CN102452925A - Method for separating acetic acid from water - Google Patents
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- CN102452925A CN102452925A CN2010105298409A CN201010529840A CN102452925A CN 102452925 A CN102452925 A CN 102452925A CN 2010105298409 A CN2010105298409 A CN 2010105298409A CN 201010529840 A CN201010529840 A CN 201010529840A CN 102452925 A CN102452925 A CN 102452925A
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Abstract
The invention relates to a method for separating acetic acid from water, which mainly solves the problems of high energy consumption and high operating cost in an acetic acid dehydration process in the prior art. In the invention, distillation and dehydration are carried out by pressurizing an acetic acid dehydration tower, water is used as a heat exchange medium in heat pump circulation, the heat released by condensing the discharged material at the top of the acetic acid dehydration tower is absorbed by a heat exchange medium in a closed heat pump process, the heat exchange medium after absorbing the energy of the discharged material at the top of the tower is compressed by a compressor so as to raise temperature, the high-temperature steam is used for carrying out heat exchange with the discharged material at the bottom of the tower in a tower kettle reboiler, the steam subjected to heat exchange in the tower kettle enters a gas-liquid separation tank after decompression, the separated liquid phase enters a condenser at the top of the tower to carry out heat exchange, and the separated gas phase is mixed with the gas at the outlet of the condenser at the top of the tower to enter the compressor, thereby being used for carrying out heat exchange again with the tower kettle. The technical scheme provided by the invention better solves the problems and can be applied to industrial production for separating acetic acid from water.
Description
Technical field
The present invention relates to a kind of method that is used for separating acetic acid and water.
Background technology
Produce in the process of terephthalic acid at p xylene oxidation, use acetic acid usually as organic solvent.The big water gaging that generates in the oxidising process has diluted acetate solvate, and the acetate solvate of reaction needed suitable concn.In order to guarantee the concentration of acetic acid in the solvent, use acetic acid dehydrating tower to isolate water unnecessary in the solvent usually.Along with production-scale expansion, the process cost of acetic acid dehydrating tower grows to even greater heights.
Conventional direct rectifying and dewatering is owing to the less cause of relative volatility when the acetic acid lower concentration; Usually adopt the method that increases stage number and increase reflux ratio to reduce the concentration of acetic acid in the cat head discharging, the plant investment cost is risen.Consider from economy on the engineering that general cat head acetate concentration requires to be lower than 0.8 weight %, the cat head discharging is discharged as waste water.
Document GB1576787 discloses method separating acetic acid and the water that adopts azeotropic distillation.This method adopts the series connection of two towers, and first tower is entrainer with the acetates, and the cat head discharging is the aqueous solution of acetic acid, and wherein acetate concentration is less than 0.1 weight %, and acetates is about 5 weight %, and the aqueous solution also contains the minor by-products ritalin.Acetates entrainer in second tower recycle-water returns a tower.The steam consumption of adopting said method generally is 60% of simple rectifying.Cat head concentration can be controlled at 0.1 weight %.The simple rectifying of this method has significantly reduced energy consumption, has also reclaimed more acetic acid.Still can contain acetate in minute ester class in the waste water after but two towers reclaim, and the price of acetates is higher, so acetic acid consumption has been offset in entrainer consumption; And acetates is inflammable medium, during practical applications, also need increase the expense of safety features.
Heat pump distillation has been widely used in the various chemical processs as a kind of power-saving technology that can effectively improve rectified heat efficient.But possibly there is gas-liquid two-phase in the heat transferring medium water in the heat pump when getting into condensing surface, can cause equipment loss, and process cost increases.
In a word, exist acetic acid dehydration process energy consumption high in the prior art, the problem that process cost is high.
Summary of the invention
Technical problem to be solved by this invention is to exist acetic acid dehydration process energy consumption high in the prior art, and the problem that process cost is high provides a kind of new method that is used for separating acetic acid and water.It is low that this method has energy consumption, the characteristics that process cost is low.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is following: a kind of method that is used for separating acetic acid and water may further comprise the steps:
A) aqueous acetic acid 1 gets into acetic acid dehydrating tower 2 from the middle part, and after rectifying separation, cat head obtains gaseous stream 3, and the tower still obtains liquid phase stream 7; Logistics 3 is divided into logistics 5 and logistics 6 after condensing surface 4 heat exchange condensations, logistics 5 gets into flow as the overhead product discharging, and acetic acid dehydrating tower 2 tops are returned in logistics 6; Logistics 7 is divided into logistics 9 and logistics 10 after reboiler 8 heat exchange, acetic acid dehydrating tower 2 bottoms are returned in logistics 9, and logistics 10 gets into flow as the discharging of tower still product;
B) heat transferring medium water is vaporizated into water vapor after condensing surface 4 and gaseous stream 3 heat exchange, and water vapor gets into compressor 11 compressions and heats up, and the water vapor after the intensification gets into reboiler 8 and tower bottoms logistics 7 heat exchange mutually; Water vapor in reboiler 8 after the heat exchange gets into knockout drum 13 after reducing pressure through expenditure and pressure equipment 12, after the gas-liquid separation, obtains liquid phase stream 15 and gaseous stream 14; Gaseous stream 14 gets into compressor 11; Liquid phase stream 15 get into overhead condensers 4 once more with gaseous stream 3 heat exchange.
In the technique scheme, the operational condition of acetic acid dehydrating tower 2: the stage number preferable range is 60～120, and more selecting scope is 80～100; Tower still temperature preferable range is 105～160 ℃, and more preferably scope is 110～150 ℃; The tower top temperature preferable range is 100～135 ℃, and more preferably scope is 100～125 ℃; The working pressure preferable range is 0.1～0.4MPa, and more preferably scope is 0.1～0.25MPa; Logistics 6 is 0.5～10 with the weight ratio preferable range of logistics 5, and more preferably scope is 2～4; Logistics 9 is 1～17 with the weight ratio preferable range of logistics 10, and more preferably scope is 4～9.The operational condition of condensing surface 4: tube side working pressure preferable range is 0.1～0.4MPa, and more preferably scope is 0.1～0.25MPa; The service temperature preferable range is 100～135 ℃, and more preferably scope is 100～125 ℃.Shell side working pressure preferable range is 0.1～0.3MPa, and more preferably scope is 0.1～0.25MPa; The service temperature preferable range is 100～125 ℃, and more preferably scope is 100～120 ℃.The operational condition of reboiler 8: tube side working pressure preferable range is 0.1～0.4MPa, and more preferably scope is 0.1～0.25MPa; The service temperature preferable range is 105～160 ℃, and more preferably scope is 110～150 ℃.Shell side working pressure preferable range is 0.15～0.8MPa, and more preferably range operation is 0.25～0.7MPa; The temperature preferable range is 110～400 ℃, and more preferably scope is 130～400 ℃.The operational condition of knockout drum 13: the working pressure preferable range is 0.1～0.3MPa, and more preferably scope is 0.1～0.25Mpa; The service temperature preferable range is 100～125 ℃, and more preferably scope is 100～120 ℃.By weight percentage, the content of acetic acid is 20～80% in the aqueous acetic acid 1, and the content of water is 20～80%.Heat transferring medium water preferred version is a shell side of walking condensing surface 4 and reboiler 8, and logistics 3 preferred versions are the tube side of walking condensing surface 4, and logistics 7 preferred versions are the tube side of walking reboiler 8.
In the inventive method, heat transferring medium water is after condensing surface 4 and gaseous stream 3 heat exchange, and the temperature preferable range of the water vapor that obtains is 100～125 ℃, and the pressure preferable range is 0.1～0.3MPa.Water vapor is after compressor compresses heats up, and the temperature preferable range is 110～400 ℃, and the pressure preferable range is 0.15～0.8MPa.After water vapor entering reboiler 8 after the intensification was given tower bottoms phase logistics 7 heating, the temperature preferable range was 110～180 ℃, and the pressure preferable range is 0.1～0.8MPa.After water vapor in reboiler 8 after the heat exchange got into 12 decompressions of expenditure and pressure equipment, the temperature preferable range was 100～125 ℃, and the pressure preferable range is 0.1～0.3MPa.
The inventive method is on the basis of acetic acid conventional rectification dehydration tower production equipment; Carry out pressurized operation through the Dichlorodiphenyl Acetate dehydration tower, and set up a cover enclosed heat pump circulating system, with water as heat transferring medium; Overhead condenser heat-obtaining from the lower temperature position; After compressor compresses, improve energy grade, be used for the heat supply of tower still reboiler, reached energy saving purposes.The inventive method heat transferring medium is after reboiler and tower still logistics heat exchange; Separate gas-liquid two-phase through knockout drum; Only be that the liquid phase that obtains is used for the overhead condenser heat exchange once more; Avoid gas-liquid two-phase to get into condensing surface simultaneously and caused equipment loss, improved the stability of overhead condenser, reduced process cost.Compare with the direct rectifying and dewatering technical process of routine, adopt the inventive method, energy consumption descends 50～80%; Simultaneously, in the heat pump cycle flow process, increased knockout drum after, the device operational stability improves, and has obtained better technical effect.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Among Fig. 1,1 is the aqueous acetic acid charging, and 2 is acetic acid dehydrating tower, and 3 is the discharging of cat head gas phase; 4 is overhead condenser, and 5 is the overhead product discharging, and 6 are trim the top of column stream strand, and 7 is liquid phase discharging at the bottom of the tower; 8 is reboiler, and 9 is reflow stream thigh at the bottom of the tower, and 10 is dense acetate products discharging, and 11 is compressor; 12 is expenditure and pressure equipment, and 13 is knockout drum, and 14 is the gas phase heat transferring medium that knockout drum, and 15 is the liquid phase heat transferring medium that knockout drum.
Among Fig. 1, for the process stream flow process, raw material dilute acetic acid aqueous solution 1 gets into acetic acid dehydrating tower 2 from the middle part, and after conventional simple rectifying separation, cat head obtains gaseous stream 3, and the tower still obtains liquid phase stream 7.Logistics 3 is divided into logistics 5 and logistics 6 after condensing surface 4 heat exchange condensations.Logistics 5 is the aqueous solution of acetic acid content≤1 weight %, and it gets into flow as the overhead product discharging.Acetic acid dehydrating tower 2 tops are returned in logistics 6.Logistics 7 is divided into logistics 9 and logistics 10 after reboiler 8 heat exchange.Acetic acid dehydrating tower 2 bottoms are returned in logistics 9.Logistics 10 is the aqueous acetic acid of 90～95 weight % for acetic acid content, and it gets into flow as the discharging of tower still product.
For the heat pump cycle flow process, with water as heat transferring medium.Heat transferring medium water is vaporizated into water vapor after condensing surface 4 and gaseous stream 3 heat exchange, water vapor gets into compressor 11 compressions and heats up, and the water vapor after the intensification gets into reboiler 8 and tower bottoms logistics 7 heat exchange mutually; Water vapor in reboiler 8 after the heat exchange gets into knockout drum 13 after getting into expenditure and pressure equipment (like orifice plate, valve) 12 decompressions, after the gas-liquid separation, obtains liquid phase stream 15 and gaseous stream 14; Gaseous stream 14 gets into compressor 11; Liquid phase stream 15 get into overhead condensers 4 once more with gaseous stream 3 heat exchange.Be that the heat that acetic acid dehydration column overhead discharging condensation discharges absorbs through the heat transferring medium in the enclosed heat pump flowsheet; The heat transferring medium absorption tower ejects the energy of material after the temperature rising of overdraft machine compression back; Be used for discharging heat exchange at the bottom of tower reboiler and the tower, knockout drum is used to separate the heat transferring medium behind expenditure and pressure.
Through embodiment the present invention is done further elaboration below.
Embodiment
[Comparative Examples 1]
Dilute acetic acid aqueous solution adopts the mode of conventional rectification to dewater no heat pump cycle flow process.Acetate concentration is 38 quality % in the charging dilute acetic acid aqueous solution, and acetate concentration is greater than 94 quality % in the discharging at the bottom of the acetic acid dehydration Tata, and acetate concentration is less than 0.1 quality % in the cat head discharging.
The operational condition of acetic acid dehydrating tower is: stage number is 89, and tower still temperature is 131 ℃, and tower top temperature is 99.5 ℃, and the cat head working pressure is 0.11MPa, and tower still working pressure is 0.19MPa, and the overhead condenser reflux ratio is 3.2, and tower still reboiler reflux ratio is 6.3.
The operational condition of condensing surface 4 is: the tube side working pressure is 0.11MPa, and service temperature is 99.5 ℃; Shell side working pressure 0.55MPa, 33 ℃ of temperature ins, 43 ℃ of temperature outs.
The operational condition of reboiler 8 is: the tube side working pressure is 0.19MPa, and service temperature is 131 ℃; The shell side working pressure is 0.4MPa, and service temperature is 143 ℃.
The energy expenditure situation is seen table 1.
[embodiment 1]
Adopt flow process shown in Figure 1, aqueous acetic acid 1 (wherein acetate concentration is 38 quality %) gets into acetic acid dehydrating tower 2 from the middle part, and after rectifying separation, cat head obtains gaseous stream 3, and the tower still obtains liquid phase stream 7; Logistics 3 is divided into logistics 5 and logistics 6 after condensing surface 4 heat exchange condensations, logistics 5 gets into flow as the overhead product discharging, and acetic acid dehydrating tower 2 tops are returned in logistics 6; Logistics 7 is divided into logistics 9 and logistics 10 after reboiler 8 heat exchange, 2 bottoms are returned in logistics 9, and logistics 10 gets into flow as the discharging of tower still product.Acetate concentration is greater than 94 quality % in the discharging at the bottom of the acetic acid dehydration Tata, and acetate concentration is less than 0.1 quality % in the cat head discharging.
Heat transferring medium water is vaporizated into water vapor after condensing surface 4 and gaseous stream 3 heat exchange, water vapor gets into compressor 11 compressions and heats up, and the water vapor after the intensification gets into reboiler 8 and tower bottoms logistics 7 heat exchange mutually; Water vapor in reboiler 8 after the heat exchange gets into knockout drum 13 after getting into valve 12 decompressions, after the gas-liquid separation, obtains liquid phase stream 15 and gaseous stream 14; Gaseous stream 14 gets into compressor 11; Liquid phase stream 15 get into overhead condensers 4 once more with gaseous stream 3 heat exchange.
Wherein, the operational condition of acetic acid dehydrating tower 2: stage number is 89, and tower still temperature is 139 ℃; Tower top temperature is 111 ℃, and the cat head working pressure is 0..16MPa, and tower still working pressure is 0.24MPa; Logistics 6 is 3.4 with the weight ratio of logistics 5, and logistics 9 is 6.5 with the weight ratio of logistics 10.
The operational condition of condensing surface 4 is: the tube side working pressure is 0.16MPa, and service temperature is 111 ℃; Shell side working pressure 0.1MPa, service temperature is 100 ℃.
The operational condition of reboiler 8 is: the tube side working pressure is 0.24MPa, and service temperature is 139 ℃; The shell side working pressure is 0.6MPa, 363 ℃ of temperature ins, 159 ℃ of temperature outs.
The operational condition of knockout drum 13: working pressure is 0.1MPa, and service temperature is 100 ℃.
Compare with the heat pump cycle technology of no knockout drum, after the inventive method increased knockout drum, the condensing surface operational stage was more stable.When having gas phase in the logistics, the entering of gas phase part can cause the vibrations of condensing surface, loss equipment; After the gas phase part was separated, the entering of pure liquid phase stream can make the condensing surface stable operation, thereby improved the work-ing life of device, reduced process cost.
The energy expenditure situation is seen table 1.
Table 1
Annotate: steam consumption quantity numerical value is that negative indication is externally exported steam.
Can find out from table 1, compare with compression rectification, 1 ton of dense acetic acid-aqueous solution of every production, the inventive method increases the about energy consumption 64.4% of heat pump cycle flow process deutomerite.
[Comparative Examples 2]
With [embodiment 1], just there is not knockout drum, all the other operational conditions are constant.Be that heat transferring medium water is vaporizated into water vapor after condensing surface 4 and gaseous stream 3 heat exchange, water vapor gets into compressor 11 compressions and heats up, and the water vapor after the intensification gets into reboiler 8 and tower bottoms logistics 7 heat exchange mutually; After water vapor in reboiler 8 after the heat exchange gets into valve 12 decompressions, be back to condensing surface 4 once more with 3 heat exchange of cat head gaseous stream.
Heat transferring medium because gas phase directly gets into condensing surface in company with liquid phase, has caused the vibrations of condensing surface after valve 12 decompressions, influenced the work-ing life of condensing surface, and process cost is increased.
Claims (6)
1. method that is used for separating acetic acid and water may further comprise the steps:
A) aqueous acetic acid (1) gets into acetic acid dehydrating tower (2) from the middle part, and after rectifying separation, cat head obtains gaseous stream (3), and the tower still obtains liquid phase stream (7); Logistics (3) is divided into logistics (5) and logistics (6) after condensing surface (4) heat exchange condensation, logistics (5) gets into flow as the overhead product discharging, and acetic acid dehydrating tower (2) top is returned in logistics (6); Logistics (7) is divided into logistics (9) and logistics (10) after reboiler (8) heat exchange, acetic acid dehydrating tower (2) bottom is returned in logistics (9), and logistics (10) gets into flow as the discharging of tower still product;
B) heat transferring medium water is vaporizated into water vapor after condensing surface (4) and gaseous stream (3) heat exchange, and water vapor gets into compressor (11) compression and heats up, and the water vapor after the intensification gets into reboiler (8) and tower bottoms logistics mutually (7) heat exchange; Water vapor in reboiler (8) after the heat exchange gets into knockout drum (13) after reducing pressure through expenditure and pressure equipment (12), after the gas-liquid separation, obtains liquid phase stream (15) and gaseous stream (14); Gaseous stream (14) gets into compressor (11); Liquid phase stream (15) get into overhead condenser (4) once more with gaseous stream (3) heat exchange.
2. the method that is used for separating acetic acid and water according to claim 1; The operational condition that it is characterized in that acetic acid dehydrating tower (2): stage number is 60～120; Tower still temperature is 105～160 ℃, and tower top temperature is 100～135 ℃, and working pressure is 0.1～0.4MPa; Logistics (6) is 0.5～10 with the weight ratio of logistics (5), and logistics (9) is 1～17 with the weight ratio of logistics (10);
The operational condition of condensing surface (4): the tube side working pressure is 0.1～0.4MPa, and service temperature is 100～135 ℃; Shell side working pressure 0.1～0.3MPa, service temperature is 100～125 ℃;
The operational condition of reboiler (8): the tube side working pressure is 0.1～0.4MPa, and service temperature is 105～160 ℃; The shell side working pressure is 0.15～0.8MPa, and service temperature is 110～400 ℃.
The operational condition of knockout drum (13): working pressure is 0.1～0.3MPa, and service temperature is 100～125 ℃.
3. the method that is used for separating acetic acid and water according to claim 2; The operational condition that it is characterized in that acetic acid dehydrating tower (2): stage number is 80～100; Tower still temperature is 110～150 ℃, and tower top temperature is 100～125 ℃, and working pressure is 0.1～0.25MPa; Logistics (6) is 2～4 with the weight ratio of logistics (5), and logistics (9) is 4～9 with the weight ratio of logistics (10);
The operational condition of condensing surface (4): the tube side working pressure is 0.1～0.25MPa, and service temperature is 100～125 ℃; Shell side working pressure 0.1～0.25MPa, service temperature is 100～120 ℃; The operational condition of reboiler (8): the tube side working pressure is 0.1～0.25MPa, and service temperature is 110～150 ℃; The shell side working pressure is 0.25～0.7MPa, and service temperature is 130～400 ℃;
The operational condition of knockout drum (13): working pressure is 0.1～0.25MPa, and service temperature is 100～120 ℃.
4. the method that is used for separating acetic acid and water according to claim 1 is characterized in that by weight percentage, and the content of acetic acid is 20～80% in the aqueous acetic acid (1), and the content of water is 20～80%.
5. the method that is used for separating acetic acid and water according to claim 1 is characterized in that heat transferring medium water walks the shell side of condensing surface (4) and reboiler (8), and the tube side of condensing surface (4) is walked in logistics (3), and the tube side of reboiler (8) is walked in logistics (7).
6. the method that is used for separating acetic acid and water according to claim 1 is characterized in that expenditure and pressure equipment is selected from orifice plate or valve.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010529840.9A CN102452925B (en) | 2010-11-03 | 2010-11-03 | Method for separating acetic acid from water |
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| CN201010529840.9A CN102452925B (en) | 2010-11-03 | 2010-11-03 | Method for separating acetic acid from water |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285612A (en) * | 2013-01-09 | 2013-09-11 | 天津大学 | No-compressor heat-pump rectifying device and operation method thereof |
| CN102875329B (en) * | 2012-10-22 | 2016-04-20 | 莒南县凯利化工有限公司 | A kind of heat pump distillation is separated technique and the device of primary isoamyl alcohol isomers |
| CN111302922A (en) * | 2020-03-27 | 2020-06-19 | 北京诺维新材科技有限公司 | Rectification separation method and rectification system |
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| US20070068792A1 (en) * | 2005-09-23 | 2007-03-29 | Jang Jiyoung | System and method for acetic acid dehydration |
| WO2007055386A1 (en) * | 2005-11-14 | 2007-05-18 | Nichirei Industries Co., Ltd. | Gas-liquid separator and refrigerating apparatus equipped therewith |
| CN101172941A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for recycling acetic acid in dilute acetic acid |
| CN101704524A (en) * | 2009-11-20 | 2010-05-12 | 天津大学 | Production device and method of high purity trichlorosilane by using heat pump distillation |
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2010
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4824527A (en) * | 1986-06-10 | 1989-04-25 | Erickson Donald C | Nested enrichment cascade distillation of unequal mixtures |
| US20070068792A1 (en) * | 2005-09-23 | 2007-03-29 | Jang Jiyoung | System and method for acetic acid dehydration |
| WO2007055386A1 (en) * | 2005-11-14 | 2007-05-18 | Nichirei Industries Co., Ltd. | Gas-liquid separator and refrigerating apparatus equipped therewith |
| CN101172941A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for recycling acetic acid in dilute acetic acid |
| CN101704524A (en) * | 2009-11-20 | 2010-05-12 | 天津大学 | Production device and method of high purity trichlorosilane by using heat pump distillation |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875329B (en) * | 2012-10-22 | 2016-04-20 | 莒南县凯利化工有限公司 | A kind of heat pump distillation is separated technique and the device of primary isoamyl alcohol isomers |
| CN103285612A (en) * | 2013-01-09 | 2013-09-11 | 天津大学 | No-compressor heat-pump rectifying device and operation method thereof |
| CN111302922A (en) * | 2020-03-27 | 2020-06-19 | 北京诺维新材科技有限公司 | Rectification separation method and rectification system |
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