PART SCORE

Introduction (25)
Materials(20)
Methodology(30)
Data Tables(20)
References(5)

EXERCISE 2

EXPERIMENTAL ANALYSIS OF THE EFFECT OF VARYING MASSECUITE BRIX

ON FILTRATION PARAMETERS USING A LABORATORY SCALE CENTRIFUGAL

FILTER.

GROUP 2

ADRIENNE JOYCE D. EBORA

JESI C. MACAHIA

BRYAN VINCENZO C. PATANGAN

ChE 156-1L

Date Submitted: March 11, 2022

ASST. PROF RHEBNER E. AROCENA

Faculty-in-charge
 INTRODUCTION

Principles/Relevant Equations

Centrifugal filtration is the combination of two principles, filtration and centrifugal

separation. Filtration is the separation of solid particles from liquids through a pressure

difference set up that will induce fluid to flow through filter medium which then will block the

passage of larger particles, in turn, presence of build up on the mesh as porous cake

(Geankopolis, 1993). Centrifugal separation is the use of the force resulting from the rotation of

a cylindrical container about an axis at a constant radial distance to separate solids from liquids

(Geankopolis, 1993). Therefore, centrifugal filtration is the solid-liquid separation process

wherein pressure resulting from centrifugal action is applied to force the slurry through the filter

medium, leaving solids behind (McCabe, Smith, & Harriot, 1993). In contrast to other filters,

centrifugal filters are able to drain residual liquid from the porous cake through centrifugal action

making centrifugal filters a cost efficient option for processes that require subsequent drying of

the cake. Figure 1.1 shows a basic centrifugal filtration setup where ri is the inner radius of the

porous cake, r1 is inner radius of the liquid surface, and r2 is the inner radius of the basket.

Figure 1.1 Basic Centrifugal Filtration Setup (Geankopolis, 1993).

 Centrifugal filters can be classified into two, batch filtering centrifuges and continuous

filtering centrifuges. Batch filtering centrifuges are preferred when the value of the desired

product is high since it yields the highest possible product purity, lowest possible cake moisture,

and highest product recovery (Green & Perry, 2008). Continuous centrifuges on the other hand

are often preferred for its low capital cost, high unit capacity, shorter retention time, and ease of

integration in continuous manufacturing processes (Green & Perry, 2008). There are three

common types of centrifugal filters: suspended batch machines, automatic short-cycle batch

machines, and continuous conveyor centrifuges. These centrifugal filters differ according to

drum size, filter medium, rotational speed, and time per load. Table 1.1 shows the difference in

the three common centrifugal filters: suspended batch machines, automatic short-cycle batch

machines, and continuous conveyor centrifuges.

In a centrifugal filtration process, there is the presence of the following: filter medium,

cake, filtrate, and filter aid. Filter medium is a porous membrane that allows fluid to pass through

leaving the solids behind. A good filter medium is described as the following: retain solids to be

filtered giving a clear filtrate; not plug or blind; must be able to withstand process conditions;

allow the cake formed to be discharged clean and completely; and, relatively low cost (McCabe,

Smith, & Harriot, 1993). Cake is the solids that remain on the filter medium, through time as

cake builds up on the filter medium this can increase the flow resistance and subsequently affect

flow rate (McCabe, Smith, & Harriot, 1993). In contrast, filtrate is the liquid that passes through

the filter medium. Lastly, filter aids are slimy or very fine solid materials that can serve as an

initial layer to a filter medium. It can increase the porosity of the cake to be able to control the

flow to a reasonable rate (McCabe, Smith, & Harriot, 1993). Examples of filter aids that can be

used in such processes are the following: diatomaceous silica, perlite, purified wood cellulose, or
other inert porous materials (McCabe, Smith, & Harriot, 1993). According to McCabe, Smith

and Harriot, when filter cake is required to be recovered, filter aid can be easily separated by

dissolving or burning, in cases solids have no value cake and filter aid can be discarded together.

Table 1.1. Data on the Characteristics of The Common Centrifugal Filters (McCabe, Smith, &

Harriot, 1993).

Type Illustration Characteristics

Suspended Batch Basket size: 30 to 48 inches

Machines in diameter, 18 to 30inches in
depth;
Filter medium: Canvas,
fabric, woven metal cloth.
Rotational speed: 600 r/min
to 1800 r/min
Time per load: 10 to 30
minutes
Throughput: 300 to 1800
kg/hr

Automatic Basket size: 20 to 42 inches

Short-cycle Batch in diameter
Machines Filter medium: Fine metal
screens
Feed size: Finer than
150-mesh
Rotational speed: Constant
Time per load: 30 to 90 sec
Throughput: large
 Continuous Basket size: 12 to 48 inches
Conveyor in diameter
Centrifuges Filter medium: Slotted wall
Feed size: Coarse crystals,
Finer than 100-mesh
Throughput: 0.3 to 25 ton/hr

According to Green and Perry, theoretical predictions of the behavior and filtration rates

of solid-liquid mixtures in filtering centrifuges are quite difficult and have not been too

successful. This is due to the direct relationship of area of flow and driving force to the radius;

and, specific resistance and porosity which change due to the cake.

The theory of constant-pressure filtration can be modified and used where centrifugal

force instead of pressure difference causes the fluid to flow (Geankopolis, 1993). The equation

is derived from a setup where cake has already been deposited. Referring to Figure 1.1 where we

defined ri as the inner radius of the porous cake, r1 as the inner radius of the liquid surface, and r2

as the inner radius of the basket. For the succeeding equations, the following must be assumed:

(1) cake is nearly incompressible so that an average value resistance, 𝞪 (2) flow is laminar, (3)

area of flow 𝞐 is approximately constant (Geankopolis, 1993). Therefore, the velocity ν of the

liquid is

𝑞 𝑑𝑉
ν= 𝐴
= 𝐴𝑑𝑡
(Equation 1-1)

Where q is the filtrate flow rate m3/s. Relating the equation of constant pressure filtration,

the flow rate is defined as:

𝑑𝑉 −∆𝑝
𝐴𝑑𝑡
= µα𝑐𝑠 (Equation 1-2)
𝐴
(𝑉+𝑉𝑒)
Substituting Eq. 1-2 to 1-1, relating centrifugal field

𝑞µα𝑐𝑠(𝑉+𝑉𝑒)
− ∆𝑝 = 2 (Equation 1-3)
𝐴

For hydraulic head of dz m, the pressure drop is

𝑑𝑝 = 𝑝𝑔𝑑𝑧 (Equation 1-4)

2
In a centrifugal field, g will be equal to centripetal acceleration therefore 𝑔 = 𝑟ω and dz=dr

2
𝑑𝑝 = 𝑝𝑟ω 𝑑𝑟 (Equation 1-5)

Integrating between r1 and r2

2 2 2
𝑝ω (𝑟2−𝑟1)
− ∆𝑝 = 2
(Equation 1-6)

Combining Eq. 1-3 and Eq. 1-6, therefore filtrate flow at constant area A is (Geankopolis, 1993).
2 2 2 2
𝑝ω 𝐴 (𝑟2−𝑟1)
𝑞= 2(µα𝑐𝑠(𝑉+𝑉𝑒))
(Equation 1-7)

The rate of filtration at constant pressure can be described using the Carman Kozeny

Equation (Handout 2 - Centrifugal Filtration, 2022).

𝑑𝑡 µα𝑤(𝑉+𝑉𝑒)
𝑑𝑉
= 2 (Equation 1-8)
𝑔𝑐𝐴 (−∆𝑝)

2
5(1−ε)𝑆𝑜
α= 3 (Equation 1-9)
𝑝𝑠ε

Such that:

∝ - specific resistance (constant for incompressible cakes)

dV/dt- filtration rate

μ - viscosity of the liquid

w - mass of solid in feed slurry per unit volume of liquid

V - volume of filtrate

(-∆p) - pressure drop

Ve - equivalent volume

So - specific surface area

A - filtration area

ε - porosity of the cake

ρs - density

Consequently,

(Equation 1-10)

(Equation 1-11)

(Equation 1-12)

(Equation 1-13)

(Equation 1-14)
To relate raw sugar, massecuite feed, and saturated sugar solution:

(Brix x weight)massecuite = (Brix x weight) sat’d sugar sol’n + (Brix x weight) raw sugar (Equation 1-15)

Significance of the Experiment

Chemical engineers are those who are often involved in industrial plants through the

design, development and operation of manufacturing processes. It is their task to ensure that it

runs with high efficiency in the most economical way. According to Green and Perry, centrifugal

filters are preferred and more economical than using other types of filter, when high cake purity

or minimal residual moisture of cake is required. Factors such as filtrate volume equivalents,

specific cake resistance, cake porosities, and cake specific surfaces must be evaluated on how it

affects the product yield in order to know how to run the process efficiently and economically.

Centrifugal filtration is widely applied in the production of sugar, therefore understanding the

effect of brix massecuite to the efficiency of separation process.

Objectives of the Experiment

The general objective of this experiment is to evaluate filtration characteristics using a

laboratory-scale centrifugal filter with perforated basket/drum. Specifically, the study aims to:

1. Illustrate the effect of brix massecuite on the plot of change in time per change in volume

of filtrate(Δt/ΔV) versus volume of filtrate(V);

2. Calculate and compare corresponding filtrate volume equivalents, specific cake

resistance, cake porosities, and cake specific surfaces; and

3. Evaluate the sugar recovery.

 MATERIALS AND METHODS

Materials

For the experiment, the materials, and miscellaneous include: (1) stirring rod, (3) spatula,

(5) beakers, (1) 5-mL volume interval graduated cup, (1) 12 inch ruler, (1) thermometer, a

centrifugal filter (Fig. 1.2), a refractometer (Fig 1.2), an analytical top loading balance, an

electrical water heater, a timer, a video recorder, tap water, masking tape, raw brown sugar and/or

syrup.

Figure 1.2 Top Loading Batch Centrifugal Filter (Handout 2 - Centrifugal Filtration, 2022).

Figure 1.3 Brix Refractor and Graduation through Eyepiece (Handout 2 - Centrifugal Filtration,

2022).
Methodology

Calibration of Brix Refractometer

1. Place 3 to 5 drops of water into the refractometer.

2. Make sure that there is no bubble formation

3. Make sure that the reading is zero.

Determination of the actual brix number of raw sugar and saturated sugar syrup

1. Dissolve 5g of raw sugar with 25g of water, making sure that the solution is thoroughly

mixed.

2. Compute for the dilution factor using.

𝑉𝑖 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑡𝑜𝑐𝑘
𝐷𝐹 = 𝑉𝑓
= 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑡𝑜𝑐𝑘 + 𝑑𝑖𝑙𝑢𝑒𝑛𝑡
(Equation 1-16)

3. Place 3 to 5 drops of the solution into the refractometer and record the reading.

4. Calculate the actual brix number of the raw sugar by multiplying the dilution factor with

the refractometer reading.

𝐵𝑟𝑖𝑥 = 𝐷𝐹 𝑥 𝑅𝑒𝑓𝑟𝑎𝑐𝑡𝑜𝑚𝑒𝑡𝑒𝑟 𝑟𝑒𝑎𝑑𝑖𝑛𝑔 (Equation 1-17)

5. The brix of the saturated sugar syrup was set at 66°Bx.

Preparation of the massecuite samples

1. Calculate the required mass of raw sugar and saturated sugar syrup for 2000g of 85, 87

and 89°B massecuite samples using Equation 1-15.

2. Mix and stir the required amount of raw sugar and syrup for each sample until the

mixture becomes homogeneous.

3. Prepare 2 samples for each brix number to have two sets of trials.

Batch Centrifugal filtration

1. At the start of each run, clean and dry the equipment using water and rugs.

2. Transfer the massecuite sample into the centrifugal filter.

3. Turn the power on and place a graduated cup at the bottom of the equipment to collect the

filtrate.

4. Start the timer when the first drop is observed.

5. In the span of 2 minutes, record the time for every 10mL filtrate of 85°Bx, 10mL filtrate

of 87°Bx, and 5mL filtrate of 89°Bx collected.

6. Dry each filter cake in the centrifugal filter by spinning it for another 5 minutes.

7. Using a ruler, measure the height and thickness of each cake at different points and

calculate for the average height and thickness of each cake.

8. Collect the cake from the filter and weigh to obtain the percent recovery of the sugar.

9. For each collected filtrate, measure 5g and dilute it with 25g water.

10. Record the refractometer reading of the diluted filtrate by placing 3 to 5 drops of the

diluted solution into the refractometer.

11. Clean and dry the centrifugal filter in preparation for the next run.
 DATA TABLES/BLANKS

Table 1.2. Batch centrifugal filter specifications.

Height of the filtration basket, in

Radius of the basket, cm

Table 1.3. Determination of the actual brix of the raw sugar

Mass of brown sugar, g

Mass of water, g

Dilution factor

°Bx reading

Actual Brix, °Bx

Table 1.4. Preparation of massecuite samples

Massecuite Raw Mass, g

component concentration,
°Bx 85°Bx 87°Bx 89°Bx

Raw sugar

Saturated sugar
syrup
Table 1.5. Data for change in volume with respect to change in time.

85°Bx 87°Bx 89°Bx

V, mL t, s V, mL t, s V, mL t, s

Table 1.6. Determination of the cake properties and filtrate of each massecuite.

85°Bx 87°Bx 89°Bx

Height of cake, mm

Thickness of cake, mm

Mass of sugar recovered, kg

Brix of filtrate, °Bx

 REFERENCES

Foust, A. S. (1980). Principles of Unit Operations. New York: Wiley.

Geankopolis, C. J. (1993). Transport Processes and Unit Operations (3rd ed.). Englewood

Cliffs, New Jersey, United States of America: PTR Prentice-Hall Inc.

Green, D. W., & Perry, R. H. (2008). Perry's Chemical Engineering Handbook (8th ed.). The

McGraw-Hill Companies, Inc.

(2022). Handout 2 - Centrifugal Filtration. Los Banos: Department of Chemical Engineering,

UPLB.

McCabe, W. L., Smith, J. C., & Harriot, P. (1993). Unit Operations of Chemical Engineering

(5th ed.). McGraw-Hill Book Inc.