NaOH Alkalinasi
NaOH Alkalinasi
NaOH Alkalinasi
(51) International Patent Classification: Bangi, Kajang, Selangor, 43000 (MY). CHOO, Yuen
D21C 3/02 (2006.01) D21C 11/00 (2006.01) May; c/o MALAYSIAN PALM OIL BOARD, No. 6, Per
D21C 3/04 (2006.01) CIOL 1/02 (2006.01) siaran Institusi, Bandar Baru Bangi, Kajang, Selangor,
D21C 5/00 (2006.01) 43000 (MY). XUEBING, Zhao; Department of Chemical
Engineering, Institute of Nuclear and New Energy Techno
(21) International Application Number:
logy, Tsinghua University, Haidian District, Beijing,
PCT/MY20 15/050002
100084 (CN). DEHUA, Liu; Department of Chemical En
(22) International Filing Date: gineering, Institute of Nuclear and New Energy Techno
19 January 2015 (19.01 .2015) logy, Tsinghua University, Haidian District, Beijing,
100084 (CN).
(25) Filing Language: English
(74) Agent: MIRANDAH ASIA (MALAYSIA) SDN BHD;
(26) Publication Language: English Suite 3B-19-3, Plaza Sentral, Jalan Stesen Sentral 5, 50470
(30) Priority Data: Kuala Lumpur (MY).
PI2014000163 20 January 2014 (20.01.2014) MY (81) Designated States (unless otherwise indicated, for every
(71) Applicants: MALAYSIAN PALM OIL BOARD kind of national protection available): AE, AG, AL, AM,
[MY/MY]; No. 6, Persiaran Institusi, Bandar Baru Bangi, AO, AT, AU, AZ, BA, BB, BG, BH, BN, BR, BW, BY,
Kajang, Selangor, 43000 (MY). TSINGHUA UNIVER¬ BZ, CA, CH, CL, CN, CO, CR, CU, CZ, DE, DK, DM,
SITY [CN/CN]; Haidian District, Beijing, 100084 (CN). DO, DZ, EC, EE, EG, ES, FI, GB, GD, GE, GH, GM, GT,
HN, HR, HU, ID, IL, IN, IR, IS, JP, KE, KG, KN, KP, KR,
(72) Inventors: LOH, Soh Kheang; c/o MALAYSIAN PALM KZ, LA, LC, LK, LR, LS, LU, LY, MA, MD, ME, MG,
OIL BOARD, No. 6, Persiaran Institusi, Bandar Baru MK, MN, MW, MX, MY, MZ, NA, NG, NI, NO, NZ, OM,
[Continued on nextpage]
(54) Title: AN INTEGRATED PROCESS FOR FRACTIONATION OF OIL PALM EMPTY FRUIT BUNCH AND CONVER
SION OF THE CELLULOSIC SOLID TO ETHANOL
(57) Abstract: The invention relates to an integrated process
for fractionation of oil palm empty fruit 5 bunch (EFB) to
obtain cellulosic solid, hemicellulosic sugars and high-purity
lignin, and conversion of the cellulosic solid to ethanol by
enzymatic hydrolysis and microbial fermentation. The end-
products of the disclosed integrated process comprises at
least a cellulosic solid, hemicellulosic sugars, high-purity
lignin and cellulosic ethanol. 10
w o 2015/108409 Ai III III II II III I I11 III I 11III I I I llll III I
II II
PA, PE, PG, PH, PL, PT, QA, RO, RS, RU, RW, SA, SC, Declarations under Rule 4.17:
SD, SE, SG, SK, SL, S , ST, SV, SY, TH, TJ, TM, TN,
— as to applicant's entitlement to apply for and be granted
TR, TT, TZ, UA, UG, US, UZ, VC, VN, ZA, ZM, ZW.
a patent (Rule 4.1 7( ))
(84) Designated States (unless otherwise indicated, for every — of inventorship (Rule 4. 7(iv))
kind of regional protection available): ARIPO (BW, GH,
GM, KE, LR, LS, MW, MZ, NA, RW, SD, SL, ST, SZ, Published:
TZ, UG, ZM, ZW), Eurasian (AM, AZ, BY, KG, KZ, RU, — with international search report (Art. 21(3))
TJ, TM), European (AL, AT, BE, BG, CH, CY, CZ, DE,
DK, EE, ES, FI, FR, GB, GR, HR, HU, IE, IS, IT, LT, — before the expiration of the time limit for amending the
LU, LV, MC, MK, MT, NL, NO, PL, PT, RO, RS, SE, claims and to be republished in the event of receipt of
SI, SK, SM, TR), OAPI (BF, BJ, CF, CG, CI, CM, GA, amendments (Rule 48.2(h))
GN, GQ, GW, KM, ML, MR, NE, SN, TD, TG).
AN INTEGRATED PROCESS FOR FRACTIONATION OF OIL PALM EMPTY FRUIT
FIELD OF INVENTION
The invention discloses an integrated process for fractionation of oil palm empty fruit bunch
(EFB) to obtain cellulosic solid, hemicellulosic sugars and high-purity lignin, and conversion
of the cellulosic solid to ethanol by enzymatic hydrolysis and microbial fermentation. The
BACKGROUND ART
Lignocellulose is one of the most abundant organic materials on the planet and has long
been recognized as a potential feedstock for producing fuels, chemicals and materials.
interest all over the world due to the shortage of fossil-based oil and increasing
and hemicelluloses) and an aromatic polymer (lignin), all of which show promising uses in a
biorefinery platform.
such as to make paper or other pulp-derived products. The cellulose can also be converted
into glucose which can be further used as carbon source for producing many fuels and
substituted polymer of sugars with degree of polymerization ~ 70 to 200. After hydrolysis, the
both. Lignin obtained from lignocellulosic biomass has value as a solid fuel and also as an
It will be beneficial to fractionate lignocellulosic biomass and further utilize the resulting
technologies is that the process is usually conducted using high temperatures with
associated high pressures. For example, the ethanol organosolv delignification process is
usually conducted at higher than 160 °C in order to effectively remove lignin (Zhao et al.,
bagasse by aqueous formic acid with direct recycle of spent liquor to increase cellulose
digestibility - the Formiline process"; Bioresour Technol. 7:23 - 32; 2012). Traditional
biomass pulping (to produce paper and related goods) is also a biomass fractionation
process, in which cellulose is recovered in high yields, but lignin is primarily consumed by
combustion for heat recovery. Moreover, the lignin products are always not of high purity
Publication) disclosed a method for utilization of lignocellulose waste of palm oil production,
first of all, empty fruit bunches (EFB) after separation of oil-bearing fruit. The method for
utilization is based on peculiarities of the structure of cell tissue of bunches and provides
obtaining soluble sugars useful for ethanol production and obtaining solid fuel enriched in
lignine. '330 Publication disclosed a method which consists of several stages including
conversion of polysaccharides (cellulose and hemicellulose) of lignocellulose feedstock into
microorganisms. '330 Publication acknowledges the fact that the presence of lignine in the
feedstock. Lignine inhibits action of enzymes as it covers cellulose fibers hindering access of
enzymes to the substrate. Therefore the first task is efficient shredding of the plant substrate
consisting mainly of cell walls, and creation of defects in the form of disordered and
amorphous sites of cellulose. Chemical composition of the bunches shows that they contain
a large amount of water- and acid-soluble compounds. Their removal from the bunches
should affect the structure, and, therefore, mechanical strength of the material.
However, it must be taken into account that the importance of process of simultaneous
microorganisms as highlighted in the present invention was not disclosed in '233 Patent.
One of the most challenging technical obstacles in biomass fractionation processes is that
the recovered cellulose is often recalcitrant to subsequent hydrolysis to form glucose. The
hydrolysis is often done enzymatically, and the resistance of the cellulose to hydrolysis is
often compensated for by using high enzyme loading. For conventional pulping process, the
objective of delignification is to remove lignin and maintain fiber strength and degree of
polymerization (DP) of cellulose. However, during biomass pretreatment for increasing the
obtain the individual components. The lignin products obtained are often highly condensed
and not suitable for further modification and application. A disadvantage of the prior art
pretreatment processes is that lignin is not sufficiently removed from the lignocellulosic
biomass. The lignin that remains present in the cellulosic solid has a negative effect on an
enzymatic hydrolysis, and can give higher handing costs in downstream processing. In
particular the presence of residual lignin can irreversibly adsorb cellulase enzymes and thus
Oil palm empty fruit bunch (EFB) is a by-product of palm oil extraction and milling process.
EFB has become an attractive biomass for biorefinery since a large amount of EFB is
produced along with palm oil production. Malaysia has a ready source of biomass in EFB
conveniently collected and available for exploitation in all palm oil mills. As a lignocellulosic
biomass, EFB similarly shows many applications in various fields (Sumathi et al., "Utilization
Energy Reviews 12(9):2404 - 2421 ; 2008). However, if EFB is fractionated into its primary
components such as cellulose, hemicellulosic sugars and lignin, it would be used more
pretreatment which has been recognized as a promising biomass fractionation due to the
following advantages:
(1) organic solvents are always easy to recover by distillation and recycled for
pretreatment;
(2) the chemical recovery in organosolv pretreatment can isolate lignin as a solid
material and hemicellulose as syrup, both of which show promise as chemical feedstocks;
(3) the isolated lignin are of high purity, which can be used for polymer substitution
One aspect of the present invention is to provide an integrated process for fractionation of oil
A further aspect of the present invention is to provide an integrated process for converting
the said cellulosic solid into ethanol and specifically employing simultaneous saccharification
In another aspect of the present invention is to provide a process for utilizing the produced
spent liquor comprises lignin product and hemicellulosic sugars in more beneficial way via
The present invention consists of features and a combination of parts hereinafter fully
described and illustrated in the accompanying drawings, it being understood that various
changes in the details may be made without departing from the scope of the invention or
To further clarify various aspects of some embodiments of the present invention, a more
thereof, which are illustrated, in the appended drawings. It is appreciated that these
drawings depict only typical embodiments of the invention and are therefore not to be
considered limiting of its scope. The invention will be described and explained with additional
FIG. 1 is the flow sheet of the integrated process for fractionation of EFB into cellulosic solid
FIG. 2 is the graph showing enzymatic hydrolysis of cellulosic solid at different solid
consistency characterized in the form of (a) Sugar concentration; (b) Enzymatic glycan
conversion
cellulosic solid for ethanol production characterized independently in the form of (a) Glucose
FIG. 4 is the flow sheet of the general mass balance of fractionation of EFB for ethanol,
The present invention relates to an integrated process for fractionation of oil palm empty fruit
bunch (EFB) to obtain cellulosic solid, hemicellulosic sugars and high-purity lignin, and
It has been well known that biomass pretreatment is a prerequisite step for effective
increase cellulose accessibility and thus cellulase enzymes can contact cellulose to perform
the hydrolysis process. Conventional biomass pretreatment such as steam explosion, dilute
digestibility. However, in these processes, lignin is often of low quality and only can use as a
fuel.
It has been known that removing lignin from lignocellulose is more important than removing
the following advantages: (1) organic solvents are always easy to recover by distillation and
recycled for pretreatment; (2) the chemical recovery in organosolv pretreatment can isolate
lignin as a solid material and hemicellulose as syrup, both of which show promise as
chemical feedstocks; (3) the isolated lignin are of high purity, which can be used for polymer
organosolv pretreatment has been well investigated for biomass pretreatment under acid
for enzymatic hydrolysis"; Applied Microbiology and Biotechnology 82 (5): 8 1 5-827; 2009).
However, ethanol actually does not have a high solubility to lignin, so that a relatively high
liquid-to-solid ratio is often used for an effective delignification. However, even so there is
still a high residual lignin content in the cellulosic pulp. It has been known that a good solvent
for lignin should have a solubility parameter (δ value) around 11 cal 2/cm 2. Therefore,
actually organic acids, such as formic acid and acetic acid with δ values of 12.1 and 10.1
cal 2/cm 2 respectively, are better solvents for lignin than ethanol.
Accordingly, the present invention provides a process for fractionation of oil palm empty fruit
bunch (EFB) for producing cellulosic solid (pulp), hemicellulosic sugars and lignin as
a) mixing EFB with aqueous organic acid solution containing at least 50-90% by
weight of organic acid in a digester at a temperature in the range of 50-1 60°C, thereby
b) separating the said first mixture ( 1 ) into a first solid phase (2) and a first liquid
c) washing the said solid phase (2) with fresh aqueous organic acid solution to obtain
a second mixture (4), and separating the said second mixture (4) into a second solid phase
d) heating the said second solid phase (5) to recover organic acid under vacuum to
obtain a evaporated solid phase (7) and gas phase, and condensing the said gas phase to
e) washing the evaporated solid phase (7) with water to obtain a cellulosic solid and
f) mixing the first liquid stream (3) and second liquid stream (6) in a spent liquor
g) distillating the liquid stream (9) for recovering organic acid to obtain a top liquid
h) recycling the top liquid stream ( 1 0) and the third liquid stream (8) for EFB cooking
j) separating the said mixture stream ( 1 3) to obtain lignin product and hemicellulosic
sugars.
The process advantageously produces cellulose pulp from EFB which can be further used
for paper production. In addition, the produced celluose is suitable for enzymatic hydrolysis
into sugars, which can be further fermented into alcohols such as ethanol and/or butanol.
Preferably, the said organic acid is selected from formic acid, acetic acid or propanoic acid;
more preferably, the said organic acid is formic acid. Since organic acid, in particular formic
acid and acetic acid have δ value around 11 cal 2/cm 2, they are good solvents for lignin
fragmentation. Moreover, the carboxyl group of organic acid can easily form hydrogen bond
with lignin molecule, thus aqueous organic acids have high lignin solubility. Therefore, during
fractionation of EFB, the required liquid-to-solid ratio could be reduced compared with other
organosolv processes. On the other hand, the FT dissociated from organic acid can play as
More preferably, the used aqueous organic acid should have an organic acid concentration
of 50-90%. Too low organic acid concentration is negative to lignin solubilization; however,
too high organic acid concentration can lead to high acylation of cellulose, which can further
affect the utilization of cellulose. More preferably, the organic acid concentration should not
be higher than 90% by weight in order to control the acyl group content of lower than 5% by
weight. However, the organic acid concentration should not be less than 50% by weight, in
after separation the said solid phase contains dry solid mater of 20-50% by weight. It should
be careful to control the liquid content of the obtained solid phase. In a preferable
embodiment of this invention, after squeezing the liquid content should not be less than 50%
(corresponding dry solid matter content higher than 50%); otherwise the mechanical
pressing power would collapse the pore structure of the cellulosic solid, which whereby could
In order to further remove the residual lignin fragments remaining in the said solid phase (2)
obtained in step b), the solid phase (2) must be washed with fresh organic acid as shown in
step c). Preferably, the said organic acid in step c) is selected from formic acid, acetic acid or
propanoic acid; more preferably, the said organic acid is the same as that used for cooking
in both organic acid type and concentration. The said solid phase (2) cannot be directly
washed with water in order to avoid the precipitation of dissolved lignin onto cellulosic fiber
which will affect the subsequent enzymatic hydrolysis of cellulose. The washing step can be
conducted by either batch or continuous flow. Preferably, the solid phase (2) is washed with
fresh medium comprising the same organic acid as that used in step a) in a counter flow or
cross flow manner. In another preferable embodiment of this invention, after washing the
solid phase (2), a separating step is performed as that used in step b) to obtain a solid phase
(5). The said solid phase (5) is wet with some residual organic acid that must be recovered.
Preferably, in step d) the said solid phase (5) is heated under vacuum to recover the residual
organic acid by evaporation and obtained an evaporated solid phase (7). The evaporation
temperature should be well controlled. Too high a temperature might cause significant
hornification of the said cellulosic solid, and whereby decreases the subsequent enzymatic
80 °C under pressure of 1- 1 3 kPa; more preferably, the recovery condition meets the
demand that the said evaporated solid phase (7) has a liquid content of less than 5% by
weight. By this evaporation process, more than 95% of the residual organic acid can be
recovered.
The evaporated solid phase (7) still contains some residual organic acid, which might inhibit
the microorganism growth in the subsequent fermentation process. Therefore, the said
evaporated solid phase (7) is further washed with water to remove the residual organic acid.
Preferably, the said washing process in step e) is conducted at 30-60 °C with water-to-solid
ratio of 20-5:1 by weight. More preferably, the said washing process is conducted in a
This invention also comprises a step for recovering the organic acid from the spent liquor
obtained in step b) and c). The spent liquor contains dissolved lignin and sugars that mainly
come from hemicellulose hydrolysis. In a preferable embodiment of this invention, the said
spent liquor is evaporated under vacuum to recover organic acid. Preferably, the spent liquor
is distillated under vacuum to obtain the recovered fresh aqueous organic acid at the top as
the top liquid stream ( 1 0) and a concentrated spent liquor stream ( 1 1). The said top liquid
stream (10) is further recycled to step a) for delignification of EFB and step c) for washing
the said solid phase 2). More preferably, 90% of the organic acid in spent liquor should be
recovered by distillation.
The concentrated spent liquor stream ( 1 1) is further treated for lignin and hemicellulosic
sugar recovery. Lignin can be easily precipitated from the concentrated spent liquor as a
solid phase while hemicellulosic sugars are recovered as a liquid syrup. Preferably, the
volume of the water added to the said concentrated spent liquor should be at least five times
that of the concentrated spent liquor. More preferably, the water added to the concentrated
a) treating the said cellulosic solid with alkali solution or suspension at liquid-to-solid
b) adjusting the pH value of the said first slurry mixture obtained in step a) to 4.5-6.5
c) converting the said second slurry mixture to ethanol by adding cellulase enzyme
During delignification, cellulose can be acylated to a certain extent, which can limit the
binding of cellulase enzyme onto cellulose. Therefore, the cellulosic solid should be further
treated to remove acyl group. In a preferable embodiment of this invention, alkali is used to
catalyze the deacylation process. Preferably, the said alkali is selected from sodium
hydroxide, potassium hydroxide, lime or ammonia. More preferably, the said alkali is
selected from lime or ammonia, since lime is cheap and ammonia can be used as nitrogen
The alkali loading is important to deacylation. Preferably, the used alkali loading is 0.1 -10%
by weight based on the dry cellulosic solid. However, liquid-to-solid ratio is also important
since it can affect the alkali concentration for deacylation. In a preferable embodiment of this
invention, the liquid-to-solid ratio is 20-3:1 . More preferably, when alkali loading is low, a low
liquid-to-solid ratio should be used, but the mixing might not be homogenous at a low liquid-
to-solid ratio. Deacylation temperature also significantly affects the degree of deacylation.
Preferably, the temperature should be in the range of 20-120 °C. Most preferably, the
deacylation condition should meet the requirement i.e. the treated cellulosic solid has an acyl
by a SSF process. However, the slurry mixture is preferably neutralized and its pH adjusted
in the range of 4.5-6.5. More preferably, in most cases, since the released organic acid by
deacylation process can react with the excess alkali, no other acid is required to adjust the
pH value of the slurry. The neutralized slurry is thus suitable for ethanol production.
Preferably, the said SSF is conducted with 5-30 FPU/g solid of cellulase loading, at 30-40 °C
The celulosic solid obtained by this invention showed very good enzymatic digestibility, and
can obtain a high ethanol concentration. Removing most of the lignin by organic acid
delignification not only eliminates the physical barrier of lignin, but also decreases the no n
productive adsorption of cellulase enzymes onto the residual lignin matrix. Moreover, the
high cellulose content in the obtained cellulosic solid would increase glucose concentration
in the enzymatic hydrolyzate, which whereby would increase the subsequent ethanol
observed at an ethanol concentration below 4%. However, with the process provided by this
invention, ethanol concentration can be higher than 5%, which is important to decrease the
In another embodiment of this invention, the said hemicellulosic sugars obtained in the
process provided are further utilized for the production of corresponding products by
biological or chemical ways; more preferably, the said hemicellulosic sugars is converted to
furfural and 5-(Hydroxymethyl)-furfural (5-HMF); most preferably, the said conversion of the
hemicellulosic sugars to furfural and 5-HMF is employed under the catalysis of the residual
organic acid and no additional mineral acids need to be added. The obtained lignin product
The oil palm EFB's main chemical components were determined according to Laboratory
30 gram of EFB was packed in a 1-L three-neck flask followed by addition of 300 ml 78%
(by weight) formic acid. The mixture was then heated to the normal boiling point at
atmospheric pressure for 1.5 hours. A mechanical stirring was employed to ensure a good
reaction. After the reaction, the mixture was filtered to obtain a solid phase with liquid
content of about 75%. The obtained solid phase was first washed by 300 m l 78% (by weight)
formic acid and then filtered to remove as much liquid as possible. After further washed by
tap water till neutrality, the solid was deformylated with 4% Ca(OH) 2 based on dry pulp
weight at 120 °C for 1 hour. The solid was washed with water till neutrality and dried for
analysis.
The main chemical components of the dried pretreated solid are shown in Table 2 . It can be
calculated according to mass balance that after the treatment, 7.9% of cellulose, 89.32% of
hemicellulose and 87.27% of lignin were respectively dissolved into the liquid phase,
solid phase. This result indicates that aqueous formic acid treatment can obtain a good
vti ti
30 gram of EFB was packed in a 1-L three-neck flask followed by addition of 300 ml 80% (by
weight) acetic acid and 0.3% (by weight) sulfuric acid as a catalyst. The mixture was then
heated to the normal boiling point at atmospheric pressure for 1.5 hours. A mechanical
stirring was employed to ensure a good reaction. After reaction, the mixture was filtered to
obtain a solid phase with liquid content of about 75%. The obtained solid phase was first
washed by 300 m l 80% (by weight) acetic acid and then filtered to remove as much liquid as
possible. After further washed by tap water till neutrality, the solid was deacetylated with 4%
Ca(OH) 2 based on dry pulp weight at 120 °C for 1 hour. The solid was washed with water till
The main chemical components of the dried pretreated solid are shown in Table 3 . It can be
calculated according to mass balance that after the treatment, 9.6% of cellulose, 73.4% of
hemicellulose and 68.7% of lignin were respectively dissolved into the liquid phase,
solid phase. This example indicates that aqueous acetic acid treatment also can obtain a
30 gram of EFB was packed in a 1-L three-neck flask followed by addition of 300 ml 50-88%
(by weight) formic acid. The mixture was then heated to the normal boiling point at
atmospheric pressure for 1.5 hours. A mechanical stirring was employed to keep a good
reaction. After the reaction, the mixture was filtered to obtain a solid phase with liquid
content of about 75%. The obtained solid phase was first washed by 300 m l aqueous formic
acid solution - the same as that used in delignification. The solid was washed by water till
The main chemical components of the dried pretreated solid are shown in Table 4 .
Generally, solid recovery, xylan and klason lignin contents decreased with increasing formic
acid concentration, and vice versa for glucan contents. Moreover, degree of formylation
different concentrations
weight) formic acid. The mixture was then heated to the normal boiling point at atmospheric
pressure for 1.5 hours. A mechanical stirring was employed to ensure a good reaction. After
the reaction, the mixture was filtered to obtain a solid phase with liquid content of about 75%.
The obtained solid phase was first washed by 300 m l 78% (by weight) formic acid and then
filtered to remove as much liquid as possible. After further washed by tap water till neutrality,
the solid was deformylated with 4% Ca(OH) 2 based on dry pulp weight at 120 °C for 1 hour.
The solid was washed with water until neutrality and stored at 4°C in a fridge prior to
enzymatic hydrolysis.
The cellulosic solid was further digested by cellulase loading of 15 FPU/g solid at 50±0.5°C
and pH 4.8 (0.1 M sodium acetate buffer) in an air-bath shaker at 130 rpm for 5 days. The
solid consistency was 2.5-10%. The enzymatic digestibility of the cellulosic solid was
defined as follows:
where w u se , wbeiiobiose and x iose are the weight of glucose, cellobiose and xylose produced
by enzymatic hydrolysis; |G i is the weight of initial total glycan (glucan+xylan) of the solid.
The results are illustrated in FIG. 2 , which indicate that the cellulosic solid could be very well
30 gram of EFB was packed in a 1-L three-neck flask followed by addition of 300 ml 78% (by
weight) formic acid. The mixture was then heated to the normal boiling point at atmospheric
pressure for 1.5 hours. A mechanical stirring was employed to ensure a good reaction. After
the reaction, the mixture was filtered to obtain a solid phase with liquid content of about 75%.
The obtained solid phase was first washed by 300 m l 78% (by weight) formic acid and then
filtered to remove as much liquid as possible. After further washed by tap water till neutrality,
the solid was deformylated with 4% Ca(OH) 2 based on dry pulp weight at 120 °C for 1 hour.
The solid was washed with water until neutrality and stored at 4°C in a fridge prior to SSF.
The SSF was performed in 150-ml Erienmeyer flasks with 50 m l liquid medium. The yeast
used was Saccharomices cerevisiae CICC 31014. The liquid medium contained 2 g/L
(NH 4)2S0 4, 5 g/L KH2P0 4, 5 g/L yeast extracts, 1 g/L MgS0 4 and 0.2 g/L CaCI 2. The
cellulosic solid was mixed with the liquid medium until the solid consistency was 15% (w/v)
solid of /3-glucansidase were then added to the mixture followed by inoculation with 10%
(v/v) yeast inocula. The SSF process was conducted at 37-38°C and 130 rpm in an air-bath
shaker. The pH value was not controlled during SSF. The experimental results are illustrated
in FIG. 3 .
A general mass balance of fractionation of EFB for ethanol, lignin and hemicellulosic syrup
The present invention may be embodied in other specific forms without departing from its
only as illustrative and not restrictive. The scope of the invention is, therefore indicated by
the appended claims rather than by the foregoing description. All changes, which come
within the meaning and range of equivalency of the claims, are to be embraced within their
scope.
CLAIMS
1. A process for fractionation of oil palm empty fruit bunch (EFB) comprising the steps
of:
a) mixing EFB with aqueous organic acid solution containing at least 50-90% by
weight of organic acid in a digester at a temperature of 50-1 60°C, thereby producing a first
mixture (1);
b) separating the said first mixture ( 1 ) into a first solid phase (2) and a first liquid
c) washing the said solid phase (2) with fresh aqueous organic acid solution to obtain
a second mixture (4), and separating the said second mixture (4) into a second solid phase
d) heating the said second solid phase (5) to recover organic acid under vacuum to
obtain a evaporated solid phase (7) and gas phase, and condensing the said gas phase to
e) washing the evaporated solid phase (7) with water to obtain a cellulosic solid and
f) mixing the first liquid stream (3) and second liquid stream (6) in a spent liquor
g) distilling the liquid stream (9) for recovering organic acid to obtain a top liquid
h) recycling the top liquid stream ( 1 0) and the third liquid stream (8) for EFB cooking
i) precipitating lignin from the said concentrated spent liquor stream ( 1 1) by adding
j) separating the said mixture stream ( 1 3) to obtain lignin product and hemicellulosic
sugars.
2. The process according to Claim 1, wherein the said mixing EFB with aqueous
3. The process according to Claim 1 and 2 , wherein the said organic acid are selected
from formic acid, acetic acid or propanoic acid; preferably, the said organic acid is formic
acid.
4. The process according to Claim 1, wherein the said separating the mixture in step b)
5. The process according to Claim 1, wherein in step c) the said organic acid is selected
from formic acid, acetic acid or propanoic acid; preferably, the said organic acid is the same
6. The process according to Claim 1, wherein the said heating the said second solid
phase (5) to recover organic acid in step d) is conducted at 20-80°C under pressure of 1-13
kPa; preferably, the recovery condition meets the demand that the said evaporated solid
7. The process according to Claim 1, wherein the said washing the evaporated solid
phase (7) with water in step e) is conducted at 30-60 °C with water-to-solid ratio of 20-5:1 .
conversion of the hemicellulosic sugars to furfural and 5-HMF is under the catalysis of the
polymer substitutes and/or is further modified for the production of derivatives such as
surfactant.
10. The process according to Claim 9 , wherein the said lignin products used as polymer
11. A process for converting the said cellulosic solid to ethanol comprising the steps of:
a) treating the said cellulosic solid with alkali solution or suspension at liquid-to-solid
b) adjusting the pH value of the said first slurry mixture obtained in step a) to 4.5-6.5
c) converting the said second slurry mixture to ethanol by adding cellulase enzyme
12. The process according to Claim 11, wherein the said alkali is selected from sodium
13. The process according to Claim 11 and 12 , wherein the said alkali is used at a
14. The process according to Claim 11, wherein the said SSF is conducted with 5-30
PCT/MY2015/05Q002
A . CLASSIFICATION O F SUBJECT MATTER
INV. D21C3/Q2 D21C3/04 D21C5/O0 D21C11/00 ClOLl/02
ADD.
According to International Patent Classification (IPC) or to both national classification and IPC
B. FIELDS SEARCHED
Minimum documentation searched (classification system followed by classification symbols)
D21C CIOL
Documentation searched other than minimum documentation to the extent that such documents are included in the fields searched
Electronic data base consulted during the international search (name of data base and, where practicable, search terms used)
Category* Citation of document, with indication, where appropriate, of the relevant passages Relevant to claim No.
/ -
X Further documents are listed in the continuation of Box C . See patent family annex.
Date of the actual completion of the international search Date of mailing of the international search report
PCT/MY2015/05Q002
C(Continuation). DOCUMENTS CONSIDERED TO BE RELEVANT
Category * Citation of document, with indication, where appropriate, of the relevant passages Relevant to claim No.