CN102452926B - Method for separating acetic acid and water - Google Patents
Method for separating acetic acid and water Download PDFInfo
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- CN102452926B CN102452926B CN201010530473.4A CN201010530473A CN102452926B CN 102452926 B CN102452926 B CN 102452926B CN 201010530473 A CN201010530473 A CN 201010530473A CN 102452926 B CN102452926 B CN 102452926B
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Abstract
The invention relates to a method for separating acetic acid and water, mainly solving the problems in the prior art that the energy consumption is high in acetic acid dehydrating process and equipment manufacturing cost is high. The technical scheme of the method is as follows: rectifying and dehydrating by adding pressure to an acetic acid dehydrating tower; using water as a heat-transfer medium during a heat pump cycle; absorbing heat released from condensation on materials discharged from the acetic acid dehydrating tower top by the heat-transfer medium in a closed heat pump flow; compressing the heat-transfer medium having absorbed the energy of the materials discharged from the tower top by a compressing machine, wherein the temperature of the medium is raised then; desuperheating the high temperature superheated steam by a desuperheating device to form saturated steam, and filling the steam in a tower kettle reboiler to exchange heat with the discharged materials from the tower bottom. The method with the above technical scheme better solves the problems in the prior art, and can be applied in industrial production for separating acetic acid and water.
Description
Technical field
The present invention relates to a kind of method of separating acetic acid and water.
Background technology
Produce in the process of terephthalic acid at p xylene oxidation, 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 ensure 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 the concentration that increases acetic acid in the discharging of the method reduction of stage number and increase reflux ratio tower top, when causing energy consumption index high, also make plant investment cost increase.In engineering, consider for economy, general tower top acetate concentration requires lower than 0.8 % by weight, and tower top discharging is discharged as waste water.
Document GB1576787 discloses the method separating acetic acid of azeotropic distillation and the method for water of adopting.This method adopts cascade towers, and first tower is taking 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, therefore acetic acid consumption has been offset in entrainer consumption; And acetates is inflammable medium, when 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 existence of superheated vapour can reduce the heat exchange efficiency of reboiler in heat pump, need to increase reboiler heat interchanging area, thereby cause the increase of equipment and materials expense.This is because the heat transfer coefficient of superheated vapour is much smaller compared with saturation steam.Superheated vapour is that vapour phase is conducted heat, and saturation steam condensation rapidly forms liquid film at steam side, greatly increases rate of heat transfer.This is particularly important for using this point of expensive titanium material tube heat-exchanger.And due to the corrodibility of acetic acid, acetic acid dehydrating tower exactly needs to select expensive titanium steel material as tower bottom reboiler material.
In a word, in prior art, there is the problem that acetic acid dehydration process energy consumption is high and device fabrication cost is high.
Summary of the invention
Technical problem to be solved by this invention is in prior art, to have the problem that acetic acid dehydration process energy consumption is high and device fabrication cost is high, and a kind of method of new separating acetic acid and water is provided.It is high that the method has heat transfer efficiency, and energy consumption is low, the feature that device fabrication 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 of separating 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 enters compressor 11 compression intensifications after condenser 4 and gaseous stream 3 heat exchange; Heat transferring medium after intensification enters desuperheater 13 desuperheatings; The heat transferring medium of desuperheating reduces pressure through expenditure and pressure equipment 12 after entering reboiler 8 and 7 heat exchange of tower reactor liquid phase stream, be back to condenser 4 again with top gaseous phase logistics 3 heat exchange; Wherein, described heat transferring medium is water.
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 DEG C, and more preferably scope is 110～150 DEG C; Tower top temperature preferable range is 100～135 DEG C, and more preferably scope is 100～125 DEG C; 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 DEG C, more preferably 100～125 DEG C of scopes.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 DEG C, and more preferably scope is 100～120 DEG C.The operational condition of desuperheater 13: tube side working pressure preferable range is 0.1～0.4MPa, more preferably scope is 0.1～0.3MPa; Service temperature preferable range is 100～160 DEG C, and more preferably scope is 100～150 DEG C; Shell side working pressure preferable range is 0.1～0.8MPa, and more preferably scope is 0.15～0.8MPa; Service temperature preferable range is 100～400 DEG C, and more preferably scope is 110～400 DEG C.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 DEG C, and more preferably scope is 110～150 DEG C.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 DEG C, and more preferably scope is 130～400 DEG C.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, desuperheater 13 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 in condenser 4 and gaseous stream 3 heat exchange, and the temperature preferable range of the water vapor that heat exchange obtains is 100～125 DEG C, and pressure preferable range is 0.1～0.3MPa.Water vapor is after compressor 11 compressions heat up, and temperature preferable range is 110～400 DEG C, and pressure preferable range is 0.15～0.8MPa.Water vapor after intensification enters after desuperheater desuperheating, obtains saturation steam.This heat transfer process can be used for heating cycle water to produce more low-grade byproduct steam, or for other process-stream of preheating.Saturated-steam temperature preferable range is 140～200 DEG C, and pressure preferable range is 0.15～0.8MPa.Saturation steam enter reboiler 8 to 7 heating of tower reactor liquid phase stream after, temperature preferable range is 110～180 DEG C, pressure preferable range is 0.1～0.8MPa.Heat transferring medium enters after 12 decompressions of expenditure and pressure equipment, and temperature preferable range is 100～125 DEG C, and pressure preferable range is 0.1～0.3MPa.
The inventive method, on the basis of acetic acid conventional rectification dehydration tower production equipment, is carried out pressurized operation by Dichlorodiphenyl Acetate dehydration tower, and sets up a set of enclosed heat pump circulating system; Using water as heat transferring medium, from the overhead condenser heat-obtaining of lower temperature position, after compressor compression, improve energy grade, high-grade steam is converted into saturation steam after by desuperheater heat exchange, this saturation steam, for the heat supply of tower reactor reboiler, has reached energy-saving and cost-reducing object.Saturation steam condensation rapidly, forms liquid film at steam side, greatly increases rate of heat transfer.And if directly the superheated vapour of employing after compressor compresses is for reboiler heat exchange, superheated vapour is that vapour phase is conducted heat, heat transfer coefficient is much smaller compared with saturation steam.The reduction of heat exchange efficiency of reboiler, need to increase reboiler heat interchanging area, thereby causes the increase of equipment and materials expense.For using, this point of acetic acid dehydrating tower reboiler of expensive titanium material pipe is particularly important.The present invention is by increasing a desuperheating interchanger head it off: high-grade steam is converted into saturation steam after by desuperheater heat exchange, this saturation steam is for the heat supply of tower reactor reboiler, avoid superheated vapour directly to enter reboiler, improve heat exchange efficiency, reduce heat interchanging area, thereby reduced the consumption of titanium material during reboiler is manufactured, and the desuperheating interchanger increasing is carbon steel equipment, thereby can reduces device fabrication cost.Adopt the inventive method, compared with the direct rectifying and dewatering technical process of routine, energy consumption declines 50～80%; , in heat pump cycle flow process, increased after desuperheater, heat transfer efficiency can improve 10～20% meanwhile, thereby reboiler manufacturing expense has reduced by 10～20%, has obtained good technique effect.
Brief description of the drawings
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 is 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, 10 is dense acetate products discharging, and 11 is compressor, and 12 is expenditure and pressure equipment, 13 is desuperheater, and 14 is desuperheater heat transferring medium.
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.Water vapor after intensification enters desuperheater 13 and logistics 14 heat exchange; Wherein, logistics 14 needs the process-stream of preheating for recirculated water or other.Logistics 14 produces byproduct steam or is preheated after desuperheater 13 heat exchange, makes the water vapor in heat pump cycle become saturation steam simultaneously.The saturation steam obtaining 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 12 (as orifice plate, valve) decompression, be back to condenser 4 again with top gaseous phase logistics 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, heat transferring medium absorption tower ejects after the energy of material temperature after the compression of overdraft machine and raises, again after desuperheater desuperheating, for discharging heat exchange at the bottom of tower reboiler and tower; Meanwhile, the heat in desuperheater, in order to produce low-grade byproduct steam, or is used it for to other process-stream of preheating.
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 DEG C, and tower top temperature is 99.5 DEG C, 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 DEG C; Shell side working pressure 0.55MPa, 33 DEG C of temperature ins, 43 DEG C of temperature outs.
The operational condition of reboiler 8 is: tube side working pressure is 0.19MPa, and service temperature is 131 DEG C; Shell side working pressure is 0.4MPa, and service temperature is 143 DEG C.
Energy Expenditure Levels is in table 1, and heat transfer efficiency and equipment cost are in table 2.
[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 after desuperheater 13 heat exchange; 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.
Wherein, the operational condition of acetic acid acetic acid dehydrating tower 2: stage number is 89, tower reactor temperature is 139 DEG C, tower top temperature is 111 DEG C, 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 DEG C; Shell side working pressure 0.1MPa, service temperature is 100 DEG C.
The operational condition of desuperheater 13 is: tube side working pressure is 0.3MPa, and service temperature is 133 DEG C; Shell side working pressure 0.6MPa, service temperature is 159～363 DEG C.
The operational condition of reboiler 8 is: tube side working pressure is 0.24MPa, and service temperature is 139 DEG C; Shell side working pressure is 0.6MPa, 159 DEG C of temperature ins, 159 DEG C of temperature outs.
Energy Expenditure Levels is in table 1.
[comparative example 2]
With [embodiment 1], just, in heat pump cycle flow process, heat transferring medium, without desuperheater, directly enters reboiler, and 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 transfer efficiency and equipment cost are in table 2.
Table 1
Note: steam consumption quantity numerical value is that negative indication is externally exported steam.
As can be seen from Table 1, compared with conventional pressurized rectifying, 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.
Table 2
As can be seen from Table 2, compared with heat pump cycle technique without desuperheater, the inventive method has increased after desuperheater in heat pump cycle flow process, and the heat transfer efficiency of reboiler has improved 22%, heat interchanging area has reduced 18%, thereby the manufacturing cost of reboiler has reduced by 18%.
Claims (5)
1. a method for separating acetic acid and water, comprises the following steps:
A) aqueous acetic acid (1) enters acetic acid dehydrating tower (2) from middle part, 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 acetic acid dehydrating tower tower reactor the first logistics (9) and acetic acid dehydrating tower tower reactor the second logistics (10), acetic acid dehydrating tower (2) bottom is returned in acetic acid dehydrating tower tower reactor the first logistics (9), and acetic acid dehydrating tower tower reactor the second logistics (10) enters follow-up flow process as tower reactor product discharge;
B) heat transferring medium enters compressor (11) compression intensification after condenser (4) and acetic acid dehydrating tower top gaseous phase logistics (3) heat exchange; Heat transferring medium after intensification enters desuperheater (13) desuperheating; The heat transferring medium of desuperheating enters after reboiler (8) and acetic acid dehydrating tower tower reactor liquid phase stream (7) heat exchange through expenditure and pressure equipment (12) decompression, be back to condenser (4) again with acetic acid dehydrating tower top gaseous phase logistics (3) heat exchange; Wherein, described heat transferring medium is water;
The operational condition of acetic acid dehydrating tower (2): stage number is 60～120, tower reactor temperature is 105～160 DEG C, tower top temperature is 100～135 DEG C, 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 acetic acid dehydrating tower tower reactor the first logistics (9) is 1～17 with the weight ratio of acetic acid dehydrating tower tower reactor the second logistics (10);
The operational condition of condenser (4): tube side working pressure is 0.1～0.4MPa, service temperature is 100～135 DEG C; Shell side working pressure 0.1～0.3MPa, service temperature is 100～125 DEG C;
The operational condition of desuperheater (13): tube side working pressure is 0.1～0.4MPa, service temperature is 100～160 DEG C; Shell side working pressure 0.1～0.8MPa, service temperature is 100～400 DEG C;
The operational condition of reboiler (8): tube side working pressure is 0.1～0.4MPa, service temperature is 105～160 DEG C; Shell side working pressure is 0.15～0.8MPa, and service temperature is 110～400 DEG C.
2. the method for separating acetic acid according to claim 1 and water, it is characterized in that the operational condition of acetic acid dehydrating tower (2): stage number is 80～100, tower reactor temperature is 110～150 DEG C, tower top temperature is 100～125 DEG C, 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 acetic acid dehydrating tower tower reactor the first logistics (9) is 4～9 with the weight ratio of acetic acid dehydrating tower tower reactor the second logistics (10);
The operational condition of condenser (4): tube side working pressure is 0.1～0.25MPa, service temperature is 100～125 DEG C; Shell side working pressure 0.1～0.25MPa, service temperature is 100～120 DEG C;
The operational condition of desuperheater (13): tube side working pressure is 0.1～0.3MPa, service temperature is 100～150 DEG C; Shell side working pressure 0.15～0.8MPa, service temperature is 110～400 DEG C;
The operational condition of reboiler (8): tube side working pressure is 0.1～0.25MPa, service temperature is 110～150 DEG C; Shell side working pressure is 0.25～0.7MPa, and service temperature is 130～400 DEG C.
3. the method for separating acetic acid according to claim 1 and water, 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 acetic acid according to claim 1 and water, it is characterized in that heat transferring medium water walks the shell side of condenser (4), desuperheater (13) 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 acetic acid according to claim 1 and water, is characterized in that expenditure and pressure equipment is selected from orifice plate or valve.
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| CN112169364B (en) * | 2020-09-29 | 2021-12-24 | 江苏博颂化工科技有限公司 | Fractionating tower heat pump system adopting external circulating working medium |
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| US4240267A (en) * | 1978-12-04 | 1980-12-23 | The Coca-Cola Company | System for vaporizing carbon dioxide utilizing the heat by-product of the refrigeration system as a heat source |
| 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 |
| CN101310154A (en) * | 2005-11-14 | 2008-11-19 | 日冷工业株式会社 | Gas-liquid separator and refrigerating apparatus equipped therewith |
| 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4240267A (en) * | 1978-12-04 | 1980-12-23 | The Coca-Cola Company | System for vaporizing carbon dioxide utilizing the heat by-product of the refrigeration system as a heat source |
| CN101310154A (en) * | 2005-11-14 | 2008-11-19 | 日冷工业株式会社 | 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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