CHE59700-012 PARTICLE DESIGN AND PROCESSING Final Exam Spring Semester 2011

2 hours for working. This is an open book exam. Do all questions. Total marks = 60

Name: PUID: Signature:

QUESTION 1 (a) During batch granulation, induction time behaviour is sometimes observed ie. there is little or no change in granule size for a long time followed by a sudden sharp increase in granule size (see diagram below).

Granule Size
Increasing Liquid Content

Granulation Time

Explain why this phenomenon occurs in terms of your understanding of granule consolidation and growth. If the feed powder size is decreased, how will induction time change? Why? [5 marks]

(b) A fluidised bed is used to make porous granules for an instantised food product ie. the product will quickly disperse and dissolve when added to water. Explain why a fluid bed granulator is a good approach for making low density, porous granules by agglomeration of fine powders. Is there a limit to how fine the feed powder can be? I would like to use my fluid bed granulator to make coated microspheres. In this process, I want to spray a polymer solution onto the outside of the spheres from a single spray nozzle in the fluidised bed. The solvent evaporates to leave a uniform polymer coating on each sphere. The following data is available (with symbols as defined in lecture notes): dp = 100m db = 0.03m = 1Pa.s p = 1500 kg.m-3 -1 Ub = 0.08 m.s St* = 4

Are single coated particles possible? Justify your answer quantitatively using an appropriate regime analysis. [7 marks] (c) A pharmaceutical product is produced in a 300 litre vertical shaft high shear mixer granulator. The product leaving the granulator has a very wide size distribution with some large high liquid content granules and lumps, and some fine dry powder. A troubleshooting team is put together to analyse the problem. They establish that the problem is due to poor powder wetting and nucleation but disagree on how to solve the problem. The formulation scientist proposes to add surfactant to the liquid binder to make it wet the powder better by reducing the contact angle from 70 to 10. The process engineer proposes increasing the number of nozzles from one to four to better distribute the liquid spray.

The values of tp and for this system are 1.5s and 0.6 respectively. Using a sketch of the nucleation regime map, locate the current operating regime for the mixer granulator. Calculate the expected change to tp and for each proposed change to conditions. Comment critically on whether either (or both) of the changes will achieve better nucleation and liquid distribution. [6 marks] (d) The breakage function for a roll mill is given below. Based on this breakage function, is the mode of breakage in the roll mill more likely to be cleavage or attrition? Explain why.
0 0 0 0 0 0.6 0 0 0 0 0.4 0.6 0 0 0 = 0 0 . 4 0 . 6 0 0 0 0 0.4 0.6 0 0 0 0 0.4 1.0 0 0 0 0 0 0

Using concepts from fracture mechanics, explain why the breakage constant Si for breakage by cleavage generally decreases with decreasing particle size. [5 marks] (e) To manufacture a granulated detergent powder, highly concentrated surfactant solution is added to fine zeolite powder in a continuous high shear mixer granulator. The mixer has an impeller speed of 500rpm and an impeller diameter of 0.7m. Analysis of the granules leaving the granulator shows that granule properties are: dg = 1mm g = 2000 kg.m-3 s = 0.85 min = 0.31 The properties of the feed are: dp = 5m = 7 Pa.s lv = 35*10-3 N.m-1 = 20 where the symbols are as defined in lecture notes. You may assume that the zeolite particles are spherical. Estimate the dynamic yield strength of the granules under granulator conditions. Use the regime map analysis to establish the type of granule growth behaviour that is expected in the granulator. [7 marks]

[TOTAL FOR QUESTION 1 = 30 marks]

QUESTION 2 A stirred media mill is used to grind cocoa solids during chocolate manufacturing. The batch grinding equation for such an operation is:
dmi = dt

j =1

j ,i S j m j

S i mi

where the symbols are as defined in lectures. (a) In one experiment, 1kg of a single size fraction of solids (45-63m) is used as the feed material. The mass fraction of solids remaining in the size fraction is shown as a function of time in the figure below. What is the breakage rate constant Si for the 45-63m size fraction in this mill? [6 marks]

1 0.8 0.7 0.6 0.5

m(t) / m 0

0.4 0.3

0.2

0.1 0 0.5 1 1.5 2 2.5 3 3.5 4

Time (hr)
The same mill is reconfigured to run in continuous mode to grind 1 kg/hr of cocoa solids feed with the following size distribution: Size interval (m) 45 - 63 37.5 - 45 22.5 - 37.5 <22.5 Mass fraction 0.4 0.3 0.2 0.1

For this system we know that the breakage rate can be expressed as:
x Si = k i x1
0.5

where xi is the top size of size interval i, and the breakage function matrix function is:
0 0 0 0.2 0 0 = 0.3 0.2 0 0.5 0.8 1.0 0 0 0 0

(b)

If the mill residence time is one hour, what proportion of the cocoa solids leaving the mill are less than 37.5m? You may assume the mill is operating at steady state and is well mixed. [9 marks] [TOTAL FOR QUESTION 2 = 15 marks]

QUESTION 3 The ACME explosives company produces ammonium nitrate (AN) particles by a prilling (spray cooling) process for use in explosive manufacture. The AN prills are very circular and have a very tight size distribution (effectively 1.4mm diameter monosized). The company wishes to diversify its product range by producing fertilizer granules which need to be in the size range 1.7 2.0mm. Engineers propose to do this using a single stage continuous fluidized bed to fatten the AN prills by spraying AN melt onto the granules so that they grow by layering (agglomeration is undesirable and will be avoided). (a) The population balance model for the product granule size distribution n(x) from the continuous granulator can be reduced to:
dn( x) N in ( x xin ) n( x) = dx G List clearly all assumptions that are made in developing this model from the general form of the population balance. Sketch the expected form of the product size distribution (n(x) vs x). Why is the product size distribution so broad? [5 marks] (b) If the product granule size distribution has a mean size x3, 0 = 1.85mm and the feed rate of seed AN prill particles is 1 tonne per hour, what is the feed rate of AN melt to the granulator? [5 marks]
Starting from the general moments form of the population balance, derive an in terms of expression for the 3rd moment of the product size distribution 3 moments of the prill seed distribution j , in for j =0, 1,2,3 and G . [5 marks]

(c)

[TOTAL FOR QUESTION 3 = 15 marks]