CN104086363A - Energy-saving process for recycling n-butyl acetate and butyl alcohol from waste acid water - Google Patents
Energy-saving process for recycling n-butyl acetate and butyl alcohol from waste acid water Download PDFInfo
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- CN104086363A CN104086363A CN201410334841.6A CN201410334841A CN104086363A CN 104086363 A CN104086363 A CN 104086363A CN 201410334841 A CN201410334841 A CN 201410334841A CN 104086363 A CN104086363 A CN 104086363A
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Abstract
The invention relates to an energy-saving process for recycling n-butyl acetate and butyl alcohol from waste acid water. According to the energy-saving process for recycling the n-butyl acetate and butyl alcohol from the waste acid water, aiming at the characteristics that n-butyl acetate, butyl alcohol and water in the waste acid water can form binary azeotrope and ternary azeotrope in different compositions at different pressures and the azeotrope formed by n-butyl acetate and butyl alcohol during pressurization can move toward a direction in which butyl alcohol content is increased, a countercurrent double-effect rectifying technology is adopted, one condenser is omitted at the top of a tower, and steam at the top of a pressurization tower can be used for heating a feed liquid at bottom of a vacuum tower, so that the aim of saving energy is realized; meanwhile, qualified n-butyl acetate and butyl alcohol are obtained in a single tower by virtue of the conventional rectification. The energy-saving process for recycling the n-butyl acetate and butyl alcohol from the waste acid water has the advantages that a method that azeotropic distillation and the conventional distillation are combined is adopted, and a heat pump technology and a countercurrent double-effect rectification technology are utilized for recycling n-butyl acetate and butyl alcohol in the single tower, so that the energy consumption can be greatly reduced, and obvious economic benefit is obtained.
Description
Technical field
The present invention relates to a kind of energy-saving reclaiming process method of N-BUTYL ACETATE and butanols in waste acid water, concrete technology is the method that adopts azeotropic distillation and conventional rectification combination, utilizes heat pump techniques, flow-reversing dual-purpose distillation technology recovery of acetic acid butyl ester and butanols.
Background technology
In medicine production, as the extraction agent of effective ingredient in fermented liquid or the solvent of reaction process, N-BUTYL ACETATE and butanols often remain in the raffinate of production process discharge, and its content is generally between 0.1-9%wt.If this trade effluent directly discharges, on the one hand, serious environment pollution; On the other hand, can cause serious waste.Therefore, before discharge, need organic solvent wherein to carry out resource utilization recycling.
In penicillin production process, N-BUTYL ACETATE and butanols are two kinds of important solvents, due to the feature of production process, these two kinds of solvents can inevitably appear in waste water, adopt energy-conservation method to be isolated, obtain two kinds of qualified solvents and realize recycling, there is higher realistic meaning.
Factory adopts chemical conversion to process more at present.This process is: in the mixed solution of butanols and N-BUTYL ACETATE, add alkali, make N-BUTYL ACETATE be hydrolyzed into acetic acid and butanols, acetic acid and alkali reaction generate acetate, can utilize rectificating method butyl alcohol extraction out.But this chemical treatment method is the inverse process of esterification, not only cause physical resources waste, increase energy consumption, and hydrolytic process produces a large amount of acetate waste water, waste discharge causes environmental pollution.
CN101811965A discloses a kind of azeotropic distillation and has reclaimed N-BUTYL ACETATE in waste water and the technique of butanols, its technique is to adopt multitower thermal coupling transformation azeotropic distillation technique, with recovery of acetic acid butyl ester and butanols, these technique three tower operations all adopt azeotropic distillation, all need the heating to water to carry out rectifying, caused unnecessary energy wastage, and at the bottom of first rectifying tower the large water gaging of extraction, energy consumption is higher.
Summary of the invention
The object of the present invention is to provide the energy-saving reclaiming process of N-BUTYL ACETATE and butanols in a kind of waste acid water, this technology utilization heat pump techniques, flow-reversing dual-purpose distillation technology recovery of acetic acid butyl ester and butanols, can significantly be reduced in the energy consumption in waste acid water rectifying.
For reaching this object, the present invention by the following technical solutions:
An energy-saving reclaiming process for N-BUTYL ACETATE and butanols in waste acid water, described technique comprises the following steps:
1) the distillate heat exchange in First Heat Exchanger through the first reboiler of tower reactor by the waste acid water containing N-BUTYL ACETATE, butanols and atmospheric distillation tower, then be transported in mixing tank, with the feed liquid from the second phase splitter, mix, by the middle and upper part charging of atmospheric distillation tower, carry out enrichment purification;
2) gas mixture of atmospheric distillation column overhead is after compressor compression, with the feed liquid from tower reactor through the first reboiler heat exchange, steam after heat exchange is through the first water cooler, be transported to the first phase splitter and carry out phase-splitting, after phase-splitting, heavy phase water refluxes, light is the mixture of N-BUTYL ACETATE, fourth alcohol and water mutually, enters rectification under vacuum tower and carries out enrichment purification, and atmospheric distillation tower tower reactor obtains pure water;
3) rectification under vacuum column overhead steam, after the second water cooler is cooling, is transported to the second phase splitter and carries out phase-splitting, after phase-splitting, gently refluxes mutually, and heavy phase water is transported to mixing tank, is mixed into atmospheric distillation tower carries out enrichment purification with the waste acid water from First Heat Exchanger; The steam of compression rectification column overhead is as the thermal source of the second reboiler of rectification under vacuum tower tower reactor, and tower reactor obtains only containing the distillate of N-BUTYL ACETATE and butanols;
4) rectification under vacuum tower distillate is transported to pump pressurization, then through the second interchanger and the heat exchange of compression rectification tower tower reactor distillate, then feed liquid is transported to compression rectification tower, carries out enrichment purification;
5) compression rectification tower tower reactor adopts reboiler heating, and through conventional rectification, tower top obtains finished product butanols, and tower reactor obtains finished product N-BUTYL ACETATE.
Step 1) in, the temperature of waste acid water is generally 20～30 ℃.Preferably, described waste acid water temperature after First Heat Exchanger is 70～75 ℃.Temperature after described heat exchange can be selected 70.1 ℃, and 70.8 ℃, 72.3 ℃, 73 ℃, 73.6 ℃, 74 ℃, 74.4 ℃, 74.9 ℃ etc.
Step 2) in, the gaseous tension of the gas mixture of atmospheric distillation column overhead after compressor compression is 2.5～3atm, and temperature is 200～222 ℃.Described pressure can be selected 2.51atm, 2.56atm, 2.62atm, 2.68atm, 2.71atm, 2.78atm, 2.85atm, 2.94atm, 2.99atm etc.; Described temperature can be selected 200.4 ℃, and 202.3 ℃, 204.6 ℃, 206 ℃, 208.8 ℃, 213 ℃, 217.5 ℃, 220 ℃, 221.8 ℃ etc.
Gas after described compression is with the feed liquid from tower reactor through the first reboiler heat exchange, and after heat exchange, steam is cooled to 75～90 ℃ through the first water cooler.Described temperature can be selected 75.03 ℃, and 77 ℃, 78.6 ℃, 79.6 ℃, 83 ℃, 86.4 ℃, 88 ℃, 89.5 ℃ etc.
Step 2) in, atmospheric distillation column overhead temperature is 95～98 ℃, and when tower reactor temperature is 100～103 ℃, tower reactor obtains pure water.Described tower top temperature can be selected 95.02 ℃, and 95.2 ℃, 95.7 ℃, 96.2 ℃, 96.8 ℃, 97.3 ℃, 97.8 ℃ etc.; Described tower reactor temperature can be selected 100.02 ℃, and 100.1 ℃, 100.6 ℃, 101 ℃, 101.4 ℃, 101.9 ℃, 102.4 ℃, 102.9 ℃ etc.
Step 3) in, the working pressure of rectification under vacuum tower is 10～15kPa; Preferably, rectification under vacuum column overhead steam is cooled to 30～37 ℃ through the second water cooler.Described working pressure can be selected 10.03kPa, 10.3kPa, 10.9kPa, 11.3kPa, 12.5kPa, 13.2kPa, 13.8kPa, 14.2kPa, 14.9kPa etc.Described temperature can be selected 30.05 ℃, and 30.4 ℃, 31 ℃, 31.6 ℃, 32.1 ℃, 33 ℃, 33.8 ℃, 34.2 ℃, 35.2 ℃, 36.3 ℃, 36.8 ℃ etc.
Step 3) in, rectification under vacuum column overhead temperature is 49～56 ℃, and when tower reactor temperature is 59 ℃～68 ℃, tower reactor obtains only containing the distillate of N-BUTYL ACETATE and butanols.Described tower top temperature can be selected 49 ℃, and 51.2 ℃, 53 ℃, 54.6 ℃, 55.5 ℃, 55.8 ℃ etc.Described tower reactor temperature is 59.1 ℃, 59.8 ℃, and 60.4 ℃, 62 ℃, 63.7 ℃, 64.2 ℃, 66 ℃, 67.5 ℃ etc.
Step 4) in, rectification under vacuum tower distillate is transported to pump and is pressurized to 10～11atm.Described pressure can be selected 10.01atm, 10.3atm, 10.36atm, 10.45atm, 10.59atm, 10.7atm, 10.84atm, 10.96atm etc.Preferably, the pressurization of rectification under vacuum tower distillate is by the second interchanger heat exchange to 130～135 ℃.Described temperature can be selected 130.01 ℃, and 130.2 ℃, 130.9 ℃, 131.4 ℃, 131.8 ℃, 132.4 ℃, 132.9 ℃, 134 ℃, 134.8 ℃ etc.
Step 5) in, compression rectification tower working pressure is 4.5～5atm.Described working pressure can be selected 4.51atm, 4.58atm, 4.63atm, 4.7atm, 4.76atm, 4.83atm, 4.9atm, 4.96atm etc.
Step 5) in, compression rectification column overhead temperature is 168～172 ℃, and when tower reactor temperature is 189～194 ℃, tower top obtains finished product butanols, and tower reactor obtains finished product N-BUTYL ACETATE.Described tower top temperature can be selected 168.02 ℃, and 168.3 ℃, 169 ℃, 169.4 ℃, 170 ℃, 170.6 ℃, 171.2 ℃, 171.8 ℃ etc.Described tower reactor temperature can be selected 189.03 ℃, and 189.6 ℃, 190 ℃, 191.2 ℃, 192 ℃, 192.5 ℃, 193 ℃, 193.8 ℃ etc.
An energy-saving reclaiming process for N-BUTYL ACETATE and butanols in waste acid water, described technique comprises the following steps after optimization of process conditions:
1) distillate heat exchange to 70 in First Heat Exchanger～75 ℃ through the first reboiler of tower reactor by the waste acid water containing N-BUTYL ACETATE, butanols and atmospheric distillation tower, then be transported in mixing tank, with the feed liquid from the second phase splitter, mix, by the middle and upper part charging of atmospheric distillation tower, carry out enrichment purification;
2) gas mixture of atmospheric distillation column overhead compresses through compressor, gaseous tension after compression is 2.5～3atm, temperature is 200～222 ℃, after compression with from the feed liquid of tower reactor through the first reboiler heat exchange, steam after heat exchange is cooled to 75～90 ℃ through the first water cooler, is transported to the first phase splitter and carries out phase-splitting, and after phase-splitting, heavy phase water refluxes, light is the mixture of N-BUTYL ACETATE, fourth alcohol and water mutually, enters rectification under vacuum tower and carries out enrichment purification; Tower top temperature is 95～98 ℃, and when tower reactor temperature is 100～103 ℃, atmospheric distillation tower tower reactor obtains the pure water that purity is greater than 99.99%;
3) working pressure of rectification under vacuum tower is 10～15kPa, overhead vapours is cooled to after 30～37 ℃ through the second water cooler, be transported to the second phase splitter and carry out phase-splitting, after phase-splitting, gently reflux mutually, heavy phase water is transported to mixing tank, is mixed into atmospheric distillation tower carries out enrichment purification with the waste acid water from First Heat Exchanger; The steam of compression rectification column overhead is as the thermal source of the second reboiler of rectification under vacuum tower tower reactor; Tower top temperature is 49～56 ℃, and when tower reactor temperature is 59 ℃～68 ℃, rectification under vacuum tower tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate that is 0.38～0.67;
4) rectification under vacuum tower distillate is transported to pump and is forced into 10～11atm, then through the second interchanger and compression rectification tower tower reactor distillate heat exchange to 130～135 ℃, then feed liquid is transported to compression rectification tower, carries out enrichment purification;
5) working pressure of compression rectification tower is 4.5～5atm, tower reactor adopts reboiler heating, through conventional rectification, tower top temperature is 168～172 ℃, and when tower reactor temperature is 189～194 ℃, tower top obtains butanols, biodiversity percentage concentration <0.5% wherein, ester mass percentage concentration <5%, tower reactor obtains N-BUTYL ACETATE, its mass percentage concentration >99%.
The present invention is directed to that N-BUTYL ACETATE in waste acid water, fourth alcohol and water can form the different binary that form, ternary azeotrope under different pressures and feature that direction that N-BUTYL ACETATE and butanols form when high pressure azeotrope can increase towards butanol content move, adopt flow-reversing dual-purpose distillation technology, tower top has saved a condenser, make the steam of compression rectification column overhead to the feed liquid heating of rectification under vacuum tower tower reactor, thereby reach energy-conservation object, can at Dan Tazhong, obtain qualified N-BUTYL ACETATE and butanols by conventional rectification simultaneously.The present invention on the basis of three tower continuous production devices, has set up a set of compression heat pump system simultaneously, and tower top has saved condenser, by consuming a small amount of electric energy, from condenser lower temperature position heat-obtaining, for the heat supply of reboiler, thereby reaches energy-conservation object.
Compare with prior art scheme, the present invention has following beneficial effect:
(1) the present invention is on the basis of three tower continuous production devices, by setting up a set of compression heat pump system, tower top mixing steam is heated up by compressor, at the bottom of tower, after heat release condensation, returning to phase splitter, overhead vapours becomes high potential temperature from low-temperature level, can save heating steam, greatly improve the energy consumption efficiency of process;
(2) the present invention is by transformation technique, the feature that the direction that the azeotrope that while utilizing pressurization, N-BUTYL ACETATE and butanols form can increase towards butanol content moves, adopt flow-reversing dual-purpose distillation technology, make pressurizing tower overhead vapours to the feed liquid heating of vacuum distillation tower tower reactor, make full use of the used heat of pressurizing tower tower reactor simultaneously, realize energy-conservation object;
(3) adopt the separate mode of azeotropic distillation and conventional rectification combination, the unnecessary energy expenditure that while having avoided azeotropic distillation, heating causes to water, obtains qualified N-BUTYL ACETATE and butanols through conventional rectification at Dan Tazhong, thereby realizes energy-conservation object;
(4) this technique is transformed on the basis of current technology, easy and simple to handle and reduced investment.
Accompanying drawing explanation
Fig. 1 is the energy-saving reclaiming process schema of N-BUTYL ACETATE and butanols in waste acid water.
In figure: 1-First Heat Exchanger; 2-mixing tank; 3-atmospheric distillation tower; 4-compressor; 5-the first phase splitter; 6-the first water cooler; 7-the first reboiler; 8-rectification under vacuum tower; 9-the second water cooler; 10-the second phase splitter; 11-the second reboiler; 12-pump; 13-the second interchanger; 14-compression rectification tower.
Below the present invention is described in more detail.But following example is only simple and easy example of the present invention, does not represent or limit the scope of the present invention, and protection scope of the present invention is as the criterion with claims.
Embodiment
Below in conjunction with accompanying drawing and by embodiment, further illustrate technical scheme of the present invention.
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1:
Will be containing N-BUTYL ACETATE 6%wt, butanols 4%wt, water 90%wt, flow is that the waste acid water of 0.130 ton/hour is transported to First Heat Exchanger 1 and is preheating to 75 ℃, heat transferring medium is that atmospheric distillation tower 3 is through the distillate of the first reboiler 7 of tower reactor, again waste acid water is transported to mixing tank 2, with after mixing from the feed liquid of the second phase splitter 10 by the middle and upper part charging of atmospheric distillation tower 3, the number of theoretical plate of atmospheric distillation tower 3 is 7, working pressure is normal pressure, the mixing steam of tower top is through compressor 4, gaseous tension after compression is 3atm, temperature is 221.8 ℃, in the first reboiler 7, carry out heat exchange with the feed liquid from tower reactor, steam after heat exchange is cooled to 90 ℃ through the first water cooler 6, be transported to the first phase splitter 5 and carry out phase-splitting, after phase-splitting, heavy phase water refluxes, be gently N-BUTYL ACETATE mutually, the mixture of fourth alcohol and water, be transported to rectification under vacuum tower 8 and carry out enrichment purification, when tower top temperature is 97.8 ℃, when tower reactor temperature is 101.4 ℃, it is 99.99% water that tower reactor obtains purity, rectification under vacuum tower 8 number of theoretical plates are 14, working pressure is 15kPa, overhead vapours is cooled to 30 ℃ through the second water cooler 9, be transported to the second phase splitter 10 and carry out phase-splitting, after phase-splitting, gently reflux mutually, heavy phase is transported to mixing tank 2, after mixing with the waste acid water from First Heat Exchanger 1, be transported to atmospheric distillation tower 3 and carry out enrichment purification, the steam of compression rectification tower 14 tower tops is as the thermal source of the second reboiler 11 of rectification under vacuum tower 8, tower top temperature is 55.7 ℃, when tower reactor temperature is 67.7 ℃, tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate that is 0.67, rectification under vacuum tower 8 distillates are transported to pump 12 and are pressurized to 10atm, through the second interchanger 13, heat exchange to 130 ℃, its heat transferring medium is compression rectification tower 14 tower reactor distillates, then feed liquid is transported to compression rectification tower 14, compression rectification tower 14 number of theoretical plates are 35, and working pressure is 5atm, tower reactor adopts reboiler heating, through conventional rectification, tower top temperature is 172.1 ℃, when tower reactor temperature is 194.3 ℃, tower top obtains finished product butanols, and wherein biodiversity percentage concentration is 8.8 * 10
-7%, ester mass percentage concentration is 2.3%, and tower reactor obtains N-BUTYL ACETATE, and its mass percentage concentration is 99.99%.
By analysis, in three tower continuous flow procedures, complete identical throughput, when not setting up a set of compression heat pump system, atmospheric distillation tower 3 tower reactors adopt reboiler to heat the 755.26kw that need to consume energy, and 0.3MPa steam saving amount is 1.26 tons/hour, by 130 yuan of calculating of steam per ton, 10080 tons of year steam savings, nearly 1,310,000 yuan of economic benefit; Rectification under vacuum tower 8 and compression rectification tower 14 adopt conventional rectification, reboiler need consume energy respectively for 43.44kw, 64.95kw, when adopting flow-reversing dual-purpose distillation technology, rectification under vacuum tower 8 reboiler institute heat requirements can be provided by compression rectification tower tower 14 overhead vapours, only need to consume the compression rectification tower 14 heat requirement 64.95kw of reboiler institute, realizing energy-conservation is 40.1%.
Embodiment 2:
Will be containing N-BUTYL ACETATE 8%wt, butanols 3%wt, water 89%wt, flow is that the waste acid water of 0.20 ton/hour is transported to First Heat Exchanger 1 and is preheating to 75 ℃, heat transferring medium is that atmospheric distillation tower 3 is through the distillate of the first reboiler 7 of tower reactor, again waste acid water is transported to mixing tank 2, with after mixing from the feed liquid of the second phase splitter 10 by the middle and upper part charging of atmospheric distillation tower 3, the number of theoretical plate of atmospheric distillation tower 3 is 7, working pressure is normal pressure, the mixing steam of tower top is through compressor 4, gaseous tension 2.5atm after compression, temperature is 208.9 ℃, in the first reboiler 7, carry out heat exchange with the feed liquid from tower reactor, steam after heat exchange is cooled to 75 ℃ through the first water cooler 6, be transported to the first phase splitter 5 and carry out phase-splitting, after phase-splitting, heavy phase water refluxes, be gently N-BUTYL ACETATE mutually, the mixture of fourth alcohol and water, be transported to rectification under vacuum tower 8 and carry out enrichment purification, when tower top temperature is 96.8 ℃, when tower reactor temperature is 102.9 ℃, it is 99.99% water that tower reactor obtains purity, rectification under vacuum tower 8 number of theoretical plates are 11, working pressure is 10kPa, overhead vapours is cooled to 30 ℃ through the second water cooler 9, be transported to the second phase splitter 10 and carry out phase-splitting, after phase-splitting, gently reflux mutually, heavy phase is transported to mixing tank 2, after mixing with the waste acid water from First Heat Exchanger 1, be transported to atmospheric distillation tower 3 and carry out enrichment purification, the steam of compression rectification tower 14 tower tops is as the thermal source of the second reboiler 11 of rectification under vacuum tower 8, tower top temperature is 49.1 ℃, when tower reactor temperature is 59 ℃, tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate that is 0.38, rectification under vacuum tower 8 distillates are transported to pump 12 and are pressurized to 11atm, through the second interchanger 13, heat exchange to 135 ℃, its heat transferring medium is compression rectification tower 14 tower reactor distillates, then feed liquid is transported to compression rectification tower 14, compression rectification tower 14 number of theoretical plates are 39, and working pressure is 4.5atm, tower reactor adopts reboiler heating, through conventional rectification, tower top temperature is 167.9 ℃, when tower reactor temperature is 189.3 ℃, tower top obtains finished product butanols, and wherein biodiversity percentage concentration is 3.3 * 10
-7%, ester mass percentage concentration is 3.3%, and tower reactor obtains N-BUTYL ACETATE, and its mass percentage concentration is 99.99%.
By analysis, in three tower continuous flow procedures, complete identical throughput, when not setting up a set of compression heat pump system, atmospheric distillation tower 3 tower reactors adopt reboiler to heat the 1211.28kw that need to consume energy, and 0.3MPa steam saving amount is 2.01 tons/hour, by 130 yuan of calculating of steam per ton, 16090 tons of year steam savings, nearly 2,090,000 yuan of economic benefit; Rectification under vacuum tower 8 and compression rectification tower 14 adopt conventional rectification, reboiler need consume energy respectively for 57.72kw, 85.60kw, when adopting flow-reversing dual-purpose distillation technology, rectification under vacuum tower 8 reboiler institute heat requirements can be provided by compression rectification tower 14 overhead vapours, only need to consume the compression rectification tower 14 heat requirement 85.60kw of reboiler institute, realizing energy-conservation is 40.3%.
Embodiment 3
Will be containing N-BUTYL ACETATE 7%wt, butanols 1%wt, water 92%wt, flow is that the waste acid water of 0.15 ton/hour is transported to First Heat Exchanger 1 and is preheating to 70 ℃, heat transferring medium is that atmospheric distillation tower 3 is through the distillate of the first reboiler 7 of tower reactor, again waste acid water is transported to mixing tank 2, with after mixing from the feed liquid of the second phase splitter 10 by the middle and upper part charging of atmospheric distillation tower 3, the number of theoretical plate of atmospheric distillation tower 3 is 7, working pressure is normal pressure, the mixing steam of tower top is through compressor 4, gaseous tension 2.5atm after compression, temperature is 200.4 ℃, in the first reboiler 7, carry out heat exchange with the feed liquid from tower reactor, steam after heat exchange is cooled to 80 ℃ through the first water cooler 6, be transported to the first phase splitter 5 and carry out phase-splitting, after phase-splitting, heavy phase water refluxes, be gently N-BUTYL ACETATE mutually, the mixture of fourth alcohol and water, be transported to rectification under vacuum tower 8 and carry out enrichment purification, when tower top temperature is 95.2 ℃, when tower reactor temperature is 100.1 ℃, it is 99.99% water that tower reactor obtains purity, rectification under vacuum tower 8 number of theoretical plates are 12, working pressure is 10kPa, overhead vapours is cooled to 36.8 ℃ through the second water cooler 9, be transported to the second phase splitter 10 and carry out phase-splitting, after phase-splitting, gently reflux mutually, heavy phase is transported to mixing tank 2, after mixing with the waste acid water from First Heat Exchanger 1, be transported to atmospheric distillation tower 3 and carry out enrichment purification, the steam of compression rectification tower 14 tower tops is as the thermal source of the second reboiler 11 of rectification under vacuum tower 8, tower top temperature is 53.8 ℃, when tower reactor temperature is 65.2 ℃, tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate that is 0.59, rectification under vacuum tower 8 distillates are transported to pump 12 and are pressurized to 11atm, through the second interchanger 13, heat exchange to 135 ℃, its heat transferring medium is compression rectification tower 14 tower reactor distillates, then feed liquid is transported to compression rectification tower 14, and compression rectification tower 14 number of theoretical plates are 37, working pressure is 4.5atm, tower reactor adopts reboiler heating, and through conventional rectification, tower top temperature is 170.6 ℃, when tower reactor temperature is 192.5 ℃, tower top obtains finished product butanols, and wherein, biodiversity percentage concentration is 7.2 * 10
-7%, ester mass percentage concentration is 2.6%, and tower reactor obtains N-BUTYL ACETATE, and its mass percentage concentration is 99.99%.
By analysis, in three tower continuous flow procedures, complete identical throughput, when not setting up a set of compression heat pump system, atmospheric distillation tower 3 tower reactors adopt reboiler to heat the 885.56kw that need to consume energy, and 0.3MPa steam saving amount is 1.47 tons/hour, by 130 yuan of calculating of steam per ton, 11760 tons of year steam savings, nearly 1,530,000 yuan of economic benefit; Rectification under vacuum tower 8 and compression rectification tower 14 adopt conventional rectification, reboiler need consume energy respectively for 47.52kw, 70.85kw, when adopting flow-reversing dual-purpose distillation technology, rectification under vacuum tower 8 reboiler institute heat requirements can be provided by compression rectification tower 14 overhead vapours, only need to consume the compression rectification tower 14 heat requirement 70.85kw of reboiler institute, realizing energy-conservation is 40.1%.
Applicant's statement, the present invention illustrates technique of the present invention by above-described embodiment, but the present invention is not limited to aforesaid operations step, does not mean that the present invention must rely on aforesaid operations step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of the selected raw material of the present invention and ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible array modes.
In addition, between various embodiment of the present invention, also can carry out arbitrary combination, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. an energy-saving reclaiming process for N-BUTYL ACETATE and butanols in waste acid water, is characterized in that, described technique comprises the steps:
1) the distillate heat exchange in First Heat Exchanger (1) through first reboiler (7) of tower reactor by the waste acid water containing N-BUTYL ACETATE, butanols and atmospheric distillation tower (3), then be transported in mixing tank (2), with the feed liquid from the second phase splitter (10), mix, by the middle and upper part charging of atmospheric distillation tower (3), carry out enrichment purification;
2) gas mixture of atmospheric distillation tower (3) tower top is after compressor (4) compression, with the feed liquid from tower reactor through the first reboiler (7) heat exchange, steam after heat exchange is through the first water cooler (6), be transported to the first phase splitter (5) and carry out phase-splitting, after phase-splitting, heavy phase water refluxes, light is the mixture of N-BUTYL ACETATE, fourth alcohol and water mutually, enters rectification under vacuum tower (8) and carries out enrichment purification, and atmospheric distillation tower (3) tower reactor obtains pure water;
3) rectification under vacuum tower (8) overhead vapours is after the second water cooler (9) is cooling, be transported to the second phase splitter (10) and carry out phase-splitting, after phase-splitting, gently reflux mutually, heavy phase water is transported to mixing tank (2), is mixed into atmospheric distillation tower (3) carries out enrichment purification with the waste acid water from First Heat Exchanger (1); The steam of compression rectification tower (14) tower top is as the thermal source of second reboiler (11) of rectification under vacuum tower (8) tower reactor, and tower reactor obtains only containing the distillate of N-BUTYL ACETATE and butanols;
4) rectification under vacuum tower (8) distillate is transported to pump (12) pressurization, then through the second interchanger (13) and the heat exchange of compression rectification tower (14) tower reactor distillate, then feed liquid is transported to compression rectification tower (14), carries out enrichment purification;
5) compression rectification tower (14) tower reactor adopts reboiler heating, and through conventional rectification, tower top obtains finished product butanols, and tower reactor obtains finished product N-BUTYL ACETATE.
2. technique as claimed in claim 1, is characterized in that step 1) in the temperature of waste acid water be 20～30 ℃; Preferably, described waste acid water temperature after First Heat Exchanger (1) is 70～75 ℃.
3. technique as claimed in claim 1 or 2, is characterized in that step 2) in the gas mixture of atmospheric distillation tower (3) the tower top gaseous tension after compressor (4) compression be 2.5～3atm, temperature is 200～222 ℃;
Preferably, the gas after described compression is with the feed liquid from tower reactor through the first reboiler (7) heat exchange, and after heat exchange, steam is cooled to 75～90 ℃ through the first water cooler (6).
4. the technique as described in one of claim 1-3, is characterized in that step 2) in atmospheric distillation tower (3) tower top temperature be 95～98 ℃, when tower reactor temperature is 100～103 ℃, tower reactor obtains pure water.
5. the technique as described in one of claim 1-4, is characterized in that step 3) in the working pressure of rectification under vacuum tower (8) be 10～15kPa; Preferably, rectification under vacuum tower (8) overhead vapours is cooled to 30～37 ℃ through the second water cooler (9).
6. the technique as described in one of claim 1-5, is characterized in that step 3) in rectification under vacuum tower (8) tower top temperature be 49～56 ℃, when tower reactor temperature is 59 ℃～68 ℃, tower reactor obtains only containing the distillate of N-BUTYL ACETATE and butanols.
7. the technique as described in one of claim 1-6, is characterized in that step 4) in rectification under vacuum tower (8) distillate be transported to pump (12) and be pressurized to 10～11atm; Preferably, the pressurization of rectification under vacuum tower (8) distillate is by the second interchanger (13) heat exchange to 130～135 ℃.
8. the technique as described in one of claim 1-7, is characterized in that step 5) in compression rectification tower (14) working pressure be 4.5～5atm.
9. the technique as described in one of claim 1-8, is characterized in that step 5) in compression rectification tower (14) tower top temperature be 168～172 ℃, when tower reactor temperature is 189～194 ℃, tower top obtains finished product butanols, tower reactor obtains finished product N-BUTYL ACETATE.
10. the technique as described in one of claim 1-9, is characterized in that, described technique comprises the following steps:
1) distillate heat exchange to 70～75 ℃ in First Heat Exchanger (1) through first reboiler (7) of tower reactor by the waste acid water containing N-BUTYL ACETATE, butanols and atmospheric distillation tower (3), then be transported in mixing tank (2), with the feed liquid from the second phase splitter (10), mix, by the middle and upper part charging of atmospheric distillation tower (3), carry out enrichment purification;
2) gas mixture of atmospheric distillation tower (3) tower top compresses through compressor (4), gaseous tension after compression is 2.5～3atm, temperature is 200～222 ℃, after compression with from the feed liquid of tower reactor through the first reboiler (7) heat exchange, steam after heat exchange is cooled to 75～90 ℃ through the first water cooler (6), be transported to the first phase splitter (5) and carry out phase-splitting, after phase-splitting, heavy phase water refluxes, light is the mixture of N-BUTYL ACETATE, fourth alcohol and water mutually, enters rectification under vacuum tower (8) and carries out enrichment purification; Tower top temperature is 95～98 ℃, and when tower reactor temperature is 100～103 ℃, atmospheric distillation tower (3) tower reactor obtains the pure water that purity is greater than 99.99%;
3) working pressure of rectification under vacuum tower (8) is 10～15kPa, overhead vapours is cooled to after 30～37 ℃ through the second water cooler (9), be transported to the second phase splitter (10) and carry out phase-splitting, after phase-splitting, gently reflux mutually, heavy phase water is transported to mixing tank (2), is mixed into atmospheric distillation tower (3) carries out enrichment purification with the waste acid water from First Heat Exchanger (1); The steam of compression rectification tower (14) tower top is as the thermal source of second reboiler (11) of rectification under vacuum tower (8) tower reactor; Tower top temperature is 49～56 ℃, and when tower reactor temperature is 59～68 ℃, rectification under vacuum tower (8) tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate that is 0.38～0.67;
4) rectification under vacuum tower (8) distillate is transported to pump (12) and is forced into 10～11atm, again through the second interchanger (13) and compression rectification tower (14) tower reactor distillate heat exchange to 130～135 ℃, then feed liquid is transported to compression rectification tower (14), carries out enrichment purification;
5) working pressure of compression rectification tower (14) is 4.5～5atm, tower reactor adopts reboiler heating, through conventional rectification, tower top temperature is 168～172 ℃, and when tower reactor temperature is 189～194 ℃, tower top obtains butanols, biodiversity percentage concentration <0.5% wherein, ester mass percentage concentration <5%, tower reactor obtains N-BUTYL ACETATE, its mass percentage concentration >99%.
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