CN106977409B - A kind of separation method of triethylamine and water - Google Patents
A kind of separation method of triethylamine and water Download PDFInfo
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- CN106977409B CN106977409B CN201710321637.4A CN201710321637A CN106977409B CN 106977409 B CN106977409 B CN 106977409B CN 201710321637 A CN201710321637 A CN 201710321637A CN 106977409 B CN106977409 B CN 106977409B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
Abstract
The invention discloses the separation methods of a kind of triethylamine and water, it is intended to provide purity is high after a kind of separation and is not required to the triethylamine of additional separating medium and the separation method of water, its key points of the technical solution are that the separation method of a kind of triethylamine and water, comprising the following steps: one, will triethylamine aqueous solution place heater in heating be separated into water content≤5% triethylamine solution and amount containing triethylamine≤5% aqueous solution；Two, the triethylamine solution of water content≤5% is purified into triethylamine by first rectifying column and Second distillation column；Three, the aqueous solution of amount containing triethylamine≤5% is tentatively extracted by third distillation column, then the triethylamine tentatively extracted and water mixed liquid is imported in second step and purified, the purification technique field of present invention triethylamine suitable for water.
Description
Technical field
The present invention relates to a kind of purification technique field of triethylamine in water, more specifically, it relates to a kind of triethylamine with
The separation method of water.
Background technique
Triethylamine is a kind of important industrial chemicals, since it is a kind of volatile, liquid easily miscible with water at low temperature
Body in production carries out it mostly the separation method of triethylamine and water being with its contained humidity of piece Alkali absorption, Huo Zhejia in industry
Enter entrainer azeotropic distillation, but there are the following problems: pure using piece alkali carries if triethylamine content is lower in 1, water, consumption
Greatly, and the lye of generation will cause secondary pollution；2, according to being added entrainer azeotropic distillation, then triethylamine after separating or
Entrainer impurity can be remained in water, influence purity；3, after separating, triethylamine residual quantity is high in waste liquid.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide purity is high after a kind of separation and be not required to outer
Add the triethylamine of separating medium and the separation method of water.
To achieve the above object, the present invention provides the following technical scheme that the separation method of a kind of triethylamine and water, special
Sign is: the following steps are included:
One, triethylamine aqueous solution is placed in heater and is heated to 30 DEG C, be separated into the triethylamine solution of water content≤5%
With the aqueous solution of amount containing triethylamine≤5%；
Two, the triethylamine solution of water content≤5% is added to first rectifying column, by the triethylamine solution of water content≤5%
Heating vaporization, triethylamine-water azeotropic mixture steam enters the first condenser from tower top and is condensed after vaporization, and condensate liquid is collected into first
In return tank, condensate liquid is layered in the first return tank, forms water layer and triethylamine layer, and the water layer in the first return tank is back to
In first rectifying column, the triethylamine layer in the first return tank is imported in Second distillation column, three second of Second distillation column overhead collection
Amine-water azeotropic mixture steam is condensed by the second condenser, and is recycled in first rectifying column, and water is discharged from first rectifying column tower bottom
To the first water tank, triethylamine is expelled in finished product box from Second distillation column tower bottom, and the design of pressure of first rectifying column is
Normal pressure, the design of pressure of Second distillation column are greater than the pressure value of first rectifying column；
Three, the water in the aqueous solution of the amount containing triethylamine isolated in heater≤5% and the first water tank is directed into
Heating vaporization in three rectifying columns, triethylamine-water azeotropic mixture steam enters third condenser from third distillation column tower top after vaporization, the
The condensate liquid that three condensers are collected is sent into the second return tank, and condensate liquid is layered in the second return tank, forms water layer and three second
Amine layer, the water layer in the second return tank are back to third distillation column, and the triethylamine layer in the second return tank imports first rectifying column,
Water is expelled in the second water tank from third distillation column tower bottom.
The present invention is further arranged to: passing through the control of first flow controller between first return tank and first rectifying column
System, controls between the first return tank and Second distillation column by second flow controller, the second condenser and first rectifying column it
Between controlled by third flow measuring unit, between the second return tank and third distillation column by the 4th flow controller control, second time
It flows and is controlled between tank and first rectifying column by the 5th flow controller.
The present invention is further arranged to: first return tank includes liquid collecting bucket, water storage chamber and storage triethylamine chamber, collection
Liquid bucket bottom is communicated with U-tube, and U-tube liquid outlet height is greater than feed liquor open height, and condensate liquid flows into liquid collecting bucket in advance, in liquid collecting
Water is layered in advance with triethylamine in struggling against, and water layer exports through U-tube and flows into water storage cavity room, and the aqueous solution of water storage chamber is back to first
Rectifying column, triethylamine liquid suction pipe is additionally provided on liquid collecting bucket, and triethylamine layer flows into storage triethylamine chamber, storage by triethylamine liquid suction pipe
Triethylamine chamber is connected with reverse osmosis membrane, and triethylamine layer pressurizes and passes through reverse osmosis membrane filtration, filters out and be slightly soluble in triethylamine
Moisture, the moisture filtered out is back to water storage chamber, and filtered triethylamine is directed into Second distillation column.
The present invention is further arranged to: first condenser includes air collecting chamber, the first condenser pipe and the second condenser pipe, and
It is connected at the top of the inlet end of one condenser pipe and air collecting chamber, the inlet end of the second condenser pipe is connected to the bottom of air collecting chamber, air collecting chamber
It being connected to the first overhead, liquid collecting bucket also accordingly uses two, it is respectively used to the first condenser pipe of connection and the second condenser pipe,
Upper layer is mainly water vapour in air collecting chamber, and lower layer is mainly triethylamine steam in air collecting chamber, and water and three second are first carried out before condensation
The initial gross separation of amine, then be layered by the first return tank.
The present invention is further arranged to: being connected between the third distillation column and third condenser by being equipped with gas separator
Logical, gas separator includes gas filtration film, air inlet, water vapour gas outlet and triethylamine gas outlet, and third condenser includes
Third condenser pipe and the 4th condenser pipe, triethylamine-water azeotropic vaporization pressurization enter air inlet, are filtered by gas filtration film, mistake
Water after filter steam enters third condensing tube condensation from water vapour gas outlet and is back to third distillation column, and the triethylamine not filtered steams
Vapour enters the 4th condensing tube condensation from triethylamine gas outlet, then is layered in the second return tank.
The present invention is further arranged to: the temperature of first return tank and the second return tank is controlled at 30-35 DEG C.
By using above-mentioned technical proposal, have the advantage that
1, the present invention uses the azeotropic distillation of triethylamine and water, realizes and efficiently separates to triethylamine and water mixed liquid,
And because triethylamine and water after separation do not have entrainer impurity, purity is high without using entrainer；
2, the water in the aqueous solution and the first water tank of amount containing triethylamine≤5% isolated to heating passes through third rectifying
Tower rectifying again, and be recycled in first rectifying column, the purification amount of triethylamine is improved, containing for discharge Shi Shuizhong triethylamine is reduced
Amount；
3, separating for several times and layering are carried out by the first condenser and the first return tank, improves purification purity, reduced in water
The content of triethylamine；
4, it does not need not will form aqueous slkali using piece alkali and cause secondary pollution.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the separation method implementing procedure of a kind of triethylamine of the present invention and water.
Fig. 2 is that separation method the first condenser of implementation of a kind of triethylamine of the present invention and water and the structure of the first return tank are shown
It is intended to.
Specific embodiment
It is described further referring to figs. 1 to separation method embodiment of the Fig. 2 to a kind of triethylamine of the present invention and water.
A kind of separation method of triethylamine and water, comprising the following steps:
One, by temperature at 18.7 DEG C or more, triethylamine is slightly soluble in water, and finds that water can also remain in three in production practices
In ethylamine solution, so can be layered after 30 DEG C being heated in triethylamine aqueous solution placement heater, it is separated into water content≤5%
Triethylamine solution and amount containing triethylamine≤5% aqueous solution, the mixed liquor of triethylamine and water is separated in advance, is imported different
In rectifying column, separation is synchronized, the purity after improving the rate of departure, and separation.
Two, the design of pressure of first rectifying column 100 is normal pressure, and the design of pressure of Second distillation column 200 is greater than first
The pressure value of rectifying column 100, the pressure value of Second distillation column 200 are preferably 0.3MPa, using in triethylamine-water azeotropic mixture composition
The triethylamine content principle reduced with pressure rise, triethylamine is come out from triethylamine-water Azeotrope separation.
The triethylamine solution of water content≤5% is added to first rectifying column 100, by the triethylamine solution of water content≤5%
Heating vaporization, triethylamine-water azeotropic mixture steam enters the first condenser 10 from tower top and is condensed after vaporization, and condensate liquid is collected into the
In one return tank 40, the temperature of the first return tank 40 is controlled at 30-35 DEG C, and condensate liquid is layered in the first return tank 40, is formed
Water layer and triethylamine layer, water layer are back in first rectifying column 100 by first flow controller 1, and triethylamine layer passes through second
Flow controller 2 imports in Second distillation column 200, and triethylamine-water azeotropic mixture steam of 200 overhead collection of Second distillation column passes through
Second condenser 20 condensation, and being recycled in first rectifying column 100 by third flow controller 3, water is from first rectifying column 100
Tower bottom is expelled in the first water tank 11, triethylamine content≤2% in water in the first water tank 11, and triethylamine is from Second distillation column
200 tower bottom are expelled in finished product box 12, and the triethylamine purity in finished product box 12 can reach 99.95% or more.
Three, due in the water in the first water tank 11 can also residual fraction triethylamine, so by the first water storage in step 2
The aqueous solution for amount containing triethylamine≤5% separated in water and step 1 in case 11, which is directed into third distillation column 300, to be heated
Vaporization, triethylamine-water azeotropic mixture steam enters third condenser 30, third condenser from 300 tower top of third distillation column after vaporization
30 condensate liquids collected are sent into the second return tank 50, and the temperature of the second return tank 50 is also controlled at 30-35 DEG C, makes the second reflux
Condensate liquid in tank 50 is separated into water layer and triethylamine layer, the water layer in water content≤5%, the second return tank 50 of triethylamine layer
It is back to third distillation column 300 by the 4th flow controller 4, the triethylamine layer in the second return tank 50 passes through the 5th flow control
Device 5 processed imports first rectifying column 100, and multi-cycle separation, water are expelled in the second water tank 13 from 300 tower bottom of third distillation column again,
Amount containing triethylamine≤0.02% in water in second water tank 13.
As shown in Fig. 2, the first return tank includes liquid collecting bucket 41, water storage chamber 42 and storage triethylamine chamber 43, liquid collecting bucket 41
Bottom is communicated with U-tube 44, and 44 liquid outlet height of U-tube is greater than feed liquor open height, and condensate liquid flows into liquid collecting bucket 41 in advance, collecting
Water is layered in advance with triethylamine in liquid bucket 41, and water layer density is bigger to flow into water storage chamber 42 through 44 liquid outlet of U-tube, due to water
Liquid separation is collected in collector tube 41 with triethylamine solution, and water-yielding stratum is separated by U-tube 44, can be improved in water storage chamber 42
The purity of aqueous solution, the aqueous solution of water storage chamber 42 are back to first rectifying column 100, and 41 are additionally provided with triethylamine drawing liquid on liquid collecting bucket
Pipe 45, triethylamine layer flow into storage triethylamine chamber 43 by triethylamine liquid suction pipe 45, and storage triethylamine chamber 43 is connected with reverse osmosis
Film 46, triethylamine layer pressurizes and passes through reverse osmosis membrane 46 and filters, since organic solution is difficult to through reverse osmosis membrane, so by anti-
Permeable membrane 46 filters out the moisture content being slightly soluble in triethylamine, further purifies to triethylamine layer, the water content of triethylamine layer
≤ 0.5%, purity when being directed into Second distillation column is improved, the moisture filtered out is back to water storage chamber by diversion pipe 47
42。
First condenser includes air collecting chamber 14, the first condenser pipe 15 and the second condenser pipe 16, the air inlet of the first condenser pipe 15
It holds and is connected at the top of air collecting chamber 14, the inlet end of the second condenser pipe 16 is connected to the bottom of air collecting chamber 14, air collecting chamber 14 and first
The connection of 100 tower top of destilling tower, liquid collecting bucket 41 is also corresponding to use two, is respectively used to the first condenser pipe 15 of connection and the second condenser pipe
16, since water phase is less than the relative steam density of triethylamine to vapour density, so upper layer is mainly water vapour in air collecting chamber 14,
Lower layer is mainly triethylamine steam in air collecting chamber 14, and the initial gross separation of water and triethylamine is first carried out before condensation, then passes through liquid collecting
Struggle against 41 pairs of triethylamines and water secondary clearing again, improves separation purity.
It is connected between third distillation column 300 and third condenser 30 by being equipped with gas separator 400, gas separator
400 include gas filtration film 401, air inlet 402, water vapour gas outlet 403 and triethylamine gas outlet 404, air inlet 402 and the
The connection of three rectifying columns 300, air inlet 402 are connected to water vapour gas outlet 403 by gas filtration film 401, third condenser 30
Including third condenser pipe 31 and the 4th condenser pipe 32, water vapour gas outlet 403 and third distillation column 300 pass through third condenser pipe 31
Connection, triethylamine gas outlet 404 are connected to the second return tank 50 by the 4th condenser pipe 32.
Triethylamine-water azeotropic vaporization pressurization enters air inlet 402, is filtered by gas filtration film 401, water vapour after filtering
Enter third condenser pipe 31 from water vapour gas outlet 403 to be condensed back to third distillation column 300, the triethylamine steam not filtered
Enter the 4th condenser pipe 32 from triethylamine gas outlet 404 to condense, then be layered reflux in the second return tank 50, part water vapour is logical
Crossing gas filtration film 401 and being directly condensed back reduces the layering required waiting time to third distillation column 300, can be improved
Water vapour reflux rate, and water vapour by gas filtration film 401 be directly condensed back when, the purity of water is higher, reduces three
The reflux of ethamine improves the rectifying rate of third distillation column 300.
The temperature of first return tank 40 and the second return tank 50 is controlled at 30-35 DEG C, temperature control at 30-35 DEG C.
The temperature of first return tank 40 and the second return tank 50 is controlled at 30-35 DEG C, makes triethylamine and water secondary clearing again, temperature
When degree is as between 20-30 DEG C, the layering rate of triethylamine and water is gradually increased, and the mutual solubility of water and triethylamine also gradually increases
Add, when temperature is higher than 35 DEG C, layering rate increase is unobvious, and water content tends to be steady in triethylamine, preferably 30 DEG C, 32 DEG C
With 35 DEG C so temperature control is conducive to the layering of triethylamine and water at 30-35 DEG C.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, and those skilled in the art exists
Common variations and alternatives are carried out within the scope of technical solution of the present invention should all be included within the scope of the present invention.
Claims (3)
1. the separation method of a kind of triethylamine and water, it is characterized in that: the following steps are included:
One, triethylamine aqueous solution is placed in heater and is heated to 30 DEG C, be separated into the triethylamine solution of water content≤5% and contain
The aqueous solution of triethylamine amount≤5%；
Two, the triethylamine solution of water content≤5% is added to first rectifying column, the triethylamine solution of water content≤5% is added
Hot vapour, triethylamine-water azeotropic mixture steam enters the first condenser from tower top and is condensed after vaporization, and condensate liquid is collected into first time
It flows in tank, condensate liquid is layered in the first return tank, forms water layer and triethylamine layer, and the water layer in the first return tank is back to the
In one rectifying column, the triethylamine layer in the first return tank is imported in Second distillation column, the triethylamine-of Second distillation column overhead collection
Water azeotropic mixture steam is condensed by the second condenser, and is recycled in first rectifying column, and water is expelled to from first rectifying column tower bottom
In first water tank, triethylamine is expelled in finished product box from Second distillation column tower bottom, and the design of pressure of first rectifying column is normal
Pressure, the design of pressure of Second distillation column are greater than the pressure value of first rectifying column；
Three, the water in the aqueous solution of the amount containing triethylamine isolated in heater≤5% and the first water tank is directed into third
Heating vaporization in rectifying column, triethylamine-water azeotropic mixture steam enters third condenser, third from third distillation column tower top after vaporization
The condensate liquid that condenser is collected is sent into the second return tank, and condensate liquid is layered in the second return tank, forms water layer and triethylamine
Layer, the water layer in the second return tank is back to third distillation column, and the triethylamine layer in the second return tank imports first rectifying column, water
It is expelled in the second water tank from third distillation column tower bottom；
It is controlled between first return tank and first rectifying column by first flow controller, the first return tank and the second rectifying
It is controlled between tower by second flow controller, is controlled between the second condenser and first rectifying column by third flow measuring unit, the
It is controlled between two return tanks and third distillation column by the 4th flow controller, is passed through between the second return tank and first rectifying column
The control of 5th flow controller；
First return tank includes liquid collecting bucket, water storage chamber and storage triethylamine chamber, and liquid collecting bucket bottom is communicated with U-tube, U-shaped
Pipe liquid outlet height is greater than feed liquor open height, and condensate liquid flows into liquid collecting bucket in advance, and water is layered in advance with triethylamine in liquid collecting bucket,
Water layer exports through U-tube and flows into water storage cavity room, and the aqueous solution of water storage chamber is back to first rectifying column, is additionally provided with three on liquid collecting bucket
Ethamine liquid suction pipe, triethylamine layer flow into storage triethylamine chamber by triethylamine liquid suction pipe, and storage triethylamine chamber is connected with reverse osmosis
Film, triethylamine layer pressurize and pass through reverse osmosis membrane filtration, filter out the moisture being slightly soluble in triethylamine, the moisture reflux filtered out
To water storage chamber, filtered triethylamine is directed into Second distillation column；
First condenser includes air collecting chamber, the first condenser pipe and the second condenser pipe, the inlet end and gas collection of the first condenser pipe
Top of chamber connection, the inlet end of the second condenser pipe are connected to the bottom of air collecting chamber, and air collecting chamber is connected to the first overhead, collection
Liquid bucket also accordingly uses two, is respectively used to the first condenser pipe of connection and the second condenser pipe, and upper layer is mainly that water steams in air collecting chamber
Vapour, lower layer is mainly triethylamine steam in air collecting chamber, the initial gross separation of water and triethylamine is first carried out before condensation, then pass through first
Return tank is layered.
2. the separation method of a kind of triethylamine and water according to claim 1, it is characterized in that: the third distillation column and
It is connected between three condensers by being equipped with gas separator, gas separator includes gas filtration film, air inlet, water vapour outlet
Mouthful and triethylamine gas outlet, third condenser include third condenser pipe and the 4th condenser pipe, triethylamine-water azeotropic vaporization pressurize into
Enter air inlet, filtered by gas filtration film, water vapour enters the reflux of third condensing tube condensation from water vapour gas outlet after filtering
To third distillation column, the triethylamine steam not filtered enters the 4th condensing tube condensation from triethylamine gas outlet, then at second time
Flow layering in tank.
3. the separation method of a kind of triethylamine and water according to claim 1, it is characterized in that: first return tank and
The temperature of two return tanks is controlled at 30-35 DEG C.
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| CN108658785B (en) * | 2017-09-08 | 2019-04-16 | 杭州九清科技有限公司 | The separation method of difficult separation system containing triethylamine |
| CN109369419B (en) * | 2018-12-03 | 2024-01-19 | 烟台国邦化工机械科技有限公司 | Process method and device for separating triethylamine from industrial waste liquid |
| CN109607920B (en) * | 2018-12-28 | 2021-06-11 | 浙江建业化工股份有限公司 | System and process for producing ethylamine by membrane separation-hydrolysis treatment of wastewater |
| CN110180327A (en) * | 2019-05-13 | 2019-08-30 | 天津大学 | A kind of method and system of the tail gas resource utilization containing organic amine |
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| EP1070717B1 (en) * | 1999-07-23 | 2002-02-27 | Basf Aktiengesellschaft | Process for the preparation of pure triethylenediamine |
| CN102442913A (en) * | 2010-10-07 | 2012-05-09 | 阎成华 | Production method of triethylamine extracted from waste liquid by batch distillation method |
| EP2484421A1 (en) * | 2011-02-07 | 2012-08-08 | Basf Se | Method for separating sulphur from low boiling point components from a mixture containing hexamethylendiamine |
| CN103772205B (en) * | 2012-10-25 | 2015-07-08 | 中国石油化工股份有限公司 | Method for separating ethidene diamine and water |
| CN103539675B (en) * | 2013-10-21 | 2015-05-13 | 西安近代化学研究所 | Separation method of ethylenediamine and water azeotrope |
| CN204454715U (en) * | 2015-01-27 | 2015-07-08 | 中国人民解放军63977部队 | A kind of triethylamine retrieving arrangement |
| CN104771926B (en) * | 2015-03-23 | 2017-01-04 | 烟台国邦化工机械科技有限公司 | The rectifier unit of a kind of recovery of acetic acid from aqueous acetic acid and process |
| CN204676014U (en) * | 2015-04-21 | 2015-09-30 | 江苏金凯树脂化工有限公司 | A kind of Trimethylamine 99 retrieving arrangement |
| CN105523889B (en) * | 2016-01-17 | 2017-12-08 | 济南大学 | A kind of tert-butyl alcohol triethylamine azeotropic mixture extraction rectifying method |
| CN105693446B (en) * | 2016-01-17 | 2017-10-13 | 济南大学 | A kind of isopropanol triethylamine azeotropic mixture extraction rectifying method |
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