三氯蔗糖的收率为65%~70%。该方法为工业化生产三氯蔗糖提供了一个可行的方法。     

HBsAg缺失型乙型肝炎病毒复制细胞模型的建立及其对乙型肝炎病毒复制的影响

目的体外构建HBsAg缺失型乙型肝炎病毒(HBV)复制细胞模型,并探讨HBsAg对HBV复制的影响。方法定点突变pch9质粒上HBV 1.1倍体基因S蛋白表达区,构建HBV1.1倍体HBsAg突变质粒,并进行测序鉴定;将鉴定正确的突变质粒瞬时转染HepG2细胞,设未突变pch9质粒转染细胞作为对照,采用ELISA法检测转染72 h的细胞培养上清中HBsAg的表达;Southern blot及Real-time PCR法检测转染72 h的细胞内HBV DNA的复制水平。结果定点突变质粒经测序证实构建正确;突变质粒转染72 h的细胞培养上清中HBsAg A450值为(0.06±0.003),表达呈阴性,对照细胞A450值为(1.82±0.010),表达呈阳性,转染突变质粒72 h的细胞内HBV DNA条带浓度明显高于转染未突变质粒的细胞;转染突变质粒的细胞内HBV DNA绝对拷贝数分别为9.33×106、5.26×106,约为转染未突变质粒(6.91×105)的7.6～13.5倍。结论已成功构建了HBsAg缺失型HBV复制细胞模型,为HBV DNA复制及相关研究提供了实验依据;推测HBsAg是HBV DNA形成的自限性因素,能够负调控HBVDNA复制。     

非对称同向双螺杆端面造型对混合行为影响数值模拟

提出了同向自洁型双螺杆挤出机端面非对称造型的新概念。以符合Carreau定律的纯黏性流体为加工对象,建立相应的数学模型。采用Polyflow软件,基于叠加网格技术,对两种螺杆造型端面内的周期性流动和混合情况进行数值模拟。将粒子示踪技术及分离尺度相结合,研究了流场内分布混合能力;将分散准数与剪切速率相结合,表征了流场的分散混合能力。当两组螺杆单位时间转过的总圈数一致时,螺杆转速比为2∶3的组合混合能力稍优于转速比为2∶1的组合。     

稻壳吸附剂的制备及其吸附聚丙烯酰胺的应用研究

采用稻壳为原料,使用浓硫酸炭化活化稻壳方法制备稻壳活性炭。将所制备的活性炭吸附处理聚丙烯酰胺污水,确定了活性炭最佳吸附能力的制备工艺条件,并通过一系列实验得出了稻壳吸附剂吸附溶液中HPAM的最佳实验条件,并深入研究了其吸附处理HPAM过程的吸附动力学,确定了其等温吸附线模型。实验结果表明,采用浓硫酸处理稻壳的方法制备活性炭具有方法简单、处理效果好的特点,因此在含聚污水的前期预处理中具有良好的应用前景。     

Pulsation error in a rotameter

The effect of square-wave pulsations in gas flow on the performance of a rotameter has been studied. The experimental variables were pulsation frequency (1–24 Hz), gas flow rate, gas density, float mass, and the gas volume between the pulse generator and the flowmeter. The fluctuation in float position was found to decrease with increasing frequency and this was in agreement with a simplified theoretical model. Pulsation caused the rotameter to over-read by as much as 100% and in some cases the error was appreciable even when the float was almost stationary. The error decreased as the damping volume was increased. The factor of error was correlated empirically with the above variables. The results were also compared with other published data and theory, and with a numerical solution of the equations of motion of the float. The numerical solution was found to predict the error satisfactorily in cases where a damping chamber was used and where float bouncing did not occur.     

D-对羟基苯甘氨酸的制备

采用乙醛酸法合成DL-对羟基苯甘氨酸,再用氯化亚砜法将DL-对羟基苯甘氨酸酯化后与L-(+)-酒石酸成盐,甲醇做溶剂,水杨醛作消旋剂,利用不对称转化法制得D-对羟基苯甘氨酸甲酯酒石酸盐,经水解,中和得到D-对羟基苯甘氨酸。考察了酯化条件及消旋剂的用量,并对水解条件进行了优化。拆分总收率为70.7%,光学纯度99.8%。同时,采用1H NMR对化合物物结构进行了表征。     

Influence of molecular weight on the fracture properties of aliphatic polyketone terpolymers

The influence of polymer molecular weight on the mechanical properties of aliphatic polyketones was investigated. The molecular weight varied from 100,000 to 300,000 g mol⁻¹. The crystallinity was found to be independent of polymer molecular weight, as was the glass transition temperature. The yield strength and stiffness of the aliphatic polyketone terpolymers were also found to be independent of molecular weight. The post yield behaviour showed strong dependency on polymer chain length. The draw stress was increased significantly with higher molecular weight material. The impact resistance was increased with molecular weight, resulting in ductile fractures with large energy consumption upon fracture. The brittle-to-ductile transition temperature was lowered with increasing chain length. The difference in material deformation was linked to the higher mechanical connectivity and more stable post yield behaviour of the polymers with an increased molecular weight.     

液相色谱法测定环氧乙烷和乙二醇装置中气体和液体的醛含量

衍生技术与液相色谱法相结合,将样品与过量的2,4-二硝基苯肼衍生液混合,样品中的甲醛、乙醛分别与2,4-二硝基苯肼发生衍生反应,生成甲醛、乙醛的腙衍生物,用高效液相色谱ODS柱分离,采用DAD检测器在254nm波长下分别测量峰面积,应用标准曲线外标方法计算结果,准确定量测定样品中的甲醛、乙醛含量,解决了环氧乙烷装置反应器出口气中、乙二醇水溶液中以及环氧乙烷和乙二醇产品中的甲醛、乙醛分别定量测定的技术难题,高效、灵敏、准确。     

沙棘叶中总黄酮的提取与测定

研究沙棘中总黄酮的提取条件及含量测定。通过实验得出最佳条件是:乙醇的浓度为80%。pH为9,时间为6h,样品前处理是用石油醚除去油脂、色素等杂质。这种方法简单易行,用芦丁制出标准曲线,推出计算公式,计算沙棘叶中总黄酮的含量(以芦丁计)。     

利用往复扰动螺棱强化单螺杆挤出机内混合模拟表征

提出了采用副螺棱轴向往复运动提高单螺杆挤出机混合的结构并建立了相应的数学模型。对挤出机内牛顿流体三维周期性流动和混合过程进行了数值模拟。采用有限体积方法,变量分布采用交错网格,副螺棱的周期性运动边界通过叠加网格方式实现。采用4阶Runge-Kutta方法实现流体追踪计算,得到了示踪剂界面增长及累积停留时间分布。采用Poincaré 截面揭示混沌混合存在的区域,证实了副螺棱往复运动能够产生混沌混合效应提高螺槽内的混合效果,与其位置固定时相比,缩短了平均停留时间,停留时间分布变窄。作为对比,同时分析了常规的副螺棱位置固定的单螺杆挤出机内的相应混合行为。     

Reversible crosslinking in cellulose. VI. Formation of sulfonium derivatives by the reaction of cellulose β-mercaptoethylaminocarboxylate with methyl iodide

The reaction of methyl iodide with cellulose β-mercaptoethylaminocarboxylate (RDTC) made from cotton was investigated. The product was found to contain dimethyl sulfonium groups in addition to S-methyl groups, with accompanying hydrolytic cleavage of some of urethane linkages. The iodide counterions could be easily exchanged with hydroxide and chloride ions. The dyeabilty of RDTC and its sulfonium derivatives toward Direct Sky Blue A was studied. The equilibrium uptake of the dye by RDTC decreased with increasing sulfur content, while the uptake by the sulfonium derivatives was higher than that of control cotton and increased with increasing sulfonium content. The counterions did not affect the dyeability. The dye adsorbed onto the sulfonium derivatives was very fast against solvent extraction, and could be extracted only with Cadoxen containing 0.5% sodium hydroxide. The equilibrium uptake of the dye was much more than the amount calculated on basis of the 1 : 1 ionic bonding between the sulfonic acid group in the dye molecule and the sulfonium group in the modified cotton. The spatial effect in the dye–sulfonium bonding is discussed.     

Studies on disulfide-crosslinked nylon. II. Stress relaxation of disulfide-crosslinked polycaprolactam fibers in water

The stress relaxation at 100% elongation in water was investigated for disulfide-crosslinked polycaprolactam (DSPC) fibers prepared from N-mercaptomethyl polycaprolactam. The stress decreased faster with increasing temperature and with increasing mercaptan content of the fiber. Little stress decay took place when the fiber was treated with a mercaptan-blocking reagent. It was concluded that the controlling mechanism of the stress relaxation was the mercaptan/disulfied (SH/SS) interchange reaction. The remanent stress observed for the stress relaxation was fairly high and increased with decreasing mercaptan content of the fiber. The stress decay curve was not Maxwellian. It has been suggested that the concentration of mercaptan that could not participate in the interchange with stressed disulfide bonds increased with increasing cycles of the interchange reaction. A kinetic equation is presented and the activation energy of the SH/SS interchange reaction was evaluated as 22.3–23.9 kcal/mole. The stress relaxation of DSPC fibers in dilute β-mercaptoethanol was also studied. The stress decreased more rapidly to almost zero and the decay curve was Maxwellian. The activation energy of the reaction was 17.1 kcal/mole. These results were compared with the stress relaxation of wool fibers.