Continuous Reaction Crystallization of Struvite in a DTM Type Crystallizer With Jet Pump of Ascending Suspension Flow in a Mixing Chamber–Kinetic Approach of the Process

Reaction crystallization of struvite in water solutions containing 0.20 mass % of phosphate(V) ions by magnesium and ammonium ions addition was investigated experimentally. Process was carried out in DTM type crystallizer with liquid jet pump device in 298 K assuming stoichiometric conditions. Struvite crystals of mean size Lm 5.2-23.0 μm were produced depending on pH (9-11) and mean residence time of suspension in a crystallizer τ (900-3600 s). Under these conditions linear growth rate of struvite crystals (SIG MSMPR kinetic model) decreased 2-time with the increase in pH and 3-time with the elongation of mean residence time of crystal suspension from 7.11×10-9 m/s (pH 9, τ900 s) to 1.65×10-9 m/s (pH 11, τ3600 s). Nucleation rate varied within the 7.9×108-1.8×1010 1/(sm3) limits. Struvite product of maximal linear size exceeded 100 μm with 10 vol. % of < 3 μm fraction corresponded to pH 9 and τ3600 s.

Reaction Crystallization of Struvite in a Continuous FB MSZ Type Crystallizer with Jet Pump Driven by Compressed Air

The results of struvite reaction crystallization from diluted water solutions of phosphates （V） （0.20 mass% of PO43-） by means of magnesium and ammonium ions are presented. Continuous FB MSZ crystallizer with jet pump driven by compressed air was used. Influence of pH and mean residence time of suspension on the crystal product quality was determined. Increase in pH from 9 to 11 resulted that mean crystal size decreased nearly two-time： from 27.1 to 15.1μm for mean residence time of suspension 900 s. Elongation of this time from 900 to 3,600 s influenced struvite crystal size advantageously-it increased from 27.1 to 41.2 μm at pH 9. From the population density distributions nucleation and growth rates of struvite were calculated based on the simplest SIG model of mass crystallization kinetics in MSMPR crystallizer. Linear growth rate ofstruvite crystals decreased nearly two-time with the increase in environment pH from 9 to 11, and more than 2.5-time with the elongation of mean residence time of crystal suspension in a crystallizer from 900 to 3,600 s from 1.34× 10-8 m/s （pH 9, τ= 900 s） to 2.60×10-9 m/s （pH 11, τ= 3,600 s）.

Controlling Nonlinear Dynamics in Continuous Crystallizers

Crystallization is used to produce vast quantities of materials. For several applications, continuous crystallization is often the best operation mode because it is able to reproduce better crystal size distributions than other operation modes. Nonlinear oscillation in continuous industrial crystallization processes is a well-known phenomenon leading to practical difficulties such that control actions are necessary. Nonlinear oscillation is a consequence of the highly nonlinear kinetics, different feedbacks between the variables and elementary processes taking place in crystallizers units, and the non-equilibrium thermodynamic operation. In this paper the control of a continuous crystallizer model that displays oscillatory behavior is addressed via two practical robust control approaches： （i） modeling error compensation, and （ii） integral high order sliding mode control. The controller designs are based on the reduced-order model representation of the population balance equations resulting after the application of the method of moments. Numerical simulations show good closed-loop performance and robustness properties

Progress of Pharmaceutical Continuous Crystallization

Crystallization is an important unit operation in the pharmaceutical industry. At present, most pharmaceutical crystallization processes are performed in batches. However, due to product variability from batch to batch and to the low productivity of batch crystallization, continuous crystallization is gaining increasing attention. In the past few years, progress has been made to allow the products of continuous crystallization to meet different requirements. This review summarizes the progress in pharmaceutical continuous crystallization from a product engineering perspective. The advantages and disadvantages of different types of continuous crystallization are compared, with the main difference between the two main types of crystallizers being their difference in residence time distribution. Approaches that use continuous crystallization to meet different quality requirements are summarized. Continuous crystallization has advantages in terms of size and morphology control. However, it also has the problem of a process yield that may be lower than that of a batch process, especially in the production of chirality crystals. Finally, different control strategies are compared.

CONTINUOUS CASTING TECHNOLOGY OF SINGLE CRYSTAL COPPER ROD

ＣＯＮＴＩＮＵＯＵＳＣＡＳＴＩＮＧＴＥＣＨＮＯＬＯＧＹＯＦＳＩＮＧＬＥＣＲＹＳＴＡＬＣＯＰＰＥＲＲＯＤ①ＸｕＺｈｅｎｇｍｉｎｇ，ＬｉＪｉａｎｇｕｏａｎｄＦｕＨｅｎｇｚｈｉＳｔａｔｅＫｅｙＬａｂｏｒａｔｏｒｙｏｆＳｏｌｉｄｉｆｉｃａｔｉｏｎＰｒｏｃｅｓ...

Relationships between the surface quality of a single crystal copper ingot and the process parameters of a heated mould continuous casting method

The relationships between the surface quality of a single crystal copper ingot and the process parameters of heated mould continuous casting method were studied experimentally using our own design of horizontal heated mould continuous casting apparatus, and the mechanism by which process parameters affect the surface quality of a single crystal copper ingot is analyzed in the present paper. The results show that the process parameters affect the surface quality of a pure copper ingot by affecting the position of the liquid-solid interface in the mould. The position of the liquid-solid interface in the mould must be controlled carefully within an appropriate range, which is determined through a series of experiments, in order to gain a single crystal copper ingot with good surface quality.

Crystallization Growth of Single Crystal Cu by Continuous Casting

Crystallization growth of single-crystal Cu by continuous casting has been investigated using self-designed horizontal continuous casting equipment and XRD. Experimental results showed that the crystallization plane of (311), (220) and (ill) were eliminated sequentially in evolutionary process. The final growth plane of crystal was (200), the direction of crystallization was [100], the growth direction of both sides of the rod inclined to axis, and the degree of deviation of direction [100] from the crystal axis was less than 10°. In order to produce high quality single crystal, the solid-liquid interface morphology must be smooth, even be planar.

Effect of Copper (II) Ions on Quality of Struvite Produced in Continuous Reaction Crystallization Process at the Magnesium Ions Excess

The research results concerning continuous removal of phosphate (V) ions from solutions containing 1.0 or 0.20 mass % of phosphate (V) ions and 0.2 or 0.5 mg/kg of copper (II) ions using magnesium and ammonium ions addition are presented. Continuous reaction crystallization of struvite MgNH4PO4 × 6H2O ran both under stoichiometric conditions and at 20% excess of magnesium ions (pH 9, t 900 s). It was concluded, that presence of copper (II) ions in a process system influenced product quality moderately advantageously. Mean size of struvite crystals enlarged by ca. 6% only. Lower concentration of phosphate (V) ions and excess of magnesium ions caused, that products of ca. 9% - 13% larger crystal mean size (up to ca.40mm) were removed from the crystallizer. Presence of struvite crystals and copper (II) hydroxide were detected analytically in the products (Cu in a product varied from 6 to 90 mg/kg). Presence of copper (II) ions favored crystallization of struvite in the form of tubular crystals.

The effect of in-situ dynamic mold flux melting and crystallization on heat transfer in continuous casting

A mold flux is widely used to modify heat transfer rates in continuous casting,and crystallization of the mold flux has been identified as a primary factor that influences heat flux from the strand to the mold.As the harsh environment and the very high transient nature of the mold caster,the study of dynamic mold flux melting and crystallization as well as their effects on heat transfer has not been conducted widely.By using an infrared radiation emitter,a high level heat flux was applied to a copper mold covered with solid mold flux disk to simulate the heat transfer phenomena in continuous casting.By this technique it is possible to have a liquid layer,a crystalline layer and a glassy layer in contact with one another and,by varying the energy input,it is possible to study the dynamic nature of the film and its effect on the heat transfer rate.A general heat transfer model was also developed to allow the prediction of the effect of varying the thickness of the three potential layers in the flux film.

Process Parameters of Manufacturing Single Crystal Copper by Heated Mold Continuous Casting

The effect of process parameters on the surface quality of single crystal copper ingot was studied through experiment with a self-designed horizontal heated mould continuous casting apparatus,and the mechanism was analyzed.The results show that the process parameters affect the surface quality of pure copper ingot by affecting the position of the liquid-solid interface in the mould.The position of the liquid-solid interface in the mould must be controlled carefully in an appropriate range determined through experiments in order to gain a single crystal copper ingot with a high surface quality.

Pyrene Nanocrystals Crystallized by a Continuous Flow Microreactor

Pyrene solution and distilled water were flowed through a microreactor at a predetermined flow rate to generate pyrene crystals. Pyrene nanocrystals were crystallized by a Continuous Flow Microreactor. The particle size and luminescence properties of pyrene nanocrystals produced were evaluated. The crystal mean size between 60 nm and 400 nm could be controlled by the operating conditions. The crystal mean size decreased with increasing flow rate and solution concentration. In addition, the crystal morphology also changed. In the case of slow flow conditions, a needle-like crystal morphology was obtained. The crystal morphology became spherical on increasing the flow rate. Pyrene crystals with size about 400 nm exhibited luminescence at about 470 nm. As the crystal size decreased, the intensity of the luminescence also declined. The luminescence wavelength was in the range of about 370 to 400 nm.

Investigation of the trajectory uniformity in water dissolution ultraprecision continuous polishing of large-sized KDP crystal

Large-sized potassium dihydrogen phosphate(KDP)crystals are an irreplaceable nonlinear optical component in an inertial confinement fusion project.Restricted by the size,previous studies have been aimed mainly at the removal principle and surface roughness of small-sized KDP crystals,with less research on flatness.Due to its low surface damage and high machining efficiency,water dissolution ultraprecision continuous polishing(WDUCP)has become a good technique for processing large-sized KDP crystals.In this technique,the trajectory uniformity of water droplets can directly affect the surface quality,such as flatness and roughness.Specifically,uneven trajectory distribution of water droplets on the surface of KDP crystals derived from the mode of motion obviously affects the surface quality.In this study,the material removal mechanism of WDUCP was introduced.A simulation of the trajectory of water droplets on KDP crystals under different eccentricity modes of motion was then performed.Meanwhile,the coefficient of variation(CV)was utilized to evaluate the trajectory uniformity.Furthermore,to verify the reliability of the simulation,some experimental tests were also conducted by employing a large continuous polisher.The results showed that the CV varied from 0.67 to 2.02 under the certain eccentricity mode of motion and varied from 0.48 to 0.65 under the uncertain eccentricity mode of motion.The CV of uncertain eccentricity is always smaller than that of certain eccentricity.Hence,the uniformity of trajectory was better under uncertain eccentricity.Under the mode of motion of uncertain eccentricity,the initial surface texture of the100 mm×100 mm×10 mm KDP crystal did achieve uniform planarization.The surface root mean square roughness was reduced to 2.182 nm,and the flatness was reduced to 22.013μm.Therefore,the feasibility and validity of WDUCP for large-sized KDP crystal were verified.

Continuous-wave mid-infrared intracavity singly resonant optical parametric oscillator based on periodically poled lithium niobate

This paper reports a continuous-wave （CW） mid-infrared intracavity singly resonant optical parametric oscillator based on periodically poled lithium niobate （PPLN） pumped by a diode-end-pumped CW Nd：YVO4 laser. Considering the thermal lens effects, it adopted an optical ballast lens and the near-concentric cavity for better operation. At the PPLN＇s grating period of 28.5 μm and the temperature of 140℃, the maximum idler output power of 155 mW at 3.86 μm has been achieved when the 808 nm pump power is 8.5 W, leading to an optical-to-optical conversion efficiency of 1.82%.

High efficiency continuous-wave tunable signal output of an intracavity singly resonant optical parametric oscillator based on periodically poled lithium niobate

In this paper we report on a continuous-wave （CW） intracavity singly resonant optical parametric oscillator （ICSRO） based on periodically poled LiNbO3 （PPLN） pumped by a diode-end-pumped CW Nd：YVO4 laser. Considering the thermal lens effects and diffraction loss, an optical ballast lens and a near-concentric cavity are adopted for better operation. Through varying the grating period and the temperature, the tunable signal output from 1406 nm to 1513 nm is obtained. At a PPLN grating period of 29 pm and a temperature of 413 K, a maximum signal output power of 820 mW at 1500 nm is achieved when the 808 nm pump power is 10.9 W, leading to an optical-to-optical conversion efficiency of 7.51%.

High-strength aluminum alloys hollow billet prepared by two-phase zone continuous casting

The two-phase zone continuous casting(TZCC)technique was used to continuously cast high-strength aluminum alloy hollow billets,and a verified 3D model of TZCC was used to simulate the flow and temperature fields at casting speeds of 2-6 mm·min^(-1).Hollow billets under the same conditions were prepared,and their macro/microstructures were analyzed by an optical microscope and a scanning electron microscope.During the TZCC process,a circular fluid flow appears in front of the mushy zone,and the induction heated stepped mold and convective heat transfer result in a curved solidification front with depressed region near the inner wall and a vertical temperature gradient.The deflection of the solidification front decreases and the average cooling rate in the mushy zone increases with increasing casting speed.Experimental results for a 2D12 alloy show that hot tearing periodically appears in the hollow billet accompanied by macrosegregation near the inner wall at casting speeds of 2 and 4 mm·min^(-1),while macroscopic defects of hot tearing and macrosegregation weaken and the average size of columnar crystals in the hollow billets decreases with further increasing casting speed.2D12 aluminum alloy hollow billets with no macroscopic defects,the finest columnar crystals,and excellent mechanical properties were prepared by TZCC at a casting speed of 6 mm·min^(-1),which is beneficial for the further plastic forming process.

基于CFD-PBE耦合的连续结晶过程数值模拟

通过CFD(计算流体力学)与PBE(粒数衡算方程)耦合对连续结晶过程进行数值模拟。采用QMOM(积分矩方法)求解PBE。在考虑成核、生长、聚并和破碎的情况下,通过网格独立性验证确定计算网格数量。在此基础上研究挡板设置、停留时间、搅拌转速以及搅拌桨类型等因素对CSD(晶体粒径分布)演变的影响,结果表明:挡板的设置增强了结晶器内湍流程度;高转速和低停留时间会获得平均粒径较小的颗粒。对比3种搅拌桨对CSD演变的影响,轴流式的螺旋桨功耗小,适用于大颗粒晶体结晶过程,而径流式的圆盘涡轮桨适用于微粒结晶过程。

小方坯连铸机直轧品种钢的工艺装备优化

某炼钢厂为适应品种钢浇铸工艺,对小方坯连铸机进行了工艺设备优化,设备优化后兼顾了普通钢种生产模式,且生产的品种钢方坯满足工艺技术要求。该连铸机配有铸坯在线保温设施,高温铸坯经剪切后温降减小,通过直轧辊道快速输送至轧钢工序,满足了轧线免加热、直接轧制的工艺要求。连铸机经优化后具有明显的经济效益,在行业里具有示范作用。

连续结晶器研究进展

结晶是化工领域重要的分离纯化单元之一。随着人们对精细化工产品纯度和质量稳定性要求越来越高,近年来结晶技术的研究受到广泛关注。连续结晶克服了间歇结晶过程中不同批次产品质量不一致、生产效率低和成本高等缺点,具有晶体粒度分布窄、产品质量稳定,并且可以连续生产特定晶型或手性晶体的优点,是近年来结晶技术研究的重点方向。结晶器是连续结晶研究的重点之一,本文概述了连续结晶器中混合悬浮混合出料(MSMPR)结晶器和管式结晶器的研究现状,总结了目前连续结晶器的种类和优势,以及存在的问题和解决的方法,展望了未来连续结晶器的发展方向。

基于有限元模拟的水平连铸TP2铜管坯一次冷却结构优化研究

对比多种结晶器结构下温度场、速度场等分布状态及石墨模具内部温度变化趋势,探究其对铜套、石墨模具等易损件及铜管铸坯温度变化的影响。结果表明,在一次冷却结构增设12道Φ10 mm且倾斜角度为30°的流槽,可使冷却水流态平稳均衡,铜套受热均匀,有利于铸坯周向同时凝固。本文通过有限元软件模拟铜管水平连铸过程一次冷却结构优化对温度的影响,为生产企业改善产线冷却效果,提高产品质量,降低模具成本和延长使用寿命,提供了实验参照和理论指导。

水平连铸结晶器内真实换热边界计算及传递模型

连铸结晶器内冷却水的流动、传热和金属液的传热、凝固全耦合计算时,模型计算效率低、收敛性差,而不考虑真实冷却水流场只进行金属液传热-凝固耦合时,模型计算精度较低,可将冷却水流动-传热和金属液传热-凝固过程分别建模,并基于二次开发的温度场量原位传递程序,将模型串联耦合。结果表明,通过耦合流场计算得到的真实冷却边界替代传统均匀界面换热系数的边界条件施加方式,在保证模型计算效率和计算精度的前提下,可准确模拟铸坯晶粒的尺寸、取向和数量,经试验验证,模拟结果与试验结果高度吻合。