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Practical1:BallMilling|TFLab1

TF Lab 1
A fine presentation of lab work

Practical 1 : BallMilling
December 23, 2013
Practical 1:

Experiment 1

Title: Ball Milling

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Sieve. The sieving process in this


experiment uses a stack of sieves
which have the smallest mesh above
a collector tray followed by meshes
which get progressively coarser
towards the
top of the stack.
Objective:
To grind the coarse salt to a smaller size by using a ball mill and to obtain the particle size distribution
of the initial and the sieved final mixture.
Introduction:
Ball milling is a method used to break down the solids to smaller sizes or into a powder. A ball mill is
a type of grinder which consists of a cylinder. It is used in grinding (or mixing) materials like ores,
chemicals, ceramic raw materials and paints. The cylinder rotates around a horizontal axis. It is
partially filled with the grinding medium and the material to be ground. Materials which can be used
as media are ceramic balls, pebbles and stainless steel balls. Large to medium-sized ball mill is
mechanically rotated on its axis, but small one (as in our laboratory) has its container sits on two
drive sha s (where pulleys and belts are utilised to transmit rotary motion).
There are dierent types of milling equipment used in which they can be categorized according to the
principal method applied. No matter what principal method is applied, the extent of size reduction is
always associated to the milling time. We have cutting methods, impact method, compression
method and attrition method. Ball mills uses combined impact and attrition methods.
In this experiment, we are required to break the coarse salt down using a ball mill and then by using a
sieve, the particle size distribution is known.
Method:
Materials:

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Coarse Salt
Apparatus:
Ball milling machine
Steel balls (of two dierent sizes)
Weighing boat
Weighing balance
Sieve
Procedures:
1. 300-500g coarse salt was weighed.
2. Ball bearings of various sizes were inserted into the mill.
3. Coarse salt was added into the mill.
4. The process of milling was started for between 10 or 20 minutes with the appropriate speed. (refer
Result)
5. The product obtained was weighed again.
6. The powder obtained was si ed by using sieving method (sieve nest).
7. A graph (histogram) of particle size distribution was plotted.
Result and Calculations:

Particle

5rpm10

5rpm20 min

3rpm 10 min

3rpm20 min

Before
size (mm)

312.50
min

400.00

340.79

327.15

501

281.85

358.87

311.14

296.67

301-500

14.11

30.18

12.92

18.56

251-300

4.10

3.78

4.14

1.49

milling
A er milling
Mass of
course salt
collected/
g

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151-250

5.79

3.37

2.05

0.27

1-150

3.83

2.48

0.00

0.06

Total

309.68

398.68

330.25

317.05

Graph of Mass of Coarse Salt Collected(g) Against Particle Size (mm) 3rpm, 10minutes

Graph of Mass of Coarse Salt Collected(g) Against Particle Size (mm) 3rpm, 20minutes

Graph of Mass of Coarse Salt Collected(g) Against Particle Size (mm) 5rpm, 10minutes

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Graph of Mass of Coarse Salt Collected(g) Against Particle Size (mm) 5rpm, 20minutes

Questions:
1. What are the factors which influence the process of particle size reduction (milling)?
Particle size, number of balls, particle density, hardness, number of media used, time of grinding, and
speed of the ball mill (rpm) are factors which will aect the process of milling.
Size: The smaller the media particles, the smaller the particle size of the final product. Meanwhile, the
size of grinding media particles should be larger than the material to be ground.
Density: The grinding media should be denser than the material being ground. It becomes a problem
if the grinding media floats on top of the material to be ground.

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Hardness: The grinding media needs to be durable enough to grind the material, but not to be too
hard that it could wear down the tumbler at a fast pace.
Number of media used: The more the number of media, the faster the process of size reduction. But
at the same time, there will be less capacity le the mill, less production. In fact, using a mixture of
two dierent sizes of media can produce much faster results, than milling with either size of media
alone.
Time of grinding: The longer the time of grinding, the faster the process of particle size reduction.
Speed of the ball mill (rpm): The faster the speed of ball mill, the faster the process of size reduction.
2. What tools can be used to reduce the size of the particles?
A microfluidizer achieve uniform particle size reduction by bottom-up crystallization and eicient cell
disruption.
A homogenizer reduces particle sizes under very high pressures, sheer, turbulence, acceleration and
impact.
A mixer transports phases or ingredients into a main continuous phase (liquid), with which it would
normally be immiscible. An array of rotors is used to create shear in a tank or pipe through which the
solution passes.
Mills grind the particles using the mill or milling media and can quickly produce fine powders from
coarse grains. Mills are commonly used in the mining industry. In cutter mill, size reduction occurs by
fracture of particles between the two sets of knives. In hammer mill, size reduction occurs by impact,
by four hammers attaching on a central sha . In end-runner and edge-runner mills, compression is
carried out on a small scale in a mortar-and-pestle form. In roller mills, the principle of attrition is
used where material is sheared as it passes through a gap and is transferred from slower roll to a
faster roll, and is removed by a scraper. In ball mill, size reduction is done by both impact and attrition
of particles. Rod mill is similar to ball mills but it uses long rods for grinding media. Autogenous mill is
a self-grinding mill which is used in breakage of larger rocks. SAG (Semi-Autogenous Grinding) mill is
an autogenous mill which uses grinding balls, it is similar to ball mill but has large diameter and short
length. Vertical mill is used in grinding material at smaller particle sizes, which is used a er ball mill.
Pebble mill is used when product contamination by iron from steel balls must be avoided.
Fluid energy or jet mill consists of a hollow toroid. A fluid, usually air, is injected as a high-pressure jet
through nozzles at the bottom of the loop. High velocity of air creates zones of turbulence into which
solid particles are fed. The high kinetic energy causes particles to collide with momentum for fracture
to occur. The turbulence produces the impact and attrition.
Together with ball mill and jet mill, pin mill also acts by producing impact and attrition. Two discs
with closely spaced pins rotate against one another at high speeds. Particles experience impaction
with pins and attrition between pins when they travel outwards under influence of centrifugal force.
3. What are the factors which influence the selection of a device for particle size reduction?

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Particle shape desired: Particle shape may vary due to methods (e.g. impact or attrition).
Fineness of particles desired: Some other properties of powder will be altered if the fineness is
changed. The degree of size reduction depends on the use of a powder (where is it applied to)
Particle size desired: When small particle size is desired, more time is needed in the size reduction
process, thus cost of size reduction also increases.
Hardness of the particle to be ground: The harder the particle, the tougher the device should be and
more abrasion is needed in the process.
Contamination of product: Pebble mill is used to prevent product contamination by iron from steel
balls.
Discussion:
From the result the size reduction increases as we increase the number of rotations of the ball milling.
Meanwhile, increase in the time taken for ball milling will also increase the size reduction. From the
graphs, we can see that as the size reduction increases, the particle sizes obtained will form a less
steep curve in the graph. This can be correlated with the values in our table due to the following
reason. As we can see in the table, more and more particles can go through to the smaller meshes and
thus the weight of particles remained in the first mesh decreases. A less steep curve can then be
obtained.
Another thing to consider is that our curves had all been skewed to the le (negatively skewed). This
indicated that majority of our particles size has been distributed to the le side. However, this may be
due to the fact that we do not have sieves which have aperture of >500mm or else we might be able
to have a plot of particle size distribution (histogram) showing normal distribution (no skew).
Finally, less weight is obtained a er milling compared to before milling because some particles were
le in the ball mill. Not all particles can be removed from ball mill as some particles which are small
tend to stick to wall and some were baled by the narrow opening of the ball mill.
Conclusion:
Size reduction increases as the number of rotations and time taken for ball milling increases. Meshes
of larger aperture should be used in sieving to obtain a complete curve of particle size distribution.
Some particles were lost when transferring them out of the ball milling, which results in lighter weight
obtained a er ball milling.
References:
1. M. E. Aulton. (1988) Pharmaceutics The Science Of Dosage Form Design. 2nd Edition. Churchill
Livingstone, UK. Pg. 166-172
2. Robert E. Schilling, Union Process Inc. (n.d.) Citing Websites. Choose The Right Grinding Mill.
Retrieved date. 21st December 2013. From
http://www.unionprocess.com/tech_papers/ChooseTheRightGrindingMill.pdf
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3. Citing Websites. Rod Mills, How Do They Work? (1994-2012) Retrieved date. 21st December 2013.
From http://www.mine-engineer.com/mining/rodmill.htm
4. Citing Websites. Ball Mills. (2013) Retrieved date. 21st December 2013. From
http://www.unitednuclear.com/index.php?main_page=index&cPath=25_35
5. A. Sahoo* and G. K. Roy. (2008) Citing Websites. Correlations for the Grindability of the Ball Mill As a
Measure of Its Performance. From
http://dspace.nitrkl.ac.in/dspace/bitstream/2080/879/1/correlations1.p
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Practical 2 : Sieving
In "Experiment 1"

Practical 5 : Shape And


Particle Size Analysis Using
A Microscope
In "Experiment 1"

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Practical 4 : Angle Of Repose


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