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PA M A N TA S A N N G LU N G S O D N G M AY N I L A

Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

RAW MATERIALS PRETREATMENT


A. Washing
Sargassum was obtained at the benthic (deep) part of the sea around Quezon
Province and contain significant amounts of sand, salt ions (Ca 2+, Mg2+, Na+, Cl-, SO42-),
and other foreign matter that can potentially interfere to the succeeding chemical
reaction. Thus, washing with tap water is necessary to eliminate these interferents.
1. Determination of Sargassum to Tap Water Mass Ratio
a. Materials and Apparatus

Sargassum
Analytical Balance
Plastic Containers
Tap Water
b. Objective

To determine the mass ratio of sargassum to tap water that will significantly

reduce the adhering foreign matters in the sargassum.


To determine the washing time that will significantly reduce the adhering foreign
matters in the sargassum.

c. Hypothesis
The mass ratio of sargassum to tap water, and the washing time that will
significantly reduce the adhering foreign matters in the sargassum is 1:9 and 30 minutes,
respectively.
d. Procedure
1. Weigh two hundred grams of Sargassum in eight separate plastic containers using an
analytical balance.
2. Pour 400 g, 600 g, 800 g, 1000 g, 1200 g, 1400 g, 1600 g and 1800 g of tap water in
the eight containers respectively and allow the mixture to stand for ten minutes.
3. Drain the washed Sargassum from the wash water

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

5. Weigh the washed Sargassum seaweeds


6. Weigh the wash water
e. Laboratory Setup

Figure 5.2: Sargassum Washing


f. Data and Observations
Run

Mass of

Mass of

Sargassum-

Mass of

Mass of

Mass of

Sargassum

tap

water mass

washed

wash

impurities

water

ratio

Sargassum

water

200 g

400 g

1:2

206.9 g

389.4 g

3.64 g

200 g

600 g

1:3

213.88 g

582.3 g

3.82 g

200 g

800 g

1:4

203.8 g

791.6 g

4.6 g

200 g

1000 g

1:5

210.8 g

984.4 g

4.8 g

200 g

1200 g

1:6

210.6 g

1184.2 g

5.2 g

200 g

1400 g

1:7

212.4 g

1382.4 g

5.2 g

7
8

200 g
200 g

1600 g
1800 g

1:8
1:9

204.2 g
201.4 g

1590.6 g
1792.8 g

5.4 g
5.8 g

200 g

2000 g

1:10

g. Observations and Analysis

5.8 g

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

It can be observed from the table above that as the Sargassum-water mass ratio
increases, the amount of impurities removed from the Sargassum also increased.
Although significant amount of impurities was removed from the Sargassum after
washing, its final mass (mass of washed Sargassum) consistently remained greater than
its original/feed mass in all the runs.
After washing, the water turned dark brown and significant amount of suspended
solids can be observed at the bottom of the container. The impurities removed from the
Sargassum include fine to coarse sand particles, dirt, shells, stems and leaves of other
seaweed species, and small dismembered parts of Sargassum.

Figure 5.3: Sargassum wash water

Figure 5.4: Washed Sargassum


At mass ratios 1:2 up to 1:7, the Sargassum is not completely soaked in the
water. It is confirmed that after washing the Sargassum samples using these runs, the

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

wash water obtained were saturated with a dark brown color and suspended solids and
the washed Sargassum still have some adhering dirt and sand particles which has a
distinct rough texture to touch. The tiny particulates suspended in the wash liquid have
inertial forces that are appreciably negligible and motion that assumes that of the fluid.
However, since the Sargassum occupies more volume than water, it hinders the motion
and settling not only of the tiny particulates but also of some coarse particles. Thus the
reduction of impurities is not efficient using these runs. At 1:8-mass ratio, the Sargassum
level is almost even to that of the water level in the container. However, the quality of
wash water and the amount of impurities removed using this run does not significantly
differ to that of the aforementioned runs. At mass ratio of 1:9, the Sargassum is
thoroughly soaked under water. After washing the highest amount of impurities with
amounting in 5.8 grams of foreign matter is removed. The opportunity for the dirt
adhering in the Sargassum to contact water is increased since the Sargassum is totally
submerged. Moreover, with more water molecules occupying the container, the
hindrance in the motion and settling of tiny particles that adhered to the Sargassum is
lessen.
The salt content of Sargassum is diluted when soaked with significant amount of
tap water since tap water contains less hardness ions compared to that of the seawater
that adhered inthe seaweed thereby establishing a concentration gradient which then
promotes diffusion of these ions. The consistent increase in mass of the Sargassum feed
in all the runs after washing is attributed to nutrient/essential element concentration
gradient across the tap water environment to the cellular structure of the seaweed. Since
the cells of Sargassum is hypotonic relative to the tap water environment, the tap water
molecules will tend to diffuse through the Sargassum cells to equalize the concentration
of nutrients present in these cells.

h. Conclusion
The Sargassum is effectively washed with tap water at a Sargassum-water mass ratio of
1:9.

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

2. Determination of Sargassum Washing Time


a. Materials and Apparatus

Sargassum
Analytical Balance
Plastic Containers

Tap Water
Timer

b. Objective
To determine the suitable washing time that will significantly reduce the adhering foreign
matters in the seaweed.
c. Hypothesis
Significant washing time will allow the reduction of adhering foreign matter in raw
Sargassum.
d. Procedure
1. Weigh two hundred grams of Sargassum and pour 1800 grams of tap water in six
separate plastic containers.
2. Allow the six mixtures to stand for 5, 10, 15, 20, 25 and 30 minutes respectively.
3. Drain the Sargassum seaweeds from the wash water
4. Weigh the washed Sargassum seaweeds
5. Weigh the wash water

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

e. Laboratory Setup

Figure 5.5: Sargassum Washing Setup

f. Experimental Data
Run

1
2
3
4
5
6

Mass of

Mass of

Washin

Mass of

Mass of

Mass of

Sargassum

tap water

g Time

washed

wash

impuritie

5 mins
10 mins
15 mins
20 mins
25 mins
30 mins

Sargassum
201.4 g
201.6 g
200.4 g
203.2 g
202.8 g
204 g

water
1792.8 g
1792.6 g
1793.6 g
1790.6 g
1791 g
1789.2 g

s
5.8 g
5.8 g
6.0 g
6.2 g
6.2 g
6.8 g

200 g
200 g
200 g
200 g
200 g
200 g

1800 g
1800 g
1800 g
1800 g
1800 g
1800 g

g. Observation and Analysis


It can be observed from the table above that the mass of impurities removed increases
as the washing time of Sargassum increases. Also, the mass of the washed Sargassum
consistently remained greater than the original feed mass used in each run. After
washing, a mixture of dirt, sand particles, shells and small dismembered seaweed parts
were collected as impurities. No significant change in the color of the wash water was
observed.

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

Longer washing time or hydraulic retention time (the time that a specific volume of water
remain in a container) allows large amount of small particles to contact the water
molecules and settle at the bottom of the container. It provided an opportunity for the
large portion of small particles to transition from being suspended near the bottom region
of the container to being compressed at the bottom region by virtue of density
differences and gravitational action.
The hypotonic environment of Sargassum upon being soaked in tap water established a
nutrient concentration gradient between the cells of Sargassum and the tap water
environment thereby promoting the tendency of the Sargassum cells to absorb water
molecules via osmosis to equalize the nutrient concentrations across. This more than
compensates for the impurities loss after washing since the final mass of the wet
Sargassum is greater than that of the original mass fed in the washing container.
h. Conclusion
The suitable washing time to remove significant amount of impurities from the
Sargassum is thirty minutes.

B. Drying
Washed Sargassum comprises of significant amount of unbound moisture which can
affect the succeeding reaction. Moreover, the wet Sargassum is bulky thereby occupying large
amount of space when being handled. Drying operation is therefore necessary to reduce the
water interferent in the reaction for ease of subsequent process parameter control and material
handling.

DRYING

Washed
Sargassum

Dried Sargassum

1. Determination of Drying Time and Temperature and Moisture Content of Wet


Sargassum
a. Materials and Apparatus

Wet Sargassum
Oven
Metal plate
Analytical Balance
Tongs

Timer
Thermometer
Silica crystals or beads (desiccant)
Desiccator

b. Objective

To determine the required drying time and temperature that will remove the moisture of
sargassum.

c. Hypothesis

The drying time and temperature that will remove the moisture of sargassum is
2.5 hours and 120C, respectively.

d. Procedure

1. Weigh 204 g of wet Sargassum in five separate metal plates using an analytical
balance

2. Dry the samples at temperatures 80 , 90 , 100 , 110

and 120

for thirty minutes.

3. Cool the samples to a desiccator with silica beads or crystals as desiccant for another
thirty minutes.

4. Weigh the cooled samples using an analytical balance.

5. Repeat steps 2-4 until the mass of each sample becomes constant

e. Laboratory Setup

Figure 5.6: Sargassum Drying


(Dryer)

Figure 5.7: Sargassum in a


desiccators

Figure 5.8: Dried Sargassum

f. Experimental Data

Run

Mass
of
Wet
Sarga
ssum

Mass
of
Bone
Dried
Sarga
ssum

204 g

17.8 g

Dryin
g
Temp
eratu
re

Dryin
g
Time

80

4 hrs

4 hrs

92.35
%

4 hrs

92.76
%

3 hrs

93.05
%

2.5
hrs

92.59
%

204 g

15.6 g

90

Perce
nt
Moist
ure
Cont
ent
(wet
basis
)
91.27
%

3
4
5

204 g
204 g
204 g

14.77
g

14.18
g

15.11
g

100

110

120

g. Observation and Analysis


It can be observed that the moisture content of the wet Sargassum was
significantly reduced after being oven-dried. More than 90% of the original feed mass

was lost in all the runs after drying. The free moisture content of Sargassum is therefore
significantly larger than the equilibrium moisture content retained in its structure.
Moreover, it can also be observed that as the drying temperature increases, the amount
of time needed to obtain a bone-dried product decreases. The long drying time it took for
drying the same mass of the wet Sargassum at lower temperature (lower energy input)
was compensated with an increased energy input for drying the same mass of the
sample at a lower residence time.

All the bone-dried Sargassum has a crisp texture and a deep dark brown color.
Moreover, there is no significant difference in the bone-dried mass of the Sargassum in
every run. Therefore, the run with the least amount of drying time requirement will be
chosen to be suitable for drying the wet Sargassum feed.

h. Conclusion
The suitable drying time for wet Sargassum is two and a half hours at 120
degrees Celsius. The free moisture content of the wet Sargassum is taken as the
average of the moisture content lost after drying and is equal to 92.40%.

C. Size Reduction

Though the dried Sargassum is now less bulky, its elongated structural symmetry
and appendages could be problematic in handling it especially during transport and
reaction. Size reduction is hence necessary in order to even enhance Sargassum
handling and to hasten the proceeding chemical reaction by exposing the cellulose in the
feedstock with maximized surface area.

SIZE
REDUCTION

Dried Sargassum

Sized Reduced
Sargassum

1. Determining the Particle Size Distribution of Size-Reduced Sargassum

a. Materials and Apparatus

Dried Sargassum
Blender
Analytical Balance

Tyler Standard screen (Mesh

numbers 8, 16, 40, 100 and 200)


Plastic containers

b. Objective

To determine the particle size distribution of size-reduced dried sargassum that will serve
as the basis for designing the size-reduced dried sargassum handling equipment.

c. Hypothesis

The size-reduced dried Sargassum has a large surface area exposed

d. Procedure

1. Weigh 20 g of dried Sargassum in four separate containers using an analytical


balance

2. Size reduce each sample of bulky dried Sargassum using a blender until it occupies
the least space it can inside the blender container.

3. Using a Tyler standard screen with mesh numbers 8, 16, 40, 100 and 200, screen
each sampleand weigh the mass of the retained portion (oversized, +) in each mesh and
that passed through (undersized, -) the last mesh (portion left in the pan) using an
analytical balance.

4. Report the particle size distribution of the size-reduced Sargassum by taking the
average of the mass percentage retained in each of the six section of the screen.

e. Laboratory Setup

Figure 5.9: Sargassum Size


Reduction Setup

f. Experimental Data

Figure 5.10: Size-reduced


Sargassum Sieving Setup (Tyler
Standard Screen)

Mes
h
Nu
mbe
r

16

40

100

200

Pan

Part
icle
Size
Ran
ge

>2.3
8
mm
1.19
mm2.38
mm
0.42
0
mm1.19
mm
0.14
9
mm0.42
0
mm
0.07
4
mm0.14
9
mm
<0.0
74
mm
Tota
l

Mass of Retained Sargassum particles


(g)

1st
ru
n
0.3

5.5

5.3

6.4

9.3

10.
2

10.
3

3.8

3.4

0.8

0.6

0.3

20

g. Observation and Analysis

2nd
ru
n
0.0
6

3rd
ru
n
0.0
4

4th
ru
n
0.0
4

%M
ass
of
size
red
uce
d
Sar
gas
sum

0.55
%

6.1

29.1
3%

10.
5

50.3
8%

3.0

2.9

16.3
8%

0.2

0.5

2.62
%

0.4
5

0.0

0.0

0.94
%

20.
01

19.
94

20.
04

100
%

During size reduction operation, the bulky structure of the dried Sargassum
occupies a lot of space in the blender container. Overcrowding of the feed inside the
container is not ideal since the Sargassum becomes stagnant at the topmost part of the
container, giving only the opportunity for the Sargassum near the blades at the bottom to
be size-reduced. Intermittent feeding of dried Sargassum was done in order to allow the
contact of all the seaweeds with the blades and to avoid leaving a stagnant portion of
Sargassum in the container during operations.

The reported particle size distribution of size-reduced Sargassum in each run


consistently showed least percentages of the coarse (>2.38 mm) and fine (<0.74 mm)
particles. The Sargassum portion with the particle size range 0.420 mm 1.19 mm
which is about half of the total mass of the size-reduced samples in all the runs is
consistently the highest in all the distributions. With the least amount of fines and coarse,
the handling of size-reduced Sargassum can be carried out easily since the particle
sizes will not significantly require further size reduction (for coarse) and no significant
losses will be incurred upon transport (for fines).

h. Conclusions

The size reduced Sargassum has the following particle size distribution:

Particle Size range


>2.38 mm
1.19 mm 2.38 mm
0.420 mm 1.19 mm
0.149 mm 0.420 mm
0.074 mm 0.149 mm
<0.074 mm

Mass percent (%)


0.55
29.13
50.38
16.38
2.62
0.94

HYDROLYSIS

Cellulose-rich feedstock like Sargassum can be directly converted to levulinic


acid using various metal chloride and acid catalysts. The conversion of cellulose from
the dried Sargassum to levulinic acid is a complex multistep process. It is generally
believed that the polymer chains of cellulose are broken down into low molecular weight
fragments

and

finally

to

glucose.

Then,

the

glucose

is

decomposed

to

hydroxymethylfurfural, which is further converted into levulinic acid and formic acid.

Figure 5.11: Reaction mechanism of Cellulose Hydrolysis to Levulinic Acid

Hydrolysis can be done by introducing the cellulose and water into the reactor
along with certain concentration of catalyst. The reactor will be heated for some time.
After the reaction, the cellulose residue will be filtered and the levulinic acid crystals will
be allowed to crystallize in the filtrate at ambient conditions. The crystals formed will
finally be filtered and then dried at ambient temperature.

HYDROLYSIS

Sized Reduced
Sargassum

Levulinic Acid

1. Determination of the type of Catalyst to be used

a. Materials and Apparatus

Dried Sargassum

Ferric chloride
Aluminum chloride
Sulfuric acid
Hydrochloric acid
Nitric acid
Distilled water
Analytical balance

Hot plate
Thermometer
1-L Beaker
500-mL beaker
Watch glass
Funnel
Iron ring
Iron Stand
Filter paper

b. Objective

To determine the catalyst type, catalyst concentration, sargassum-to-catalyst


solution mass ratio and reaction time that will produce the highest amount of
levulinic acid from size-reduced sargassum.

c. Hypothesis
The catalyst that will yield the highest amount of levulinic acid is sulfuric acid. The
suitable concentration of the catalyst for hydrolysis is 6 w/w%. The sargassum-to-mass
ratio that will produce the highest amount of levulinic acid, and at the same time will
keep the sargassum submerged is 1:25. The reaction time that will produce the highest
amount of levulinic acid is 4 hours.

d. Procedure

1. Prepare 377.75 g of 4% (w/w) of AlCl 3, FeCl3, H2SO4, HNO3 and HCl in five
separate 1-L beakers

2. Weigh 15.11 g of dried Sargassum in five separate watch glass.

3. Add the Sargassum samples to the solutions.

4. Heat and stir the reaction mixture for 120 minutes at 100 C .

5. Filter the solution from the cellulose residue using a Whatman 1 filter paper,
funnel, beaker, iron ring and iron stand.

6. Allow the levulinic acid to crystallize in the filtrate as it cools down at ambient
temperature.
7. Filter the crystals using a 500-ml beaker, filter paper and funnel
8. Allow the crystal residue to dry at ambient temperature
9. Weigh the dried levulinic acid crystals using an analytical balance

e. Laboratory Setup

Figure 5.12: Catalytic Conversion of Sargassum to Levulinic Acid Setup

Figure 5.14: Levulinic Acid Filtration


Setup

Figure 5.13: Cellulose residue


Filtration Setup

f. Data and Observations


Ma

Catal

Cataly

Sar

Tem

ss

yst

st

gas

perat

ss

of

type

Conce

sum

ure

dri

ntratio

Lev

ed

Cat

ulin

Sar

alys

ic

gas

Aci

su

Mas

rec

rati

ove

of

Ma

15.

Ferri

11

chlor

15.

ide
Alu

11

minu

4%

(w/w)

4%

1:2

red

(w/w)

1:2

100

100

100

100

100

0g

0g

0g

0.7

chlor

15.

11

g
15.
g
15.

11

ide
Nitri
acid
Sulf
acid
Hydr

11

ochl

oric

(w/w)

uric

4%

4%

4%

(w/w)

1:2

1:2

(w/w)

1:2
5

7g

0g

acid

g. Observations and Analysis


Sulfuric acid solely produced levulinic acid crystals from the Sargassum
feedstock among all the catalysts used for the catalytic conversion process. The

absence of levulinic acid yield using other catalysts in the processis due to the less
reactive nature of such catalysts at the given concentration and temperature as
compared to sulfuric acid in penetratingand breaking down the crystalline cellulose
structure of Sargassum and in converting the cellulose to levulinic acid. In addition, the
presence of other components in the Sargassum could have led to other selective
reactions that favored the formation of only the intermediate or other by-products in lieu
of levulinic acid.

Levulinic Acid Yield using various Catalysts

Figure 5.15: Levulinic Acid Yield using various Catalysts

During the reaction, dark-colored mixture of the catalyst and Sargassum was
observed using sulfuric acid, hydrochloric acid, ferric chloride and aluminum chloride
whereas the nitric acid catalyst produced a greenish-yellow mixture with the seaweed
substrate. As the temperature of the system exceeds 100 degrees Celsius temperature,

the mixture tends to evaporate significant amount of water at a fast rate leading to the
entrainment of sulfuric acid at the aluminum cover at the top of the reactor (beaker)
which eventually leads to the corrosion of the cover and catalyst loss. Moreover, the
observed temperature of the reaction mixture for the process does not significantly
exceed 105 degrees Celsius. This is so because under atmospheric conditions, sulfuric
acid solutions no more than 20% by weight has a boiling temperature near 100 degrees
Celsius. For these reasons, the maximum reaction temperature for all the runs in this
process will be kept at 100 degrees Celsius.

During the process of separating the cellulose residue from the filtrate, the
levulinic acid crystals start to grow as the heat applied to the reaction started to subside.
This is so since the melting point of levulinic acid is 34 degrees Celsius which means
that the cellulose residue should be filtered out from the filtrate before the reaction
mixture cools down in order to avoid levulinic acid crystallization in the cake (cellulose
residue). The dried levulinic acid product has a distinct fiber-like structure. The filtrate
with the levulinic acid crystals is not cooled at temperatures less than 8 degress Celsius
since formic acid, a by-product of the reaction, could crystallize which is undesirable.

h. Conclusion

Sulfuric acid is the suitable catalyst for the hydrolysis of Sargassum into levulinic acid.

2. Determination of the concentration of catalyst

a. Materials and Apparatus

Dried Sargassum
Distilled water
Analytical balance
Magnetic Hot plate
Thermometer
1-L beaker
500-mL beaker

Whatman 1 Filter paper


Funnel
Iron ring
Iron stand
Thermometer
Timer

b. Objective
To determine the concentration of suitable catalyst to be used that would yield
the highest amount of levulinic acid from Sargassum.

c. Hypothesis
The higher the concentration of the catalyst, the more Sargassum will be
converted into levulinic acid

d. Procedure

1. Prepare 377.75 g of 2%, 4%, 6%, 8%, 10% and 12% of H 2SO4catalyst solution in six
separate beakers.

2. Weigh 15.11 g of dried Sargassum in eight separate watch glass.

3. Add the Sargassum samples to the solutions.

4. Heat it for 120 minutes at 100 C.

5. Filter the solution from the cellulose residue using a Whatman 1 filter paper, funnel,
500-ml beaker, iron ring and iron stand.

6. Allow the levulinic acid to crystallize in the filtrate as it cools down at ambient
temperature.

7. Filter the crystals using a 500-ml beaker, filter paper and funnel

8. Allow the crystal residue to dry at ambient temperature

9. Weigh the dried levulinic acid crystals using an analytical balance

e. Laboratory Setup

Figure 5.16. Hydrolysis Setup

f. Experimental Data

Ma

Catal

Cataly

ss

yst

st

of

type

Conce

Ma

Temp

eratu

Ti

Mass
of

re

Levuli

drie

ntratio

nic

Acid

Sar

yield

gas
su
m

15.

Sulf

11

uric

g
15.

acid
Sulf

11

uric

acid

15.1

1g

Sulf

2%

1:

4%

1:

6%

uric

100

100
C

1:

100
C

0g

0.77 g

0.913 g

0.56 g

acid

15.

Sulf

8%

100

11

g
15.

uric

acid
Sulf

11

uric

g
15.

acid
Sulf

11

uric

acid

1:

10 %

1:

12 %

1:

100
C

100
C

0.311
g

0.53 g

g. Analysis

It can be observed from the experimental data obtained that the highest conversion of
Sargassum was attained using 6% (w/w) of H2SO4 solution. The levulinic acid conversion
increases from concentrations 2% up to 6% by weight. Beyond 6% (w/w) acid
concentration, levulinic acid conversions showed an erratic behavior as the
concentration increases.

Levulinic Acid Yield at various Concentrations

Levulinic Acid Yield

Figure 5.17: Levulinic acid Yield at various Sulfuric Acid Concentrations

h. Conclusion

Sulfuric acid solution at 6 % (w/w) concentration is the suitable catalyst concentration for
the hydrolysis of Sargassum into levulinic acid

3. Determination of Catalyst Solution-Sargassum Mass Ratio

a. Materials and Apparatus

Dried Sargassum

Distilled water
Analytical balance

Magnetic Hot plate


Thermometer
1-L beaker
500-mL beaker
Whatman 1 Filter paper

Funnel
Iron ring
Iron stand
Thermometer
Timer

b. Objective
To determine the suitable mass ratio of dried Sargassum to catalyst solution that will
yield the highest amount of levulinic acid.

c. Hypothesis

At higher mass-ratio, high amount of levulinic acid product can be produced

d. Procedure

1. Prepare 151.1 g, 226.65 g, 302.2 g, 377.75 g and 453.3 g of6 % (w/w) of sulfuric acid
catalyst solution in five separate beakers.

2. Weigh 15.11 g of dried Sargassum in eight separate watch glass.

3. Add the Sargassum samples to the solutions.

4. Heat it for 120 minutes at 100 C.

5. Filter the solution from the cellulose residue using a Whatman 1 filter paper, funnel,
500-ml beaker, iron ring and iron stand.

6. Allow the levulinic acid to crystallize in the filtrate as it cools down at ambient
temperature.

7. Filter the crystals using a 500-ml beaker, filter paper and funnel

8. Allow the crystal residue to dry at ambient temperature

9. Weigh the dried levulinic acid crystals using an analytical balance

e. Laboratory Setup

f. Experimental Data

Ma

Figure 5.18: Hydrolysis Setup

Cataly

Tem

(Sargassum:

pera

ture

Mass ratio

ss

st

of

Conce

Sulfuric

dri

ntrati

Acid

ed

on

solution)

Sar

gas

su

a
s

v
t

li

i
c
A
c
i
d

y
i
e
l
d

15.

6%

1:10

(w/w)

100

11

r
i
c
a
c
i

15.

d
S

6%

1:15

(w/w)

100

11

r
i
c
a
c
i

15.

d
S

6%
(w/w)

1:20

100

11

r
i
c
a
c
i
d

15.

6%

1:25

(w/w)

100

11

i
c

a
c
i
d

15.

6%

1:30

100

i
c
a
c
i
d

(w/w)

11

g. Observations and Analysis

At mass ratios 1:10 up to 1:25, the levulinic acid yield increases with increased sulfuric
acid mass.Within this range of mass ratio, increased sulfuric acid solution mass offers
increased selectivity towards the formation of the desired levulinic acid product.
However, at mass ratio of 1:30, the yield drastically dropped to 0.58 g which is about half
of the yield at 1:25-mass ratio run.

Levulinic Acid Yield at various Sargassum-Sulfuric Acid Solution Mass Ratio

Figure 5.19: Levulinic Acid Yield at various Sargassum-Sulfuric Acid Mass Ratio

h. Conclusion

The suitable Sargassum to sulfuric acid solution mass ratio for the hydrolysis reaction is
1:25.

4. Determination of Reaction Time and Reaction Order

a. Materials and Apparatus

Dried Sargassum

Distilled water
Analytical balance
Magnetic Hot plate
Thermometer
1-L beaker

500-mL beaker
Whatman 1 Filter paper
Funnel
Iron ring
Iron stand
Thermometer
Time

b. Objective

To determine the reaction time of dried Sargassum with the catalyst solution that will
yield the highest amount of levulinic acid.

c. Hypothesis

Long reaction times yield high amounts of levulinic acid product

d. Procedure

1. Prepare 377.75 g of 6% (w/w) of sulfuric acid catalyst solution in seven separate


beakers.

2. Weigh 15.11 g of dried Sargassum in seven separate watch glass.

3. Add the Sargassum samples to the solutions.

4. Heat it for 30, 60, 90,120, 150, 180, and 210 minutes at 100 C.

5. Filter the solution from the cellulose residue using a Whatman 1 filter paper, funnel,
500-ml beaker, iron ring and iron stand.

6. Allow the levulinic acid to crystallize in the filtrate as it cools down at ambient
temperature.

7. Filter the crystals using a 500-ml beaker, filter paper and funnel

8. Allow the crystal residue to dry at ambient temperature

9. Weigh the dried levulinic acid crystals using an analytical balance

e. Laboratory Setup

Figure 5.19: Hydrolysis Setup

f. Experimental Data
Ma

Cata

Cataly

Ma

Temp

ss

lyst

st

eratu

of

type

Conce

re

drie

ntratio

(degr

ees

Sar

Celsi

gas

us)

Ti

Mass
of
Levuli

nic
Acid

(ho

yield

su
m

15.

11

g
15.
11

H2S

O4

H2S
O4

6%
(w/w)

6%
(w/w)

100

1:

1:

0.11 g

0.25 g

0.5

100

g
15.

11

g
15.
g
15.

g
15.

g
15.

H2S

H2S

11

H2S

6%
(w/w)

O4

6%
(w/w)

O4

11

H2S

6%
(w/w)

O4

11

O4

11

H2S

6%
(w/w)

O4

6%
(w/w)

100

1:

100

100

0.913
g

1.94 g

3.772

2.5

100

1:

1:

0.51 g

1.5

1:

100

1:

6.28 g

8.39 g

3.5

15.1
1g

H2S
O4

6%
(w/w)

1:

100

g. Observation and Analysis

It can be observed from the table above that as the reaction time increases, the levulinic
acid yield also increases. The longer reaction time allows longer time for the feedstock to
contact the catalyst and the catalyst to penetrate the crystalline cellulose in the
Sargassum and hydrolyze it into levulinic acid. Hence, longer reaction time allows the
completion of the reaction which leads to increased reaction yield and selectivity

h. Conclusions

The suitable hydrolysis reaction time is 3.5 hours.

OXIDATION PROCESS

Treatment of levulinic acid with the inexpensive, simple oxidant hydrogen

peroxide under the catalytic action of sulfuric acid gives succinic acid in high yield and enables
facile product isolation by simple distillation of the volatile catalyst and by-products. Oxidation of
levulinic acid to produce succinic acid is done by reacting it with an acid catalyst and oxidizing
agent at a certain temperature. The reaction is shown below.

Process Flow Diagram

Oxidation

Levulinic Acid

Succinic Acid

1. Determination of sulfuric acid concentration

a. Materials and Apparatus

Levulinic Acid

Sulfuric Acid
Hydrochloric acid
Nitric Acid
Hydrogen peroxide
Magnetic Hot plate

Thermometer
1-L beaker
Filter paper
Funnel
500-ml beaker
Timer
Distilled water

b. Objective

To determine the sulfuric acid concentration and levulinic acid-to-hydrogen


peroxide mass-to-volume ratio that will produce the highest amount of succinic
acid.

c. Hypothesis

The sulfuric acid concentration that will produce the highest amount of succinic
acid is 3 M. The levulinic-to-hydrogen peroxide mass-to-volume ratio that will yield the
highest amount of succinic acid, and at the same time will keep the levulinic acid
submerged is 1:4.

d. Procedure
1. Mix 8.39 g of levulinic acid with 83.9 mL of 1 M, 2 M, 3 M and 4 M sulfuric acid
2.
3.
4.
5.

solution in four separate beakers.


Carefully add 33.56 mL of 30% H2O2 (v/v) to the solution
Heat the solution using a magnetic hotplate for 2 hours at 90C and stir continuously.
Allow the mixture to cool at room temperature.
Filter the slurry mixture using a filter paper, funnel and 500-ml beaker and wash it

with known volume of tap water


6. Sun-dry the succinic acid obtained

e. Laboratory Setup

Figure 5.19: Oxidation Setup

f. Experimental Data
Ma

Catal

Ca

Temp

Ti

Mass

ss

yst

tal

eratu

of

of

type

yst

re

Lev

Co

as

ic Acid

ulin

nc

s-

yield

ic

ent

aci

rati

ci

on

Succin

Vo
lH
P
Vo
l
ra
tio

8.3

Sulf

1:

90C

2.56 g

9g

uric

8.3
9g

acid
Sulf

uric

10

8.3
9g

Sulf
uric

8.3
9g

Sulf
uric

3.81 g

4.01 g

3.98 g

1:

90C

10

:4

4
M

acid

90C

:4

acid

10

acid

:4
1:

1:
10

90C

:4

*HP Hydrogen Peroxide; Vol - Volume

g. Observations and Analysis


It can be observed from the data that the succinic acid yield increases with
increased molarity of sulfuric acid solution. At 4 M concentration, the succinic acid yield
amount has a 0.50% deviation with respect to the succinic acid yield at 3 M. The
succinic acid yield at 2 M is 4.99% away relative to the value of the succinic acid yield at
3 M. The highest yield of succinic acid is therefore 4.01 g given by 3 M of sulfuric acid
solution.

Upon mixing the levulinic acid with sulfuric acid solution, a white homogeneous
solution is formed. The eventual addition of hydrogen peroxide increases the oxidizing
power of the solution since more water is protonated upon the decomposition of the
oxidant (H2O2). The premixing of hydrogen peroxide and sulfuric acid solutions before
the addition of levulinic acid should be avoided since a highly exothermic reaction occurs
leading to violent boiling of the solution that may impose potential hazards. The reaction
mixture forms a white slurry after an hour of heating and stirring. White solids at the
bottom of the reactor (beaker) can be observed during the reaction which could indicate
the presence of succinic acid. Succinic acid starts to melt at 184 degrees Celsius while
the other by-products of the process which are formic and acetic acids melt at 8.4 and
16.9 degrees Celsius respectively.

h. Conclusion

The suitable sulfuric acid catalyst concentration for the levulinic acid oxidation is 3 M.

2. Determination of Levulinic acid mass to H2O2 solution volume ratio

a. Materials and Apparatus

Levulinic Acid

Sulfuric Acid
Hydrogen peroxide

Hot plate
Thermometer

1-L beaker
Stirring rod
Filter paper
Graduated Cylinder
Distilled water

b. Objective

To determine the mass of levulinic acid to volume of hydrogen peroxide solution


ratio that will yield the highest amount of succinic acid

c. Hypothesis

High mass to volume ratio of levulinic acid with hydrogen peroxide solution will
yield significant amount of cellulose product

d. Procedure
1. Mix 8.39 g of levulinic acid with 83.9 mL of 3 M H2SO4 in five separate beakers.
2. Carefully add 16.78 mL, 33.56 mL, 50.34 mL, 67.12 mL and 83.9 mL of 30% H2O2
3.
4.
5.
6.

(v/v) to the solutions


Heat the solution using a magnetic hotplate for 2 hours at 90C and stir continuously.
Allow the mixture to cool at room temperature.
Filter the slurry mixture using a filter paper, funnel and 500-ml beaker
Sun-dry the succinic acid obtained.

e. Laboratory Setup

Figure 5.20: Levulinic Acid Oxidation Setup

Mass

Figure 5.21: Succinic acid powder product

f. Experimental Data

Catalys

LA Mass-HP

Volume ratio

Tempe

rature

Tim

Mass of

of

at

Succini

Levuli

al

Concen

c Acid

nic

ys

tration

yield

Acid

t
ty
p
e

8.39

H2

3M

1:2

90C

3.51 g

4.01 g

4.02 g

3.99 g

3.78 g

O
4

8.39 g

H2

3M

1:4

90C

O4

8.39

H2

3M

1:6

90C

O
4

8.39

H2

3M

1:8

90C

O
4

8.39
g

H2
S

3M

1:10

90C

O
4

g. Observations and Analysis

The highest succinic acid yield was obtained at 1:6 weight to volume ratio of levulinic
acid to H2O2 solution with 4.02 g of the desired product. Though the amount of product
produced at 1:6 weight to volume ratio is the highest among the runs, it is not
reasonable to conclude that it is the suitable process parameter since it is only 0.25%
higher in mass than that of the product produced using 1:4 ratio and it also required
lesser amount of the oxidant solution.

h. Conclusion

The suitable levulinic acid mass to hydrogen peroxide solution volume ratio for the
oxidation process is 1:4.

I.

SUMMARY OF
CHOSEN
PARAMETERS

The following are the values that were able to give the highest product yield in
each process.

Washing

Drying

Hydrolysis

Oxidation

Feed-to-Water Ratio

CHOSEN
VALUE
1:9

Washing Time

30 min

Drying Time

2.5 hrs

Temperature

Catalyst

1:25

Catalyst Concentration
Feed-to-Catalyst
Solution
Ratio
Reaction Time

120C
Sulfuric
Acid
6.0 w/w%

Catalyst Type

Catalyst Concentration
Feed-to-Catalyst
Solution
Ratio

4 hrs
Sulfuric
Acid
3M

1:4

PROCESS

PARAMETER

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Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

II.

EXPERIMENTAL FLOWCHART

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College of Engineering and Technology
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III.

ANALYTICAL TEST
RESULTS

A FTIR Analysis of Levulinic Acid

Levulinic acid is an essential intermediate produced from the hydrolysis of


sargassum. It is a major component for the production of succinic acid. To verify if the
produced crystals from the hydrolysis of sargassum is levulinic acid, Fourier Transform
Infrared (FTIR) Spectroscopy was conducted. The FTIR result is shown in Figure 5.22.

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Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

Figure 5.22. FTIR Spectra of Levulinic Acid synthesized from Sargassum

The FTIR spectra showed that the sample contained the major functional groups
in levulinic acid which are ketone and a carboxyl group. Thus confirming that the test
sample is levulinic acid.

D. FTIR Analysis of Succinic Acid


To verify if the proposed process was able to produce succinic acid, FTIR spectroscopy
was conducted. The FTIR spectra showed that the test sample contain the major functional
groups found in succinic acid. The FTIR spectra was able to show the carboxyl group, -C=O
group, C-O-H in-plane Bending and the Out-of-plane Bonding of the Bended O-H. Thus, the
FTIR spectra confirmed that the test sample is succinic acid. The FTIR spectra of succinic
acid is found on figure 5.23

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Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

Figure 5.23. FTIR Spectra of Succinic Acid derived from Oxidizing Levulinic Acid

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Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

Several physicochemical properties of the produced succinic acid were tested


and compared to the standard. The summary of the physicochemical properties are
presented in the succeeding table.

PRO
PERT
Y
Phas
e
Color

pH

Water
Solubi
lity
Meltin
g
Point
FTIR
Peaks

TEST METHOD

STANDARD

SAMPLE SUCCINIC
ACID

Sensory Test

Solid

Solid

Sensory Test

White

White

pH Meter

Water Solubility Test

Capillary Tube Test

FTIR
Spect
rosco
py

Broa
d OH
C-H
Stret
ch
C=O
Gro
up
C-OH inplan
e
ben
d
C-O
stret
ch
vibra
tion
O-H
outof-

2.7 at 0.1 M

1g/13mL

3300-2500

2635,2534

1g/12mL

188C

2.81 at 0.1 M

190C

3412.02

2606.95, 2490.67

1692

1416

1400

1307

1350

909

1630.38

673.25*

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Intramuros, Manila
College of Engineering and Technology
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plan
e
ben
d
*According to Reusch,W., the Range for O-H out-of-plane Bending is 660-900.
With the result of both FTIR spectroscopy and physicochemical tests, we have
verified that the sample is succinic acid.

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Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

IV.

OVERALL

PERCENTAGE YIELD

The overall percentage yield is calculated using the selected

values per process. The calculation is shown below.

Percent Yield=

Actual Yield
100
Theoretical Yield

Percent Yield=

mass of product obtained


100
mass of reactant

Percent Yield Hydrolysis=

8.39 g Levulinic Acid


100
65.50 g cellulose
15.11 g Sargassum x(
)
100 g sargassum

Percent Yield Hydrolysis=84.77


Percent Yield Oxidation=

4.01 g Succinic Acid


100
8.39 g Levulinic Acid

Percent Yield Oxidation=47.79

Overall Yield=( Yield Hydrolysis)( YieldOxidation)

Overall Yield=(0.8477)(0.4779) 100

Overall Yield=40.51

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College of Engineering and Technology
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The overall yield for this study is 40.51%. This will serve as a

basis for the upscale manufacturing process in the technical study.

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

V.

EXPERIMENTAL
STUDY CONCLUSION

The Sargassum feedstock which comprises of 65.50% of cellulose in a dry mass

basis is converted into levulinic acid via hydrolysis and the levulinic acid into succinic acid via
oxidation. The hydrolysis process produced 8.39 g of levulinic acid. The overall percentage yield
was found to be 40.51%.

Using one-factor at a time optimization, the suitable parameters for the washing

operation were found to be 1:9 Sargassum-to-water mass ratio and 30 minutes of washing, for
the drying operation were 120 degrees Celsius of drying temperature for 2.5 hours, for
hydrolysis reaction were 6% (w/w) sulfuric acid solution at 100 degrees Celsius and 1:25
Sargassum-to-sulfuric acid solution mass ratio for 4 hours and for the oxidation process, 3 M of
sulfuric acid solution at 90 degrees Celsius and 1:10:4 levulinic acid mass to sulfuric acid
solution volume to hydrogen peroxide solution volume for two hours of reaction.

Using Fourier-Transform Infra-Red (FTIR) Spectroscopy, the functional groups

present in the levulinic acid intermediate and succinic acid product were determined and
compared to the standard results.

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
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College of Engineering and Technology
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VI.

UPSCALE OF

EXPERIMENTATION

A WASHING OF SARGASSUM

Washing is a method of removing dirt usually with water and often some kind of

surfactants. Sargassum samples are collected from Agdangan, Quezon Province, within the
area of the West Philippine Sea. The average total dissolved solids of Philippine seawater
ranges from 34000-40000 ppm. It contains 54.78% chloride, 30.61% sodium, 7.68% sulfate,
3.66% magnesium etc. The presence of these ions in hard water produces undesirable salt
byproducts in a chemical reaction. Washing with water is the most convenient way to remove
these impurities from harvested sea raw materials. Our harvested raw material contains
significant amounts of sand, salt ions (Ca2+, Mg2+, Na+, Cl-, SO42-), and other foreign matter
that can potentially interfere to the succeeding chemical reaction. Thus, washing with tap water
is necessary to eliminate these interferents.

LABORATORY SCALE

INDUSTRIAL SCALE

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

Plastic Tubs

Bubble Drum Type Washer

Bubble Drum Type Washer:

The main principle is that the device is equipped with a strong flow of air drying

equipment, air bubbles in the pool by the high pressure air, let the water tumbling, tumbling to
achieve the purpose of the product. Upper end of the device is equipped with high-pressure
spray, the product roll in the pool, then there is the impact of high-pressure water, to wash sand
kelp mucosa role of surface impurities float through the overflow overflow, sand filtered through
the water cycle, the impurity precipitation tank.

The Bubble Drum Type Washer has features which include:


Device in addition to the motor, bearings and other standard parts are made of stainless
steel SUS304 / 2B material, in full compliance with the export of food hygiene
requirements. The device has a bubble generating device, so that the material was
tumbling state, with wash clean, energy-saving, water-saving, stable and reliable

equipment.
Conveyor section SUS304 stainless steel mesh belt, smooth operation, long life and

other characteristics, in line with food hygiene requirements.


The washing equipment uses advanced design, interior structure, in terms of cleaning up

contaminants, to no dead ends, clean, easy to clean features retentate.


The equipment adopts 2mm thick stainless steel tank body is made of 304 stainless
steel.

I.

DRYING OF SARGASSUM

Drying is a mass transfer process consisting of the removal of water A source of

heat and an agent to remove the vapor produced by the process are often involved In the most

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common case, a gas stream, e.g., air, applies the heat by convection and carries away the
vapor as humidity.

Washed Sargassum comprises of significant amount of unbound moisture which

can affect the succeeding reaction. Moreover, the wet Sargassum is bulky thereby occupying
large amount of space when being handled. Drying operation is therefore necessary to reduce
the water interferent in the reaction for ease of subsequent process parameter control and
material handling.

LABORATORY SCALE

INDUSTRIAL SCALE

Oven Dryer, Dessicator

Continuous Belt Dryer

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Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

Continuous Belt Dryer:

This equipment is a continuous penetrating flow drying equipment applied for

drying pieces strip and particles state materials with good ventilation. The equipment is suitable
for leafy materials, for which the water contents are high and high drying temperature is not
allowed. The equipment owns the advantages, of fast drying speed, high evaporation capacity
and good product quality.

The materials are uniformly distributed by the material feeder. The dryer is

composed of several sections. For each section, the hot air is circulated separately. Part of
exhausted gas is exhausted by a special moisture exhaust blower. The waste gas is controlled
by an adjustment valve. The hot air passes through the belt will bring water material away. The
belt moves slowly, running speed can be freely adjusted according to the material property. The
final products after the drying process will fall into the material collector continuously. The top
and low circulation units can be freely equipped according to the user's requirements. The
number of section might be selected according to the production demands.

The Continuous Belt Dryer has features which include:

Amount of air, heating temperature, time of material sticking on the belt and velocity of

feeding material can be adjusted in order to obtain the best drying effect.
Hot air can be circularly applied, the energy is greatly saved.
Unique air dividing device, it makes hot air distribute uniformly; this can guarantee

products quality.
Heating source can be selected from steam, conducting heat oil, electricity, and coal

furnace and oil burner


The equipment body is made of 304 stainless steel.

E. SIZE REDUCTION OF SARGASSUM

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College of Engineering and Technology
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Grinding reduces the size of solid materials by mechanical action, dividing them

into smaller particles In the grinding process, materials are reduced in size by fracturing them.
The mechanism of fracture is not fully understood, but in the process, the material is stressed by
the action of mechanical moving parts in the grinding machine and initially the stress is
absorbed internally by the material as strain energy.

Though the dried Sargassum is now less bulky, its elongated structural symmetry

and appendages could be problematic in handling it especially during transport and reaction.
Size reduction is hence necessary in order to even enhance Sargassum handling and to hasten
the proceeding chemical reaction by exposing the cellulose in the feedstock with maximized
surface area.

LABORATORY SCALE

INDUSTRIAL SCALE

PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

Blender & Tyler Mesh Screens

Fine Mesh Seaweed Grinder w/


Screener

Fine Mesh Seaweed Grinder:

The machine is composed of feeder, grading wheel, pulverizing blades, gears,

pulverizing motor, discharging gate, fans, collection box, dust collection box and etc. The raw
material is fed into the grind chamber through the upper feeder, is pulverized by high-speed
running blades. The fineness of the finished products is regulated via the distance adjustment of
grading wheel and grading plate. The high-speed running fans will lead those pulverized
material from grinding chamber to discharge gate via negative pressure while those unpulverized remained in the chamber. The dust from grinding is filtered and recycled via the cloth
bag.

The Fine Mesh Seaweed Grinder has features which include:

Equipped with features of cool air and sieve or screen


It is not limited by the viscosity, hardness, softness or fiber shape of the raw materials
Good effect to all materials, especially to those with fibers and those with oils.
Made of stainless steel SS304/SS316
Easy structure ;convenient operation and cleaning, low noise
High capacity without dust flying in production.

F. HYDROLYSIS OF SARGASSUM

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College of Engineering and Technology
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Acid hydrolysis is a process in which a protic acid is used to catalyze the

cleavage of a chemical bond via a nucleophilic substitution reaction. Cellulose-rich feedstock


like Sargassum can be directly converted to levulinic acid (LA) using various metal chloride and
acid catalysts.

The conversion of cellulose from the dried Sargassum to LA is a complex

multistep process. It is generally believed that the polymer chains of cellulose are broken down
into low molecular weight fragments and finally to glucose. Then, the glucose is decomposed to
hydroxymethylfurfural, which is further converted into levulinic acid and formic acid. Hydrolysis
can be done by introducing the cellulose and water into the reactor along with certain
concentration of catalyst. The reactor will be heated for some time.

LABORATORY SCALE

INDUSTRIAL SCALE

Enclosed Beaker on Hot Plate w/


Magnetic Stirrer

Digestion Tank:

Digestion Tanks

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Intramuros, Manila
College of Engineering and Technology
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This equipment is used in the production process of hydrolysis, neutralization,

etc.. It has great acid resistance, high temperature resistance, wear resistance, and corrosion
resistance.

The Digestion Tank has features which include:

The body is made up of stainless steel SUS304


Equipped with paddle type mixer. It has a mixing structure of cycloid pin wheel reducer.
Its sealing equipment is by mechanical sealing
It uses coil pipes for heating using steam/heating oils.

G. FILTRATION OF HYDROLYZED MIXTURE

Filtration is any of various mechanical, physical or biological operations that

separate solids from fluids by adding a medium through which only the fluid can pass. Vacuum
Filtration technique is most preferred for small batch of solution in order to quickly dry out small
crystals.

LABORATORY SCALE

INDUSTRIAL SCALE

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Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

Filter Paper in Funnel

Rotary Vacuum Drum Filter

Rotary Vacuum Drum Filter:

Vacuum drum filters can process high volumes of sludge which means reduced

operating costs compared to other filtration alternatives. However, this installation not just being
used for separating solids from liquids, but foremost to obtain a output of cake with a high purity
level.

The cylinder is main part of filter. The filter cylinder is divided to some filtering

chambers by strip along the circumferential direction. These chambers are strictly sealed
without ventilation between each other. Filter plate is laid on filter chamber forming a channel for
filtrate and supporting filter cloth. There is a pipe at one end of the cylinder body which has the
same number of channels with chambers. Each channel connects with corresponding filter
chamber.

The Rotary Vacuum Drum Filter has features which include:

The large size cylinder is made of welded steel plate


the small size made of cast cylinder
The cylinder is wrapped in filter cloth in order to ensure the sealing between each

chamber.
This cake has a low moisture level at the output of the vacuum filter
Low energy consumption level of the vacuum filter in terms of economies of scale
and also in terms of absolute energy consumption.

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The transmission mechanism drives the cylinder, and could transform several
speeds.

H. CRYSTALLIZATION OF LEVULINIC ACID

Crystallization is the process where a solid forms where the atoms or molecules

are highly organized in a structure known as a crystal. Some of the ways which crystals form
are through precipitating from a solution. Crystallization is also a chemical solidliquid
separation technique, in which mass transfer of a solute from the liquid solution to a pure solid
crystalline phase occurs. Most chemical compounds, dissolved in most solvents, show the socalled direct solubility that is, the solubility threshold increases with temperature. So, whenever
the conditions are favourable, crystal formation results from simply cooling the solution.
Levulinic acid crystallizes at room temperature.

LABORATORY SCALE

INDUSTRIAL SCALE

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Beaker

Fletcher Smith Continuous Vacuum


Pan

In view of energy saving Fletcher Smith Continuous Vacuum Pan has designed

Dual Continuous Pan which can be operated for two different grades of liquor simultaneously.
This pan is having the provision to stop any one of the liquor crystallization without affecting the
crystallization. The pan shall be equipped with multi baffle type SS 304 construction entrainment
separator.

The Fletcher Smith Continuous Vacuum Pan has features which include:

Heart-shaped profile of Pan to enhance natural circulation.


Fully automated.
Low temperature crystallization
Equipped with multi-baffle entrainment arrestor in stainless steel construction.
Simultaneous crystallization of two different grades of liquor.
Less initial investment compared to individual pans for two different grades for the same

type of liquor.
Lesser space is required than the individual pans.
Only one pan crystallizerr is required instead of two.
Made up of Stainless Steel 304

I.

FILTRATION OF LEVULINIC ACID

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Centrifugal filters provide fast sample processing and promote high sample

recoveries, even in dilute samples,

LABORATORY SCALE

INDUSTRIAL SCALE

Filter Paper in Funnel

Centrifuge Filters

Centrifuge Filters:

The centrifugal separator is adept industrial grade SS304 material. The

centrifuge is widely used in solid-liquid separating, the drum is high-speed rotation when running
so that the solid will stay in filter bag under the centrifugal force and liquid filtrate was
discharged.

The Centrifuge Filter has features which include:

The machine and material contact parts all made of stainless steel 304 or 316
Single or multilayer of grid structure, without dead parts, easy to clean.
Discharge part, 360 degree adjustable, more suitable for mass or line production.
With waterproof spring aprons, to prevent dust from entering the motor.
Inlet and outlet parts, with a de-ironing separator, to clean the metallic impurities in
material.

J. OXIDATION OF LEVULINIC ACID

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Treatment of levulinic acid with the inexpensive, simple oxidant hydrogen

peroxide under the catalytic action of sulfuric acid gives succinic acid in high yield and enables
facile product isolation by simple distillation of the volatile catalyst and byproducts. Oxidation of
Levulinic acid to produce succinic acid is done by reacting it with an acid catalyst and oxidizing
agent at a certain temperature

LABORATORY SCALE

INDUSTRIAL SCALE

Beaker on Hot Plate w/ Magnetic


Stirrer

Oxidation Reactor Vessel

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The reactor tank is consisted of tank body and mixing part. The mixing tank

made of stainless steel with jacket for heating or cooling and insulating layer for outer. According
to technological requirements, the mixing part can choose high shear, high speed dispersion or
low speed anchor mixing. Reactor is typically used to install floor-mounted legs, also can use
lug support on the platform.

The Oxidation Reactor Vessel has features which include:

It is an inner coil steam-heated reactor


Made up of stainless steel 304
Component: Cover, Body, Jacket, Mixer, Shaft gland driving device, Supporting and
others
Shaft gland is mechanically sealed.
Stirring mode is anchor type

K. FILTRATION OF SUCCINIC ACID

Vacuum Filtration technique is most preferred for small batch of solution in order

to quickly dry out small crystals.

LABORATORY SCALE

INDUSTRIAL SCALE

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Filter Paper in Glass Funnel

Rotary Vacuum Drum Filter

Rotary Vacuum Drum Filter:

Vacuum drum filters can process high volumes of sludge which means reduced

operating costs compared to other filtration alternatives. However, this installation not just being
used for separating solids from liquids, but foremost to obtain a output of cake with a high purity
level.

The cylinder is main part of filter. The filter cylinder is divided to some filtering

chambers by strip along the circumferential direction. These chambers are strictly sealed
without ventilation between each other. Filter plate is laid on filter chamber forming a channel for
filtrate and supporting filter cloth. There is a pipe at one end of the cylinder body which has the
same number of channels with chambers. Each channel connects with corresponding filter
chamber.

The Rotary Vacuum Drum Filter has features which include:

The large size cylinder is made of welded steel plate


the small size made of cast cylinder

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The cylinder is wrapped in filter cloth in order to ensure the sealing between each

chamber.
This cake has a low moisture level at the output of the vacuum filter
Low energy consumption level of the vacuum filter in terms of economies of scale

and also in terms of absolute energy consumption.


The transmission mechanism drives the cylinder, and could transform several
speeds.

L. DRYING OF SUCCINIC ACID

Spray drying is a method of producing a dry powder from a liquid or slurry by

rapidly drying with a hot gas. A consistent particle size distribution is a reason for spray drying
some industrial products such as catalysts. Air is the heated drying medium; however, if the
liquid is a flammable solvent such as ethanol or the product is oxygen-sensitive then nitrogen is
used.

LABORATORY SCALE

INDUSTRIAL SCALE

Blower

Spray Dryer

Spray drying plant is a kind of centrifugal or pressurized atomizer ,which

atomizes liquid materials such as solution, suspensions, emulsion or paste into tiny droplet
(surface area increased) and dry them into powder product at once(several seconds) by
contacting with hot air . Air is transferred into hot air by passing through the heater, and goes

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into the hot air separator on the top of the dryer, then goes into the drying room evenly. As the
same time, liquid materials are sent to the centrifugal atomizer on the top of the dryer by the
screw pump with stepless speed regulation, and atomized into tiny droplets which will contact
hot air, then dried into dry product within short time. The finished product will be discharged by
the whirlwind separator on the bottom of the drying tower and waste air is exhausted by air fan.

The spray drying speed is very fast, liquid material after atomizing will increase

its surface area largely and can be evaporated its moisture 65-98% instantly in the hot air flow
so as to finish drying within 5 to 15 seconds. It is specially suitable for drying of heat sensitive
material. The dried product have even granule , good flowability and solubility , high purity and
good quality

The wall of the tower has sandwich cooling device to ensure liquid cone body which

has large taper.


The wall can pulsate the tube by compressed air to shake down powder which is stuck

on the tube.
All contact place inside the dryer have plain or round surface , and is ground and

polished to avoid sand hole and dead angle etc.


The contact surface is made of stainless steel to ensure materials free of pollution.
The driving parts have good sealing to prevent water and oil.
Materials discharge is done by sealed butterfly valve to avoid air leaking .
Minimum of 95% Dried Powder Collection
Positive Pressure System Condition
Tower body is equipped with automatic vibration device.
Tower body and pipe line have cleaning hole and sewage discharge hole that can

open quickly.
Equipped with thermostat feeding tank

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Intramuros, Manila
College of Engineering and Technology
Chemical Engineering Department

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PA M A N TA S A N N G LU N G S O D N G M AY N I L A
Intramuros, Manila
College of Engineering and Technology
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