CN102452925B - Method for separating acetic acid from water - Google Patents
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- CN102452925B CN102452925B CN201010529840.9A CN201010529840A CN102452925B CN 102452925 B CN102452925 B CN 102452925B CN 201010529840 A CN201010529840 A CN 201010529840A CN 102452925 B CN102452925 B CN 102452925B
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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 for separating of acetic acid and water.
Background technology
At p xylene oxidation, produce in the process of terephthalic acid, conventionally use acetic acid as organic solvent.The large water gaging generating in 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 solvent, conventionally use acetic acid dehydrating tower to isolate water unnecessary in solvent.Along with production-scale expansion, the process cost of acetic acid dehydrating tower grows to even greater heights.
Conventional direct rectifying and dewatering is due to the less cause of relative volatility when the acetic acid lower concentration, conventionally adopt and increase the concentration that the method for stage number and increase reflux ratio reduces acetic acid in tower top discharging, when causing energy consumption index high, also make plant investment cost increase.In engineering, for economy, consider, general tower top acetate concentration requires lower than 0.8 % by weight, and tower top discharging is discharged as waste water.
Document GB1576787 discloses method separating acetic acid and the water that adopts azeotropic distillation.This method adopts cascade towers, and first tower be take acetates as entrainer, and tower top discharging is vinegar aqueous acid, and wherein acetate concentration is less than 0.1 % by weight, and acetates is about 5 % by weight, and the aqueous solution also contains a small amount of by-product methyl acetate.Acetates entrainer in second tower recycle-water, returns to a tower.The steam consumption of adopting said method is generally 60% of simple rectifying.Tower top concentration can be controlled at 0.1 % by weight.The simpler rectifying of this method has significantly reduced energy consumption, has also reclaimed more acetic acid.In the waste water after but two towers reclaim, still can contain acetate in minute ester class, and the price of acetates is higher, so acetic acid consumption has been offset in entrainer consumption; And acetates is inflammable medium, during engineering application, also need to increase the expense of safety features.
Heat pump distillation, as a kind of power-saving technology that can effectively improve rectified heat efficiency, has been widely used in various chemical processs.But the heat transferring medium water in heat pump may exist gas-liquid two-phase while entering condenser, can cause equipment loss, process cost increases.
In a word, in prior art, exist acetic acid dehydration process energy consumption high, the problem that process cost is high.
Summary of the invention
Technical problem to be solved by this invention is in prior art, to exist acetic acid dehydration process energy consumption high, and the problem that process cost is high provides a kind of new method for separating of acetic acid and water.It is low that the method has energy consumption, the feature that process cost is low.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method for separating of acetic acid and water, comprises the following steps:
A) aqueous acetic acid 1 enters acetic acid dehydrating tower 2 from middle part, and after rectifying separation, tower top obtains gaseous stream 3, and tower reactor obtains liquid phase stream 7; Logistics 3, after condenser 4 heat exchange condensations, is divided into logistics 5 and logistics 6, and as overhead product, discharging enters follow-up flow process in logistics 5, and acetic acid dehydrating tower 2 tops are returned in logistics 6; Logistics 7, after reboiler 8 heat exchange, is divided into logistics 9 and logistics 10, and acetic acid dehydrating tower 2 bottoms are returned in logistics 9, and logistics 10 enters follow-up flow process as tower reactor product discharge;
B) heat transferring medium water is vaporizated into water vapor after condenser 4 and gaseous stream 3 heat exchange, and water vapor enters compressor 11 compressions and heats up, and the water vapor after intensification enters reboiler 8 and 7 heat exchange of tower reactor liquid phase stream; Water vapor in reboiler 8 after heat exchange enters knockout drum 13 after reducing pressure by expenditure and pressure equipment 12, after gas-liquid separation, obtains liquid phase stream 15 and gaseous stream 14; Gaseous stream 14 enters compressor 11; Liquid phase stream 15 enter overhead condenser 4 again with gaseous stream 3 heat exchange.
In technique scheme, the operational condition of acetic acid dehydrating tower 2: stage number preferable range is 60～120, more selecting scope is 80～100; Tower reactor temperature preferable range is 105～160 ℃, and more preferably scope is 110～150 ℃; Tower top temperature preferable range is 100～135 ℃, and more preferably scope is 100～125 ℃; 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 condenser 4: tube side working pressure preferable range is 0.1～0.4MPa, more preferably scope is 0.1～0.25MPa; 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; 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, more preferably scope is 0.1～0.25MPa; 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; Temperature preferable range is 110～400 ℃, and more preferably scope is 130～400 ℃.The operational condition of knockout drum 13: working pressure preferable range is 0.1～0.3MPa, more preferably scope is 0.1～0.25Mpa; Service temperature preferable range is 100～125 ℃, and more preferably scope is 100～120 ℃.By weight percentage, in aqueous acetic acid 1, the content of acetic acid is 20～80%, and the content of water is 20～80%.Heat transferring medium water preferred version is the shell side of walking condenser 4 and reboiler 8, and logistics 3 preferred versions are the tube side of walking condenser 4, and logistics 7 preferred versions are the tube side of walking reboiler 8.
In the inventive method, heat transferring medium water is after condenser 4 and gaseous stream 3 heat exchange, and the temperature preferable range of the water vapor obtaining is 100～125 ℃, and pressure preferable range is 0.1～0.3MPa.Water vapor is after compressor compression heats up, and temperature preferable range is 110～400 ℃, and pressure preferable range is 0.15～0.8MPa.Water vapor after intensification enter reboiler 8 to 7 heating of tower reactor liquid phase stream after, temperature preferable range is 110～180 ℃, pressure preferable range is 0.1～0.8MPa.Water vapor in reboiler 8 after heat exchange enters after 12 decompressions of expenditure and pressure equipment, and temperature preferable range is 100～125 ℃, and pressure preferable range is 0.1～0.3MPa.
The inventive method is on the basis of acetic acid conventional rectification dehydration tower production equipment, by Dichlorodiphenyl Acetate dehydration tower, carry out pressurized operation, and set up a set of enclosed heat pump circulating system, using water as heat transferring medium, overhead condenser heat-obtaining from lower temperature position, after compressor compression, improve energy grade, for the heat supply of tower reactor reboiler, reached energy-saving and cost-reducing object.The inventive method heat transferring medium is after reboiler and tower reactor logistics heat exchange, through the separated gas-liquid two-phase of knockout drum, only again for overhead condenser heat exchange by the liquid phase obtaining, avoided gas-liquid two-phase to enter condenser simultaneously and caused equipment loss, the stability that has improved overhead condenser, has reduced process cost.Compare with the direct rectifying and dewatering technical process of routine, adopt the inventive method, energy consumption declines 50～80%; , in heat pump cycle flow process, increased after knockout drum, device operational stability improves, and has obtained good technique effect meanwhile.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
In Fig. 1,1 is aqueous acetic acid charging, and 2 is acetic acid dehydrating tower, 3 is top gaseous phase discharging, and 4 is overhead condenser, and 5 is overhead product discharging, 6 are trim the top of column stream strand, and 7 is liquid phase discharging at the bottom of tower, and 8 is reboiler, 9 is reflow stream thigh at the bottom of tower, and 10 is dense acetate products discharging, and 11 is compressor, 12 is expenditure and pressure equipment, 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.
In Fig. 1, for process stream flow process, raw material dilute acetic acid aqueous solution 1 enters acetic acid dehydrating tower 2 from middle part, and after the simple rectifying separation of routine, tower top obtains gaseous stream 3, and tower reactor obtains liquid phase stream 7.Logistics 3, after condenser 4 heat exchange condensations, is divided into logistics 5 and logistics 6.Logistics 5 is the aqueous solution of acetic acid content≤1 % by weight, and as overhead product, discharging enters follow-up flow process for it.Acetic acid dehydrating tower 2 tops are returned in logistics 6.Logistics 7, after reboiler 8 heat exchange, is divided into logistics 9 and logistics 10.Acetic acid dehydrating tower 2 bottoms are returned in logistics 9.Logistics 10 for acetic acid content be the aqueous acetic acid of 90～95 % by weight, it enters follow-up flow process as tower reactor product discharge.
For heat pump cycle flow process, using water as heat transferring medium.Heat transferring medium water is vaporizated into water vapor after condenser 4 and gaseous stream 3 heat exchange, and water vapor enters compressor 11 compressions and heats up, and the water vapor after intensification enters reboiler 8 and 7 heat exchange of tower reactor liquid phase stream; Water vapor in reboiler 8 after heat exchange enters after expenditure and pressure equipment (as orifice plate, valve) 12 decompressions, enters knockout drum 13, after gas-liquid separation, obtains liquid phase stream 15 and gaseous stream 14; Gaseous stream 14 enters compressor 11; Liquid phase stream 15 enter overhead condenser 4 again with gaseous stream 3 heat exchange.Be that the heat that acetic acid dehydration column overhead discharging condensation discharges absorbs by the heat transferring medium in enclosed heat pump flowsheet, the energy that heat transferring medium absorption tower ejects material raises by the rear temperature of overdraft machine compression, for discharging heat exchange at the bottom of tower reboiler and tower, knockout drum is for separating of the heat transferring medium after expenditure and pressure.
Below by embodiment, the present invention is further elaborated.
Embodiment
[comparative example 1]
Dilute acetic acid aqueous solution adopts the mode of conventional rectification to dewater, without heat pump cycle flow process.In charging dilute acetic acid aqueous solution, acetate concentration is 38 quality %, and at the bottom of acetic acid dehydrating tower tower, in discharging, acetate concentration is greater than 94 quality %, and in tower top discharging, acetate concentration is less than 0.1 quality %.
The operational condition of acetic acid dehydrating tower is: stage number is 89, and tower reactor temperature is 131 ℃, and tower top temperature is 99.5 ℃, and tower top working pressure is 0.11MPa, and tower reactor working pressure is 0.19MPa, and overhead condenser reflux ratio is 3.2, and tower reactor reboiler reflux ratio is 6.3.
The operational condition of condenser 4 is: 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: tube side working pressure is 0.19MPa, and service temperature is 131 ℃; Shell side working pressure is 0.4MPa, and service temperature is 143 ℃.
Energy Expenditure Levels is in Table 1.
[embodiment 1]
Adopt flow process shown in Fig. 1, aqueous acetic acid 1 (wherein acetate concentration is 38 quality %) enters acetic acid dehydrating tower 2 from middle part, and after rectifying separation, tower top obtains gaseous stream 3, and tower reactor obtains liquid phase stream 7; Logistics 3, after condenser 4 heat exchange condensations, is divided into logistics 5 and logistics 6, and as overhead product, discharging enters follow-up flow process in logistics 5, and acetic acid dehydrating tower 2 tops are returned in logistics 6; Logistics 7, after reboiler 8 heat exchange, is divided into logistics 9 and logistics 10, and 2 bottoms are returned in logistics 9, and logistics 10 enters follow-up flow process as tower reactor product discharge.At the bottom of acetic acid dehydrating tower tower, in discharging, acetate concentration is greater than 94 quality %, and in tower top discharging, acetate concentration is less than 0.1 quality %.
Heat transferring medium water is vaporizated into water vapor after condenser 4 and gaseous stream 3 heat exchange, and water vapor enters compressor 11 compressions and heats up, and the water vapor after intensification enters reboiler 8 and 7 heat exchange of tower reactor liquid phase stream; Water vapor in reboiler 8 after heat exchange enters after valve 12 decompressions, enters knockout drum 13, after gas-liquid separation, obtains liquid phase stream 15 and gaseous stream 14; Gaseous stream 14 enters compressor 11; Liquid phase stream 15 enter overhead condenser 4 again with gaseous stream 3 heat exchange.
Wherein, the operational condition of acetic acid dehydrating tower 2: stage number is 89, tower reactor temperature is 139 ℃, tower top temperature is 111 ℃, and tower top working pressure is 0..16MPa, and tower reactor 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 condenser 4 is: 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: tube side working pressure is 0.24MPa, and service temperature is 139 ℃; 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, service temperature is 100 ℃.
Compare with the heat pump cycle technique without knockout drum, the inventive method increases after knockout drum, and condenser operational stage is more stable.While there is gas phase in logistics, gas phase part enter the vibrations that can cause condenser, loss equipment; After gas phase part is separated, entering of pure liquid phase stream can make condenser stable operation, thereby improves the work-ing life of device, reduces process cost.
Energy Expenditure Levels is in Table 1.
Table 1
Note: steam consumption quantity numerical value is that negative indication is externally exported steam.
As can be seen from Table 1, compare with compression rectification, 1 ton of dense Acetic Acid-Water solution of every production, the inventive method increases the about energy consumption 64.4% of heat pump cycle flow process deutomerite.
[comparative example 2]
With [embodiment 1], just there is no knockout drum, all the other operational conditions are constant.Be that heat transferring medium water is vaporizated into water vapor after condenser 4 and gaseous stream 3 heat exchange, water vapor enters compressor 11 compressions and heats up, and the water vapor after intensification enters reboiler 8 and 7 heat exchange of tower reactor liquid phase stream; Water vapor in reboiler 8 after heat exchange enters after valve 12 decompression, be back to condenser 4 again with top gaseous phase logistics 3 heat exchange.
Heat transferring medium, after valve 12 decompressions, because gas phase directly enters condenser in company with liquid phase, has caused the vibrations of condenser, has affected the work-ing life of condenser, and process cost is increased.
Claims (5)
1. for separating of a method for acetic acid and water, comprise the following steps:
A) aqueous acetic acid (1) enters acetic acid dehydrating tower (2) from middle part, and after rectifying separation, tower top obtains acetic acid dehydrating tower top gaseous phase logistics (3), and tower reactor obtains acetic acid dehydrating tower tower reactor liquid phase stream (7); Acetic acid dehydrating tower top gaseous phase logistics (3) is after condenser (4) heat exchange condensation, be divided into acetic acid dehydration column overhead the first logistics (5) and acetic acid dehydration column overhead the second logistics (6), as overhead product, discharging enters follow-up flow process in acetic acid dehydration column overhead the first logistics (5), and acetic acid dehydrating tower (2) top is returned in acetic acid dehydration column overhead the second logistics (6); Acetic acid dehydrating tower tower reactor liquid phase stream (7) is after reboiler (8) heat exchange, be divided into reflow stream thigh (9) and dense acetate products discharging (10) at the bottom of tower, at the bottom of tower, reflow stream thigh (9) returns to acetic acid dehydrating tower (2) bottom, and dense acetate products discharging (10) enters follow-up flow process as tower reactor product discharge;
B) heat transferring medium water is vaporizated into water vapor after condenser (4) and acetic acid dehydrating tower top gaseous phase logistics (3) heat exchange, water vapor enters compressor (11) compression and heats up, and the water vapor after intensification enters reboiler (8) and acetic acid dehydrating tower tower reactor liquid phase stream (7) heat exchange; After water vapor in reboiler (8) after heat exchange reduces pressure by expenditure and pressure equipment (12), enter knockout drum (13), after gas-liquid separation, obtain knockout drum liquid phase stream (15) and knockout drum gaseous stream (14); Knockout drum gaseous stream (14) enters compressor (11); Knockout drum liquid phase stream (15) enter overhead condenser (4) again with acetic acid dehydrating tower top gaseous phase logistics (3) heat exchange;
The operational condition of acetic acid dehydrating tower (2): stage number is 60～120, tower reactor temperature is 105～160 ℃, tower top temperature is 100～135 ℃, working pressure is 0.1～0.4MPa, acetic acid dehydration column overhead the second logistics (6) is 0.5～10 with the weight ratio of acetic acid dehydration column overhead the first logistics (5), and at the bottom of tower, reflow stream thigh (9) is 1～17 with the weight ratio of dense acetate products discharging (10);
The operational condition of condenser (4): tube side working pressure is 0.1～0.4MPa, service temperature is 100～135 ℃; Shell side working pressure 0.1～0.3MPa, service temperature is 100～125 ℃;
The operational condition of reboiler (8): tube side working pressure is 0.1～0.4MPa, service temperature is 105～160 ℃; 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, service temperature is 100～125 ℃.
2. the method for separating of 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 80～100, tower reactor temperature is 110～150 ℃, tower top temperature is 100～125 ℃, working pressure is 0.1～0.25MPa, acetic acid dehydration column overhead the second logistics (6) is 2～4 with the weight ratio of acetic acid dehydration column overhead the first logistics (5), and at the bottom of tower, reflow stream thigh (9) is 4～9 with the weight ratio of dense acetate products discharging (10);
The operational condition of condenser (4): tube side working pressure is 0.1～0.25MPa, service temperature is 100～125 ℃; Shell side working pressure 0.1～0.25MPa, service temperature is 100～120 ℃;
The operational condition of reboiler (8): tube side working pressure is 0.1～0.25MPa, service temperature is 110～150 ℃; 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, service temperature is 100～120 ℃.
3. the method for separating of acetic acid and water according to claim 1, is characterized in that by weight percentage, and in aqueous acetic acid (1), the content of acetic acid is 20～80%, and the content of water is 20～80%.
4. the method for separating of acetic acid and water according to claim 1, it is characterized in that heat transferring medium water walks the shell side of condenser (4) and reboiler (8), the tube side of condenser (4) is walked in acetic acid dehydrating tower top gaseous phase logistics (3), and acetic acid dehydrating tower tower reactor liquid phase stream (7) is walked the tube side of reboiler (8).
5. the method for separating of 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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| 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 |
| CN103285612B (en) * | 2013-01-09 | 2015-01-14 | 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 |
Citations (4)
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| US4824527A (en) * | 1986-06-10 | 1989-04-25 | Erickson Donald C | Nested enrichment cascade distillation of unequal mixtures |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20070068792A1 (en) * | 2005-09-23 | 2007-03-29 | Jang Jiyoung | System and method for acetic acid dehydration |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4824527A (en) * | 1986-06-10 | 1989-04-25 | Erickson Donald C | Nested enrichment cascade distillation of unequal mixtures |
| 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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