Preparation of CaO granules using the granulation method

ABSTRACT

Improving the hydration resistance of CaO particle in manufacturing and application of free CaO-containing materials has practical significance. In this study, CaO granules was made from Ca(OH)₂ particles, which were fabricated by the granulation method. The results showed that the hydration resistance of the CaO granules which was prepared under 1700?r?min^?1 was the best, the CaO granules was sintered well in calcination process, the shell of CaO granules was relatively dense, which improves the hydration resistance of CaO granules, and the rate of hydration weight increment was 0.58% after placed in the air for 20 days under a temperature of 10–14°C and a relative humidity of 57–81%.     

Steady states in granulation of pharmaceutical powders with application to scale-up

Theoretical and experimental evidence is given to show that steady states can be reached during agglomerate growth and break-up in high-shear granulation of fine powders. An earlier theoretical model [G.I. Tardos, I.M. Khan and P.R. Mort, Critical parameters and limiting conditions in binder granulation of fine powders, Powder Technology, 94, 245-258 (1997).], based on simple energy-dissipation considerations hinted at the existence of these states at the point where growth is counterbalanced by breakage. Further theoretical evidence is obtained from molecular dynamic simulations of wet and dry particles situated in a constant shear field [I. Talu, G.I. Tardos and M.I. Khan, Computer simulation of wet granulation, Powder Technology, 110, 59-75 (2000).], where the size distribution of initially identical particles, shifts in time to reach a dynamic steady state. Under the conditions of this steady state, the number of breaking agglomerates approximately equals the number of forming ones to yield a time independent final-size distribution.Experimental evidence to support the theoretical findings is obtained during the present research by measuring particle size distributions at line at crucial points during granulation of a typical pharmaceutical powder in a high-shear mixer. In order to reach a steady state, binder addition has to be slow enough and wet massing has to be long enough so that neither has an influence on the final properties of the granules. We show experimentally that if binder is spread properly and homogeneously in the powder and continuous shearing of the wet mass ensures homogeneous, equal growth of the granules, the steady state will only be a function of the total amount of fluid added provided that the shear forces in the machine are maintained constant.These findings are important in that they show that under carefully controlled conditions of binder addition and shear in the mixer, the granulation process is robust and controllable and can, in principle, be scaled up with ease once the powder ingredients and the total amount of binder are fixed.     

Manufacturing pharmaceutical granules: Is the granulation end-point a myth?

The moist agglomeration process by high-shear mixing/granulation, i.e. the wet massing, screening and subsequent drying is a wide spread but critical unit operation. Since for decades formulators are looking for the correct “end-point” of this important process, i.e. when do you need to stop massing or stop with the addition of granulating liquid? What is the correct amount of granulating liquid? A similar situation exists in case of the moist agglomeration in fluidized bed equipment. In the latter case the simultaneous drying of the still moist granules have to be taken into account. Recently a science-based virtual equipment simulator could be developed mimicking the granule size evolution in a fluidized bed granulator during the addition of granulating liquid. For the simultaneous drying the Mollier chart is used. With this virtual equipment simulator it is possible to simulate “crash situations”, i.e. by overwetting or by an incorrect use of the parameter setting. However the determination of the “end-point” depends only on the operator, who desires a certain granule size distribution and a well-defined final moisture content of the batch. Thus the existence of a process intrinsic “end-point” has to be questioned. The same situation can be reported in case of high-shear mixing/granulation based on many years of research. In fact nobody could clearly show the existence of an intrinsic “end-point”. However during the continuous addition of a granulating low viscous liquid a sudden increase in power consumption can be measured, which levels off. Such a measurement depends on the formulation and leads to an “early signal” not to the “end-point”. This signal can be used for a tight control of the granulation process and leads to a low batch to batch variability in the final granule size distribution. The latter is the goal of the PAT (Process Analytical Technology) Initiative emphasizing “Quality by Design”.     

Influence of the properties of refractory powders on their granulation and the properties of the granules

Conclusions A study was made of the properties of aluminosilicate powders of various compositions and their influence on the densification during granulation.We established relationships between the porosity and density of the granules with various concentrations of Al₂O₃ with bulk densities and angles of natural slope. It is shown that to obtain dense and strong green articles and fired aluminosilicate granules with the minimum shrinkage, it is necessary to use bodies with a high bulk density and low internal friction, which is attained for alumina by using batches with the maximum concentration of -Al₂O₃ and grains with a pore-free structure, and for aluminosilicate refractories — an increased content of Al₂O₃ within the limits of each type of article.Translated from Ogneupory, No. 8, pp. 6–10, August, 1985.     

Scale-up in the 4th dimension in the field of granulation and drying or how to avoid classical scale-up

In the pharmaceutical industry, the production of granules is based on a batch concept. This concept offers many advantages, as a batch can be accepted or rejected. However, the scale-up of the batch size may lead to problems. The variety of the equipment involved does not facilitate the scale-up process and the capital invested in space and equipment is high. An alternative approach is the use of a continuous process. However, continuous processes have the disadvantage among others that the batch size is not well defined. Thus, a special quasi-continuous production concept was developed, taking into account the advantages of a batch type and a continuous process. This concept was developed in cooperation with the Institute of Pharmaceutical Technology of the University of Basel, Glatt CH-4133 Pratteln and F. Hoffmann-La Roche, CH-4070 Basel. The equipment allows to implement a “Just in Time Production Concept” as a large batch B consists of n subunit (SU) batches b, i.e. B=nb. The subunit batch b corresponds to, e.g. 7-kg material for the production of pharmaceutical granules for further processing such as tabletting. At the Roche production site, this novel process equipment was used to manufacture batch sizes B with n=10, n=100 and so far up to n=600 subunits. This leads to an optimal use of capital invested in GMP space and equipment. The difference to the classical scale-up is the following: with classical scale-up, the dimensions of the equipment x, y, z is enlarged and the process time is more or less kept constant. With this novel concept, the dimension x, y, z of the equipment is kept constant and the process is repeated in the 4th dimension “n times”. Thus, for the scale-up in the 4th dimension, i.e. in the time, the equipment needs to show a “self-cleaning” property and appropriate formulations. The novel concept is of special interest, as the quality of the product is not changed during scale-up.     

Increases in the strength of Si-additive mixture granules by presintering

In order to preserve a spherical granule shape in a porous sintered body, presintering technology was developed to enhance the strength of Si-mixture granules containing Y₂O₃-Al₂O₃-CaO as sintering additives prior to shaping. The fracture strength of the granules measured by a compression test was ≤0.2 MPa and ≤20 MPa for as-spray dried granule and presintered granules, respectively. Furthermore, the flowability of the presintered granules was retained by the presintering process done to 1300 °C.     

Effect of process parameters on the melt granulation of pharmaceutical powders

Co-melt granulation of lactose and PEG was investigated in a fluidised bed granulator. The effect of process parameters such as binder content and binder viscosity were correlated to granulation time and particle size distribution. The experimental data indicated that after initial nucleation the granulation mechanism was dependent upon binder content and binder viscosity. When the binder content was increased above 18% (w/w) de-fluidisation of the bed occurred and granulation moved to the slurry regime. As the process involved the melt granulation of relatively high molecular weight (6-20 k) and thus high viscosity PEG (500-19000 mPa s), it was found that binder viscosity had a significant affect on the granule growth mechanism. Granulation with a binder viscosity of 500 mPa s resulted in granule growth by coalescence, however, an increase in binder viscosity resulted in less coalescence and a lower granule growth rate. Furthermore, the granulation data were characterised by Stokes number analysis.     

导热油进口速度对造粒模板造粒带温度均匀性影响

造粒模板是切粒系统的主要部位之一,造粒模板内部包括加热通道与物料通道,通道内部流动介质分别为导热油和聚乙烯.探究在同等条件下,导热油进口速度分别为0.01、0.05、0.1 m/s的情况下物料挤出速度与造粒带温度分布的均匀性.应用SolidWorks软件对造粒模板进行三维建模,采用ANSYS软件对聚合物与导热油的流动与...     

AZF工艺返料质量对造粒的影响

返料是参与喷浆造粒工艺生产NPK复合肥造粒环节不可缺少的一部分。分析和讨论返料粒度分布、返料湿度和温度对造粒液固质量比、成粒率及造粒稳定性的影响。     

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.

     

Further observations on the scale-up of aerated mixing vessels

The unsteady-state rate of dissolution of oxygen in water was used to measure k_La in a large aerated mixing vessel. Results are compared with those previously observed in smaller, geometrically similar vessels, from which it is found that the problem of scale-up with equal mass-transfer rates is complex and difficult to resolve on the laboratory scale. However, it is apparent that scale-up with geometric similarity results in a marked sacrifice in performance.     

生物反应器放大因素与方法研究

搅拌式生物反应器是最重要的一类生物反应器,广泛应用于生物化工、食品、医药等领域。由于同时涉及到生物化学反应和物理过程,因此由实验室规模到工业装置设计的放大问题成为生物工程技术的关键问题之一。对搅拌式生物反应器放大过程的影响因素进行了分析,并着重讨论了反应器内的传质、传热、混合、剪切以及表观气速等因素对放大设计的影响规律。在该基础上,就生物反应器的放大方法进行了初步总结。     

Effect of additives on the strength of kaolin briquette

Conclusions Incorporating an additition of still-pot residue in kaolin briquette increases its strength for loading into the furnace in the moist state. An addition of water glass increases the density and strength of the briquette owing to ion exchange. Magnesium-containing additive intensifies mullite formation in kaolin briquette.Incorporating a combination of these additives yields denser and stronger briquette at lower firing temperatures which reduces the quantity of fine fractions in the material, and reduces dust emission during the firing of kaolin in rotary kilns.Translated from Ogneupory, No.6, pp. 48–51, June, 1970.     

On the scale-up of plasticating extruder screws

In the most commonly used scale-up method of plasticating extruder screws, the screw channel depth is increased by the square root of the diameter ratio while the screw RPM is decreased by the square root of the diameter ratio such that the output rate increases proportionally to the square of the diameter ratio. This scale-up method, largely based on the pumping function of the screw, often leads to a higher melt temperature, a higher screw horsepower consumption per unit output rate and an inferior melt quality from the larger diameter screw. Analysis of the common scale-up method reveals that, although the shear rate in the melt is kept constant, the average residence time and the peripheral screw speed are increased for the larger diameter screw. Our recent study on the melting mechanism also reveals that the melting capacity increases less than the pumping capacity. A detailed examination of the common scale-up method in this paper shows that the pumping capacity and the solid conveying capacity increase more than necessary while the melting capacity increases insufficiently.