Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
REF-1401016
PROCESS OF PRODUCING HIGHLY PURE ALKYL ACETATES
TECHNICAL FIELD
[0001] The present disclosure is generally related to a process of producing
alkyl acetates,
particularly to a process of producing highly pure alkyl acetates using the
reactive extraction
system, and more particularly to a process of producing highly pure methyl and
ethyl acetate.
BACKGROUND
[0002] One of the most common commercial production processes of alkyl
acetates especially
methyl and ethyl acetate is the direct esterification of methanol/ ethanol
with acetic acid with an
acid catalyst. However, this process has encountered difficulty in driving the
esterification
reactions to completion, thereby resulting in acetate products contaminated
with unreacted
alcohols, which can result in a relatively expensive separation system to
purify the product.
Accordingly, the improvements in the production of acetates have dealt mainly
with finding
alternative reaction processes to produce pure acetates.
[0003] Other improvements for alkyl acetates production such as reactive
distillation or extractive
distillation systems need several complementary purification steps that are
expensive and highly
energy-consuming. Consequently, there is a need to develop a cost-effective
and highly robust
industrial process for the production of highly pure alkyl acetates using low-
cost equipment with
safe reaction conditions without any need for high temperature, and high
pressure. Moreover, there
is a need for an efficient process for producing highly pure alkyl acetates
with high yield and the
ability to recycle the extraction solvent.
SUMMARY
[0004] This summary is intended to provide an overview of the subject matter
of the present
disclosure, and is not intended to identify essential elements or key elements
of the subject matter,
nor is it intended to be used to determine the scope of the claimed
implementations. Its sole purpose
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is to present some concepts of one or more aspects in a simplified form as a
prelude to the more
detailed description that is presented later. The proper scope of the present
disclosure may be
ascertained from the claims set forth below in view of the detailed
description below and the
drawings.
[0005] In one general aspect, the present disclosure describes an exemplary
process of producing
highly pure alkyl acetates. In one exemplary embodiment, the process may
include producing a
first mixture by mixing acetic acid, a C1-C2 aliphatic alcohol, and an acid
catalyst in first mixer,
and then atomizing the first mixture using a first atomizer. In one exemplary
embodiment,
producing Cl-C2 alkyl acetate with at least 95% purity may include producing a
first reaction
product comprising a Cl-C2 alkyl acetate and water in the first reactive
extraction column, wherein
the conversion of the Cl-C2 aliphatic alcohol in the atomized first mixture to
the Cl-C2 alkyl
acetate is at maximum 70%. In one exemplary embodiment, removing high-purity
C1-C2 alkyl
acetates produced in the first reactive extraction column may include removing
an overhead stream
from the first reactive extraction column by contacting the first reaction
product with a first
extraction solvent, wherein the overhead stream comprises a first organic
phase comprising 10%
wt. C1-C2 alkyl acetate produced in the first reaction product that is
dissolved in the first extraction
solvent. In one exemplary embodiment, producing C 1 -C2 alkyl acetate with at
least 95% purity
may include separating the first organic phase into C1-C2 alkyl acetate with
at least 95% purity
and the first extraction solvent using the first distillation unit, wherein
separating the first organic
phase into C1-C2 alkyl acetate with at least 95% purity and the first
extraction solvent using the
first distillation unit comprises regenerating the first extraction solvent.
In one exemplary
embodiment, the regenerated first extraction solvent is recycled back to the
first reactive extraction
column.
[0006] In one exemplary embodiment, producing C1-C2 alkyl acetate with at
least 95% purity
may include transferring a first residual compound in the first reactive
extraction column to a
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second atomizer, wherein the first residual compound comprising unreacted
acetic acid, the Cl-
C2 aliphatic alcohol, the acid catalyst, water, and C1-C2 alkyl acetate
produced in the first reaction
product are atomized. In one exemplary embodiment, producing C1-C2 alkyl
acetate with at least
95% purity may include producing a second reaction product comprising a C1-C2
alkyl acetate
and water in the second reactive extraction column, wherein the conversion of
the Cl-C2 aliphatic
alcohol in the atomized first residual compounds to the Cl-C2 alkyl acetate is
at maximum 90%.
In one exemplary embodiment, removing high-purity Cl-C2 alkyl acetates
produced in the second
reactive extraction column may include removing an overhead stream from the
second reactive
extraction column by contacting the second reaction product with the second
extraction solvent,
wherein the overhead stream comprises a second organic phase comprising 10%
wt. C1-C2 alkyl
acetate produced in the second reaction product that is dissolved in the
second extraction solvent.
In one exemplary embodiment, producing C1-C2 alkyl acetate with at least 95%
purity may
include separating the second organic phase into C1-C2 alkyl acetate with at
least 95% purity and
the second extraction solvent using the second distillation unit, wherein
separating the second
organic phase into C1-C2 alkyl acetate with at least 95% purity and the second
extraction solvent
using the second distillation unit comprises regenerating the second
extraction solvent. In one
exemplary embodiment, the regenerated second extraction solvent is recycled
back to the second
reactive extraction column.
[0007] In one exemplary embodiment, producing C 1 -C2 alkyl acetate with at
least 95% purity
may include transferring a second residual compound in the second reactive
extraction column to
a second mixer, wherein the second residual compounds comprising unreacted
acetic acid, the Cl-
C2 aliphatic alcohol, the acid catalyst, water, and C1-C2 alkyl acetate
produced in the second
reaction product. In one exemplary embodiment, producing C1-C2 alkyl acetate
with at least 95%
purity may include producing a second mixture by adding a 10% wt. salt
solution to the second
mixer, wherein the second residual compound and salt solution are mixed, and
then atomizing the
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second mixture using a third atomizer. In one exemplary embodiment, the salt
solution may be
prepared using a salt having 10% wt. solubility in water. Salts may include,
but are not limited to,
calcium chloride, sodium sulfate, sodium acetate, potassium chloride. In one
exemplary
embodiment, producing C1-C2 alkyl acetate with at least 95% purity may include
contacting the
atomized second mixture with the third extraction solvent in the third
reactive extraction column,
wherein the Cl-C2 alkyl acetate remaining in the atomized second mixture is
extracted by the third
extraction solvent. In one exemplary embodiment, producing Cl-C2 alkyl acetate
with at least
95% purity may include removing an overhead stream from the third reactive
extraction column,
wherein the overhead stream comprises a third organic phase comprising 10% wt.
C1-C2 alkyl
acetate remained in the atomized second mixture that is dissolved in the third
extraction solvent.
In one exemplary embodiment, producing C1-C2 alkyl acetate with at least 95%
purity may
include separating the third organic phase into C1-C2 alkyl acetate with at
least 95% purity and
the third extraction solvent using the third distillation unit, wherein
separating the third organic
phase into C1-C2 alkyl acetate with at least 95% purity and the third
extraction solvent using the
third distillation unit comprises regenerating the third extraction solvent.
In one exemplary
embodiment, the regenerated third extraction solvent is recycled back to the
third reactive
extraction column.
[0008] This Summary may introduce a number of concepts in a simplified format;
the concepts
are further disclosed within the "Detailed Description" section. This Summary
is not intended to
configure essential/key features of the claimed subject matter, nor is
intended to limit the scope of
the claimed subject matter.
BRIEF DESCRIPTION OF THE DRAWINGS
[0009] The present disclosure is disclosed more in detail with reference to
the drawings in which:
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[00010] FIG. 1 is a schematic piping and instrumentation diagram
(P&ID) of producing high-
purity C1-C2 alkyl acetate, consistent with one or more exemplary embodiments
of the present
disclosure.
[00011] FIG. 2 shows a flowchart of an exemplary process for
producing high-purity C1-C2
alkyl acetate in first reactive extraction column, consistent with one or more
exemplary
embodiments of the present disclosure.
[00012] FIG. 3 shows a flowchart of an exemplary process for
producing high-purity C1-C2
alkyl acetate in second reactive extraction column, consistent with one or
more exemplary
embodiments of the present disclosure.
[00013] FIG. 4 shows a flowchart of an exemplary process for
producing high-purity C1-C2
alkyl acetate in third reactive extraction column, consistent with one or more
exemplary
embodiments of the present disclosure.
[00014] It is understood that the following description and
references to the figures concern
exemplary embodiments of the present disclosure and shall not be limiting the
scope of the claims.
DETAILED DESCRIPTION
[00015] In the following detailed description, numerous specific
details are set forth by way
of examples in order to provide a thorough understanding of the relevant
teachings. However, it
should be apparent that the present teachings may be practiced without such
details. In other
instances, well-known methods, procedures, components, and/or circuitry have
been described at
a relatively high-level, without detail, in order to avoid unnecessarily
obscuring aspects of the
present teachings.
[00016] The following detailed description is presented to enable
a person skilled in the art
to make and use the methods and devices disclosed in exemplary embodiments of
the present
disclosure. For purposes of explanation, specific nomenclature is set forth to
provide a thorough
understanding of the present disclosure. However, it will be apparent to one
skilled in the art that
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these specific details are not required to practice the disclosed exemplary
embodiments.
Descriptions of specific exemplary embodiments are provided only as
representative examples.
Various modifications to the exemplary implementations will be readily
apparent to one skilled in
the art, and the general principles defined herein may be applied to other
implementations and
applications without departing from the scope of the present disclosure. The
present disclosure is
not intended to be limited to the implementations shown but is to be accorded
the widest possible
scope consistent with the principles and features disclosed herein.
[00017]
Disclosed herein is an exemplary cost-effective and straightforward
reactive
extraction system and process for producing highly pure C1-C2 alkyl acetates
through an
esterification reaction. "Highly pure alkyl acetate" and "high-purity alkyl
acetate" may refer to at
least 95% alkyl acetate by weight. In an exemplary implementation, the
reactive extraction system
may be used for producing highly pure C1-C2 alkyl acetates, which may not only
decrease the
costs of the common methods but may also obviate the need for high temperature
and high
pressure, which may be considered as industrial obstacles. In one or more
exemplary
implementations, an exemplary C1-C2 alkyl acetate may be produced through an
esterification
reaction of an exemplary C1-C2 aliphatic alcohol with acetic acid in the
presence of an exemplary
acid catalyst at temperatures between 20 C and 35 C. An exemplary process
may further
comprise the separation of an exemplary produced C1-C2 alkyl acetate from one
or more
exemplary reactants and byproducts through dissolving C1-C2 alkyl acetate in
an exemplary
extraction solvent. An exemplary process may be considered as an efficient
process for producing
C 1-C2 alkyl acetates with high-purity by distilling the solution containing
the produced Cl-C2
alkyl acetate and extraction solvent. An exemplary process may allow for a one-
step Cl-C2 alkyl
acetate production process, which may be advantageous relative to other
processes that require
further steps to purify the Cl-C2 alkyl acetates. Each of these advantages may
be provided in a
process that may also be less expensive than alternative processes by Cl-C2
alkyl acetates
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production using the esterification reactions. Furthermore, as advantages of
the integration of the
reaction and extraction, esterification equilibrium limitations may be
overcome, and the reaction
may be carried out at temperatures between 20 C and 35 C, under atmospheric
pressure. In one
or more exemplary processes, the extraction solvent may be recycled into an
exemplary reaction
column. According to one or more exemplary embodiments, C1-C2 alkyl acetates
may be
produced using an exemplary continuous, semi-continuous, or batch processes.
Using one or more
exemplary embodiments of the processes, high-purity methyl acetate and/ or
ethyl acetate may be
produced.
[00018] FIG. 1 is a schematic piping and instrumentation diagram
(P&ID) 100 of producing
high-purity C1-C2 alkyl acetates, consistent with one or more exemplary
embodiments of the
present disclosure. Exemplary P&ID 100 may include reactive extraction column
104, reactive
extraction column 114, and reactive extraction column 134 for producing high-
purity C1-C2 alkyl
acetates through an esterification reaction. "Reactive extraction column" may
refer to a reaction
column in which both reaction and extraction are performed. An exemplary
reactive extraction
column may have trays, packing, or some other type of complex internal
structure. Examples of
reactive extraction columns may include scrubbers, strippers, absorbers,
adsorbers, packed
columns, and columns having valve, sieve, or other types of trays. Exemplary
reactive extraction
columns may employ weirs, downspouts, internal baffles, temperature control
elements, and/or
pressure control elements. In one or more exemplary embodiments, C1-C2 alkyl
acetates may be
produced via an esterification reaction of the acetic acid with an exemplary
C1-C2 aliphatic
alcohol in the presence of an acid catalyst in one or more reactive extraction
columns.
"Esterification reaction" may refer to a process of producing an ester (RCOOR)
and water by
combining a carboxylic acid with an alcohol.
[00019] In further detail with regards to an exemplary system and
process of producing high-
purity esters in first reactive extraction column 104, FIG. 2 shows a
flowchart of
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exemplary process 200 for producing high-purity C1-C2 alkyl acetate in first
reactive extraction
column 104, consistent with one or more exemplary embodiments of the present
disclosure. An
exemplary process 200 may include producing the first mixture by mixing acetic
acid, a C1-C2
aliphatic alcohol, and an acid catalyst (step 202), atomizing the first
mixture using an atomizer
(step 204), pumping the first extraction solvent to the first reactive
extraction column (step 206),
pumping the atomized first mixture to the first reactive extraction column
(step 208), extracting
the first organic phase comprising 10% wt. Cl-C2 alkyl acetate produced in the
first reactive
extraction column that is dissolved in the first extraction solvent (step
210), distilling the first
organic phase to obtain the CI-C2 alkyl acetate with at least 95% purity and
regenerate the first
extraction solvent (step 212), transferring the first residual compounds in
the first reactive
extraction column to the second atomizer (step 214), and recycling back the
regenerated first
extraction solvent to the first reactive extraction column (step 216).
[00020] Referring to FIG. 1 and FIG. 2, in one or more exemplary
embodiments, step 202
may include producing the first mixture by mixing acetic acid, a C I-C2
aliphatic alcohol, and an
acid catalyst. In an exemplary em.bodim.ent, forming the first mixture may
include mixing the
reactants in a first mixer at controlled temperatures in the range of 20 C
and 35 C, results in
preparing the first mixture. In one or more exemplary embodiments, mixing a C1-
C2 aliphatic
alcohol with acetic acid may include mixing a C1-C2 aliphatic alcohol with
acetic acid with a
molar ratio between 1.1 to 1.3 in the presence of at least 1% wt. acid
catalyst based on acetic acid.
Acid catalyst may include, but is not limited to, sulfuric acid. In one
exemplary embodiment,
mixing a C1-C2 aliphatic alcohol with acetic acid may include mixing a C1-C2
aliphatic alcohol
with acetic acid with a molar ratio 1.2 in the presence of at least 1% wt.
acid catalyst based on
acetic acid.
[00021] In one or more exemplary embodiments, step 204 may
include atomizing the first
mixture using an atomizer. In one exemplary embodiment, atomizing the first
mixture using an
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atomizer may include transferring the first mixture to a first atomizer for
increasing the contact
area of the reactants mixture droplet via decreasing their size via atomizing
the mixture.
"Atomizer" may refer to a device for converting the substances into very fine
particles or droplets.
[00022] In one or more exemplary embodiments, step 206 may
include pumping the first
extraction solvent to the first reactive extraction column. In one exemplary
embodiment, pumping
the first extraction solvent to the first reactive extraction column may
include pumping the first
extraction solvent into first reactive extraction column 104. The
esterification reaction for C1-C2
alkyl acetate production may initiate and carry on in first reactive
extraction column 104 in the
presence of a sufficient amount of the first extraction solvent which is
adjusted regarding the level
of the compounds in first reactive extraction column 104. Thereby, the need
for much first
extraction solvent may be balanced by a dosing pump via pumping the first
extraction solvent into
first reactive extraction column 104. The first extraction solvent may have a
boiling point between
temperatures of 140 C and 220 C and a density between 0.78 g/cm3 and 0.8
g/cm3. The first
extraction solvent may include, but is not limited to, a combination of 5% wt.
aromatic compound,
and 95% wt. of a mixture of naphthenic and paraffinic compounds, wherein the
mixture of the
naphthenic compound and the paraffinic compound has a weight ratio (the
naphthenic compound:
the paraffinic compound) ranging from 20:80 to 80:20.
[00023] In one or more exemplary embodiments, step 208 may
include pumping the atomized
first mixture to the first reactive extraction column. In one exemplary
embodiment, pumping the
atomized first mixture to the first reactive extraction column may include
feeding atomized first
mixture feed 101 to first reactive extraction column 104 from the top of first
reactive extraction
column 104 as an overhead stream. In one exemplary embodiment, the first
mixture may be
transferred to first reactive extraction column 104 using a pump.
[00024] In one or more exemplary embodiments, an exemplary C1-C2
alkyl acetate may be
produced in first reactive extraction column 104 through an esterification
reaction at temperatures
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between 20 C and 35 C, and atmospheric pressure, results in producing the
first reaction product.
In one exemplary embodiment, the first reaction product in the first reactive
extraction column
104 comprises a Cl-C2 alkyl acetate and water. An exemplary produced Cl-C2
alkyl acetate may
be incompatible with the residual reactants, containing acetic acid and
aliphatic alcohol, and water
as the byproduct of the esterification reaction. On the contrary, the first
extraction solvent may be
designed to be as much as compatible with the produced C 1 -C2 alkyl acetate.
In one or more
exemplary embodiments, step 210 may include extracting the first organic phase
comprising 10%
wt. C 1 -C2 alkyl acetate produced in the first reactive extraction column
that is dissolved in the
first extraction solvent. Extracting the first organic phase comprising 10%
wt. C1-C2 alkyl acetate
produced in the first reactive extraction column that is dissolved in the
first extraction solvent may
include extracting an exemplary first organic phase comprising produced Cl-C2
alkyl acetate
dissolved in the first extraction solvent, in which the produced Cl-C2 alkyl
acetate may be
separated from the other compounds in first reactive extraction column 104 via
dissolving in the
first extraction solvent and leaving the reaction environment from the top of
first reactive
extraction column 104 as an overhead stream 106. In one exemplary embodiment,
the conversion
of the Cl-C2 aliphatic alcohol in the atomized first mixture to the Cl-C2
alkyl acetate in the first
reactive extraction column 104 is at maximum 70%. In one or more exemplary
embodiments,
overhead product stream 106 may comprise 10% wt. C1-C2 alkyl acetate produced
in column 104
in the first reaction product dissolved in the first extraction solvent.
[00025]
In one or more exemplary embodiments, step 212 may include
distilling the first
organic phase to obtain the Cl -C2 alkyl acetate with at least 95% purity and
regenerate the first
extraction solvent. In one or more exemplary embodiments, distilling the first
organic phase to
obtain the C1-C2 alkyl acetate with at least 95% purity and regenerate the
first extraction solvent
may include transferring the first organic phase as an overhead stream 106
into an exemplary first
atmospheric distillation unit 107 as a bottoms stream, wherein the high-purity
C1-C2 alkyl acetate
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and first extraction solvent may be separated. An exemplary high-purity Cl-C2
alkyl acetate 109
may be collected through an overhead stream from the top of first distillation
unit 107. In an
embodiment, overhead product stream 109 may comprise greater than about 90%,
greater than
about 95%, greater than about 96%, greater than about 97%, greater than about
98%, greater than
about 99%, or greater than about 99.5% Cl-C2 alkyl acetate by weight.
[00026] In one or more exemplary embodiments, step 214 may
include transferring the first
residual compounds in the first reactive extraction column to the second
atomizer. In one
exemplary embodiment, transferring the first residual compounds in the first
reactive extraction
column to the second atomizer may include evacuating and transferring an
exemplary first
remaining bottoms products or first residual products of first reactive
extraction column 104 from
first reactive extraction column 1.04 as a bottoms stream 11.0 into the next
system and process of
the producing high-purity Cl-C2 alkyl acetate. An exemplary first remaining
bottoms products or
first residual products of first reactive extraction column 104 may be
comprised the Cl-C2 alkyl
acetate produced in the column 104, along with unreacted aliphatic alcohol,
acetic acid, acid
catalyst, and potentially any side products produced by the esterification
reaction such as water.
In one or more exemplary embodiments, the conversion of the esterification
reaction of the CI-C2
alkyl acetate production in the first reactive extraction column 104 may be
about 65% to 70%. It
means that a portion of the reactants may remain unreacted, transferred to
another reactive
extraction system for producing high-purity C1-C2 alkyl acetate.
[00027] In one or more exemplary embodiments, step 216 may
include recycling back the
regenerated first extraction solvent to the first reactive extraction column.
In one exemplary
embodiment, separating the first organic phase into C1-C2 alkyl acetate with
at least 95% purity
and the first extraction solvent using the first distillation unit comprises
regenerating the first
extraction solvent. In one exemplary embodiment, recycling back the
regenerated first extraction
solvent to the first reactive extraction column may include recycling back the
first extraction
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solvent, which is regenerated in first distillation unit 107 (step 212), into
first reactive extraction
column 104 as a bottoms stream 108.
[00028]
In further detail with respect to an exemplary system and process of
producing high-
purity C1-C2 alkyl acetate in second reactive extraction column 114, FIG. 3
shows a flowchart of
an exemplary process 300 for producing high-purity Cl-C2 alkyl acetate in
second reactive
extraction column 114, consistent with one or more exemplary embodiments of
the present
disclosure. An exemplary process 300 may include pumping the second extraction
solvent to the
second reactive extraction column (step 302), pumping the atomized first
residual compounds to
the second reactive extraction column (step 304), extracting the second
organic phase comprising
10% wt. CI-C2 alkyl acetate produced in the second reactive extraction column
that is dissolved
in the second extraction solvent (step 306), distilling the second organic
phase to obtain the Cl-
C2 alkyl acetate with at least 95% purity and regenerate the second extraction
solvent (step 308),
transferring the second residual compounds in the second reactive extraction
column to a second
mixer (step 310), and recycling back the regenerated second extraction solvent
to the second
reactive extraction column (step 312).
[00029]
Referring to FIG. 1 and FIG. 3, exemplary process 300 may include
sending an
exemplary first residual compounds, as bottoms stream 110, from an exemplary
first reactive
extraction column 104 (see FIG. 1) to an exemplary second reactive extraction
column
114 through feed stream 111 that may comprise first residual compounds 110 and
co-feed stream
144. In an exemplary embodiment, first residual compound 110 may comprise
unextracted Cl-C2
alkyl acetate produced in first reactive extraction column 104, along with
unreacted aliphatic
alcohol, acetic acid, acid catalyst, and water. In one or more exemplary
embodiments, feed stream
111 may be passed through a second atomizer before transferring to an
exemplary second reactive
extraction column 114. In one or more exemplary embodiments, step 302 may
include pumping
an exemplary second extraction solvent into second reactive extraction column
114. An exemplary
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second extraction solvent may have a boiling point between temperatures of 150
C and 220 C
and a density between 0.72 g/cm3 and 0.74 g/cm3. An exemplary second
extraction solvent may
include, hut is not limited to, a combination of 20% wt. aromatic compound
having boiling points
between 180 C and 190 C, and 80% wt. of a mixture of naphthenic and
paraffinic compounds,
wherein the mixture of the naphthenic compound and the paraffinic compound has
a weight ratio
(the naphthenic compound: the paraffinic compound) ranging from 20:80 to
80:20. The need for
much second extraction solvent may be balanced by a dosing pump via pumping
the second
extraction solvent into second reactive extraction column 114 as a co-feed
118, as described below.
[00030] In one or more exemplary embodiments, step 304 may
include pumping the atomized
first residual compounds to the second reactive extraction column. In one
exemplary embodiment,
pumping the atomized first residual compounds to second reactive extraction
column 114 as an
overhead stream 111 from the top of second reactive extraction column 114 may
include
transferring the first residual compounds to a second atomizer, wherein the
compounds may
convert to very fine droplets with more surface area increasing the efficiency
of the Cl-C2 alkyl
acetate extraction due to increasing the contact area of the reactants mixture
droplets, results in
moving the esterification reaction forward. In one exemplary embodiment,
pumping the atomized
first residual compounds to second reactive extraction column 114 as an
overhead stream 111 from
the top of second reactive extraction column 114 may further include
transferring the atomized
first residual compounds to second reactive extraction column 114 using a
pump. The operating
temperature of feed stream 111 to column 114 may be controlled between 25 C
and 40 C.
[00031] Referring again to FIG. 1 and FIG. 3, in one or more
exemplary embodiments, the
esterification reaction of the residual unreacted reactants transferred to
second reactive extraction
column 114 through feed stream 111 may progress for assessing the efficiency
about 70%, greater
than about 80%, greater than about 90%. In one or more exemplary embodiments,
step 306 may
include extracting the second organic phase comprising 10% wt. C1-C2 alkyl
acetate produced in
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the second reactive extraction column that is dissolved in the second
extraction solvent. In one
exemplary embodiment, extracting the second organic phase comprising 10% wt. C
1 -C2 alkyl
acetate produced in the second reactive extraction column that is dissolved in
the second extraction
solvent may include producing a second reaction product comprising Cl -C2
alkyl acetate and
water in the second reactive extraction column, wherein the conversion of the
C 1 -C2 aliphatic
alcohol in the atomized first residual compounds to the Cl-C2 alkyl acetate is
at maximum 90%.
In one exemplary embodiment, step 306 may further include extracting an
exemplary second
organic phase comprising 10% wt. C1-C2 alkyl acetate produced in the second
reactive extraction
column that is dissolved in the second extraction solvent, in which the
produced C I-C2 alkyl
acetate may be separated from the other compounds in second reactive
extraction column 114 via
dissolving in the second extraction solvent and leaving the reaction
environment from the top of
second reactive extraction column 114 as an overhead stream 116. Indeed,
relatively high
conversion of the esterification reaction in column 114 may be achieved via
overcoming the
reaction equilibrium by removing the produced C I-C2 alkyl acetates through
the extraction. In
one or more exemplary embodiments, overhead product stream 116 may comprise
10% wt. Cl-
C2 alkyl acetate produced in the second reaction product that is dissolved in
the second extraction
solvent.
[00032]
In one or more exemplary embodiments, step 308 may include distilling
the second
organic phase to obtain the C1-C2 alkyl acetate with at least 95% purity and
regenerate the second
extraction solvent. In one exemplary embodiment, distilling the second organic
phase to obtain the
C1-C2 alkyl acetate with at least 95% purity and regenerate the second
extraction solvent may
include transferring the second organic phase exited as an overhead stream 116
from column 114
to an exemplary second atmospheric distillation unit 117 as a bottoms stream,
wherein the high-
purity C1-C2 alkyl acetate and second extraction solvent may be separated. An
exemplary high-
purity C 1 -C2 alkyl acetate 119 may be collected through an overhead stream
from the top of
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second distillation unit 117. In an embodiment, overhead product stream 119
may comprise
greater than about 90%, greater than about 95%, greater than about 96%,
greater than about 97%,
greater than about 98%, greater than about 99%, or greater than about 99.5% C1-
C2 alkyl acetate
by weight. In one exemplary embodiment, separating the second organic phase
into C1-C2 alkyl
acetate with at least 95% purity and the second extraction solvent using the
second distillation unit
may include regenerating the second extraction solvent.
[00033] In one or more exemplary embodiments, step 31.0 may
include transferring the
second residual compounds in the second reactive extraction column to a second
mixer. In one or
more exemplary embodiments, transferring the second residual compounds in the
second reactive
extraction column to a second mixer may include evacuating and transferring an
exemplary second
remaining bottoms products or second residual products of second reactive
extraction column 114
from second reactive extraction column 114 as a bottoms stream 120 into second
mixer 124 for
modifying before entering the next system and process of the producing high-
purity Cl-C2 alkyl
acetate. "Modification" may refer to some treatment steps which are described
below.
[00034] In one or more exemplary embodiments, step 312 may
include recycling back the
regenerated second extraction solvent to the second reactive extraction
column. In one exemplary
embodiment, the second extraction solvent which is regenerated in second
distillation unit 117
(step 308) is recycled back into second reactive extraction column 114 as
bottoms stream 118. In
an exemplary embodiment, the regenerated second solvent extraction may
comprise about 5% Cl-
C2 alkyl acetate in a continuous system and process of producing high-purity
C1-C2 alkyl acetate.
[00035] in further detail with respect to an exemplary system and
process of producing high-
purity Cl-C2 alkyl acetates in the third reactive extraction column 134, FIG.
4 shows a flowchart
of an exemplary process 400 for producing high-purity C1-C2 alkyl acetates in
third reactive
extraction column 134, consistent with one or more exemplary embodiments of
the present
disclosure. An exemplary process 400 may include producing the second mixture
by adding a 10%
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wt. salt solution to the second mixer (step 402), transferring the second
mixture to the third
atomizer (step 404), pumping the third extraction solvent to the third
reactive extraction column
(step 406), pumping the atomized second mixture to the third reactive
extraction column (step
408), extracting the third organic phase comprising 10% wt. C1-C2 alkyl
acetate remained in the
atomized second mixture that is dissolved in the third extraction solvent
(step 410), distilling the
third organic phase to obtain in the CI-C2 alkyl acetate with at least 95%
purity and regenerate
the third extraction solvent (step 412), recycling back the regenerated third
extraction solvent to
the third reactive extraction column (step 414), and transferring the third
residual compounds in
the third reactive extraction column to a distillation unit.
[00036]
Referring to FIG. 1 and FIG. 4, FIG. 4 shows a flowchart of an
exemplary process
400 where second residual compounds as a bottoms stream 120 from second
reactive extraction
column 114 illustrated in FIG. 1 is sent to second mixer 124. In an exemplary
embodiment, second
residual compound 120 may comprise unextracted C1-C2 alkyl acetates produced
in second
reactive extraction column 114 in the second reaction product, along with
unreacted Cl- C2
aliphatic alcohol, acetic acid, acid catalyst, and water. In one or more
exemplary embodiments,
step 402 may include producing the second mixture by adding a 10% wt. salt
solution 121 to
second mixer 124, wherein may be mixed with second residual compound 120. In
one exemplary
embodiment, the salt solution may be prepared using a salt having 10% wt.
solubility in water.
Salts may include, but are not limited to, calcium chloride, sodium sulfate,
sodium acetate,
potassium chloride. An exemplary second mixture in second mixer 124 may be
diluted using an
exemplary residual compound of fourth distillation unit 141 which may be
evacuated as a bottoms
stream 146 from fourth distillation unit 141 and transferred to second mixer
124 as a co-feed. An
exemplary residual compound of fourth distillation unit 141 may be comprised
an acid catalyst
and water which may be neutralized and used as a diluent for preparing the
second mixture.
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[00037] In one or more exemplary embodiments, step 404 may
include transferring the
second mixture to a third atomizer. Transferring the second mixture to third
atomizer may include
atomizing the second mixture as an exemplary feed stream of third reactive
extraction column 134,
before pumping to the column.
[00038] In one or more exemplary embodiments, step 406 may
include pumping the third
extraction solvent to the third reactive extraction column. Pumping the third
extraction solvent to
the third reactive extraction column may include transferring and pumping an
exemplary third
extraction solvent into third reactive extraction column 134. The third
extraction solvent may have
a boiling point between temperatures of 150 C and 180 C and a density
between 0.77 g/cm3 and
0.79 g/cm3. The third extraction solvent may include, but is not limited to, a
combination of 35%
wt. aromatic compound, and 65% wt. of a mixture of naphthenic and paraffinic
compounds,
wherein the mixture of the naphthenic compound and the paraffinic compound has
a weight ratio
(the naphthenic compound: the paraffinic compound) ranging from 20:80 to
80:20. The need for
much third extraction solvent may be balanced by a dosing pump via pumping the
third extraction
solvent into third reactive extraction column 134 as a co-feed 138, as
described below.
[00039] In one or more exemplary embodiments, step 408 may
include pumping the atomized
second mixture to third reactive extraction column. Pumping the atomized
second mixture to the
third reactive extraction column may include pumping the atomized second
mixture to third
reactive extraction column 134 as an overhead stream 131 exited from the top
of the second
mixture 124.
[00040] Again referring to FIG. 1 and FIG. 3, in one or more
exemplary embodiments, step
410 may include extracting the third organic phase comprising 10% wt. C1-C2
alkyl acetate
remained in the atomized second mixture that is dissolved in the third
extraction solvent.
Extracting the third organic phase comprising 10% wt. C1-C2 alkyl acetate
remained in the
atomized second mixture that is dissolved in the third extraction solvent may
include extracting
17
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REF-1401016
the third organic phase comprising 10% wt. C1-C2 alkyl acetate remained in the
atomized second
mixture that is dissolved in the third extraction solvent, in which the
remained Cl-C2 alkyl acetates
may be separated from the other compounds in third reactive extraction column
134 via dissolving
in the third extraction solvent and leaving the reaction environment from the
top of third reactive
extraction column 134 as an overhead stream 136. In one or more exemplary
embodiments, the
overhead product stream 136 may comprise 10% wt. C1-C2 alkyl acetate dissolved
in the third
extraction solvent. In one or more exemplary embodiments, no more
esterification reaction may
happen in third reactive extraction column 134. Therefore, the third
extraction solvent may extract
the remained C1-C2 alkyl acetates produced in second reactive extraction
column 114 which may
be transferred to third reactive extraction column 134 through second residual
compound 120.
In one or more exemplary embodiments, step 412 may include distilling the
third organic phase to
obtain in the C1-C2 alkyl acetate with at least 95% purity and regenerate the
third extraction
solvent. The third organic phase may transfer to an exemplary third
atmospheric distillation unit
137 as a bottoms stream 136 from the top of column 134. Distilling the third
organic phase to
obtain in the C1-C2 alkyl acetate with at least 95% purity and regenerate the
third extraction
solvent may further include separating the high-purity Cl-C2 alkyl acetate and
the third extraction
solvent through third distillation unit 137, wherein separating the third
organic phase into C1-C2
alkyl acetate with at least 95% purity and the third extraction solvent using
the third distillation
unit comprises regenerating the third extraction solvent. An exemplary high-
purity Cl-C2 alkyl
acetate may be collected through an overhead stream 139 from the top of third
distillation unit
137. In an embodiment, the overhead product stream 139 may comprise greater
than about 90%,
greater than about 95%, greater than about 96%, greater than about 97%,
greater than about 98%,
greater than about 99%, or greater than about 99.5% C1-C2 alkyl acetate by
weight.
[00041]
In one or more exemplary embodiments, step 414 may include recycling
back the
third extraction solvent, which is regenerated in third distillation unit 137
(step 412), into the third
18
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REF-1401016
reactive extraction column 134 as a bottoms stream 138. As described above, co-
feed stream 138
comprising regenerating third reaction solvent may be used for adjusting the
required level of the
solvent in column 134.
[00042] In one or more exemplary embodiments, step 416 may
include evacuating and
transferring an exemplary third remaining bottoms products or third residual
compounds from
third reactive extraction column 134 as a bottoms stream 140 into fourth
atmospheric distillation
unit 141 for separating the produced C1-C2 alkyl acetate and alcohol from the
other compounds.
In one or more exemplary embodiments, the third residual compound may be
comprised
insignificant amounts of remained Cl-C2 alkyl acetate in column 134, along
with unreacted
aliphatic alcohol, acetic acid, acid catalyst, and potentially water may be
added. In one or more
exemplary embodiments, the separated products from fourth distillation unit
141 may evacuate as
an overhead stream 144 and mix with first residual compounds 110 of column 104
before feeding
to second reactive extraction column 114. An exemplary residual compound of
fourth distillation
unit 141 may be comprised an acid catalyst and water which may be neutralized
and used as a
diluent for preparing the second mixture. Thereby, the residual compound of
fourth distillation
unit 141 may be evacuated as a bottoms stream 146 from fourth distillation
unit 141 and transferred
to second mixer 124 as a co-feed.
[00043] To better illustrate the objects, aspects and advantages
of the present disclosure, the
present disclosure will be further described with reference to specific
examples. It will be
understood by those skilled in the art that the specific embodiments described
herein are merely
illustrative of the present disclosure and are not intended to limit the
present disclosure.
[00044] In the examples, the experimental methods used were all
conventional methods
unless otherwise specified, and the materials, reagents and the like used were
commercially
available without otherwise specified.
Example 1: Production of high-purity ethyl acetate
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[00045]
In this example, ethyl acetate was produced by an exemplary reactive
extraction
system and process similar to exemplary P&ID 100 as presented in FIG. 1. At
first, a first mixture
of acetic acid, ethanol, and acid sulfuric was prepared in a 1000 cc beaker.
The temperature of the
first mixture was controlled at about 30 C. The preparation involved mixing
300 (g) of acetic acid
(99.9% purity), 10% excess weight of ethanol (99.9% purity) about 253 (g),
with 3 (g) of acid
sulfuric (98% purity), and stirred until well mixed. Then, three 20-inch
height and 4-inch diameter
glass column were packed with either ceramic saddles, stainless steel pall
rings, or trays. In the
next step, the first column was filled with the first extraction solvent. The
volume of the solvent
was 2772 g. It should be mentioned that the volume of the solvent is
proportional to separating a
10% wt. ethyl acetate solution. Then, the first mixture was added dropwise to
the first column
using a dropping funnel over 2 hours. Ethyl acetate is dissolved in the first
solvent as soon as it is
formed through the esterification reaction. Then, unreacted reactants
comprising ethanol, acetic
acid, and acid sulfuric with water as a potential byproduct produced by the
esterification reaction
were sedimented at the bottoms of the first reactive extraction column. in the
next step, the residual
compounds sedimented at the bottoms of the first reactive extraction column
were transferred to a
dropping funnel for dropwise adding to the second reactive extraction column
which is filled with
the second solvent. The esterification reaction was completed in the second
column. However,
about 80% of the produced ethyl acetate was transferred to the solvent phase.
Again, the residual
compounds were sedimented at the bottoms of the second column which may be
evacuated for the
next step. Thereafter, the residual compounds sedimented at the bottoms of the
second reactive
extraction column were mixed with water or 10% wt. salt solution with a 50:50
weight ratio and
transferred to the third reactive extraction column which is filled with the
third solvent. In one
exemplary embodiment, the salt solution may be prepared using a salt having
10% wt. solubility
in water. Salts may include, but are not limited to, calcium chloride, sodium
sulfate, sodium
acetate, potassium chloride. In the end, about 90% of ethyl acetate produced
through the
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esterification reaction was extracted in the third column. The residual
compounds seclimented at
the bottoms of the third reactive extraction column comprising ethyl acetate,
unreacted ethanol,
acetic acid, acid sulfuric and water may be transferred to a distillation
unit; then separated ethyl
acetate and unreacted ethanol formed an azeotrope with water and were added to
the second
column as a co-feed. Solvents of all three columns contained ethyl acetate and
small amounts of
ethanol which were purified to high-purity ethyl acetate using an atmospheric
distillation unit. The
separated product after di stilling each solvent may comprise greater than
about 90%, greater than
about 95%, greater than about 96%, greater than about 97%, greater than about
98%, greater than
about 99%, or greater than about 99.5% ethyl acetate by weight.
Example 2: Production of high-purity methyl acetate
[00046]
In this example, methyl acetate was produced by an exemplary reactive
extraction
system and process similar to exemplary P&ID 100 as presented in FIG. 1. At
first, a first mixture
of acetic acid, methanol, and acid sulfuric was prepared in a 1000 cc beaker.
The temperature of
the first mixture was controlled at about 30 C. The preparation involved
mixing 300 (g) of acetic
acid (99.9% purity), 10% excess weight of methanol (99.9% purity) about 176
(g), with 3 (g) of
acid sulfuric (98% purity), and stirred until well mixed. Then, three 20-inch
height and 4-inch
diameter glass column were packed with either ceramic saddles, stainless steel
pall rings, or trays.
In the next step, the first column was filled with the first extraction
solvent. The volume of the
solvent was 2330 g. It should be mentioned that the volume of the solvent is
proportional to
separating a 10% wt. methyl acetate solution. Then, the first mixture was
added dropwise to the
first column using a dropping funnel over 2 hours. Methyl acetate is dissolved
in the first solvent
as soon as it is formed through the esterification reaction. Then, unreacted
reactants comprising
methanol, acetic acid, and acid sulfuric with water as a potential byproduct
produced by the
esterification reaction were sedimented at the bottoms of the first reactive
extraction column. In
the next step, the residual compounds sedimented at the bottoms of the first
reactive extraction
21
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REF-1401016
column were transferred to a dropping funnel for dropwise adding to the second
reactive extraction
column which is filled with the second solvent. The esterification reaction
was completed in the
second column. However, about 80% of the produced methyl acetate was
transferred to the solvent
phase. Again, the residual compounds were sedimented at the bottoms of the
second column which
may be evacuated for the next step. Thereafter, the residual compounds
sedimented at the bottoms
of the second reactive extraction column were mixed with water or 10% wt. salt
solution with a
50:50 weight ratio and transferred to the third reactive extraction column
which is filled with the
third solvent. In one exemplary embodiment, the salt solution may be prepared
using a salt having
10% wt. solubility in water. Salts may include, but are not limited to,
calcium chloride, sodium
sulfate, sodium acetate, potassium chloride. In the end, about 90% of methyl
acetate produced
through the esterification reaction was extracted in the third column. The
residual compounds
sedimented at the bottoms of the third reactive extraction column comprising
methyl acetate,
unreacted methanol, acetic acid, acid sulfuric and water may be transferred to
a distillation unit;
then separated methyl acetate and unreacted ethanol formed an azeotrope with
water and were
added to the second column as a co-feed. Solvents of all three columns
contained methyl acetate
and small amounts of methanol which were purified to high-purity methyl
acetate using an
atmospheric distillation unit. The separated product after distilling each
solvent may comprise
greater than about 90%, greater than about 95%, greater than about 96%,
greater than about 97%,
greater than about 98%, greater than about 99%, or greater than about 99.5%
methyl acetate by
weight.
[00047] GC analysis of methyl acetate produced through the
reactive extraction process
explained in Example 2 shows that the purity of methyl acetate is 99.5%.
[00048] While the foregoing has described what are considered to
be the best mode and/or
other examples, it is understood that various modifications may be made
therein and that the
subject matter disclosed herein may be implemented in various forms and
examples, and that the
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REF-1401016
teachings may be applied in numerous applications, only some of which have
been described
herein. It is intended by the following claims to claim any and all
applications, modifications and
variations that fall within the true scope of the present teachings.
[00049] The scope of protection is limited solely by the claims
that now follow. That scope
is intended and should be interpreted to be as broad as is consistent with the
ordinary meaning of
the language that is used in the claims when interpreted in light of this
specification and the
prosecution history that follows and to encompass all structural and
functional equivalents.
[00050] Except as stated immediately above, nothing that has been
stated or illustrated is
intended or should be interpreted to cause a dedication of any component,
step, feature, object,
benefit, advantage, or equivalent to the public, regardless of whether it is
or is not recited in the
claims.
[00051] It will be understood that the terms and expressions used
herein have the ordinary
meaning as is accorded to such terms and expressions with respect to their
corresponding
respective areas of inquiry and study except where specific meanings have
otherwise been set forth
herein. Relational terms such as first and second and the like may be used
solely to distinguish one
entity or action from another without necessarily requiring or implying any
actual such relationship
or order between such entities or actions. An element proceeded by "a" or "an"
does not, without
further constraints, preclude the existence of additional identical elements
in the process, method,
article, or apparatus that comprises the element.
[00052] The Abstract of the Disclosure is provided to allow the
reader to quickly ascertain
the nature of the technical disclosure. It is submitted with the understanding
that it will not be used
to interpret or limit the scope or meaning of the claims. In addition, in the
foregoing Detailed
Description, it may be seen that various features are grouped together in
various implementations.
This is for purposes of streamlining the disclosure, and is not to be
interpreted as reflecting an
intention that the claimed implementations require more features than are
expressly recited in each
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REF-1401016
claim. Rather, as the following claims reflect, inventive subject matter lies
in less than all features
of a single disclosed implementation. Thus, the following claims are hereby
incorporated into the
Detailed Description, with each claim standing on its own as a separately
claimed subject matter.
[00053]
While various implementations have been described, the description is
intended to
be exemplary, rather than limiting and it will be apparent to those of
ordinary skill in the art that
many more implementations and implementations are possible that are within the
scope of the
implementations. Although many possible combinations of features are shown in
the
accompanying figures and discussed in this detailed description, many other
combinations of the
disclosed features are possible. Any feature of any implementation may be used
in combination
with or substituted for any other feature or element in any other
implementation unless specifically
restricted. Therefore, it will be understood that any of the features shown
and/or discussed in the
present disclosure may be implemented together in any suitable combination.
Accordingly, the
implementations are not to be restricted except in light of the attached
claims and their equivalents.
Also, various modifications and changes may be made within the scope of the
attached claims.
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REF-1401016
What is claimed is:
1. A process of producing a Cl-C2 alkyl acetate with at least 95% purity,
comprising:
producing a first mixture by mixing acetic acid, a C 1-C2 aliphatic alcohol,
and an acid
catalyst in first mixer;
producing a first atomized mixture by atomizing the first mixture using a
first atomizer;
pumping a first extraction solvent to a first reactive extraction column,
wherein the first
extraction solvent is a combination of 5% wt. aromatic compound, and 95% wt.
of a mixture of
naphthenic and paraffinic compounds, wherein the mixture of the naphthenic
compound and the
paraffinic compound has a weight ratio (the naphthenic compound: the
paraffinic compound)
ranging from 20:80 to 80:20, wherein the first extraction solvent has a
boiling point between 140
C and 220 C, and a density between 0.78 g/cm3 and 0.8 g/cm3;
pumping the atomized first mixture to the first reactive extraction column;
producing a first reaction product comprising a Cl-C2 alkyl acetate and water
in the first
reactive extraction column, wherein the conversion of the Cl-C2 aliphatic
alcohol in the atomized
first mixture to the Cl-C2 alkyl acetate is at maximum 70%;
removing an overhead stream from the first reactive extraction column by
contacting the
first reaction product with the first extraction solvent, wherein the overhead
stream comprises a
first organic phase comprising 10% wt. C1-C2 alkyl acetate produced in the
first reaction product
that is dissolved in the first extraction solvent;
transferring the first organic phase to a first distillation unit;
separating the first organic phase into C1-C2 alkyl acetate with at least 95%
purity and the
first extraction solvent using the first distillation unit, wherein separating
the first organic phase
into C1-C2 alkyl acetate with at least 95% purity and the first extraction
solvent using the first
distillation unit comprises regenerating the first extraction solvent;
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recycling back the regenerated first extraction solvent to the first reactive
extraction
column;
transferring a first residual compound in the first reactive extraction column
to a second
atomizer, wherein the first residual compound comprising unreacted acetic
acid, the Cl-C2
aliphatic alcohol, the acid catalyst, water, and C1-C2 alkyl acetate produced
in the first reaction
product are atomized;
pumping a second extraction solvent to a second reactive extraction column,
wherein the
second extraction solvent is a combination of 20% wt. aromatic compound having
boiling points
between 180 C and 190 C, and 80% wt. of a mixture of naphthenic and
paraffinic compounds,
wherein the mixture of the naphthenic compound and the paraffinic compound has
a weight ratio
(the naphthenic compound: the paraffinic compound) ranging from 20:80 to
80:20, wherein the
second extraction solvent has a boiling point between 150 C and 220 C, and a
density between
0.72 g/cm3 and 0.74 g/cm3;
pumping the atomized first residual compounds to the second reactive
extraction column;
producing a second reaction product comprising a Cl-C2 alkyl acetate and water
in the
second reactive extraction column, wherein the conversion of the C1-C2
aliphatic alcohol in the
atomized first residual compounds to the Cl-C2 alkyl acetate is at maximum
90%;
removing an overhead stream from the second reactive extraction column by
contacting
the second reaction product with the second extraction solvent, wherein the
overhead stream
comprises a second organic phase comprising 10% wt. C1-C2 alkyl acetate
produced in the second
reaction product that is dissolved in the second extraction solvent;
transferring the second organic phase to a second distillation unit;
separating the second organic phase into C1-C2 alkyl acetate with at least 95%
purity and
the second extraction solvent using the second distillation unit, wherein
separating the second
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REF-1401016
organic phase into C1-C2 alkyl acetate with at least 95% purity and the second
extraction solvent
using the second distillation unit comprises regenerating the second
extraction solvent;
recycling back the regenerated second extraction solvent to the second
reactive extraction
column;
transferring a second residual compound in the second reactive extraction
column to a
second mixer, wherein the second residual compounds comprising unreacted
acetic acid, the Cl-
C2 aliphatic alcohol, the acid catalyst, water, and C1-C2 alkyl acetate
produced in the second
reaction product;
producing a second mixture by adding a 10% wt. salt solution to the second
mixer, wherein
the second residual compound and 10% wt. salt solution are mixed;
transferring the second mixture to a third atomizer, wherein the second
mixture is
atomized;
pumping a third extraction solvent to a third reactive extraction column,
wherein the third
extraction solvent is a combination of 35% wt. aromatic compound, and 65% wt.
of a mixture of
naphthenic and paraffinic compounds, wherein the mixture of the naphthenic
compound and the
paraffinic compound has a weight ratio (the naphthenic compound: the
paraffinic compound)
ranging from 20:80 to 80:20, wherein the second extraction solvent has a
boiling point between
150 C and 180 C, and a density between 0.77 g/cm3 and 0.79 g/cm3;
pumping the atomized second mixture to the third reactive extraction column;
contacting the atomized second mixture with the third extraction solvent in
the third
reactive extraction column, wherein the Cl-C2 alkyl acetate remained in the
atomized second
mixture is extracted by the third extraction solvent;
removing an overhead stream from the third reactive extraction column, wherein
the
overhead stream comprises a third organic phase comprising 10% wt. C1-C2 alkyl
acetate
remained in the atomized second mixture that is dissolved in the third
extraction solvent;
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REF-1401016
transferring the third organic phase to a third distillation unit;
separating the third organic phase into C1-C2 alkyl acetate with at least 95%
purity and the
third extraction solvent using the third distillation unit, wherein separating
the third organic phase
into C1-C2 alkyl acetate with at least 95% purity and the third extraction
solvent using the third
distillation unit comprises regenerating the third extraction solvent; and
recycling back the regenerated third extraction solvent to the third reactive
extraction
column.
2. The process of producing methyl acetate with at least 95% purity of claim
1, wherein comprising
producing a first mixture by mixing acetic acid, methanol, and acid sulfuric.
3. The process of producing ethyl acetate with at least 95% purity of claim 1,
wherein comprising
producing a first mixture by mixing acetic acid, ethanol, and acid sulfuric.
4. The process of producing a C 1 -C2 alkyl acetate with at least 95% purity
of claim 1, wherein
reacting acetic acid with Cl-C2 aliphatic alcohol comprises reacting Cl-C2
aliphatic alcohol with
acetic acid with a molar ratio between 1.1 to 1.3, in the presence of at least
1%wt. acid catalyst
based on acid acetic.
5. The process of producing a C1-C2 alkyl acetate with at least 95% purity of
claims 1, wherein
producing the first mixture by mixing acetic acid, a C1-C2 aliphatic alcohol,
and an acid catalyst
comprises producing the reaction mixture by mixing acetic acid, a Cl-C2
aliphatic alcohol, and
an acid catalyst at a temperature between 20 C and 35 C.
28
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