AU2017201901B2 - Method of producing saccharified solution from biomass - Google Patents
Method of producing saccharified solution from biomass Download PDFInfo
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- AU2017201901B2 AU2017201901B2 AU2017201901A AU2017201901A AU2017201901B2 AU 2017201901 B2 AU2017201901 B2 AU 2017201901B2 AU 2017201901 A AU2017201901 A AU 2017201901A AU 2017201901 A AU2017201901 A AU 2017201901A AU 2017201901 B2 AU2017201901 B2 AU 2017201901B2
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Abstract
The present invention relates to a method of
producing saccharified solution from biomass, and more
particularly to method of producing saccharified solution
from biomass, in which acetic acid generated in a biomass
pretreatment process is recycled so that additional supply
of acid is not required, and in which corrosion of
equipment by a strong acid is prevented and acetic acid
that inhibits back-end saccharification and fermentation
is removed in the front-end process so that the efficiency
of saccharification and fermentation can be increased.
1/ 1
FIG. 1
PmB
PretntlrTrs Gd nndie water
............................
.. . . . ........ .... .... .... ..... .
... .. ..
...... ...... .....
.. ..... m. .e........
.... ... ... ... ... ... ... ... ... .... . .... ... ... ... ... ......
Description
1/ 1
FIG. 1
PmB
PretntlrTrs Gd nndie water ............................ ... . . ........ .... .... .... .....
. ... .. .. ...... ........... .. ..... .e........ m.
The present invention relates to a method of
producing saccharified solution from biomass, and more
particularly to a method of producing saccharified
solution from biomass, which comprises recovering and
reusing acetic acid which is generated during biomass
pretreatment.
Cellulosic biomass has advantages in that it is
abundant, renewable and inexpensive, and due to such
advantages, the possibility of using the cellulosic
biomass as a raw material for fuel alcohol such as ethanol
or butanol is increasing. Cellulosic biomass comprises
cellulose, hemicellulose and lignin as main components,
which are strongly bonded to one another. Thus, in order
to produce a saccharified solution from the biomass in
high yield, these three components need to be separated
from one another by pretreatment.
Among the three components, cellulose has the
properties of being thermally stable and being soluble in
acid, and hemicellulose has the properties of being
thermally unstable and being soluble in acid. On the
other hand, lignin has the properties of being thermally
stable and being soluble in alkali.
In order to efficiently separate these components
from one another, which have different properties as
described above, various pretreatment processes have been
developed. Among processes that have been developed, the
most ideal pretreatment method is to selectively remove
the lignin component without loss of the cellulose
component to thereby convert the cellulosic raw material
into a form that is easy to enzymatically saccharify.
Major pretreatment methods include mechanical
crushing, alkali swelling, dilute acid hydrolysis,
hydrothermal pretreatment and steam explosion pretreatment
methods, and combinations of such methods may also be used.
Among these methods, the hydrothermal pretreatment
method can separate hemicellulose as a liquid by water
under mild conditions while allowing cellulose and lignin
to remain as a solid. It is a method that increases the
recovery of hemicellulose having low thermal stability by
the use of mild conditions.
Furthermore, in the steam explosion pretreatment
method, a raw material is charged into a pressurized
reactor and saturated stream is blown into the reactor to
cause a pressurized reaction, and then pressure is
suddenly discharged from the reactor, whereby an exploded
raw material can be obtained. In this procedure,
hydrolysis of hemicellulose may occur, or the structure of
lignin may also be broken. This method has high energy efficiency, because the raw material does not need to be finely crushed.
In selection of an efficient pretreatment one from
various pretreatment methods, a reduction in investment in
application of an actual commercial process needs to be
considered together with an increase in sugar yield. In
the case of an acid treatment method, pretreatment
efficiency can be increased by increasing pretreatment
severity, but commercialization of the process can be
difficult due to problems associated with equipment
corrosion. In addition, when acid is continuously used,
the production cost can be increased due to an increase in
operating expenditure (OPEX).
US Patent Publication No. 2014-0154759 discloses a
process for producing low-ash biomass for combustion or
pellets. The disclosed process comprises treating biomass
with acetic acid, separating the treated biomass into a
liquid portion and a solid portion, extracting low-ash
biomass from the solid portion, and removing acetic acid
from the liquid portion by evaporation, thereby producing
saccharified solution. However, it has disadvantages in
that, because acetic acid is removed by evaporation, a
large amount of cost is required for separation of acetic
acid, and because the solid portion is used for production
of a fuel for combustion, the efficiency of production of
the saccharified solution is deteriorated.
US Patent Publication No. 2015-0051385 discloses a
method for liquid/liquid separation of lignocellulosic
biomass to produce saccharified solution. The disclosed
method comprises pretreating biomass with heated acetic
acid, separating the pretreated biomass into a lignin
containing liquid portion and a cellulose-containing solid
portion, and recycling acetic acid from the liquid portion.
However, it has disadvantages in that, because heated
acetic acid is used, much cost is required to maintain
high temperature, and because distillation is used to
separate acetic acid, the overall operating cost is high.
Accordingly, the present inventors have made
extensive efforts to solve the above-described problems,
and as a result, have found that, a xylo-oligomer
containing fraction and a fraction containing cellulose
and lignin, which are produced from biomass, are separated
from each other and saccharified, after which acetic acid
in the xylo-oligomer-containing fraction is separated by
concentration and adsorption and recycled to a process for
pretreatment of biomass and a portion of the recycled
acetic acid is introduced into the saccharification
process, so that the efficiency of the pretreatment can be
increased without supply of acid, corrosion of equipment
by a strong acid can be prevented, and the efficiency of
saccharification can be increased by performing the
saccharification process after separation of acetic acid which inhibits a back-end saccharification or fermentation reaction, thereby completing the present invention.
The present invention relates to a method in which acetic
acid produced in biomass pretreatment/saccharification processes
is recycled to thereby reduce the operating cost and which
increases the efficiency with which saccharified solution is
produced from biomass.
In one aspect there is provided a method of preparing
saccharified solution from biomass, comprising: (a) firstly
pretreating biomass and separating a pretreated biomass into a
xylo-oligomer-containing fraction and a fraction containing
cellulose and lignin; (b) secondly pretreating the fraction
containing cellulose and lignin and then saccharifying by using
enzyme, thereby obtaining C6-enriched sugar; and (c) filtering
the xylo-oligomer-containing fraction and removing substances
that inhibit monomerization and fermentation by an adsorbent
resin, and then removing a considerable amount of water by
concentration process, and then monomerizing a concentrated
fraction, thereby obtaining C5-enriched sugar, wherein the C5
enriched sugar is obtained by adsorption and desorption of
acetic acid from the monomerized liquid in the step (c), and wherein acetic acid produced in a first pretreatment and/or monomerization in the step (c) is recovered in the desorption and recycled to the first pretreatment.
FIG. 1 is a flow chart showing a method of producing
saccharified solution from biomass according to an
embodiment of the present invention.
Explanation on Symbols
: acetic acid recycled to the biomass pretreatment
process
: a portion of the recycled acetic acid introduced
into the saccharification process
@: acetic acid, furfural and HMF discharged to the
outside
Unless defined otherwise, all technical and
scientific terms used herein have the same meaning as
commonly understood by one of ordinary skill in the art to
which the invention pertains. Generally, the nomenclature
used herein and the experiment methods, which will be
described below, are those well known and commonly
employed in the art.
In an example of the present invention, biomass was
pretreated, and then a xylo-oligomer-containing fraction and a fraction containing cellulose and lignin were separated from each other and subjected to a saccharification reaction. The xylo-oligomer-containing fraction was filtered and passed through an adsorbent resin to remove fermentation-inhibiting substances such as fine powder and inorganic substances, after which it was concentrated to remove a considerable amount of water and saccharified through a monomerization process. After monomerization, the saccharified liquid was subjected to adsorption and desorption processes to separate acetic acid which was then recycled to the biomass pretreatment process. As a result, it was found that high saccharification efficiency was achieved without additional supply of acid and that the saccharification efficiency was increased as a result of performing the saccharification process after separation of acetic acid which inhibits a back-end saccharification or fermentation process.
Therefore, the present invention is directed to a
method of preparing saccharified solution from biomass,
comprising: (a) firstly pretreating biomass and separating
a pretreated biomass into a xylo-oligomer-containing
fraction and a fraction containing cellulose and lignin;
(b) secondly pretreating the fraction containing cellulose
and lignin and then saccharifying by using enzyme, thereby
obtaining C6-enriched sugar; and (c) filtering the xylo
oligomer-containing fraction and removing substances that inhibit monomerization and fermentation by an adsorbent resin, and then removing a considerable amount of water by concentration process, and then monomerizing a concentrated fraction, thereby obtaining C5-enriched sugar, wherein the C5-enriched sugar is obtained by adsorption and desorption of acetic acid from the monomerized liquid in the step (c), and wherein acetic acid produced in a first pretreatment and/or monomerization in the step (c) is recovered in the desorption and recycled to the first pretreatment.
FIG. 1 is an overall schematic view showing a
process of producing saccharified solution from biomass
according to the present invention.
1. Process for pretreatment and solid-liquid
separation of biomass (step (a))
In the first step of the method for producing
saccharified solution according to the present invention,
biomass is first pretreated (pretreatment A in FIG. 1) and
is solid-liquid separated into a xylo-oligomer-containing
fraction (pretreated fraction (PTL)) and a fraction
(pretreated biomass (PTB)) containing cellulose and lignin.
2. Saccharification process
2-1. Process for saccharification of PTB (step (b))
In the first step of the saccharification process in
the method for producing saccharified solution according
to the present invention, the fraction (PTB) containing cellulose and lignin, separated in step (a), may be pretreated (pretreatment B in FIG. 1), and then enzymatically saccharified to obtain C6 enriched-sugar.
2-2. Process for saccharification of PTL (step (c))
In the second step of the saccharification process
in the method for producing saccharified solution
according to the present invention, the xylo-oligomer
containing fraction (PTL), separated in step (a), may be
filtered and passed through an adsorbent resin to remove
fine powder and fermentation-inhibiting substances such as
cations, HMF, furfural, etc., and it may be concentrated
to remove a considerable amount of water, and then
saccharified by a physical/chemical method. Then, the
saccharified material may be subjected to an
adsorption/desorption process for AA recovery, thereby
obtaining high-purity C5-enriched sugar.
Herein, the considerable amount of water corresponds
to 40-50 vol% of the total volume of water. The amount of
water removed may preferably be 10-80 vol%, more
preferably 40-50 vol%.
Because the PTL contains a large amounts of
microbial fermentation-inhibiting components (mainly
acetic acid, HMF, and furfural), concentration and
adsorption processes for removing these components are
required.
Acetic acid (low-concentration acetic acid obtained
by concentration and high-concentration acetic acid
separated by adsorption) recovered in these processes may
be introduced into the pretreatment process to thereby
increase pretreatment efficiency.
The present invention may use a portion of acetic
acid derived from biomass that continues to be produced in
the pretreatment process, but not strong acid such as
sulfuric acid, hydrochloric acid, phosphoric acid or the
like that has been widely used in an existing pretreatment
process. The pretreatment process that is used in the
present invention is an economical and efficient
pretreatment process in which the severity of hydrothermal
treatment (a function of temperature, time and pH) is
increased while acetic acid is produced from the acetyl
group of hemicelluloses that is a component of partially
recycled biomass, thereby increasing the pretreatment
effect.
The method for producing saccharified solution
according to the present invention may further comprise a
step of supplying condensed water, separated in the
concentration process in step (c), to the desorption
process so that the supplied condensed water is used as
water for desorption in the processes for adsorption and
desorption of acetic acid.
As shown in FIG. 1, when the concentration process
is carried out after filtration and the adsorption process for removal of impurities in step (c), there are advantages in that the amount of heat required for heating in the monomerization process can be reduced and the throughput of the monomerization process can be reduced, thereby reducing capital expenditure (CAPEX). Furthermore, condensed water generated in the concentration process can be supplied to the desorption process, and may be used for desorption after heating, but is not limited thereto.
Herein, the concentration of acetic acid separated in the
desorption process is preferably 5-30 w%.
In the concentration process, acetic acid is
separated by evaporation with water. For this reason,
acetic acid that is separated in the concentration process
is diluted in water, and thus is present at a relatively
low concentration. In the desorption process, acetic acid
and impurities are adsorbed and discharged independently
of water, and thus a relatively high concentration of
acetic acid is separated.
In the present invention, a portion of the acetic
acid recycled may be introduced into the monomerization
process of step (c). In the PTL treatment process, the
oligomer is converted to C5-enriched sugar by
monomerization. When acid is supplied to the
monomerization process, the rate of conversion to C5
enriched sugar will increase. Thus, as shown in FIG. 1, a
portion of acetic acid recovered from the desorption
process may be introduced into the monomerization process to thereby increase the conversion rate of the monomerization reaction. Although the amount of acetic acid recovered and reused varies depending on the acetyl content of biomass, the amount of acetic acid generated is
0.17-1.67 ton/hr when biomass is treated in an amount of
49 dry ton/day. The ratio of the amount of acetic acid
recycled to the pretreatment process (a in FIG. 1) to the
amount of acetic acid discharged to the outside (@ in FIG.
1) is 90:10-98:2, which corresponds to a concentration of
5-30%. When low-concentration acetic acid (AA) is applied,
severity can be increased by controlling reaction
temperature and reaction time, thereby suppressing the
production of inhibitors at low pH, and when high
concentration acetic acid (AA) is applied, severity can be
reduced by controlling reaction temperature and reaction
time, thereby reducing the amount of steam used and
increasing productivity. This makes efficient production
possible. A portion of the recovered acetic acid (AA) may
be introduced into the front end of the PTL monomerization
process ("b" in FIG. 1) to thereby increase the efficiency
of monomerization of the PTL. Herein, the weight of the
AA that is introduced is preferably adjusted such that the
acetic acid (AA) concentration of the front-end stream of
the PTL monomerization process is 30-50%.
Moreover, the acetic acid recovered may be
completely recycled to the pretreatment process, and if
the concentration of acetic acid in the production system of the present invention increases to cause side reactions, a portion or all of the acetic acid may be discharged to the outside. However, the total amount of acetic acid which is recycled to the pretreatment A process, acetic acid which is introduced into the monomerization process, and acetic acid which is discharged to the outside, should be the same as the amount of acetic acid which is recovered from the acetic acid (AA) adsorption process, in order to prevent the accumulation of acetic acid in the production system to thereby minimize side reactions.
In the present invention, the concentration in step
(c) may be vacuum concentration. The concentration
process is a process of evaporating an object using heat.
Thus, as the boiling point of the object is lower,
concentration may be achieved using a smaller amount of
heat, and for this reason, the boiling point of the object
is preferably lowered. Accordingly, the concentration
process is preferably performed in a vacuum so that the
amount of heat consumed can be minimized. More preferably,
the concentration process may be performed at a pressure
of 10-300 Torr.
In the present invention, the adsorption of step (c)
may use activated carbon as an adsorbent. As the
adsorbent used in the adsorption process of the present
invention, any adsorbents can be used without any
limitation as long as they adsorb acetic acid, but
activated carbon, zeolite, silica gel, aluminum sulfate or an ion exchange resin such as a cation exchange resin is preferably used which is stable under acid conditions and does not react with water.
Hereinafter, the present invention will be described
in further detail with reference to examples. It will be
obvious to a person having ordinary skill in the art that
these examples are illustrative purposes only and are not
to be construed to limit the scope of the present
invention.
Example 1: Production of Saccharified Solution from
Biomass through Recycling of Acetic Acid
As shown in FIG. 1, biomass was first hydrothermally
pretreated at a temperature of 185°C for 5 minutes, and
then separated into a fraction containing cellulose and
lignin and a xylo-oligomer-containing fraction. The
fraction containing cellulose and lignin was treated
mechanically, pretreated, and then saccharified to produce
C6-entiched sugar. The xylo-oligomer-containing fraction
was filtered and passed through an adsorbent resin to
remove fine powder and cations, which inhibits the
corresponding process, after which it was concentrated to
remove a considerable amount of water and subjected to a
monomerization process. After the monomerization process,
the resulting material was subjected to adsorption and desorption processes using activated carbon to separate and recover acetic acid (AA). Herein, condensed water obtained in the concentration process was used as water for desorption. Furfural and HMF were separated and removed from impurities separated by the desorption process, and the remaining high-concentration (70 wt%) acetic acid was recovered and recycled to the first pretreatment process. A portion of the acetic acid recycled was introduced into the monomerization process.
Although the amount of acetic acid recovered and
reused varies depending on the acetyl content of biomass,
the amount of acetic acid generated is 0.276 ton/hr when
biomass is treated in an amount of 49 dry ton/day. The
ratio of the amount of acetic acid recycled (a+b) to the
amount of acetic acid discharged to the outside (@ ) among
the acetic acid adsorbed in the adsorption process is
90:10-98:2, which corresponds to a concentration of 5-30%.
When low-concentration acetic acid (AA) was applied,
severity can be increased by controlling reaction
temperature and reaction time, thereby suppressing the
production of inhibitors at low pH, and when high
concentration acetic acid (AA) is applied, severity can be
reduced by controlling reaction temperature and reaction
time, thereby reducing the amount of steam used and
increasing productivity. This made efficient production
possible. A portion of the recovered acetic acid (AA) was
introduced into the front end of the PTL monomerization process in order to increase the efficiency of monomerization of the PTL. Specifically, the weight of recovered acetic acid (AA) into the front end of PTL monomerization process was controlled such that the acetic acid (AA) concentration of the front-end stream of the PTL monomerization process would be 30-50 wt%.
According to the Example of the present invention,
acetic acid generated in the pretreatment process was
recovered and concentrated, and the concentrated acetic
acid was introduced into the pretreatment process to
increase the severity of the process, thereby increasing
the pretreatment effect. According to the present
invention, because acetic acid generated in the
pretreatment process is used, a separate chemical cost is
not incurred, and thus the operating expenditure does not
increase, and because a weak acid, not a strong acid, is
used, equipment corrosion does not occur, and thus
investment in plant construction decreases. In addition,
because acetic acid that acts as an inhibitor in back-end
saccharification and fermentation processes is removed in
the front-end process, the efficiency of saccharification
and fermentation can be increased. Furthermore, in the
process of recovering acetic acid, other impurities such
as furfural and HMF, etc., which are high-value-added
compounds, can also be recovered.
In the method of producing saccharified solution from
biomass according to the present invention, acetic acid is
recycled, and thus additional supply of acid is not
required in pretreatment of biomass and monomerization of
pretreated liquid. Furthermore, saccharification and
fermentation processes are performed after separation of
acetic acid that inhibits a back-end saccharification or
fermentation reaction, and thus saccharification
efficiency and fermentation efficiency increase.
Accordingly, the present invention is useful for efficient
production of saccharified solution.
Although the present invention has been described in
detail with reference to the specific features, it will be
apparent to those skilled in the art that this description
is only for a preferred embodiment and does not limit the
scope of the present invention. Thus, the substantial
scope of the present invention will be defined by the
appended claims and equivalents thereof.
_ 17_
Claims (8)
1. A method of preparing saccharified solution from biomass,
comprising:
(a) firstly pretreating biomass and separating a
pretreated biomass into a xylo-oligomer-containing fraction and
a fraction containing cellulose and lignin;
(b) secondly pretreating the fraction containing cellulose
and lignin and then saccharifying by using enzyme, thereby
obtaining C6-enriched sugar; and
(c) filtering the xylo-oligomer-containing fraction and
removing substances that inhibit monomerization and fermentation
by an adsorbent resin, and then removing a considerable amount
of water by concentration process, and then monomerizing a
concentrated fraction, thereby obtaining C5-enriched sugar,
wherein the C5-enriched sugar is obtained by adsorption
and desorption of acetic acid from the monomerized liquid in the
step (c), and
wherein acetic acid produced in the step (a) or (c) is
recovered in the desorption and recycled to the step (a).
2. The method of claim 1, further comprising supplying
condensed water produced in the concentration process in the
step (c), to the desorption so as to use as water for desorption
in adsorption and desorption of acetic acid.
3. The method of claim 1, wherein a concentration of acetic
acid separated in the desorption is 5-30 w%.
4. The method of claim 1, wherein a portion of recycled
acetic acid is introduced into the monomerization of the step
(c).
5. The method of claim 4, wherein a ratio of an amount of
recycled acetic acid to a first pretreatment to an amount of
discharged acetic acid is 90:10-98:2, and acetic acid is
introduced so as to be 30-50% of the acetic acid concentration
of a front-end stream of the monomerization.
6. The method of claim 1, wherein the concentration process
in the step (c) is vacuum concentration.
7. The method of claim 6, wherein the vacuum concentration
is performed at a pressure of 10-300 Torr.
8. The method of claim 1, wherein the adsorption of the
step (c) uses the adsorbent resin selected from the group
consisting of activated carbon, zeolite, silica gel, aluminum
sulfate and a cation exchange resin.
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| US20140113812A1 (en) * | 2009-12-11 | 2014-04-24 | Beta Renewables S.P.A. | Regenerative purification of a pretreated biomass stream |
| US20140227742A1 (en) * | 2011-09-23 | 2014-08-14 | Archer Daniels Midland Company | C1-C2 Organic Acid Treatment of Lignocellulosic Biomass to Produce Acylated Cellulose Pulp, Hemicellulose, Lignin and Sugars and Fermentation of the Sugars |
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| CA2782522A1 (en) * | 2009-12-11 | 2011-06-16 | Beta Renewables S.P.A. | Regenerative purification of a pretreated biomass stream |
| BR112014025714A8 (en) * | 2012-04-30 | 2018-02-06 | Renmatix Inc | PROCESS INVOLVING THE LIQUEFACTION OF A BIOMASS SYRUP BY TREATMENT IN HOT COMPRESSED WATER (HCW) |
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| US20140113812A1 (en) * | 2009-12-11 | 2014-04-24 | Beta Renewables S.P.A. | Regenerative purification of a pretreated biomass stream |
| US20140227742A1 (en) * | 2011-09-23 | 2014-08-14 | Archer Daniels Midland Company | C1-C2 Organic Acid Treatment of Lignocellulosic Biomass to Produce Acylated Cellulose Pulp, Hemicellulose, Lignin and Sugars and Fermentation of the Sugars |
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| Title |
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| Wickramasinghe et al, "Adsorptive membranes and resins for acetic acid removal from biomass hydrolysates", Desalination, 2008, Vol. 234, pp. 144–151. * |
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| KR20170126291A (en) | 2017-11-17 |
| AU2017201901A1 (en) | 2017-11-23 |
| KR102584351B1 (en) | 2023-10-05 |
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