四氯化硅为原料制备二氧化硅粉体的研究

以多晶硅生产中的副产物四氯化硅为原料,在碱性溶液中制备了二氧化硅.研究了碱性溶液种类、浓度以及后处理、表面活性剂对于二氧化硅性能的影响.结果表明,采用氢氧化钠质量分数为5%的氢氧化钠水溶液时,二氧化硅邻苯二甲酸二丁酯(DBP)的吸附值为2.92 mL/g,一次粒子直径在20 nm左右,BET比表面积为260.382 m2/g;不论采用何种碱液,随着碱液浓度的增大,二氧化硅的DBP吸附值都减小,相应的粒子直径也都增大;正丁醇恒沸蒸馏处理可较大幅度提高二氧化硅的DBP吸附值;制备过程中表面活性剂的加入只能一定程度上提高产品二氧化硅的DBP吸附值.     

1,4-丁二醇分离乙酸甲酯-甲醇二元恒沸物的研究

利用1,4-丁二醇与乙酸甲酯-甲醇二元恒沸物形成三元恒沸物,研究了乙酸甲酯与甲醇恒沸物的分离工艺。实验采用精馏、常压蒸馏、减压蒸馏及冷冻的方法,主要研究了各种方法对甲醇分离的影响,并获得了较佳的工艺条件。研究得出常压蒸馏法可行,乙酸甲酯纯度达到99.7%,收率98.1%,甲醇纯度96.1%,收率95.2%。     

高分散性纳米碳酸钙的制备及表面改性研究

研究了利用共沸蒸馏来克服纳米碳酸钙粒子在干燥过程中形成硬团聚的可行性,采用直接在正丁醇中加入改性剂的新工艺进行了表面改性。确定了改性剂最佳用量为3％,利用TEM、DTA-TG、BET粒度分布等手段进行了表征,探讨了共沸蒸馏克服硬团聚的机理。结果表明,共沸蒸馏后可制得分散性好的纳米碳酸钙;改性后,粒子的分散性得到了进一步的提高。     

一种精确测定二氧化硅表面羟基数量的新方法

利用二氧化硅吸附水、表面羟基和内部羟基脱水温度的差异,结合卡氏水分测试方法,建立了一种准确、高效、简单的二氧化硅表面羟基数数量测试方法。采用所建立方法对二氧化硅进行测试,研究了测试条件和测试影响因素。结果表明:该方法操作简单,结果重现性和准确性较好,对于二氧化硅工业化生产分析及品质监控具有重要的价值。     

二氧化硅消光剂生产中正丁醇回收工艺的改进

针对福建某工厂现有工艺生产二氧化硅消光剂过程,采用间歇蒸馏方式回收正丁醇存在时间长、效率低等问题,提出使用双塔精馏工艺进行改进以缩短正丁醇回收时间和提高回收效率。对改进后的工艺使用流程模拟软件进行模拟计算,获得了新的工艺条件参数。改进后,冷凝分层温度为85℃,精馏塔一塔釜液中正丁醇质量分数为99.62%,精馏塔二塔釜中正丁醇质量分数为0.31%。在此基础上搭建了实验室规模精馏装置并进行了验证试验,试验结果与模拟计算值接近,相对平均偏差为5.4%,表明模拟计算的结果可信。模拟计算结果为工业装置的优化提供了依据。改进后,正丁醇回收率将大幅提高,生产周期由原来的10 h缩短为5 h,能耗显著降低。采用此工艺生产二氧化硅消光剂可大幅降低过程成本。     

纳米二氧化硅气凝胶隔热材料的研究进展

作为一种超级隔热材料,二氧化硅气凝胶具有极高的孔隙率和极低的热导率。着重介绍了纳米二氧化硅气凝胶隔热材料的类型以及制备方法。常见的制备方法为先制成纳米孔气凝胶的颗粒和粉料,再掺入增强纤维和黏结剂,经二次成型制成复合体。分析了二氧化硅气凝胶复合隔热材料存在的问题,简要介绍了最新的改进技术,提出今后研究的主要目标,即通过廉价原料制备出较低密度下有良好强度和热导率的气凝胶复合材料,最后对其研究前景进行了展望。     

添加剂对二氧化硅包裹碳化硅材料性能的影响

本文利用碳化硅颗粒表面氧化生成的二氧化硅将碳化硅颗粒包裹起来的方法,制备了二氧化硅包裹碳化硅材料;借助XRD、SEM分析了加入不同添加剂对材料抗折强度及抗热震性等性能的影响。结果表明添加硅粉能提高二氧化硅包裹碳化硅材料的抗弯强度和抗热震性,而Cu粉和V2O5对材料的性能影响不大。     

纳米二氧化锡的多种方法制备、表征及其对比

本文采用共沸蒸馏法、水热法、溶胶-凝胶法分别制备纳米SnO2粉体,所制得的SnO2粉体利用X-射线衍射(XRD)和扫描电子显微镜(SEM)表征。结果表明,3种方法制备得的粉体均为四方金红石结构,共沸蒸馏法所得粉体平均颗粒约为20nm。水热法所得粉体的平均颗粒约为10nm。溶胶-凝胶法所得粉体的平均颗粒约为70nm。研究不同制备方法合成纳米SnO2粉体在合成工艺,生产周期,产物颗粒大小等方面的优缺点。     

提高蒸馏氢溴酸收率的方法

<正> 用溴和工业赤磷为原料生产试剂氢溴酸,常含 HBr、H_3PO_3、H_3AsO_3、HCI 等杂质,需进行蒸馏提纯。其中 H_3AsO_3恒沸物和 HCI 恒沸物沸点较低,可去头除之;H_3PO_3沸点较高,残留于蒸发锅锅底,但在实际操作中,往往由于锅炉蒸汽压力、真     

共沸精馏法制备氧化铈纳米粉体及其煅烧动力学

用碳酸氢铵做沉淀剂,采用化学共沉淀法制备纳米氧化铈的前驱体,并以正丁醇为共沸剂经过共沸精馏除去前驱体中的水分,然后再烘干、煅烧制备了纳米氧化铈晶体.通过热重和差热分析、X射线衍射和透射电镜等对颗粒结构进行表征,研究了晶体煅烧动力学.结果表明：采用该方法能够很好地抑制粉体的团聚,获得分散均匀的立方晶系结构纳米晶体,粉体的平均粒径为20～30 nm.在煅烧过程中,该体系的表观活化能为68.43 kJ/mol,且晶粒的生长过程主要受扩散作用的控制.     

亲疏水性CuBTC/PVDF复合膜应用于膜蒸馏抗油实验

采用水热法合成亲水性的CuBTC金属有机骨架(MOFs)颗粒，采用聚乙烯醇(PVA)作为黏合剂，用抽滤的方法将CuBTC颗粒附载在聚偏氟乙烯(PVDF)膜上，之后用戊二醛(GA)对PVA进行交联，制备出表层亲水、底层疏水的CuBTC/PVDF复合膜。通过场发射电子显微镜、比表面积及孔径分析仪、接触角测量仪、孔径分析仪、X射线衍射仪等对CuBTC颗粒和不同CuBTC含量的复合膜的表面特征、结构形态和稳定性进行了表征。结果表明，CuBTC颗粒有着较大的比表面积和孔容，CuBTC颗粒可以牢固地抽滤在PVDF膜表面，热稳定性高且有较好的柔韧性。与抽滤前的PVDF膜相比，随着CuBTC颗粒的增多，膜厚度有所增加，孔径和孔隙率有所减小，但对其膜蒸馏膜通量的影响不大，且在CuBTC含量在0.6 g时表现出较好的性能。在以1 g/L原油和35 g/L氯化钠混合溶液为进料液对原膜和复合膜进行直接接触膜蒸馏抗油污实验，发现原膜很快被油污染堵塞毛孔，而复合膜具有良好的抗油污染能力，可以进行长期的膜蒸馏实验。     

Preparations of silica slurry for wafer polishing via controlled growth of commercial silica seeds

Silica slurry in aqueous medium for wafer polishing was prepared by sol-gel reaction of silicon alkoxide utilizing commercial silica particles as seeds that were grown stepwise through intermittent additions of tetraethylorthosilicate (TEOS) as a silica precursor. Before the growth reaction, the commercial silica particles were pre-treated in the vibratory mill partially filled with zirconia ball and the sonicator to ensure good dispersion. The alcohol left after growth reaction was removed by vacuum distillation and repeated washings with distilled water followed by centrifugations. Then, the alcohol-free silica particles were redispersed in water. The dispersion stability of the silica slurries was examined by measuring surface charge of silica particles and rheological properties. Finally, wafer-polishing performance of the prepared silica slurries was considered by measuring the polishing (or removal) rate, and RMS (root mean square) roughness of the polished wafer surface. For the polishing, MEA (monoethanolamine) and TMAH (tetramethylammonium hydroxide) were used as polishing accelerators. The polishing result showed that the removal rate was nearly independent of the concentrations of MEA and TMAH in the range of 0.3-0.5 wt% and 100-500 ppm, respectively. One of the most interesting features is that hydrothermal treatment of the prepared silica slurries in autoclave increased the removal rate as high as ten times. Although the removal rate was increased by the increased size of the abrasive particle, surface roughness of the polished wafer surface was deteriorated.     

Preparation of monodisperse hydrophilic polymer microspheres with N,N′‐methylenediacrylamide as crosslinker by distillation precipitation polymerization

Highly crosslinked cauliflower‐like poly(N,N′‐methylenebisacrylamide) particles were prepared by distillation precipitation polymerization in neat acetonitrile with 2,2′‐azobisisobutyronitrile as initiator. Monodisperse hydrophilic polymer microspheres with various functional groups, such as amide, pyrrolidone and carboxylic acid, with a spherical shape and smooth surface in the size range 120–600 nm were prepared by distillation precipitation copolymerizations of functional comonomers including N‐isopropylacrylamide, N‐vinylpyrrolidone, methacrylic acid with N,N′‐methylenebisacrylamide as crosslinker. The polymer particles were formed and precipitated out from the reaction medium during the distillation of the solvent from the reaction system through an entropic precipitation manner. The effects of the solvent and the degree of crosslinking on the morphology and the loading capacity of the functional groups of the resultant polymer particles were investigated. The resulting polymer particles were characterized with scanning electron microscopy, transmission electron microscopy, dynamic light scattering and Fourier transform infrared spectroscopy. Copyright © 2007 Society of Chemical Industry     

自组装法制备PVDF-SiO2/PVSQ超疏水复合膜及膜蒸馏抗污染性能

采用乙烯基三甲氧基硅烷(VTMOS)对SiO₂疏水改性,通过自组装法,将改性SiO₂接枝在商业PVDF(聚偏氟乙烯)膜表面,使其表面达到超疏水。利用场发射电子显微镜、红外光谱仪、接触角测量仪及毛细流孔径分析仪等仪器对改性前后膜的表面形貌、化学组成、接触角及孔径变化等性能参数进行表征。结果表明,VTMOS不仅对SiO₂疏水改性,还通过自身的水解缩聚反应,生成了规整圆球状的聚乙烯基倍半硅氧烷(PVSQ)微粒,纳米级SiO₂分布于微米级PVSQ表面,在改性膜表面构造了多层次微/纳米粗糙表面,在低表面能疏水基团乙烯基和甲氧基的共同作用下,成功实现了超疏水改性,改性膜水接触角达到159.5°,滚动角降至8.1°。以NaCl、HA和CaCl₂混合溶液为进料液,对商业PVDF膜和改性膜进行了长期直接接触式膜蒸馏(DCMD)实验,探究其抗污染性能。结果表明,改性膜适用于长期DCMD实验,并表现出比商业PVDF膜更稳定的通量,截盐率始终大于99.99%,具有良好的稳定性和抗污染性能。     

纳米粉体干燥方法的研究进展

由于纳米粒子的表面效应，用湿法制备出的纳米粉体的前驱——胶体的干燥已不能采用传统的干燥方法。根据胶体干燥的理论，阐述了纳米粉体干燥过程的团聚机理，并综述了纳米粉体在超临界干燥、共沸蒸馏、真空冷冻干燥、微波干燥等干燥领域的研究进展。     

Three‐phase fluidized distillation

Separation efficiency in distillation operations can be improved by modifying the characteristics of the dispersions formed on the trays. The present work reports on the hydrodynamic and mass transfer characteristics of liquid‐solid‐vapour dispersions formed on sieve trays without downcomers of a distillation column operating under total reflux conditions. Murphree efficiency and the operating limits of distillation using the ethanol‐n‐butanol system are analyzed for a large range of vapour velocities and liquid mixture compositions, utilising wettable PVC particles and non‐wettable silicone, PE, and Teflonr? particles. It was verified that wettable particles show a drastic reduction in the upper operating limit of vapour velocity, but this does not occur for non‐wettable particles. Tray efficiency can be increased when non‐wettable particles are used, mainly for high vapour velocity operations.     

Effectiveness of mass transfer in a packed distillation column in relation to surface tension gradients

In packed columns large differences occur in the wetting of the particles and especially in the refreshing of the liquid on the wetted particles due to gradients in surface tension of the liquid/gas interface. Mass transfer rates may differ with a factor 2. In a column packed with Berl saddles distillation experiments were performed with a mixture n-heptane/cyclohexane. Ceramic Berl saddles of 4, 6 and 10 mm were used as well as aluminum Berl saddles of 4 mm. In some of the experiments the saddles were coated with PTFE (teflon). The driving force for mass transfer was varied over a wide range. Both negative and positive driving forces were realized. The influence of the surface tension driven refreshment of the interface is most pronounced for small particles; for larger liquid flow rates, that may be applied in beds with larger particles, the effect is obscured by the inertia of the downcoming liquid.     

模拟生物油分子蒸馏的响应面法工况优化

分子蒸馏是一种高效的生物油分离技术。本文应用刮膜式分子蒸馏装置,对模拟生物油在不同蒸馏温度、蒸馏压力和进料速率下的分离特性进行了研究,考察不同因素对族类化合物蒸出特性的影响。随后采用响应面分析法对模拟生物油分子蒸馏进行了计算机模拟,考察多种因素对分子蒸馏的交叉影响。通过ANOVA分析,模型的F值为21.25,表明模型是显著的。并以目标物酸醛酮在馏分中的质量分数为响应值得到最佳工况：蒸馏温度69.83℃,蒸馏压力1498.31Pa,进料速率5.54mL/min,此时轻质馏分中酸醛酮的质量分数为39.12%。最后在此工况下开展了模拟生物油的验证实验,结果显示馏分中目标物的质量分数为38.96%,与响应面模型吻合良好。模拟生物油经过分子蒸馏后酸醛酮的质量分数由28.50%提升至38.96%,同时酚类的质量分数由37.50%降低到25.14%。     

气相色谱法测定洗油馏程的方法探讨

介绍了气相色谱法测定洗油馏程的原理,并对其方法进行了探讨、研究.将气相色谱法和蒸馏法进行对比,结果表明,采用气相色谱法测定洗油馏程方法简便,操作快捷,准确度高,测定结果与蒸馏法基本一致.     

减压膜蒸馏过程纤维膜表面热质传递特征模拟分析

采用CFD数值模拟的方法,建立了错流式单根中空纤维减压膜蒸馏过程的三维计算模型,对纤维膜表面不同位置的局部热量和质量传递特征进行了研究。研究结果表明,纤维膜表面的速度分布、温度分布、对流传热系数分布以及蒸发速率均随着位置的改变而改变,且具有相似的规律,在相位角60°到90°之间有最大值,而在相位角0°和180°附近其值较小;料液流速显著影响纤维膜表面的热质传递参数的分布,蒸发速率和传热系数均随着流速的提高而增大;传热系数随着真空度的提高而迅速降低。本研究结果加深了对中空纤维减压膜蒸馏过程的认识,对膜过程强化具有指导意义。