Breakage of drop nucleated granules in a breakage only high shear mixer

Wet granule breakage is a significant mechanism, particularly in high shear mixer granulation. This paper presents a study of the wet breakage mechanism using a Breakage Only Granulator. Granules with varying powder and liquid binder properties were created using single drop nucleation. These granules were inserted in a Breakage Only Granulator, a high shear mixer granulator with non-granulating cohesive sand as the bulk medium. Two different impellers were used at impeller speeds of 500 and 750 rpm. An 11° beveled edge impeller was used to create both impact and shear in the granulator, and a flat plate impeller was used to minimize impact and maximize shear in the granulator. The fraction of granules which broke during the granulation process was used as a measure of granule breakage within the granulator. These results were compared with Stokes deformation numbers calculated using mean dynamic peak flow stresses measured in unconfined uni-axial compression tests. Results for the beveled edge impeller blade show increasing breakage with increasing Stokes deformation number. Significant breakage was observed at high Stokes deformation number. Increasing impeller speed increased the magnitude of breakage. The Stokes deformations number appears to be a reasonable predictor for granule breakage within the granulator. Results for the flat plate impeller show very little breakage at 500 rpm, and significant breakage for only one formulation at 750 rpm. This suggests that either impact is dominant over shear for breakage within the granulator, or that the two impeller designs give substantially different collision velocities in the granulator. The impeller speed, type and shape have a profound effect on granule breakage in high shear mixer granulators.     

粉体混合过程及搅拌功率的DEM数值模拟和实验

采用数值模拟与功率测试相结合的方法,研究直叶桨式粉体混合机搅拌过程及搅拌功率、扭矩的变化规律。对粉体混合机内球形颗粒的混合过程进行离散单元法DEM数值模拟,研究直叶桨式粉体混合机内搅拌转速、搅拌桨直径、桨叶数目等特性参数对粉体混合时搅拌功率和扭矩的影响,并拟合得到功率计算公式。搭建粉体搅拌试验台,测试粉体搅拌功率并与模拟结果比较。结果表明,直叶桨式粉体混合机内功率消耗与搅拌桨转速、搅拌桨直径、桨叶数目等特性参数有密切关系。同时,扭矩值和功率值与搅拌桨转速、搅拌桨直径和桨叶数目都呈正相关。实验得到了与模拟类似的扭矩-转速关系以及功率-转速关系,模拟值与测试值具有较好的吻合性,验证了所推导公式的准确性。     

Influence of liquid binder dispersion on agglomeration in an intensive mixer

In industrial scale mixer granulation, liquid binder is usually sprayed onto the agitated powder bed by means of a nozzle in order to enhance the agglomeration process. The early stage of this process, where granule nuclei are formed and grow, is not well understood. As it is desirable to model the agglomeration state right from the beginning of the process for the purposes of control and modeling, this nucleation step is therefore an important field of interest.To investigate the influence of binder droplet size on the nucleation stage of the agglomeration process, experiments were carried out with lactose and water in an intensive mixer. Water was sprayed in to the mixer with different nozzles to vary the size of the produced droplets. As a comparison, water was also directly poured into the turning mixer. Samples of the produced granules were taken at specific time intervals and analysed for size and water content. As the experiments were focused on examining short granulation times, the first samples were taken after only half of the water was added.Particle size distribution and liquid distribution in the wet granule samples were analyzed. It was found, that the droplet size of the binder liquid has great influence on agglomerate size and binder distribution at short mixing times, with increasing time, the mechanical stresses acting in the mixer becomes more and more dominating in the process. Preliminary comparisons are also carried out with single drop penetration tests in an attempt to correlate drop size to penetration time and also to produced granule size.In conclusion this paper studies the effect of different drop size conditions and subsequent spray flux on the behaviour of the nucleation and the early stages of the agglomeration process. The context of these findings for agglomeration in an intensive mixer is examined.     

剪切变稀体系同心双轴搅拌釜内的气液分散模拟

气液搅拌设备因其良好的适用性被广泛应用于过程工业中。为更好地比较不同工况下剪切变稀体系中的气液分散情况,通过实验研究整体气含率和相对功耗确定适宜的转动模式,进而模拟研究表观气速、体系黏度、搅拌转速对气含率和气泡尺寸的影响。结果表明,相同功率下内外双桨反向旋转模式在理想气液分散条件下,相较于单轴内桨和内外双桨同向旋转模式具有更高的气含率和更好的气体泵送能力;表观气速的增加有利于气泡的均匀分散,但气泡尺寸也会随之增大;有效黏度的增加使得搅拌桨的影响区域变小,不利于气泡的均匀分散,气泡尺寸也随之增大;搅拌转速的增加使得循环涡流的影响区域变大,高气含率区不断扩大。     

Exploring the regime map for high-shear mixer granulation

The aim of this study was to investigate the applicability of the regime map approach proposed by Litster/Iveson and co-workers [S.M. Iveson, J.D. Litster, Growth regime map for liquid-bound granules, AIChE Journal 44 (1998) 1510–1518; S.M. Iveson, P.A.L. Wauters, S. Forrest, J.D. Litster, G.M.H. Meesters, B. Scarlett, Growth regime map for liquid-bound granules: further development and experimental validation, Powder Technology 117 (2001) 83–97] over the whole parameter range, for a given material and agglomeration method. Agglomeration behaviour in a high-shear mixer granulator was investigated and categorised using the evolution of granule size distribution (GSD). MCC 102 (Microcrystalline cellulose, Avicel 102) and aqueous PEG 6k (Polyethylene Glycol 6000) were employed as solid and liquid materials. Different operating conditions were applied by changing impeller speeds and L/S (liquid-to-solid) ratios (weight of liquid/weight of solid). 12 representative settings were selected and typical agglomeration behaviours were identified, forming a regime map for the system. The effect of impeller speed was found to depend on the L/S ratio, very little effect being seen at low L/S ratio (L/S = 85/150), but much more effect at higher binder ratios. In general, the effect of L/S ratio is of paramount importance in these systems and usually determines the growth behaviour.     

Effects of process parameters on granules properties produced in a high shear granulator

Results of a study on the influence of process parameters such as impeller speed, granulation time and binder viscosity on granule strength and properties are reported. A high shear granulator (Cyclomix manufactured by Hosokawa Micron B.V., The Netherlands) has been used to produce granules. Calcium carbonate (Durcal) was used as feed powder and aqueous polyethylene glycol (PEG) as the binder. The dried granules have been analysed for their strength, density and size distribution. The results show that increasing the granulation time has a great affect on granules strength, until an optimum time has been reached. The underlying cause is an increase in granule density. Granules are consolidated more at higher impeller speeds. Moreover, the granule size distribution seems not to be affected significantly by an increase in impeller speed. Granules produced with high binder viscosity have a considerably lower strength, wide strength distribution due to poor dispersion of binder on the powder bed. Binder addition methods have showed no considerable effect on granule strength or on granule size distribution.     

Experimental investigation on micromixing characteristics of coaxial mixers in viscous system

An experimental investigation into the micromixing performance of coaxial mixers in a viscous system is reported, in which the iodide-iodate reaction system is chosen to quantitatively characterize the product distributions. The effects of feeding time, feeding position, impeller speed, inner impeller configuration, and operation mode on the segregation index, Xs, are examined. It is revealed that the feeding near the inner impeller benefits micromixing and should be regarded as the preferred position. The presence of the rotating outer impeller causes the micromixing performance of the coaxial mixer to be significantly better than the single-shaft mixer. While an increase in the outer impeller speed has a limited influence on micromixing, the inner impeller speed is the dominant influencing factor, that is, the Xs decreases obviously when the inner impeller speed is increased. On the other hand, the coaxial mixers with multiple and axial inner impellers have a better micromixing performance at the same specific power consumption, P_V, than that with single and radial inner impellers. Among the configurations consisting of a Rushton impeller (RT), six-straight-blade turbine impeller (SBT), and six-pitched (45°)-blade turbine impeller (PBT), the Xs of the coaxial mixer is always the smallest at the same P_V when the PBT + RT configuration is used as the inner impeller. In addition, it is found that the difference in Xs that results from various operation modes is small in terms of power consumption; however, the co-rotation mode is still recommended for the micromixing of the coaxial mixer due to its excellent performance in general.     

Mass transfer into simulated fermentation media

The rates of oxygen mass transfer into a simulated fermentation medium, made up of 16 kg of paper pulp per m³ of aqueous sodium sulphite solution with a cupric ion catalyst, were determined in vessels of 0·187, 0·291 and 0·451 m dia., using flat-bladed turbine impellers, and the effect of varying impeller dimensions and operating speed were investigated. Above a critical impeller tip speed the volumetric mass transfer coefficients obtained at the same speed with different power inputs (produced by variations in the impeller blade dimensions) could be represented by the sum of two terms, one depending on the impeller speed, the diameters of the impeller and vessel, and the height of pulp suspension in the vessel, and the other function of the power input per unit volume and the air velocity through the vessel. At each impeller speed the increase in the volumetric mass transfer coefficient with power input was found to be greater below a certain power input per unit volume, and a correlation for this power per unit volume was based on it corresponding to a change in the rate of air recirculation through the impeller. The expression for the mass transfer coefficient provides a more accurate basis for scale-up than the use of simple rules, such as constant power per unit volume.     

10种石灰石浆液箱搅拌机的选型与计算

通过对搅拌机各组成部分的选型分析与介绍,针对脱硫脱硝中10种常见规格的石灰石浆液箱,进行搅拌机工艺选型上的优化设计,分析在脱硫脱硝石灰石浆液箱中如何进行搅拌机的优化选型,从而达到最优的使用效果和工艺要求。目前,搅拌机的选型和内构件的设计很大程度上依赖试验和实际工程经验。产品设计的优劣可使搅拌设备的效益相差十分悬殊,因此本文在明确石灰石浆液物料性质的基础上,针对搅拌设备的各个要素,例如叶轮的形状、叶轮直径、布置层数、转速、搅拌轴大小、挡板的尺寸和个数等进行一一优化。充分利用已有业绩对比分析,对10种常见的石灰石浆液箱规格型号在设计选型上完成优化,使机械搅拌机的设计理论更加完善,也能满足日常脱硫脱硝行业中从业者对石灰石浆液箱搅拌机的选型需求。     

MICROMIXING EFFECTS ON BARIUM SULFATE PRECIPITATION IN A DOUBLE-JET SEMI BATCH REACTOR

The effects of turbulent mixing on barium sulfate precipitation in an imperfectly mixed double jet semi batch reactor were investigated experimentally and theoretically. When two feed solutions in separate streams were fed into the semi batch reactor, the precipitation was significantly altered by the impeller speed and the feeding time. Generally, in the range of low impeller speed (below 400 rpm), the suspension was segregated vertically in the reactor and the average particle size increased with increasing impeller speed. However, in the range of high impeller speed (above 400 rpm) the suspension was homogeneously dispersed in the reactor, but the trend of the turbulent mixing effect on the precipitation was opposite to that in range of the low impeller speed. The precipitation in the semi batch reactor was controlled by particle mass transfer and micromixing of the feed streams, both of which were promoted by increasing the impeller speed. At low impeller speed the influence of the mass transfer was dominant so that the particle size increased with increasing impeller speed, but at high impeller speed it was surpassed by the influence of micromixing so that the trend was reversed because enhanced micromixing generates a large number of small particles in the reactor.

To model our hypothesis for the effects of imperfect mixing on the reaction precipitation in the semi batch reactor, a micromixing-limited plug flow-ideal semi batch series reactor model was developed. The model predicts that enhanced micromixing created high supersaturation levels in the premixing region (plug flow reactor) which reduces the average particle size. The model also predicts the effect of feeding time on the precipitation in the semi batch reactor. These predictions are in excellent agreement with the experimental data. An interesting prediction of our model is that micromixing in the premixing region plays an important role in the overall reaction precipitation and its effect is greatly intensified as the turbulent mixing intensity is increased, which is opposite to our common sense.     

Granulation in high-speed mixers Part VI. Effects of process conditions on power consumption and granule growth

Effects of impeller rotation speed, liquid flow rate and liquid amount upon power consumption and granule growth are investigated by granulation in a Fielder^® PMAT 25 VG high-speed mixer. The records of power consumption demonstrate effects of the process conditions which are coincident with the effects on the granule growth. This is attributed to the effect of the liquid saturation on the mechanical properties of the moist agglomerates. Granulation end-point control by power consumption meters requires the correlation between granule growth and power consumption being established for the particular process conditions. It is suggested that the differentiated power consumption signal be recorded in order to detect the characteristic phases of the granulation process. With regard to the control of the amount of binder solution required for an uncritical process, the differentiated signal can be useful.     

放大准则对混合澄清槽混合室中混合时间和流动特性的影响

工业混合澄清槽混合室的放大设计多基于操作经验,缺乏理论基础。基于几何相似放大,采用计算流体力学(CFD)方法,针对间歇操作的单相体系,对4 种不同放大准则下混合室内混合时间和流场特性的变化规律进行研究。结果显示,混合时间的计算值与测量位置有关,但随转速的增加受测量位置的影响减小;充分湍流条件下,本研究体系的功率准数趋于常数N_P=1.3,且几何相似放大可以保证混合室中轴向流动的流型特征;等桨叶端面速度和等Reynolds 数准则下,所需混合时间长,且抽吸压头小;等循环时间准则下,可以得到与基准混合室相同的混合时间和较高的抽吸压头,但单位体积功耗急剧增加到基准槽的24 倍;等单位体积功耗准则下,在满足具有较低的混合时间和较高的抽吸压头的同时还保证了较低的单位体积功耗,优于其他3 种放大准则。     

Effect of scale of operation on granule strength in high shear granulators

Results of a study on the influence of operation scale and impeller speed of high shear mixer granulators on the strength of granlues are reported in this paper. Calcium carbonate particles have been granulated in four scales of a geometrically similar high shear granulator (Cyclomix) with 1, 5, 50 and 250 L capacities. For the smallest scale, the effect of a small deviation from geometric similarity was also investigated. An aqueous solution of polyethylene glycol was used as the binder. Three scaling rules of constant tip speed, constant shear stress and constant Froude number have been used to determine the impeller speed for the different scales of the granulators. The granules produced in these experiments have been dried and tested for strength using side crushing test method. The data have then been analysed and compared. Operation of granulators according to the constant tip speed rule produces granules with a similar strength for all four scales, followed by a similar trend for the constant shear stress rule, albeit to the less extent. The constant Froude number rule produces a heterogeneous strength distribution and is not a suitable criterion for scaling-up of high shear granulators. The distribution of granule strength has been fitted to the normal, log-normal and Weibull distributions. Weibull distribution fits the data well for the constant tip speed operations.     

Influence of the interaction between binder and powders on melt agglomeration behavior in a high-shear mixer

The purpose of this study was to investigate the effects of the different surface properties of powders on granular agglomeration in a high-shear mixer. Polyethylene glycol 6000 (PEG 6000) was used as the melting binder. Three different powders, with mean granule sizes of 75-150 μm were used as the raw materials: calcium carbonate, calcium sulfate, and sodium carbonate. The wetting properties of the raw materials were measured with a contact angle instrument. The results indicate that the speed at which the droplets sink into the powder bed and the contact angle of binder droplets on the powder surface play important roles in determining the progress of the agglomeration process. Several types of agglomeration were found: a slurry state, heterogeneous nucleation, snowballing, and induction growth behavior. Heterogeneous dispersion leads to induction behavior and subsequent growth, but a homogeneous dispersion leads to little or no nucleation and growth of agglomerate size.     

Rheology, granule growth and granule strength: Application to the wet granulation of lactose-MCC mixtures

This study aims at better understanding the wet granulation process of a binary mixture composed of microcrystalline cellulose (water insoluble) and lactose (water soluble). It investigates the effect of formulation (proportion of the different components in the mixture) on the granule growth kinetics, the evolution of granule morphology during granulation, the wet mass consistency and dry granule strength of the end product. Additionally the influence of mixer design has been studied by up scaling the process from the 1.9 L Mi-pro high shear mixer used as the reference scale to a 6 L Diosna P1-6 high shear mixer. The scale-up rules investigated were constant impeller tip speed and constant Froude number. Our results allowed us to draw the following conclusions:

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The increase in MCC content is found to increase the optimum binder requirement for granulation, wet mass consistency and dry granule strength.

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Granule growth takes place in three distinct stages: wetting, nucleation and growth. These stages can be identified with the help of the recorded torque values during the granulation process or by the evolution of granule size and granule morphology.

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The characterization of the starting materials by moisture sorption isotherms brings more insight to the role of each component during the granulation process.

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The increase of the granulation scale has little influence on the observed growth mechanism. However bi-modality of the granule size distribution is increased, wet mass consistency and dry granule strength are decreased with increasing scale of operation.

     

The effect of powder size on induction behaviour and binder distribution during high shear melt agglomeration of calcium carbonate

Growth mechanisms in high shear mixer granulation were observed over a wide range of particle size and liquid-to-solid (L/S) ratio. The materials used were calcium carbonate (CaCO₃; size fractions in the range 1.5 to 85 μm) with a binder of polyethylene glycol 6000 (PEG 6k). The binder, solid at room temperature, was added by the “melt-in” method. A 10 L vertical-axis granulator was used, with a chopper and a four-bladed impeller.

The mean granule size and granule size distribution were measured at regular intervals during the agglomeration process by careful sampling and sieving. The uniformity of binder distribution among the granules was also measured.

The growth behaviours of each grade of primary particles were classified and compared. An induction type mechanism was observed with an initial period of slow growth in mean particle size that lasted 2 to 3 min (the induction period). This was followed by a short rapid growth phase lasting 1 to 2 min. The final stage was a plateau of more or less zero growth. Interestingly, the end of the induction period and the onset of rapid growth corresponded to a change in the granule size distribution from bimodal to monomodal and a similar change in the distribution of binder. Induction period growth rate tended to be lower for granules of finer particles, but these grew more rapidly during the rapid growth stage and produced larger granules than the coarser primary particles.

The liquid-to-solid (L/S) ratio had a significant effect on the growth rate during the rapid growth stage but a minor effect on the granule size distribution and binder distribution. Primary particle size had a significant effect on the final average size of granules, the growth rate during the rapid growth stage and the distribution of granule size and binder.     

新型同心双轴搅拌器功率与混合特性的数值模拟

基于同心双轴搅拌器的结构与运行特点,建立了兼顾其流动、混合过程的三维数学模型,并以过程工业应用较多的两种不同尺寸双层组合桨作为内桨、框式桨作为外桨构成的同心双轴搅拌器为研究对象,数值模拟了其在中高黏牛顿流体中同向及反向转动模式的功率特性、流场特性及混合特性。模拟结果表明,同向转动模式下,整个系统的搅拌功耗更小、混合效率更高;外桨功耗受内桨影响较大,一般随内桨转速的增大,恒速外桨的功耗同向转动时会减小、反向转动时会增大;对由桨式搅拌器构成的组合式内桨而言,当内桨直径与釜体直径之比为0.35左右时,相同Reynolds数下的单位体积混合能更小;中高黏牛顿流体中,同心双轴搅拌器的内桨采用上层六斜叶桨+下层六直叶桨的组合形式时更高效节能,仅在体系Reynolds数小于36时,上层二斜叶桨+下层二直叶桨的内桨组合形式才具有相对优势。     

Incorporation of nanoparticle clusters into a liquid using a proprietary design mixer,Ytron Y Jet

This paper reports the comparative performance of a proprietary design mixer, Ytron Y Jet, on the incorporation of clusters of nanoscale silica powder into water. Two sets of characteristic power curves were obtained for Ytron Y Jet depending on whether the valve on feed tube was open or closed. Whilst there was little difference at low speeds, as the speed was increased entrainment from the feed tube decreased Po which would be as a consequence of a decrease of the pressure difference between the two sides of the rotating blades. Drawdown time values determined for surface additions followed the same trends reported for traditional impellers. Powder incorporation became faster with increasing power input at a given concentration and for incremental additions of 1% (w:w), incorporation rate decreased steeply with increasing concentration. With the use of the feed tube, which is part of the design, particles could be introduced into the impeller region, and incorporation rate could be maintained constant over a wide concentration range. This suggests that whilst the flow field in the vicinity of the impeller is not significantly modified with changes in viscosity and rheology, away from the impeller, close to liquid surface liquid velocities die out quickly. When a highly non-Newtonian rheology (Bingham plastic) developed with further particle addition, incorporation rate decreased. Ability to feed into the impeller region is the main advantage this design offers for this application.     

新型行星式搅拌器开发及性能研究

介绍了新型行星式搅拌器的结构和设计原理。该新型搅拌器有一个传动轴和数个行星叶轮组成,行星轮自转的驱动力来自液体阻力,行星叶轮自转速度的大小与公转速度、公转半径和自转半径有关,而与行星叶轮高度无关;自转方向与公转方向相反。测试采用IKA EUROSTAR power control搅拌装置和Labword软件,试验介质为水和甘油。通过对搅拌器的搅拌性能试验研究发现,流体质点的轴向流线为高速螺旋线,主要流型为径向流和轴向流,因此,在主轴转速较低的情况下被搅拌液体亦可获得满意的混合效果。通过对试验数据分析处理,得到测试用行星式搅拌器的功率准数、混合时间数、排液量和循环量等搅拌性能曲线及经验公式。