KR20170007571A - The ethanol dehydration system - Google Patents

The ethanol dehydration system Download PDF

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Publication number
KR20170007571A
KR20170007571A KR1020150097143A KR20150097143A KR20170007571A KR 20170007571 A KR20170007571 A KR 20170007571A KR 1020150097143 A KR1020150097143 A KR 1020150097143A KR 20150097143 A KR20150097143 A KR 20150097143A KR 20170007571 A KR20170007571 A KR 20170007571A
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KR
South Korea
Prior art keywords
ethanol
valve
separation membrane
water
pipe
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Application number
KR1020150097143A
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Korean (ko)
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KR101700220B1 (en
Inventor
노영석
장석준
육종묵
전종필
정재칠
전오성
이효현
장성민
김택우
김동현
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(주)파인텍
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Priority to KR1020150097143A priority Critical patent/KR101700220B1/en
Priority to PCT/KR2015/007179 priority patent/WO2017007053A1/en
Publication of KR20170007571A publication Critical patent/KR20170007571A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C31/02—Monohydroxylic acyclic alcohols
    • C07C31/08—Ethanol

Abstract

The present invention relates to an ethanol dehydration system which obtains high purity ethanol by separating water through a zeolite separation membrane selectively penetrating water. The ethanol dehydration system comprises: an ethanol supply pipe (1) which supplies ethanol received from an ethanol supply tank (11) storing ethanol inside through a first pump (12) and divides the received ethanol into a plurality of paths, wherein a first valve (13) is arranged on each divided path; a plurality of separation membrane modules (2) which have a plurality of LTA zeolite separation membrane tubes in multiple bundles inside and have a manometer (23) for measuring the internal vacuum pressure of the LTA zeolite separation membrane tubes while having one end of the divided ethanol supply pipe connected to one side; a water discharging pipe (3) prepared by paths extended after being connected to the inside of the LTA zeolite separation membrane tubes in the direction opposite to the manometer of the separation membrane modules, and then connected to each of the separation membrane modules; and an ethanol collecting pipe (4) combining the paths connected to each of the separation membrane modules through a second valve (41), and connected to an ethanol storage tank (43) through a third valve (42).

Description

The ethanol dehydration system

The present invention relates to an ethanol dehydration system, and more particularly, it relates to a process for separating water from ethanol to obtain higher purity ethanol. In this process, a high-purity ethanol The present invention relates to an ethanol dehydration system which is developed to make ethanol-dehydrated water-extractable.

Generally, ethanol is produced by fermentation of sugar extracted from various plants first. The concentration of ethanol initially produced is usually about 25%, and when it is distilled by heating process, the concentration of ethanol is 95 ~ 96% Ethanol can be produced.

However, in the industrial field, it is often necessary to obtain ethanol of high purity. As a method for obtaining high purity ethanol, the membrane separation method uses water-permeable but not ethanol-permeable membrane to separate dehydrated water to obtain high purity ethanol It is a way to make it possible.

In the "Water / Ethanol Separation Method Using NaA Zeolite Membrane" in Korean Patent Registration No. 10-1282237-0000 (June 28, 2013), the concentration of 95-97% by the first stage module having high selectivity and low flux , Followed by separation of water and ethanol by passing through different membrane modules of different properties that dehydrate to a concentration of 97-100% by a low-selectivity, high-flux two-stage module Respectively.

However, it is inconvenient to prepare membranes of different properties and it is necessary to increase the capacity in order to increase the dehydration effect depending on the amount and pressure of the incoming ethanol. In this case, however, Therefore, there is an inconvenience.

In the case of the NaA zeolite separation membrane, when the Na ion is replaced with Ca ion, the micropore diameter increases from 4A to 5A, and the separation efficiency is instantaneously reduced.

(Patent Document 1) Korean Patent Registration No. 10-0220576-0000 (June 22, 1999) (Patent Document 2) Korean Patent Registration No. 10-1062918-0000 (Aug. 31, 2011) (Patent Document 3) Korean Patent Registration No. 10-1128358-0000 (March 13, 2012) (Patent Document 4) Korean Patent Registration No. 10-1282237-0000 (June 28, 2013)

The present invention has been developed in order to solve the above problems, and it is an object of the present invention to develop an ethanol dewatering system capable of obtaining high purity ethanol even when the processing capacity is fluidly changed by using an LTA zeolite membrane having high selectivity and high permeability have.

It is also intended to develop an ethanol dewatering system which can treat ethanol when the concentration of ethanol is less than the target concentration to obtain a certain concentration of ethanol.

According to an aspect of the present invention, there is provided an ethanol dewatering system for separating water through a zeolite separation membrane that selectively permeates water to obtain high purity ethanol.

An ethanol supply pipe for supplying ethanol to the plurality of paths when the ethanol is supplied by the first pump in an ethanol supply tank in which ethanol is stored, the first valve being provided in each branched path;

At least one of an aqueous solution of an alkali metal hydroxide and an aqueous solution of an aqueous alkaline hydroxide hydroxide is added to an aqueous solution of an alumina-based raw material, a silica-based raw material and sodium hydroxide dissolved in water, mixed and aged to become a hydrothermal solution A plurality of LTA zeolite membrane tubes formed into a cylindrical shape by placing a porous support for growing a separation membrane in a hydrothermal solution, carrying a porous support for hydrothermal treatment and hydrothermally treating an ion-exchanged zeolite separation layer on the surface of the support, A plurality of separation membrane modules forming a pressure gauge capable of measuring the internal vacuum pressure of the LTA zeolite separation membrane tube, one end of which is connected to one end of the branched branch into an ethanol feed pipe;

A water discharge pipe connected to the interior of the LTA zeolite membrane tube in the direction opposite to the pressure gauge of the membrane module and connected to the respective membrane modules connected to each other;

And an ethanol collecting duct connected to the other end connected to the ethanol feed pipe of the separator module and connected to each of the separator modules via a second valve and connected to the ethanol storage tank through a third valve .

Further, it is connected to the ethanol supply tank after passing through the fifth valve and the meter for measuring the concentration of the fourth valve and the ethanol after branching before passing through the third valve of the ethanol collection pipe, and is branched before passing through the fourth valve A bypass conduit connected to the fifth valve through a sixth valve and then through a fifth valve and an emergency drain conduit branched from the fifth valve and connected to the ethanol feed pipe via the seventh valve, Further comprising a reprocessing line.

In addition, the water passing through the water discharge pipe is further connected to a water tank through a heat exchanger for cooling the water, and a second water pump for sucking the air inside the water tank to form a vacuum pressure, .

As described above, according to the present invention, a plurality of LTA zeolite separation membranes having high selectivity and high permeability are formed as modules and used with water, so that there is no need for a separator module having other properties, and ethanol and water can be stably separated.

In addition, the concentration of ethanol is measured before the ethanol passing through the separation membrane module reaches the ethanol storage tank, and if it is not the target value, it can be reprocessed again, thereby obtaining high purity ethanol.

FIG. 1 is a conceptual diagram according to an embodiment of the present invention.
2 is a conceptual diagram illustrating an example of the arrangement of a separation membrane module according to an embodiment of the present invention.
3 is a conceptual diagram illustrating the structure of a separation membrane module according to an embodiment of the present invention.
4 is a conceptual diagram according to another embodiment of the present invention.
5 is a conceptual diagram according to another embodiment of the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will now be described more fully hereinafter with reference to the accompanying drawings, in which exemplary embodiments of the invention are shown.

FIG. 1 is a conceptual diagram according to an embodiment of the present invention. FIG. 2 is a conceptual diagram illustrating an example of the arrangement of a separation membrane module according to an embodiment of the present invention. The present invention relates to an ethanol dehydration system for separating water through a zeolite separation membrane which selectively permeates water to obtain high purity ethanol;

The first pump 12 is provided with a first valve 13 for supplying branched ethanol to the plurality of paths when the ethanol is supplied by the first pump 12 in the ethanol supply tank 11 in which ethanol is stored, An ethanol feed pipe (1);

At least one of an aqueous solution of an alkali metal hydroxide and an aqueous solution of an aqueous alkaline hydroxide hydroxide is added to an aqueous solution of an alumina-based raw material, a silica-based raw material and sodium hydroxide dissolved in water, mixed and aged to become a hydrothermal solution A plurality of LTA zeolite membranes (21) formed in a cylindrical shape by supporting a porous support (21) for membrane growth in the hydrothermal solution and hydrothermally treating the membrane to form ion-exchanged zeolite separation layers (22) A plurality of separation membrane modules (1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, (2).

When vacuum pressure or sucking force acts on the LTA zeolite membrane tube of the separation membrane module 2, the water with a small particle enters the inside of the LTA zeolite membrane tube and ethanol can not enter. .

At this time, the LTA zeolite separation membrane tube is manufactured by the method described in Korean Patent Registration No. 10-1128358-0000 (March 13, 2012) entitled " LTA zeolite separation membrane and its production method ".

In addition, if the plurality of separation membrane modules 2 are formed as described above, it is relatively easy to add facilities for increasing the processing capacity or processing time, and if necessary, some separation membrane modules 2 can be separated from the separation membrane modules 2, The maintenance work can be carried out, thereby enabling continuous operation.

When the water is separated by the plurality of separator modules 2, the separator module 2 is connected to the inside of the LTA zeolite separator tube in the direction opposite to the pressure gauge 23 of the separator module 2 and is connected to each separator module 2 The water is discharged through the water discharge pipe 3 to which the paths are joined and connected;

The end of the separation membrane module 2 connected to the ethanol feed pipe 1 is connected to the other end of the separation membrane module 2 via the second valve 41 and connected to the separation membrane modules 2, And the ethanol is collected through the ethanol collection duct 4 connected to the ethanol storage tank 43.

4 is a conceptual diagram according to another embodiment of the present invention. The fourth valve 51 is branched before passing through the third valve 42 of the ethanol collection pipe 4 to measure the concentration of ethanol. ) And the fifth valve 53 and then connected to the ethanol supply tank 11 and branched before passing through the fourth valve 51 to pass through the fifth valve 53 after passing through the sixth valve 54 An emergency drain line 57 connected to the bypass line 55 via the fifth valve 53 and branched before the ethanol feed line 1 is branched via the seventh valve 56, And an ethanol reprocessing line (5) equipped with an ethanol reprocessing line (5).

In the above embodiment, when the concentration of ethanol can not reach a desired concentration, the ethanol is recovered and then passed through the membrane module 2 to obtain a desired concentration of ethanol. According to the embodiment, It is possible to obtain the effect.

Also, when an abnormality occurs in the ethanol storage tank 43 or when the ethanol storage tank 43 is full, it can be circulated through the emergency drain pipe 57 to cope with an emergency situation.

5 is a conceptual diagram according to another embodiment of the present invention. Water passing through the water discharge pipe 3 is connected to a water tank 62 through a heat exchanger 61 for cooling water, And a second pump (63) for sucking in the air of the second pump (62) to form a vacuum pressure.

In this embodiment, since the discharged water is in a relatively hot state of 60 to 100 degrees, it can be cooled through the heat exchanger and then sent to the water tank 62, and the second pump 63 forms vacuum pressure to suck water So that the efficiency of the separation membrane module 2 can be increased and smooth water can be discharged.

1: Ethanol feed line
11: ethanol supply tank 12: first pump
13: first valve
2: Membrane module
21: porous support 22: zeolite separation layer
23: Manometer
3: Water discharge pipe
4: Ethanol collection pipe
41: second valve 42: third valve
43: ethanol storage tank
5: Ethanol re-treatment line
51: fourth valve 52: measuring instrument
53: fifth valve 54: sixth valve
55: bypass pipe 56: seventh valve
57: Emergency drain pipe
6: Water collection pipe
61: heat exchanger 62: water tank
63: Second pump

Claims (3)

1. An ethanol dehydration system for separating water through a zeolite separation membrane which selectively passes water through ethanol to obtain high purity ethanol;
The first pump 12 is provided with a first valve 13 for supplying branched ethanol to the plurality of paths when the ethanol is supplied by the first pump 12 in the ethanol supply tank 11 in which ethanol is stored, An ethanol feed pipe (1);
At least one of an aqueous solution of an alkali metal hydroxide and an aqueous solution of an aqueous alkaline hydroxide hydroxide is added to an aqueous solution of an alumina-based raw material, a silica-based raw material and sodium hydroxide dissolved in water, mixed and aged to become a hydrothermal solution A plurality of LTA zeolite membranes (21) formed in a cylindrical shape by supporting a porous support (21) for membrane growth in the hydrothermal solution and hydrothermally treating the membrane to form ion-exchanged zeolite separation layers (22) A plurality of separation membrane modules (1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, (2);
A water discharge pipe line 3 connected to the inside of the LTA zeolite separation membrane tube in the direction opposite to the pressure gauge 23 of the separation membrane module 2 and connected to the respective separation membrane modules 2 in a combined manner;
The end of the separation membrane module 2 connected to the ethanol feed pipe 1 is connected to the other end of the separation membrane module 2 via the second valve 41 and connected to the separation membrane modules 2, And an ethanol recovery duct (4) connected to the ethanol storage tank (43).
The method according to claim 1, further comprising the steps of: measuring the concentration of ethanol in the fourth valve (51) and the fifth valve (53) before branching through the third valve (42) A bypass pipe connected to the ethanol supply tank 11 and connected to the path through the fifth valve 53 after passing through the sixth valve 54 before passing through the fourth valve 51, And an emergency drain pipe 57 branched from the fifth valve 53 via the seventh valve 56 and connected before the ethanol feed pipe 1 is branched, 5). ≪ / RTI >
The water treatment system according to claim 1 or 2, wherein the water passing through the water discharge pipe (3) is connected to a water tank (62) through a heat exchanger (61) Further comprising a water collection conduit (6) having a second pump (63) for sucking in the air and forming a vacuum pressure.
KR1020150097143A 2015-07-08 2015-07-08 The ethanol dehydration system KR101700220B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR1020150097143A KR101700220B1 (en) 2015-07-08 2015-07-08 The ethanol dehydration system
PCT/KR2015/007179 WO2017007053A1 (en) 2015-07-08 2015-07-10 Ethanol dehydration system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR1020150097143A KR101700220B1 (en) 2015-07-08 2015-07-08 The ethanol dehydration system

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KR20170007571A true KR20170007571A (en) 2017-01-19
KR101700220B1 KR101700220B1 (en) 2017-01-31

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100220576B1 (en) 1997-02-20 1999-09-15 양인모 Low pressure ethanol psa drying device using carbon dioxide
JP2002293754A (en) * 2001-03-30 2002-10-09 Syst Enji Service Kk Method and plant for isolating and recovering alcohol from waste gas containing the same
KR101062918B1 (en) 2008-09-01 2011-09-06 주식회사 창해에탄올 Multitube Type Ethanol Pressure Swing Adsorption Dewatering Device
KR101128358B1 (en) 2009-11-26 2012-03-23 한국에너지기술연구원 Lta zeolite composite membranes and method for fabricating the same
JP2012067091A (en) * 2010-08-25 2012-04-05 Mitsubishi Chemicals Corp Recovery method of alcohol from alcohol-water mixture
KR101282237B1 (en) 2012-03-21 2013-07-10 한국에너지기술연구원 Method for separating water/ethanol mixture using naa zeolite membrane

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003210950A (en) * 2003-02-12 2003-07-29 Mitsui Eng & Shipbuild Co Ltd Liquid mixture separation membrane
CA2630493A1 (en) * 2006-01-11 2007-07-19 Ngk Insulators, Ltd. Method of separating liquid mixture
JP2007275690A (en) * 2006-04-03 2007-10-25 Ngk Insulators Ltd Method for separating and recovering organic liquid from organic liquid aqueous solution
JP2008086972A (en) * 2006-10-05 2008-04-17 Mitsubishi Heavy Ind Ltd Dehydration system and dehydration method
JP2010207776A (en) * 2009-03-12 2010-09-24 Hiroshima Univ Organic acid hardly adsorbable porous body and method of selectively separating alcohol

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100220576B1 (en) 1997-02-20 1999-09-15 양인모 Low pressure ethanol psa drying device using carbon dioxide
JP2002293754A (en) * 2001-03-30 2002-10-09 Syst Enji Service Kk Method and plant for isolating and recovering alcohol from waste gas containing the same
KR101062918B1 (en) 2008-09-01 2011-09-06 주식회사 창해에탄올 Multitube Type Ethanol Pressure Swing Adsorption Dewatering Device
KR101128358B1 (en) 2009-11-26 2012-03-23 한국에너지기술연구원 Lta zeolite composite membranes and method for fabricating the same
JP2012067091A (en) * 2010-08-25 2012-04-05 Mitsubishi Chemicals Corp Recovery method of alcohol from alcohol-water mixture
KR101282237B1 (en) 2012-03-21 2013-07-10 한국에너지기술연구원 Method for separating water/ethanol mixture using naa zeolite membrane

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KR101700220B1 (en) 2017-01-31
WO2017007053A1 (en) 2017-01-12

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