CN107459448A - A kind of acetic acid is separated from water method - Google Patents
A kind of acetic acid is separated from water method Download PDFInfo
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- CN107459448A CN107459448A CN201610388973.6A CN201610388973A CN107459448A CN 107459448 A CN107459448 A CN 107459448A CN 201610388973 A CN201610388973 A CN 201610388973A CN 107459448 A CN107459448 A CN 107459448A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
- C07C51/46—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by azeotropic distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
Abstract
The invention discloses a kind of acetic acid to be separated from water method, belongs to field of chemical engineering.Technical scheme proposed by the present invention is：Soluble-salt is added in dilute acetic acid solution, dilute acetic acid solution and extractant are then introduced into extraction tower, carries out counter-current extraction, extraction phase flows out from tower top, and raffinate phase flows out from bottom of towe.Extraction phase and water are introduced into azeotropy rectification column again, extractant and water flow out from rectifying column tower top, and acetic acid flows out from rectifying tower bottom.This method technique is simple, easy to operate, and more than 95% acetic acid can be extracted from spirit of vinegar, the separating effect of extractant can be improved using saline extraction concentrate spirit of vinegar, reduces the loss of extractant, using azeotropic distillation technique, can efficiently separate extractant and acetic acid.
Description
Technical field
The invention belongs to field of chemical engineering, and in particular to a kind of production technology that acetic acid is obtained from dilute acetic acid solution.
Background technology
Acetic acid is a kind of important solvent in industrial production, and in use, acetate concentration is gradually dropped by more than 95%
It is low to less than 40%, it is necessary to acetic acid is separated from water, acetate concentration is brought up to more than 95%, to reuse acetic acid.Industry
The method that the method that upper acetic acid is separated from water mainly is combined using conventional distillation, azeotropic distillation, extraction with rectifying.Due to vinegar
The non-ideal behavior of acid-aqueous systems is fairly obvious, and with the increase of water content, Acetic Acid-Water relative volatility tends to 1, therefore, for up to
To final separating effect, conventional distillation needs higher reflux ratio and more column plate, energy consumption higher.And azeotropic distillation process
Entrainer can form low-boiling-point substance with water, the relative volatility with acetic acid be increased, so as to effectively reduce reflux ratio and column plate
Number, energy consumption can reduce by more than 30% compared with conventional distillation, but azeotropic distillation typically requires that higher (acetate concentration is more than acetic acid content
70%) when, acetate concentration is relatively low, its energy consumption is higher.Extraction is combined processing low-concentration acetic acid with azeotropic distillation, first uses
Acetic acid is concentrated into 50% or so by extraction, is then further concentrated with azeotropic distillation again, but the extracting power of extractant is not strong enough,
The loss of extractant is higher.Also there is the report using mixed extractant, use ethyl acetate and benzene as extractant, after extraction, benzene
Azeotropic liquid is formed with water, isolates high concentration acetic acid.The presence of benzene can reduce the azeotropic of solubility of the ester in water, benzene and water
Rectifying can reduce process energy consumption.But the method still suffers from the selectivity of extractant and the band outlet capacity of entrainer, distributes sparse and pole
Limit the contradiction of concentration.
The content of the invention
The extracting power that the present invention is directed to extractant in current spirit of vinegar extraction is not strong enough, and loss of extractant is higher to be showed
Shape, it is proposed that a kind of method of spirit of vinegar saline extraction, combined azeotropy distillation technique, the method for separating acetic acid and water, this method
Technique is simple, easy to operate, and more than 95% acetic acid can be extracted from spirit of vinegar.
Technical scheme proposed by the present invention is：
Soluble sodium salt, sylvite, calcium salt are added in dilute acetic acid solution, the addition of soluble-salt is dilute acetic acid solution
The 3%~15% of quality, extractant n-butyl acetate, isobutyl acetate from top introduce extraction tower, saliferous dilute acetic acid solution from
Bottom introduces extraction tower, carries out counter-current extraction, and extraction tower number of theoretical plate is 8~12 pieces, and extraction temperature is 25~30 DEG C, and pressure is
1atm, extractant are 1~4 with dilute acetic acid solution mass ratio：1, after extraction, extraction phase and water are introduced into azeotropy rectification column,
Azeotropy rectification column number of theoretical plate is 25~35 pieces, and reflux ratio is 3~6, and tower reactor boils temperature and is maintained at acetic acid boiling point again, feeds in tower
Middle part, the extractant and water of overhead extraction are after Liquid liquid Separation, bottom of towe extraction acetic acid.
Soluble-salt is added in dilute acetic acid solution, dilute acetic acid solution and extractant are then introduced into extraction tower, is carried out
Counter-current extraction, extraction phase flow out from tower top, and raffinate phase flows out from bottom of towe.Extraction phase and water are introduced into azeotropy rectification column again, extracted
Agent and water is taken to be flowed out from rectifying column tower top, acetic acid flows out from rectifying tower bottom.
In above-mentioned technical proposal, soluble-salt, the usually salt such as Na, K, Ca, the addition of soluble-salt is spirit of vinegar
The 5%~10% of solution quality.For example, NaCl, CH3COONa、KCl、CH3COOK、CaCl2Deng.
In above-mentioned technical proposal, the extractant that the present invention selects is n-butyl acetate, isobutyl acetate.
In above-mentioned technical proposal, the number of plates of extraction tower is more than 8 pieces, and saliferous dilute acetic acid solution introduces extraction from extraction tower bottom
Tower is taken, extractant introduces extraction tower at the top of extraction tower.
In above-mentioned technical proposal, extractant is 1~4 with dilute acetic acid solution mass ratio：1.
In above-mentioned technical proposal, the mass concentration of spirit of vinegar is 20%~40%.
In above-mentioned technical proposal, azeotropy rectification column number of theoretical plate is 25~35 pieces, is fed in the middle part of tower.
In above-mentioned technical proposal, azeotropy rectification column reflux ratio is 3~6.
Specifically, the step of saline extraction and rectifying group technology handle dilute acetic acid solution is as follows：By soluble sodium salt,
Sylvite, calcium salt are added in dilute acetic acid solution by a certain percentage, the addition of soluble-salt for dilute acetic acid solution quality 3%~
15%, preferably 5%~10%.Extractant n-propyl acetate introduces extraction tower from top, and saliferous dilute acetic acid solution draws from bottom
Enter extraction tower, carry out counter-current extraction, extraction tower number of theoretical plate is more than 8 pieces, and preferably more than 10 pieces, extraction temperature is 25~30
DEG C, pressure 1atm, extractant ratio is that extractant is 1~4 with dilute acetic acid solution mass ratio：1.After extraction, in extraction phase
Acetate concentration is enriched to more than 70% (being free of extractant).Extraction phase and appropriate water are introduced into azeotropy rectification column, azeotropic essence
Tower number of theoretical plate is evaporated for more than 25 pieces, reflux ratio is 3~6, and tower reactor boils temperature and is maintained at acetic acid boiling point again, feeds in the middle part of tower,
For the extractant and water of overhead extraction after Liquid liquid Separation, extractant is available for extraction tower to reuse, and water is available for azeotropic distillation tower weight
Multiple to use, bottom of towe produces more than 95% acetic acid.
Beneficial effect
In dilute acetic acid solution, acetic acid forms strong associating system with water by hydrogen bond, and conventional extraction agent is difficult to destroy this body
System, therefore the acetate concentration that obtains is not high after extracting, the loss of extractant of the solubility a larger increase of extractant in water.With
Prior art is compared, and after the present invention in acetic acid by adding soluble-salt, is destroyed acetic acid by salting-out effect and is formed with water
Strong associating system, improve extract and separate effect, be preferably enriched with acetum, simultaneously because the addition of salt, reduces extraction
Solubility of the agent in water is taken, reduces the loss of extractant.After by saline extraction, acetate concentration is enriched with, then
The characteristics of azeotropic mixture is formed by extractant and water, using azeotropic distillation technique, reduce extractant and acetic acid separated difficulty with
Energy consumption, extractant and acetic acid can be efficiently separated, so as to obtain high concentration acetic acid.
Embodiment
The embodiment of the present invention is described in detail below, it should be noted however that the protection of the present invention
Scope is not limited to these specific embodiments, but is determined by claims.
Embodiment 1
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-propyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-butyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 75.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 2
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-propyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of isobutyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 75.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 30% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 3
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
10%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 77.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 4
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
15%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 77.8% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 5
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
3%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 72.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 6
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 8, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 70.2% (being free of extractant) in extraction phase.Extraction phase is introduced into side line rectifying column, side line essence
It is 25 to evaporate tower number of theoretical plate, and reflux ratio 3, tower reactor reboiler temperature is 118 DEG C, is fed in the 12nd block of column plate, overhead extraction vinegar
The azeotropic mixture of sour n-propyl and water, n-propyl acetate is produced in the 20th block of column plate, the acetic acid that tower reactor extraction purity is 98% will extract
Take and be mutually introduced into suitable quantity of water in azeotropy rectification column, the amount of water is to extract 40% (quality) of dosage, azeotropy rectification column number of theoretical plate
For 25, reflux ratio 4, tower reactor reboiler temperature is 118 DEG C, is fed in the 12nd block of column plate, overhead extraction n-butyl acetate and water
Azeotropic mixture, after condensed layering, n-butyl acetate can return to extraction tower reuse, water can return azeotropy rectification column repetition
Use.The acetic acid that tower reactor extraction purity is 98%.
Embodiment 7
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 30 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 75.5% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 8
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 3 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 77% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column,
The amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
For 118 DEG C, the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, the positive fourth of acetic acid are fed
Ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The acetic acid that tower reactor extraction purity is 98%.
Embodiment 9
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 4 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 79.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 10
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 1 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 70.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 11
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 75.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 3, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 97%
Acid.
Embodiment 12
By the spirit of vinegar and CH that mass concentration is 30%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is 75.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 6, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 99%
Acid.
Embodiment 13
By the spirit of vinegar and CH that mass concentration is 20%3COOK is mixed, CH3COOK quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower, extraction tower theoretical plate from top
Number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower
Tower top flows out, and acetic acid content is that extraction phase and suitable quantity of water are introduced azeotropy rectification column by 70.7% (being free of extractant) in extraction phase
In, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler temperature
Spend for 118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid is just
Butyl ester can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.The vinegar that tower reactor extraction purity is 98%
Acid.
Embodiment 14
By the spirit of vinegar and CH that mass concentration is 30%3COONa is mixed, CH3COONa quality is dilute acetic acid solution quality
5%.Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower from top, and extraction tower is theoretical
Plate number is 10, and extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction
Column overhead flows out, and acetic acid content is 75.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropic distillation
In tower, the amount of water is 40% (quality) of extraction dosage, and azeotropy rectification column number of theoretical plate is 25, reflux ratio 4, tower reactor reboiler
Temperature is 118 DEG C, feeds the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, acetic acid
N-butyl can return to extraction tower reuse, and water can return to azeotropy rectification column reuse.Tower reactor extraction purity is 98%
Acetic acid.
Embodiment 15
Spirit of vinegar and NaCl that mass concentration is 30% are mixed, NaCl quality is the 5% of dilute acetic acid solution quality.Will
Saliferous dilute acetic acid solution introduces extraction tower from bottom, and n-butyl acetate introduces extraction tower from top, and extraction tower number of theoretical plate is 10,
Extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase is from extraction tower tower top stream
Go out, acetic acid content is 75.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column, water
Measure to extract 40% (quality) of dosage, azeotropy rectification column number of theoretical plate is 35, and reflux ratio 4, tower reactor reboiler temperature is 118
DEG C, the azeotropic mixture in the 16th block of column plate, overhead extraction n-butyl acetate and water is fed, after condensed layering, n-butyl acetate can
Return to extraction tower to reuse, water can return to azeotropy rectification column reuse.The acetic acid that tower reactor extraction purity is 98%.
Embodiment 16
Spirit of vinegar and KCl that mass concentration is 30% are mixed, KCl quality is the 5% of dilute acetic acid solution quality.It will contain
Salt dilute acetic acid solution introduces extraction tower from bottom, and n-butyl acetate introduces extraction tower from top, and extraction tower number of theoretical plate is 10, extraction
It is 25 DEG C to take temperature, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase flows out from extraction tower tower top,
Acetic acid content is 75.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column, the amount of water
To extract 40% (quality) of dosage, azeotropy rectification column number of theoretical plate is 25, and reflux ratio 4, tower reactor reboiler temperature is 118
DEG C, the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water is fed, after condensed layering, n-butyl acetate can
Return to extraction tower to reuse, water can return to azeotropy rectification column reuse.The acetic acid that tower reactor extraction purity is 98%.
Embodiment 17
By the spirit of vinegar and CaCl that mass concentration is 30%2Mixing, CaCl2Quality be dilute acetic acid solution quality 5%.
Saliferous dilute acetic acid solution is introduced into extraction tower from bottom, n-butyl acetate introduces extraction tower from top, and extraction tower number of theoretical plate is
10, extraction temperature is 25 DEG C, and pressure is normal pressure, and the amount of n-propyl acetate is 2 times of spirit of vinegar amount.Extraction phase from extraction column overhead
Flow out, acetic acid content is 75.2% (being free of extractant) in extraction phase.Extraction phase and suitable quantity of water are introduced into azeotropy rectification column, water
Amount be 40% (quality) of extraction dosage, azeotropy rectification column number of theoretical plate is 25, and reflux ratio 4, tower reactor reboiler temperature is
118 DEG C, feed the azeotropic mixture in the 12nd block of column plate, overhead extraction n-butyl acetate and water, after condensed layering, n-butyl acetate
Extraction tower reuse is can return to, water can return to azeotropy rectification column reuse.The acetic acid that tower reactor extraction purity is 98%.
Although the embodiment of the present invention is described in detail above in conjunction with the embodiments, need to refer to
Go out, protection scope of the present invention is not limited to these specific embodiments, but is determined by claims.This
Art personnel can carry out appropriate in the range of the technological thought of the present invention and purport is not departed to these embodiments
Change, and the embodiment after these changes is obviously also included within protection scope of the present invention.
Claims (5)
1. a kind of acetic acid is separated from water method, it is characterised in that：
Soluble sodium salt, sylvite, calcium salt are added in dilute acetic acid solution, the addition of soluble-salt is dilute acetic acid solution quality
3%~15%, extractant n-butyl acetate, isobutyl acetate introduce extraction tower from top, and saliferous dilute acetic acid solution is from bottom
Extraction tower is introduced, carries out counter-current extraction, extraction tower number of theoretical plate is 8~12 pieces, and extraction temperature is 25~30 DEG C, and pressure is
1atm, extractant are 1~4 with dilute acetic acid solution mass ratio：1, after extraction, extraction phase and water are introduced into azeotropy rectification column,
Azeotropy rectification column number of theoretical plate is 25~35 pieces, and reflux ratio is 3~6, and tower reactor boils temperature and is maintained at acetic acid boiling point again, feeds in tower
Middle part, the extractant and water of overhead extraction are after Liquid liquid Separation, bottom of towe extraction acetic acid.
2. acetic acid according to claim 1 is separated from water method, it is characterised in that：Described soluble-salt is Na, K, Ca
Salt, the addition of soluble-salt are the 5%~10% of dilute acetic acid solution quality.
3. acetic acid according to claim 2 is separated from water method, it is characterised in that：Described soluble-salt be NaCl,
CH3COONa、KCl、CH3COOK、CaCl2。
4. acetic acid according to claim 1 is separated from water method, it is characterised in that：The mass concentration of described spirit of vinegar is
20%~40%.
5. acetic acid according to claim 1 is separated from water method, it is characterised in that：The number of plates 10 of described extraction tower~
12 pieces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610388973.6A CN107459448A (en) | 2016-06-02 | 2016-06-02 | A kind of acetic acid is separated from water method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610388973.6A CN107459448A (en) | 2016-06-02 | 2016-06-02 | A kind of acetic acid is separated from water method |
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