CN106977409A - 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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- CN106977409A CN106977409A CN201710321637.4A CN201710321637A CN106977409A CN 106977409 A CN106977409 A CN 106977409A CN 201710321637 A CN201710321637 A CN 201710321637A CN 106977409 A CN106977409 A CN 106977409A
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- triethylamine
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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
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Abstract
The invention discloses a kind of triethylamine and the separation method of water, it is desirable 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, and its drip irrigation device is the separation method of a kind of triethylamine and water, is comprised the following steps：First, triethylamine aqueous solution is placed into heating in heater and is separated into the triethylamine solution of water content≤5% and the aqueous solution of amount containing triethylamine≤5%；2nd, the triethylamine solution of water content≤5% is purified into triethylamine by first rectifying column and Second distillation column；3rd, 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 into purification in second step, 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 technology
Triethylamine is a kind of important industrial chemicals, because it is a kind of volatile, easy liquid miscible with water at low temperature
Body, it is with its contained humidity of piece Alkali absorption, Huo Zhejia mostly the separation method of triethylamine and water that it, which is carried out, in production in industry
Enter entrainer azeotropic distillation, but there is problems with：It is pure using piece alkali carries the 1st, if triethylamine content is relatively low in water, consumption
Greatly, and produce alkali lye can cause secondary pollution；2nd, according to adding entrainer azeotropic distillation, then triethylamine after separating or
Entrainer impurity can be remained in water, purity is influenceed；3rd, after separating, triethylamine residual quantity is high in waste liquid.
The content of the invention
In view of the deficienciess of the prior art, it is an object of the invention to provide purity height after one kind separation and being not required to outer
Plus the triethylamine and the separation method of water of separating medium.
To achieve the above object, the invention provides following technical scheme：A kind of separation method of triethylamine and water, it is special
Levying is：Comprise the following steps：
First, 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%；
2nd, the triethylamine solution of water content≤5% is added to first rectifying column, the triethylamine solution of water content≤5% is heated
Vaporization, triethylamine-water azeotropic mixture steam is condensed from tower top into the first condenser after vaporization, and condensate liquid is collected into the first backflow
In tank, condensate liquid is layered in the first return tank, and the water layer formed in water layer and triethylamine layer, the first return tank is back to first
In rectifying column, the triethylamine layer in the first return tank is imported in Second distillation column, triethylamine-water of Second distillation column overhead collection
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 bottom of towe
In one storage tank, triethylamine is expelled in finished product box from Second distillation column bottom of towe, and the design of pressure of first rectifying column is normal pressure,
The design of pressure of Second distillation column is more than the pressure value of first rectifying column；
3rd, the water in the aqueous solution of the amount containing triethylamine isolated in heater≤5% and the first storage tank is directed into the 3rd essence
Heating vaporization in tower is evaporated, triethylamine-water azeotropic mixture steam enters the 3rd condenser from third distillation column tower top after vaporization, and the 3rd is cold
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,
Water layer in second return tank be back in third distillation column, the second return tank triethylamine layer import first rectifying column, water from
Third distillation column bottom of towe is expelled in the second storage tank.
The present invention is further arranged to：Pass through first flow controller control between first return tank and first rectifying column
System, is controlled between the first return tank and Second distillation column by second flow controller, the second condenser and first rectifying column it
Between by the 3rd flow measuring unit control, between the second return tank and third distillation column pass through the 4th flow controller control, second time
Flow between tank and first rectifying column by the control of 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 is highly more 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 bucket, and water layer flows into water storage chamber through U-tube outlet, and the aqueous solution of water storage chamber is back to first
Triethylamine liquid suction pipe is additionally provided with rectifying column, liquid collecting bucket, 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 by reverse osmosis membrane filtration, filters out and be slightly soluble in triethylamine
Moisture, the moisture filtered out is back to water storage chamber, and the triethylamine after filtering 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, the
The inlet end of one condenser pipe at the top of air collecting chamber with being connected, and the inlet end of the second condenser pipe is connected with the bottom of air collecting chamber, air collecting chamber
Connected with the first overhead, liquid collecting bucket also accordingly uses two, be respectively used to the first condenser pipe of connection and the second condenser pipe,
In air collecting chamber upper strata be mainly in water vapour, air collecting chamber lower floor be mainly triethylamine steam, advanced water-filling and three second before condensation
The initial gross separation of amine, then be layered by the first return tank.
The present invention is further arranged to：By connecting provided with gas separator between the third distillation column and the 3rd condenser
Logical, gas separator includes gas filtration film, air inlet, water vapour gas outlet and triethylamine gas outlet, and the 3rd condenser includes
3rd condenser pipe and the 4th condenser pipe, triethylamine-water azeotropic vaporization pressurization enter air inlet, pass through gas filtration membrane filtration, mistake
Water after filter steam is back to third distillation column from water vapour gas outlet into the 3rd condensing tube condensation, 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, with advantages below：
1st, the present invention is realized to triethylamine and water mixed liquid and efficiently separated using triethylamine and the azeotropic distillation of water, and
Because without using entrainer, triethylamine and water after separation do not have entrainer impurity, and purity is high；
2nd, the water in the aqueous solution of amount containing triethylamine≤5% and the first storage tank isolated to heating by third distillation column again
Secondary rectifying, and be recycled in first rectifying column, the purification amount of triethylamine is improved, the content of triethylamine in water when discharging is reduced；
3rd, separating for several times and layering are carried out by the first condenser and the first return tank, improves three second in purification purity, reduction water
The content of amine；
4th, piece alkali need not be used, aqueous slkali will not be formed and cause secondary pollution.
Brief description of the drawings
Fig. 1 is a kind of structural representation of the separation method implementing procedure of triethylamine and water of the invention.
Fig. 2 shows for the structure that the separation method of a kind of triethylamine and water of the invention implements the first condenser and the first return tank
It is intended to.
Embodiment
A kind of separation method embodiment of triethylamine and water of the invention is described further referring to figs. 1 to Fig. 2.
A kind of separation method of triethylamine and water, comprises the following steps：
First, find that water can also remain in triethylamine by when temperature is more than 18.7 DEG C, triethylamine is slightly soluble in water, and production practices
In solution, it is heated to be layered after 30 DEG C in heater so triethylamine aqueous solution is placed, is separated into the three of water content≤5%
The aqueous solution of ethylamine solution and amount containing triethylamine≤5%, the mixed liquor of triethylamine and water is separated in advance, imports different rectifying
In tower, separation is synchronized, the purity after the rate of departure, and separation is improved.
2nd, the design of pressure of first rectifying column 100 is normal pressure, and the design of pressure of Second distillation column 200 is more than first
The pressure value of rectifying column 100, the pressure value of Second distillation column 200 is preferably 0.3MPa, using in triethylamine-water azeotropic mixture composition
The principle that is reduced with pressure rise of triethylamine content, 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 is condensed from tower top into the first condenser 10 after vaporization, and condensate liquid is collected into the
In one return tank 40, the temperature control of the first return tank 40 is 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 is imported in Second distillation column 200, and triethylamine-water azeotropic mixture steam of the overhead collection of Second distillation column 200 passes through
Second condenser 20 is condensed, and is recycled to by the 3rd flow controller 3 in first rectifying column 100, and water is from first rectifying column 100
Bottom of towe is expelled in the first storage tank 11, triethylamine content≤2% in water in the first storage tank 11, and triethylamine is from Second distillation column
200 bottom of towe are expelled in finished product box 12, and the triethylamine purity in finished product box 12 can reach more than 99.95%.
3rd, due in the water in the first storage 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 one in case 11 is directed into heating in third distillation column 300
Vaporization, triethylamine-water azeotropic mixture steam enters the 3rd condenser 30, the 3rd condenser from the tower top of third distillation column 300 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 backflow
Condensate liquid in tank 50 is separated into the water layer in water layer and triethylamine layer, water content≤5%, the second return tank 50 of triethylamine layer
The triethylamine layer being back to by the 4th flow controller 4 in third distillation column 300, the second return tank 50 passes through the 5th flow control
Device 5 processed imports the multi-cycle separation again of first rectifying column 100, and water is expelled in the second storage tank 13 from the bottom of towe of third distillation column 300,
Amount containing triethylamine≤0.02% in water in second storage 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 the liquid outlet of U-tube 44 is highly more than feed liquor open height, and condensate liquid flows into liquid collecting bucket 41 in advance, in collection
Water is layered in advance with triethylamine in liquid bucket 41, and water layer density flows into water storage chamber 42 compared with conference through the liquid outlet of U-tube 44, due to water
A point liquid 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 the aqueous solution, the aqueous solution of water storage chamber 42 is back on first rectifying column 100, liquid collecting bucket 41 and is additionally provided with triethylamine drawing liquid
Pipe 45, triethylamine layer flows into storage triethylamine chamber 43 by triethylamine liquid suction pipe 45, and storage triethylamine chamber 43 is connected with counter-infiltration
Film 46, triethylamine layer pressurizes and filtered by reverse osmosis membrane 46, because organic solution is difficult to by reverse osmosis membrane, so by anti-
Permeable membrane 46 filters out the moisture content being slightly soluble in triethylamine, and further triethylamine layer is purified, the water content of triethylamine layer
≤ 0.5%, the purity being directed into when in Second distillation column is improved, the moisture filtered out is back to water storage chamber by mozzle 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
End is connected with the top of air collecting chamber 14, and the inlet end of the second condenser pipe 16 is connected with the bottom of air collecting chamber 14, air collecting chamber 14 and first
The tower top of destilling tower 100 is connected, and 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, because aqueous phase is less than the relative steam density of triethylamine to vapour density, so upper strata is mainly water vapour in air collecting chamber 14,
Lower floor is mainly triethylamine steam in air collecting chamber 14, advanced water-filling and the initial gross separation of triethylamine before condensation, then passes through liquid collecting
Struggle against 41 pairs of triethylamines and water secondary clearing again, improves separation purity.
By being connected provided with gas separator 400 between the condenser 30 of third distillation column 300 and the 3rd, 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
Three rectifying columns 300 are connected, and air inlet 402 is connected with water vapour gas outlet 403 by gas filtration film 401, the 3rd condenser 30
Including the 3rd condenser pipe 31 and the 4th condenser pipe 32, water vapour gas outlet 403 passes through the 3rd condenser pipe 31 with third distillation column 300
Connection, triethylamine gas outlet 404 is connected with 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 the condensing reflux of the 3rd condenser pipe 31 to third distillation column 300 from water vapour gas outlet 403, the triethylamine steam not filtered
Condensed from triethylamine gas outlet 404 into the 4th condenser pipe 32, then layering flows back in the second return tank 50, part water vapour leads to
The direct condensing reflux of gas filtration film 401 is crossed to third distillation column 300, the stand-by period needed for layering is reduced, can improve
Water vapour reflux rate, and water vapour by gas filtration 401 direct condensing reflux of film when, the purity of water is higher, reduces three
The backflow of ethamine, that is, improve the rectifying speed 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 control of first return tank 40 and the second return tank 50 makes triethylamine and water secondary clearing again at 30-35 DEG C, temperature
When degree is as between 20-30 DEG C, the layering speed of triethylamine and water gradually increases, and the mutual solubility of water and triethylamine also gradually increases
Plus, when temperature is higher than 35 DEG C, layering speed increase is not obvious, and water content tends to be steady in triethylamine, preferably 30 DEG C, 32 DEG C
With 35 DEG C so temperature control is at 30-35 DEG C, be conducive to the layering of triethylamine and water.
Presently preferred embodiments of the present invention is the foregoing is only, is not intended to limit the invention, those skilled in the art exists
Common variations and alternatives are carried out in the range of technical solution of the present invention all should be comprising within the scope of the present invention.
Claims (6)
1. the separation method of a kind of triethylamine and water, it is characterized in that：Comprise the following steps：
First, 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%；
2nd, the triethylamine solution of water content≤5% is added to first rectifying column, the triethylamine solution of water content≤5% is heated
Vaporization, triethylamine-water azeotropic mixture steam is condensed from tower top into the first condenser after vaporization, and condensate liquid is collected into the first backflow
In tank, condensate liquid is layered in the first return tank, and the water layer formed in water layer and triethylamine layer, the first return tank is back to first
In rectifying column, the triethylamine layer in the first return tank is imported in Second distillation column, triethylamine-water of Second distillation column overhead collection
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 bottom of towe
In one storage tank, triethylamine is expelled in finished product box from Second distillation column bottom of towe, and the design of pressure of first rectifying column is normal pressure,
The design of pressure of Second distillation column is more than the pressure value of first rectifying column；
3rd, the water in the aqueous solution of the amount containing triethylamine isolated in heater≤5% and the first storage tank is directed into the 3rd essence
Heating vaporization in tower is evaporated, triethylamine-water azeotropic mixture steam enters the 3rd condenser from third distillation column tower top after vaporization, and the 3rd is cold
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,
Water layer in second return tank be back in third distillation column, the second return tank triethylamine layer import first rectifying column, water from
Third distillation column bottom of towe is expelled in the second storage tank.
2. the separation method of a kind of triethylamine according to claim 1 and water, it is characterized in that：First return tank and
Controlled between one rectifying column by first flow controller, pass through second flow control between the first return tank and Second distillation column
Device is controlled, and is controlled between the second condenser and first rectifying column by the 3rd flow measuring unit, the second return tank and third distillation column it
Between by the 4th flow controller control, between the second return tank and first rectifying column pass through the 5th flow controller control.
3. the separation method of a kind of triethylamine according to claim 1 and water, it is characterized in that：First return tank includes
Liquid collecting bucket, water storage chamber and storage triethylamine chamber, liquid collecting bucket bottom are communicated with U-tube, and U-tube liquid outlet is highly more than inlet
Highly, condensate liquid flows into liquid collecting bucket in advance, and water is layered in advance with triethylamine in liquid collecting bucket, and water layer flows into storage through U-tube outlet
Water chamber, the aqueous solution of water storage chamber, which is back on first rectifying column, liquid collecting bucket, is additionally provided with triethylamine liquid suction pipe, and triethylamine layer is logical
Cross triethylamine liquid suction pipe and flow into storage triethylamine chamber, storage triethylamine chamber is connected with reverse osmosis membrane, and triethylamine layer pressurizes and passed through
Reverse osmosis membrane filtration, filters out the moisture being slightly soluble in triethylamine, and the moisture filtered out is back to water storage chamber, and three after filtering
Ethamine is directed into Second distillation column.
4. the separation method of a kind of triethylamine according to claim 2 and water, it is characterized in that：First condenser includes
Air collecting chamber, the first condenser pipe and the second condenser pipe, the inlet end of the first condenser pipe are connected with air collecting chamber top, the second condenser pipe
Inlet end is connected with the bottom of air collecting chamber, and air collecting chamber is connected with the first overhead, and liquid collecting bucket also accordingly uses two, respectively
For connect upper strata in the first condenser pipe and the second condenser pipe, air collecting chamber be mainly in water vapour, air collecting chamber lower floor be mainly three
Ethamine steam, advanced water-filling and the initial gross separation of triethylamine before condensation, then be layered by the first return tank.
5. the separation method of a kind of triethylamine according to claim 1 and water, it is characterized in that：The third distillation column and
By being connected provided with gas separator between three condensers, gas separator includes gas filtration film, air inlet, water vapour outlet
Mouthful and triethylamine gas outlet, the 3rd condenser include the 3rd condenser pipe and the 4th condenser pipe, triethylamine-water azeotropic vaporization pressurize into
Enter air inlet, by gas filtration membrane filtration, water vapour flows back from water vapour gas outlet into the 3rd condensing tube condensation 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 in tank and be layered.
6. the separation method of a kind of triethylamine according to claim 1 and water, 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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| CN108658785A (en) * | 2017-09-08 | 2018-10-16 | 杭州九清科技有限公司 | The separation method of difficult separation system containing triethylamine |
| CN109369419A (en) * | 2018-12-03 | 2019-02-22 | 烟台国邦化工机械科技有限公司 | The process and device of triethylamine are separated in a kind of industrial wastes |
| CN109607920A (en) * | 2018-12-28 | 2019-04-12 | 浙江建业化工股份有限公司 | UF membrane-hydrolysis process waste water ethamine production system and technique |
| 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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| CN109369419A (en) * | 2018-12-03 | 2019-02-22 | 烟台国邦化工机械科技有限公司 | The process and device of triethylamine are separated in a kind of industrial wastes |
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Address after: 317000 Taizhou City, Zhejiang Province, chemical raw material base Lin Hai Park Patentee after: Zhejiang Taizhou Lianchuang Environmental Protection Technology Co., Ltd. Address before: 317016 Zhejiang province Taizhou Zhejiang chemical raw material base Seaside Park Patentee before: Zhejiang Taizhou LIAN Environmental Protection Technology Co., Ltd. |