Raw Materials Pretreatment: A. Washing

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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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.
Intramuros, Manila
2. Determination of Sargassum Washing Time

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
Intramuros, Manila
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.
Intramuros, Manila
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
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
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

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
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
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
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
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

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
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.
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.
temperature.
e. Laboratory Setup
Figure 5.16. Hydrolysis Setup
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
Dried Sargassum
Distilled water
Analytical balance
Magnetic Hot plate

Thermometer
1-L beaker
500-mL beaker
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.
4. Heat it for 120 minutes at 100 C.
temperature.
e. Laboratory Setup
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
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
Dried Sargassum
Distilled water
Analytical balance
Magnetic Hot plate
Thermometer
1-L beaker
500-mL beaker
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.
4. Heat it for 30, 60, 90,120, 150, 180, and 210 minutes at 100 C.
temperature.
e. Laboratory Setup
Figure 5.19: Hydrolysis Setup
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
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
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
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

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
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
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
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
Intramuros, Manila
II.
EXPERIMENTAL FLOWCHART
Intramuros, Manila
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.
Intramuros, Manila
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
Intramuros, Manila
Figure 5.23. FTIR Spectra of Succinic Acid derived from Oxidizing Levulinic Acid
Intramuros, Manila
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*
Intramuros, Manila
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.
Intramuros, Manila
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
Intramuros, Manila
The overall yield for this study is 40.51%. This will serve as a
basis for the upscale manufacturing process in the technical study.
Intramuros, Manila
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.
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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.
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
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
Intramuros, Manila
REFERENCES
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Glucose from Sugarcane Bagasse. The Italian Association of Chemical Engineering.
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June 21, 2016 from http://www.intertek.com/analysis/ftir/.
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Harmsen, P. H., &Huijgen, W. J. (2010).Progress in Physical and Chemical Pretreatment

of Lignocellulosic Biomass. Biofuel Technologies, 53-96. doi:10.1007/978-3-642-345197_3
Jiang, M., Chen, K., Liu, Z., Wei, P., Ying, H., & Chang, H. (2009).Succinic Acid
Production by Actinobacillussuccinogenes Using Spent Brewer's Yeast Hydrolysate as a
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of Lignocellulosic Biomass for Efficient Hydrolysis and Biofuel Production. Industrial &
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Raw Materials Pretreatment: A. Washing

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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

RAW MATERIALS PRETREATMENT

reduce the adhering foreign matters in the sargassum.

5. Weigh the washed Sargassum seaweeds

Figure 5.2: Sargassum Washing

g. Observations and Analysis

Figure 5.3: Sargassum wash water

Figure 5.4: Washed Sargassum

2. Determination of Sargassum Washing Time

Figure 5.5: Sargassum Washing Setup

g. Observation and Analysis

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

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

for thirty minutes.

4. Weigh the cooled samples using an analytical balance.

Figure 5.6: Sargassum Drying

Figure 5.7: Sargassum in a

Figure 5.8: Dried Sargassum

g. Observation and Analysis

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

a. Materials and Apparatus

Tyler Standard screen (Mesh

numbers 8, 16, 40, 100 and 200)

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

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

Figure 5.9: Sargassum Size

Figure 5.10: Size-reduced

Mass of Retained Sargassum particles

g. Observation and Analysis

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

Particle Size range

Mass percent (%)

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

Figure 5.11: Reaction mechanism of Cellulose Hydrolysis to Levulinic Acid

1. Determination of the type of Catalyst to be used

a. Materials and Apparatus

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

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

3. Add the Sargassum samples to the solutions.

Figure 5.12: Catalytic Conversion of Sargassum to Levulinic Acid Setup

Figure 5.14: Levulinic Acid Filtration

Figure 5.13: Cellulose residue

f. Data and Observations

g. Observations and Analysis

Levulinic Acid Yield using various Catalysts

Figure 5.15: Levulinic Acid Yield using various Catalysts

2. Determination of the concentration of catalyst

a. Materials and Apparatus

Whatman 1 Filter paper

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.

8. Allow the crystal residue to dry at ambient temperature

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

Figure 5.16. Hydrolysis Setup

Levulinic Acid Yield at various Concentrations

Levulinic Acid Yield

Figure 5.17: Levulinic acid Yield at various Sulfuric Acid Concentrations

3. Determination of Catalyst Solution-Sargassum Mass Ratio

a. Materials and Apparatus

Magnetic Hot plate

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

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