添加晶种对磷酸二氢钾结晶特性的影响

采用间歇结晶法研究了磷酸二氢钾的添加晶种结晶,考察了添加晶种时的搅拌速率、温度以及添加的晶种粒度、晶种量对结晶产品粒度分布和平均粒径的影响,并与自发成核结晶进行了比较。实验结果表明:添加晶种结晶能有效改善产品粒度分布、增大平均粒径。添加晶种时适宜的结晶条件为:搅拌速率150r/min,温度70℃,晶种粒度40!60目,晶种量1%。产品粒径大于40目的晶体累计质量分数达84.23%,平均粒径为645.37μm。相比自发成核结晶,粒径大于40目的晶体累计质量分数增加了22.46%,平均粒径增大了约100μm。     

混炼工艺对天然橡胶胶料中氧化锌粒子微细化的影响

分析两个普通氧化锌样品的粒子形态,考察优化混炼工艺对天然橡胶胶料中两个氧化锌样品粒子的微细化作用。结果表明:普通氧化锌粒子聚集形成聚集体,2~#氧化锌聚集体粒子尺寸明显大于1~#氧化锌;胶料混炼时将氧化锌先于其他小料加入,能够使氧化锌粒子微细化,但效果不明显;采用一段母炼法混炼,能大幅度减小氧化锌粒径,改善硫化胶的综合性能。     

溶析结晶法制备聚苯乙烯微粒

采用溶析结晶法制备了球形聚苯乙烯(PS)亚微米粒子,并用激光粒度仪、FESEM等分析方法对粒子大小、粒度分布以及粒子形貌等进行了表征,对料液浓度、搅拌速度、料液/反溶剂体积比、结晶温度对粒径的影响进行了考察.结果表明,溶析结晶法制备的PS粒子为球形,粒径分布比较窄,平均粒径在500nm左右,比文献报道的超临界流体技术法制备的PS颗粒小;料液浓度是影响粒径的重要因素,其他因素对粒径影响较小.     

硅酸乙酯为原料反相微乳液法制备纳米二氧化硅

采用NP-5/环己烷/去离子水体系制备反相微乳液,绘制了该体系的三元相图,并以正硅酸乙酯(TEOS)为原料,在碱性条件下受控水解反应制备了纳米SiO2粒子,探讨了[n(水)∶n(表面活性剂)](用R表示)和[n(水)∶n(TEOS)](用H表示)对SiO2纳米粒子粒径的影响。通过扫描电镜(SEM)和激光粒度仪对样品形貌和粒子大小和粒径分布进行了表征。结果显示:扫描电镜下观察到的SiO2粒子为无定型球形颗粒,粒径在200～500 nm的范围,激光粒度仪分析得到的平均粒径随着R和H的增大而增大。     

硝酸钾结晶生长特性的研究

利用5LMSMPR结晶器,通过改变停留时间、过饱和度和搅拌速度等因素,对硝酸钾结晶的粒度分布、平均粒径、主粒径、成核及生长速率等动力学特性进行了研究,并在结晶温度25℃、过饱和度2℃、搅拌速度400r/min和停留时间10～50min条件下,建立了硝酸钾晶体生长动力学模型:B°=6.19×1022G2.02。研究结果表明:当停留时间大于30min、搅拌速度为400r/min时,晶体的平均粒径和主粒径较大;过饱和度的减小也会使晶体粒径增大,但其影响较小。     

碱洗氧化工艺中杂质对硫酸钠结晶粒度的影响

针对碱洗氧化工艺脱硫废水中硫酸钠的蒸发结晶,设计开发了硫酸钠蒸发结晶放大实验装置,重点研究了废水中碳酸钠、铁离子和亚硫酸钠杂质对硫酸钠蒸发结晶晶体粒度的影响。结果表明：1.0%（质量分数）的碳酸钠对硫酸钠晶体的粒径影响可忽略;铁以沉淀物形式存在时,易引起硫酸钠晶体结块且粒径变小; 铁以溶解形式存在时,对硫酸钠晶体的粒径影响较小;亚硫酸钠的存在易引起硫酸钠晶体的粒径变小,氧化消除溶液中的亚硫酸钠后,结晶得到的硫酸钠晶体粒径变大。工业装置经过改造后,无水Na₂SO₄产品的平均粒径由106.71 μm提高至129.99 μm。     

超临界CO2辅助挤出制备PP/POE共混物微观形态与性能

采用带有超临界CO2注人装置的双阶挤出机组制备了聚丙烯/乙烯一辛烯共聚物(PP/POE)(100/10)共混物。采用扫描电子显微镜观察了PP/POE共混物脆断面的微观形态,利用ImagePro Plus软件定量分析了弹性体POE粒子在PP基体中分散的平均粒径和粒径分布,通过差示扫描量热仪和偏光显微镜考察了PP/POE共混物的结晶过程。结果表明,当超临界CO2注人量为2. 5份(样品PP2. 5)时,弹性体POE粒子在PP基体中的分散粒径最小,粒径分布最窄;其中最小平均粒径为0.34 μm,粒径分布为1. 44;样品PP2. 5的结晶度最高,为53. 57%,且具有最细小致密的晶体形态。     

微悬浮法PVC糊树脂的合成研究

采用三氯乙烯作为氯乙烯模拟液,研究主/助乳化剂结构、用量和比例等对分散液滴粒径及粒度分布的影响。采用5 L高压夹套釜进行氯乙烯微悬浮聚合,研究主/助乳化剂结构、用量、比例和水油比对PVC初级粒子平均粒径和粒度分布的影响。发现以十二烷基硫酸钠(SDS)为主乳化剂时分散液滴的尺寸最小,PVC胶乳稳定,粒度分布窄;随着脂肪醇助乳化剂链长的增加,分散液滴尺寸明显减小,十六醇、十八醇或两者的混合醇是氯乙烯微悬浮聚合适宜的助乳化剂;随着十六醇或十六~十八混合醇与SDS用量比的增加,分散液滴和PVC胶乳粒子的尺寸逐渐减小,粒度分布趋窄。微悬浮聚合PVC糊树脂包含粒径范围较宽但呈连续分布的初级粒子,通过主/助乳化剂用量比的改变,可调节PVC初级粒子的平均粒径及粒度分布。     

锐钛型二氧化钛的合成及其性能研究

采用均匀沉淀法制备了锐钛型二氧化钛,然后在适当酸度、DBS浓度、处理温度及反应物浓度环境下将二氧化钛进行了处理,对处理后样品进行了XRD、N2吸附、粒度分析表征样品的结构、晶体形貌、物性情况及粒度分布情况,发现二氧化钛物性情况有较为明显的改善,处理后的TiO2样品比表面积达346 m2·g-1,孔容达0.31 mL·g-1,TiO2粒子平均粒径不大于10 nm.     

团聚对亚微米5A分子筛粒度分析的影响

为了考察小晶粒分子筛团聚对亚微米级5A分子筛粒度分布结果的影响以及适宜的测定条件,实验以水为分散介质,六偏磷酸钠为分散剂,在超声波辅助作用下,用电位/粒度分析仪测定研究了试样浓度、分散剂用量和超声时间对亚微米级5A分子筛分散性的影响。结果表明,当分子筛含量大于5 g/L时,晶粒团聚现象严重,粒度分布呈现单峰(假象),导致粒度测量结果偏大;加入少量(0.005~0.195 g/L)的六偏磷酸钠,有缓解晶粒团聚作用,可将较大团聚粒子(大于2.8μm)分散为较小粒子(1.3μm左右),少量团聚粒子分散成单个晶粒,可测得较小晶粒粒径;超声作用可使较大团聚粒子(0.85~2.80μm)分布峰强度降低,相对较小粒子(0.30~0.85μm)分布峰强度增加。超声时间不宜太长,否则将加剧粒子间团聚,使得测定粒径偏大。当试样中5A分子筛含量为5 g/L,六偏磷酸钠浓度0.195 g/L、超声时间4 min条件下,测得5A分子筛试样粒径分布0.25~0.80μm,峰顶对应粒径为0.473μm,中位径(d50)为0.784μm,与电镜分析结果一致,说明是较为准确的粒度分析方法。     

Contributions of TMAH Surfactant on Hierarchical Structures of PVA/Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>–TMAH Ferrogels by Using SAXS Instrument

The magnetic hydrogels combining polyvinyl-alcohol (PVA) and Fe₃O₄ (magnetite)–TMAH (tetra-methyl ammonium hydroxide) have been successfully fabricated via a Freezing-thawing route. The magnetite nanoparticles were prepared from iron sands by using coprecipitation method. The transmission electron microscopy image revealed that the magnetite nanoparticles with a reaction temperature of 30 °C had the average particle size of 12 nm in clusters of aggregation. The result was similar to the particle size obtained from X-ray diffraction data analyzed by Scherer equation. Furthermore, synchrotron small angle X-ray scattering data were analyzed by using two lognormal distributions to calculate the distribution of the individual magnetite particles. Meanwhile, Teubner-Strey and Beaucage models were employed to observe the distribution of magnetite particles coated by TMAH as a surfactant. The data analysis showed that the magnetite particles within the magnetic hydrogels formed aggregations with diameters of cluster particles in the range from 13.1 to 31.8 nm. Interestingly, the diameter of clusters particle increased from 13.1 to 31.8 nm along with the increasing concentration of ferrofluids from 1 to 15 wt%. This phenomenon was predicted to result from the effect of TMAH as a surface reactant agent that prevented the aggregation by coating the surface of the magnetite nanoparticles.     

Brownian dynamics simulation of the aggregation of submicron particles in static gas

A Brownian dynamics simulation was conducted to investigate the formation of aggregates that are composed of submicron particles such as soot. Three models were considered for aggregation: a diffusion-limited aggregation model, in which an aggregate grows around a fixed particle; a particle–cluster aggregation model, in which a single aggregate grows by collisions between particles and the aggregate; and a cluster–cluster aggregation (CCA) model, in which many particles and aggregates form multiple aggregates. A comparison of the three aggregation models showed that the CCA model resulted in a soot-like branching shape. The aggregation was investigated by employing the CCA model; it was determined that increase in gas temperature affected the shielding effect of the aggregate branch by changing the displacement and velocity of Brownian particles. Furthermore, these simulations demonstrated that the size and aspect ratio of the field and the particle density also affected aggregation shape.     

Application of inline imaging for monitoring crystallization process in a continuous oscillatory baffled crystallizer

In this study, an in situ imaging system has been analysed to characterize the crystal size, the shape and the number of particles during a continuous crystallization process in a Continuous Oscillatory Baffled Crystallizer (COBC). Two image analysis approaches were examined for particle characterization in the suspension containing both small nuclei and larger grown crystals (nonspherical and irregular in shape). The pattern matching approach, in which the particles are approximated to be spherical, did result in an overestimation of the size. Alternatively, a segmentation‐based algorithm resulted in reliable crystal size and shape characteristics. The laser diffraction analysis in comparison to the image analysis overestimated the particle sizes due to the agglomeration of particles upon filtration and drying. The trend in the particle counts during the start of crystallization process, including nucleation, determined by the image analysis probe was comparable with the one measured by FBRM, highlighting the potential of in situ imaging for process monitoring. © 2018 American Institute of Chemical Engineers AIChE J, 64: 2450–2461, 2018     

Preparation and reshaping of composite microparticles for color toner based on the encapsulated nanoparticles

In this paper, the styrene–acrylic resin-encapsulated organic pigment composite nanoparticles were synthesized by mini-emulsion polymerization first, and then the aggregated microparticles used for color toner were prepared via the emulsion aggregation method. Transmission electron microscopy, dynamic light scattering, and zeta potential analysis manifest that when the emulsifier dosage was 5 wt% of the monomer, the composite nanoparticles owned clearly core-shell structure, uniform size, and appropriate zeta potential, which was conducive to the subsequent aggregation. The evolution of aggregated particle size and morphology under different stirring rates, coagulant concentrations, and temperatures was investigated by mastersizer and scanning electron microscopy. The result shows that when the stirring rate was 1,000 rpm, coagulant concentration was 0.2 mol/L, and the curing temperature was 65°C, aggregated particles with suitable size, narrow size distribution, and regular shape could be obtained. The reshaping of aggregated particles can further improve their morphology. When the reshaping temperature was 75°C, the product particles owned perfect spherical shape, and there were almost no cracks and pores on the surface of the particles. This synthesis strategy is believed to provide a guide for the fabrication of composite microparticles with controllable particle size and morphology.     

无水醋酸钠结晶过程中析晶温度和颗粒粒径在线测量

结晶过程是化工单元操作中一种高效节能的固液分离与提纯技术,广泛应用于食品、医药、染料等生产过程。结合超声法、图像法和光学浊度法研究了无水醋酸钠的结晶过程,通过超声模型结合最优正则化反演算法求解晶体颗粒粒度分布,在线测量了不同降温速率和搅拌速率下的析晶温度、晶体尺寸和形貌变化。结果表明：较快的降温速率可促进晶体生长,搅拌速率较快初期晶体尺寸较大,但后期由于颗粒磨损致平均尺寸减小;相同条件下光学浊度法较超声法较早测得析出晶体,实验中析晶温度偏差低于15%;图像法直观观察到了晶体生长过程并较好表征了晶粒形貌,与超声法具有接近的晶粒增长趋势,当晶体稳定析出后两者体积中位径偏差在15%以内,均较好地反映了实验条件对结晶晶体尺寸的影响。光学方法可更精细体现结晶初期特征,而在结晶后期超声法仍可对粒径进行有效测量。     

Al2O歧化法制备微细Al2O3/Al复合粉体

真空条件下,以Al2O3和Al为原料,通过Al2O歧化法制备微细Al2O3/Al复合粉体.XRD和SEM分析表明:在反应温度为1200～1400℃时,随着温度的升高,粉体中氧化铝含量升高;冷凝温度约为550～750℃时,复合粉体中的氧化铝包括稳定晶型和不稳定晶型;冷凝温度约为1100～1300℃时,复合粉体中的氧化铝全部为稳定晶型;冷凝温度约为550～650℃时,复合粉体的平均粒径小于0.5μm;冷凝温度约为750℃时,铝熔化、微粒团聚;冷凝温度约为1100～1200℃时,铝形成铝珠,氧化铝为不规则状、平均粒径小于2μm;冷凝温度约为1300℃时,氧化铝为片状.因此,通过选取合适的反应温度、冷凝温度,可以控制Al2O3/Al复合粉体中氧化铝的含量、晶型和粒径.     

Variation of particle size and its distribution during the synthesis of silicalite-1 nanocrystals

Recent studies imply that the external surface area of the nanozeolite product may, at least in some cases, be related to the average size of the particle population participating in aggregative nucleation, a population which itself is a product of aggregation of even smaller primary nanoparticles. This possibility puts more importance on our understanding of the variation of particle size and its distribution during the crystallization of zeolite nanoparticles. Variation of the particle size and PSD during nanoparticle silicalite-1 crystallization was followed with respect to time by a laser light scattering device with a scattering angle of 173°, for several starting synthesis compositions. Effects of varying TPAOH and water contents in the starting synthesis mixtures on the variation with time of the particle sizes and PSDs, especially across the two distinct aggregation events, were investigated. The products were also analyzed by XRD and AFM. Parallel to the decrease in the average particle size of the final product population with increasing alkalinity and organic template content, its PSD was observed to become narrower too. A reversal in the dependence on TPAOH content, of the average size of the population formed by aggregation, with respect to that of the population participating in aggregation, was observed across both aggregation events, implying that smaller particles aggregated to form larger particles, while larger particles aggregated to form smaller particles during these processes, and this was also seen from the AFM images, to be reflected to the surface features of the final product particles.     

Measurement of coal particle size and shape with concentrated coal-water mixtures

The behavior of concentrated coal-water mixtures having narrow particle size ssfractions of coal was investigated. The pulverized coal was fractionated into six distinct particle size ranges, i.e. -70+80, -80+120, -120+140,-140+200, -200+400 and -400 mesh sizes by using a series of sieves. Settling rates were determined as functions of solids concentration for suspensions in water of coal particles to establish the measurement of particle size and shape factor and to assess concentration effect upon the observed hindered settling rates. The settling rates were modelled using the Richardson-Zaki model with the exponent n variable to account for the nonspherical shape of the coal particles. The data was also correlated with the Michaels-Bolger model which explicitly account for the excess water which is dragged down along with the particles undergoing sedimentation. In addition, coal particles and suspensions were characterized by coal analysis, heating value, solid heat capacity and thermal conductivity, densities, maximum packing concentrations and pore size distributions.     

在线分析乙醇及超声波对硫酸钾晶核粒度的影响

目前,国内外生产的硫酸钾产品普遍存在粒度小、形貌差等问题。先用在线粒度仪分析无水乙醇加入量、搅拌转速、超声波功率等条件对硫酸钾起晶晶核的影响,然后研究硫酸钾晶核在浓缩的含硫酸钾洗脱液中生长的产品晶形的特点,为企业利用糖蜜酒精废液中的钾离子生产大颗粒硫酸钾提供理论支持。实验结果表明：在低温浴槽温度为30 ℃、搅拌转速为250 r/min、超声波功率为50 W、无水乙醇与饱和硫酸钾溶液质量比为1∶1条件下起晶,制得的硫酸钾晶核尺寸均匀、表面完整,颗粒平均弦长为14.5 μm。将制备的硫酸钾晶核投入到浓缩的从糖蜜酒精废液中分离出来的含硫酸钾的洗脱液中生长,可以得到粒度较大、晶形完整的硫酸钾产品,硫酸钾产品中粒度大于385 μm的晶体质量占结晶体质量的81.2%左右,钾离子结晶回收率约为85.8%。