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冷却结晶是经典的溶液结晶过程,常用于分离溶解度随温度变化较大的物质,制备高品质晶体产品。直接进行降温会导致成核速率不可控,得到的晶体产品质量差。在工业中通常选择在溶液结晶介稳区内投放适量晶种来诱导成核,但晶种制备过程复杂,而且成功的添加晶种过程取决于晶种的粒度分布、数量、投放时机和操作人员的经验等因素,降低了产品质量的批次重复性。本文利用聚四氟乙烯(PTFE)中空纤维膜组件为结晶溶液和冷却液提供换热界面,结晶溶液温度降低,在膜界面处形成较均匀的过冷度梯度,进而在低过饱和度下发生异相成核,实现膜辅助添加晶种的过硫酸铵冷却结晶过程调控。膜组件中产生的晶种进入结晶釜中继续生长,将成核和生长过程进行解耦。在线结晶检测系统捕捉到的照片证实了通过控制膜组件使用温度和时长两个操作参数便可得到具有较好的形貌、较窄的粒度分布的晶种。相比直接冷却结晶,在相近的降温速率下,膜辅助添加晶种过程制备的晶体产品具有更大的平均粒径,且粒度分布更集中,表面更加光滑。因此,膜辅助冷却结晶呈现了良好的成核控制能力,有望实现晶种自动制备和添加功能,为高附加值晶体产品的冷却结晶过程开发提供了新方向。 相似文献
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晶种添加量对硝酸钾溶液间歇结晶过程的影响研究 总被引:1,自引:0,他引:1
针对添加晶种的间歇结晶过程,基于DL定律和粒数衡算方程,建立了晶体生长溶液浓度与晶种量及其生长速率的数学表达式。实验考察了晶种添加量对KNO3-H2O间歇冷却结晶过程的影响。结果表明:随着晶种量的增加,模拟溶液浓度与实测浓度之差DC减小;同时体系相对过饱和度逐步受到抑制,其变化范围和幅度均呈现下降趋势;当晶种添加量达到或超过0.332g(100gH2O)-1时,DC在整个过程接近于0,体系基本无新核产生,过程以生长为主导,即对于添加晶种的结晶过程存在最小晶种量。由实时测定的溶液浓度和透光率得到的参数DC可确定相应工艺条件下的最小晶种添加量,为结晶产品的质量控制和优化提供了分析手段。 相似文献
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以90℃的Na2CrO4-NaOH-H2O体系相图为依据,采用蒸发盐析结晶的方法从体系中分离铬酸钠晶体,研究了搅拌强度、蒸发速度、结晶温度、晶种添加等因素对工艺过程的影响规律,得到最优工艺操作条件:搅拌强度为能使晶体离底悬浮所需的最小转速;每1 050 g原料的蒸发速率约为140 mL/h;结晶温度为90℃;并添加一定量的晶种。在以上操作条件下制备出的铬酸钠晶体粒度较大,尺寸均一。同时研究了不同氢氧化钠浓度下体系压力与沸点间的关系,为铬酸钠结晶过程的温度控制提供了基础数据。 相似文献
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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。 相似文献
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低温控温结晶法分离提纯1,8-桉叶油素的工艺 总被引:1,自引:0,他引:1
《化工进展》2016,(2)
采用全结晶工艺对原料桉叶油[w(cineole)=63.24%]进行分离提纯,在无晶种添加下,降温速率4℃/h、结晶终温-30℃、发汗速率5℃/h、发汗终温-19℃时,可将原料油提纯至77.52%。添加晶种后,可有效提高操作温度,缩小结晶温度的操作范围,提高产品的纯度,在降温速率4℃/h、结晶终温-25℃、发汗速率4℃/h、发汗终温-6℃的操作条件下,将原料油提纯至89.63%。实验得到了低温控温添加晶种结晶法分离提纯1,8-桉叶油素的适宜工艺流程和操作参数,该方法相对其他分离方法具有较为明显的优势。 相似文献
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针对头孢拉定反应结晶工艺,设计了双股进料结晶体系,将结晶环境控制在介稳区,有效避免自发成核,操作简单,容易控制。采用单因素法研究了结晶液初始浓度、料液流加速率、搅拌速率、结晶p H值范围、晶种添加量以及养晶时间对结晶产品收率、晶习及粒度分布的影响,确定了优化的工艺参数:结晶液初始浓度(溶质质量/溶剂质量)0.43 g/g,料液流加速率2 m L/min,p H值2.5~2.7,晶种添加量按公式计算,养晶时间60 min,搅拌速率为140 r/min可以得到均匀的棒状晶体,搅拌速率为70 r/min可以得到均匀的簇状聚结体,晶习完整,粒度分布均匀,收率可以达到92%。 相似文献
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In order to overcome the elementary heterogeneous nucleation while octahydro trisodium salt of fructose-1,6-diphosphate(FDPNa3 8H2O) is crystallized with ethanol precipitation at low temperature, a new crystallization method with alcohol precipitation combined with salt precipitation has been presented. The ethanol-sodium acetate system for crystallization of salt of fructose-1,6-diphosphate is based on the mechanism of crystallization of FDPNa3 8H2O in the ethanol-low temperature system. It is found that crystal size may be controlled by regulating temperature or pH value of solution in the crystallization process, and the crystal yield increases to 95% from 78% which obtained in the ethanol-low temperature system. 相似文献
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湿法氟化铝一般采用常压结晶工艺生产,其存在产品结晶水含量高、结晶时间长、产能低等弊端。对此,研究了氟化铝加压结晶工艺技术,考察了结晶压力、结晶时间、晶种添加量、加料温度等因素对氟化铝结晶水含量的影响。优化工艺及条件:将氟硅酸溶液加入反应槽中,加热到70~80 ℃,按照氟硅酸和氢氧化铝物质的量比为1.1:1加入氢氧化铝,在95~105 ℃反应30 min,过滤得到氟化铝溶液和硅胶沉淀;将氟化铝溶液转入高压结晶釜中,添加15%(质量分数)的氟化铝晶种,控制结晶釜内的温度为170 ℃,维持结晶压力为0.7 MPa,结晶时间为3 h;将高压结晶釜内的温度降到80~90 ℃,对结晶后的料浆进行真空抽滤,再经洗涤得到氟化铝软膏;将氟化铝软膏置于120~180 ℃下干燥脱去附着水,再逐步升温至400~600 ℃进行煅烧,除去产品中的结晶水,冷却后得到氟化铝产品。实验结果表明,采用加压结晶工艺制备氟化铝,不仅降低了产品结晶水含量和生产成本,提高了产品质量和产量,而且解决了制约磷化工、氟化工和电解铝行业发展的瓶颈问题。 相似文献
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Walter Gsele Wolfgang Egel-Hess Klaus Wintermantel Friedrich Richard Faulhaber Alfons Mersmann 《化学,工程师,技术》1990,62(7):544-552
Formation of solids by crystallization and precipitation. Formation of solids from solutions can take place by crystallization or precipitation. The principal factor is the relationship between solubility and supersaturation. In crystallization, the solubility of the crystallising substance is so high that the formation of solids occurs largely in the metastable zone in the immediate vicinity of the solubility limits. Crystal growth and nucleation are functions of supersaturation. If a high supersaturation is required at low substance-specific growth rates for an adequate crystal growth, high nucleation rates and hence small crystals will result. On this basis, the authors present information for the specific design of crystallization processes. In contrast, the solubility of the precipitated product must be very low for precipitation. Direct crystal formation is possible only for substance systems of high solubility. As a rule, however, the precipitated substance is so insoluble that solids are formed via amorphous intermediates. The results of a large number of experiments show the influence of various parameters of the precipitation process on the filtrability of the precipitated product. 相似文献
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The aim of this article is to introduce a new technology for the production of Dead Sea potassium chloride. The new technology depends on using the power of ultrasound waves during a crystallization process to enhance potassium chloride precipitation and to improve the end-use properties of the produced crystals. This environmentally clean technology, which is called sonocrystallization, has received very intensive research in the past few years. It was used in this study to modify the crystallization process of potassium chloride from the decomposition of Dead Sea carnallite. Two crystallization runs were done; the first was performed without the application of ultrasound waves and the second was performed with this application. The effect of sonication on the crystallization process time and on crystal size distribution as well as on the purity of the crystals was studied. It was found that the required time for the un-sonicated process was about 150 min. This time was reduced to about 50 min when sonication was applied. The produced crystals were sieved, and the crystal size distribution (CSD) was determined for the two runs. For the sonicated process, finer but more uniform crystals were obtained with a mean average size of 0.2643 mm in comparison with 0.5727 mm for the un-sonicated process. The produced crystals were found to be of 96.07% KCl for the un-sonicated process and this purity was improved to 97.31% KCl by the application of ultrasound waves. Based on the results of this study, it seems to be feasible and economical to scale up the proposed technology for industrial applications. 相似文献
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