CN104086363B - The energy-saving reclaiming process of N-BUTYL ACETATE and butanols in waste acid water - Google Patents
The energy-saving reclaiming process of N-BUTYL ACETATE and butanols in waste acid water Download PDFInfo
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- CN104086363B CN104086363B CN201410334841.6A CN201410334841A CN104086363B CN 104086363 B CN104086363 B CN 104086363B CN 201410334841 A CN201410334841 A CN 201410334841A CN 104086363 B CN104086363 B CN 104086363B
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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Abstract
The present invention relates to the energy-saving reclaiming process of N-BUTYL ACETATE and butanols in a kind of waste acid water.The present invention is directed to the feature that N-BUTYL ACETATE in waste acid water, fourth alcohol and water can form the direction movement that the binary of different composition, ternary azeotrope and N-BUTYL ACETATE and butanols are formed when pressurizeing azeotrope can increase towards butanol content at various pressures, adopt flow-reversing dual-purpose distillation technology, tower top eliminates a condenser, the steam of pressurizing tower tower top is heated to the feed liquid of vacuum distillation tower tower reactor, thus reach energy-conservation object, qualified N-BUTYL ACETATE and butanols can be obtained by conventional rectification at Dan Tazhong simultaneously.The method that the present invention adopts azeotropic distillation and conventional rectification to combine, utilize heat pump techniques, flow-reversing dual-purpose distillation technology is recovery of acetic acid butyl ester and butanols in single tower, significantly can reduce energy consumption, has significant economic benefit.
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 adopting azeotropic distillation and conventional rectification to combine, and utilizes heat pump techniques, flow-reversing dual-purpose distillation technology recovery of acetic acid butyl ester and butanols.
Background technology
As the extraction agent of effective ingredient in fermented liquid or the solvent of reaction process in medicine production, 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, serious waste can be caused.Therefore, need before discharge to carry out resource utilization recycling to organic solvent wherein.
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.
Current factory many employings chemical conversion treatment.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 to waste, increase energy consumption, and hydrolytic process produces a large amount of acetate waste water, and waste discharge causes environmental pollution.
CN101811965A discloses the technique that a kind of azeotropic distillation reclaims N-BUTYL ACETATE in waste water and butanols, its technique adopts multitower thermal coupling transformation azeotropic distillation technique, with recovery of acetic acid butyl ester and butanols, the operation of this technique three tower all adopts azeotropic distillation, then all need to carry out rectifying to water heating, cause 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, significantly can 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) by containing the distillate heat exchange in First Heat Exchanger through the first reboiler of tower reactor of N-BUTYL ACETATE, the waste acid water of butanols and atmospheric distillation tower, then be transported in mixing tank, mix with the feed liquid from the second phase splitter, 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, heavy phase water backflow after phase-splitting, be gently the mixture of N-BUTYL ACETATE, fourth alcohol and water mutually, enter vacuum rectification tower and carry out enrichment purification, atmospheric distillation tower tower reactor obtains pure water;
3) vacuum rectification tower overhead vapours is after the second water cooler cooling, be transported to the second phase splitter and carry out phase-splitting, gently reflux mutually after phase-splitting, 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 vacuum rectification tower tower reactor, and tower reactor obtains the distillate only containing N-BUTYL ACETATE and butanols;
4) vacuum rectification 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 be generally 20 ~ 30 DEG C.Preferably, described waste acid water temperature after First Heat Exchanger is 70 ~ 75 DEG C.Temperature after described heat exchange can select 70.1 DEG C, 70.8 DEG C, 72.3 DEG C, 73 DEG C, 73.6 DEG C, 74 DEG C, 74.4 DEG C, 74.9 DEG C etc.
Step 2) in atmospheric distillation column overhead gas mixture through compressor compression after gaseous tension be 2.5 ~ 3atm, temperature is 200 ~ 222 DEG C.Described pressure can select 2.51atm, 2.56atm, 2.62atm, 2.68atm, 2.71atm, 2.78atm, 2.85atm, 2.94atm, 2.99atm etc.; Described temperature can select 200.4 DEG C, 202.3 DEG C, 204.6 DEG C, 206 DEG C, 208.8 DEG C, 213 DEG C, 217.5 DEG C, 220 DEG C, 221.8 DEG C etc.
Gas after described compression and the feed liquid from tower reactor are through the first reboiler heat exchange, and after heat exchange, steam is cooled to 75 ~ 90 DEG C through the first water cooler.Described temperature can select 75.03 DEG C, 77 DEG C, 78.6 DEG C, 79.6 DEG C, 83 DEG C, 86.4 DEG C, 88 DEG C, 89.5 DEG C etc.
Step 2) in atmospheric distillation column overhead temperatures be 95 ~ 98 DEG C, when bottom temperature is 100 ~ 103 DEG C, tower reactor obtains pure water.Described tower top temperature can select 95.02 DEG C, 95.2 DEG C, 95.7 DEG C, 96.2 DEG C, 96.8 DEG C, 97.3 DEG C, 97.8 DEG C etc.; Described bottom temperature can select 100.02 DEG C, 100.1 DEG C, 100.6 DEG C, 101 DEG C, 101.4 DEG C, 101.9 DEG C, 102.4 DEG C, 102.9 DEG C etc.
Step 3) in the working pressure of vacuum rectification tower be 10 ~ 15kPa; Preferably, vacuum rectification tower overhead vapours is cooled to 30 ~ 37 DEG C through the second water cooler.Described working pressure can select 10.03kPa, 10.3kPa, 10.9kPa, 11.3kPa, 12.5kPa, 13.2kPa, 13.8kPa, 14.2kPa, 14.9kPa etc.Described temperature can select 30.05 DEG C, 30.4 DEG C, 31 DEG C, 31.6 DEG C, 32.1 DEG C, 33 DEG C, 33.8 DEG C, 34.2 DEG C, 35.2 DEG C, 36.3 DEG C, 36.8 DEG C etc.
Step 3) in rectification under vacuum column overhead temperatures be 49 ~ 56 DEG C, when bottom temperature is 59 DEG C ~ 68 DEG C, tower reactor obtains the distillate only containing N-BUTYL ACETATE and butanols.Described tower top temperature can select 49 DEG C, 51.2 DEG C, 53 DEG C, 54.6 DEG C, 55.5 DEG C, 55.8 DEG C etc.Described bottom temperature is 59.1 DEG C, 59.8 DEG C, 60.4 DEG C, 62 DEG C, 63.7 DEG C, 64.2 DEG C, 66 DEG C, 67.5 DEG C etc.
Step 4) in vacuum rectification tower distillate be transported to pump and be pressurized to 10 ~ 11atm.Described pressure can select 10.01atm, 10.3atm, 10.36atm, 10.45atm, 10.59atm, 10.7atm, 10.84atm, 10.96atm etc.Preferably, vacuum rectification tower distillate pressurization after through the second interchanger heat exchange to 130 ~ 135 DEG C.Described temperature can select 130.01 DEG C, 130.2 DEG C, 130.9 DEG C, 131.4 DEG C, 131.8 DEG C, 132.4 DEG C, 132.9 DEG C, 134 DEG C, 134.8 DEG C etc.
Step 5) in compression rectification tower working pressure be 4.5 ~ 5atm.Described working pressure can select 4.51atm, 4.58atm, 4.63atm, 4.7atm, 4.76atm, 4.83atm, 4.9atm, 4.96atm etc.
Step 5) in compression rectification column overhead temperatures be 168 ~ 172 DEG C, when bottom temperature is 189 ~ 194 DEG C, tower top obtains finished product butanols, and tower reactor obtains finished product N-BUTYL ACETATE.Described tower top temperature can select 168.02 DEG C, 168.3 DEG C, 169 DEG C, 169.4 DEG C, 170 DEG C, 170.6 DEG C, 171.2 DEG C, 171.8 DEG C etc.Described bottom temperature can select 189.03 DEG C, 189.6 DEG C, 190 DEG C, 191.2 DEG C, 192 DEG C, 192.5 DEG C, 193 DEG C, 193.8 DEG C 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) by containing N-BUTYL ACETATE, the waste acid water of butanols and atmospheric distillation tower through distillate heat exchange to 70 in First Heat Exchanger ~ 75 DEG C of the first reboiler of tower reactor, then be transported in mixing tank, mix with the feed liquid from the second phase splitter, 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 DEG C, 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 DEG C through the first water cooler, is transported to the first phase splitter and carries out phase-splitting, heavy phase water backflow after phase-splitting, be gently the mixture of N-BUTYL ACETATE, fourth alcohol and water mutually, enter vacuum rectification tower and carry out enrichment purification; Tower top temperature is 95 ~ 98 DEG C, and when bottom temperature is 100 ~ 103 DEG C, atmospheric distillation tower tower reactor obtains the pure water that purity is greater than 99.99%;
3) working pressure of vacuum rectification tower is 10 ~ 15kPa, overhead vapours is after the second water cooler is cooled to 30 ~ 37 DEG C, be transported to the second phase splitter and carry out phase-splitting, gently reflux mutually after phase-splitting, 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 vacuum rectification tower tower reactor; Tower top temperature is 49 ~ 56 DEG C, and when bottom temperature is 59 DEG C ~ 68 DEG C, vacuum rectification tower tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate being 0.38 ~ 0.67;
4) vacuum rectification 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 DEG C, 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 DEG C, and when bottom temperature is 189 ~ 194 DEG C, tower top obtains butanols, wherein biodiversity percentage concentration <0.5%, ester mass percentage concentration <5%, tower reactor obtains N-BUTYL ACETATE, its mass percentage concentration >99%.
The present invention is directed to the feature that N-BUTYL ACETATE in waste acid water, fourth alcohol and water can form the direction movement that the binary of different composition, ternary azeotrope and N-BUTYL ACETATE and butanols are formed when high pressure azeotrope can increase towards butanol content at various pressures, adopt flow-reversing dual-purpose distillation technology, tower top eliminates a condenser, the steam of compression rectification column overhead is heated to the feed liquid of vacuum rectification tower tower reactor, thus reach energy-conservation object, qualified N-BUTYL ACETATE and butanols can be obtained by conventional rectification at Dan Tazhong simultaneously.The present invention is simultaneously on the basis of three tower continuous production devices, and set up a set of compression heat pump system, tower top eliminates condenser, by consuming a small amount of electric energy, from condenser comparatively low-temperature level heat-obtaining, for the heat supply of reboiler, thus reaches energy-conservation object.
Compared 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, phase splitter is returned after exothermic condensation at the bottom of tower, overhead vapours becomes high-temperature position from low-temperature level, heating steam can be saved, the energy consumption efficiency of very big raising process;
(2) the present invention is by transformation technique, the feature of the direction movement utilizing the azeotrope that when pressurizeing, N-BUTYL ACETATE and butanols are formed can increase towards butanol content, adopt flow-reversing dual-purpose distillation technology, pressurizing tower overhead vapours is heated to the feed liquid of vacuum distillation tower tower reactor, make full use of the used heat of pressurizing tower tower reactor simultaneously, realize energy-conservation object;
(3) separate mode adopting azeotropic distillation and conventional rectification to combine, heats to water the unnecessary energy expenditure caused when avoiding azeotropic distillation, obtains qualified N-BUTYL ACETATE and butanols, thus realize energy-conservation object through conventional rectification at Dan Tazhong;
(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-first phase splitter; 6-first water cooler; 7-first reboiler; 8-vacuum rectification tower; 9-second water cooler; 10-second phase splitter; 11-second reboiler; 12-pump; 13-second interchanger; 14-compression rectification tower.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, and do not represent or limit the scope of the present invention, protection scope of the present invention is as the criterion with claims.
Embodiment
Technical scheme of the present invention is further illustrated by embodiment below in conjunction with accompanying drawing.
For better the present invention being described, 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 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 DEG C, heat transferring medium is the distillate of atmospheric distillation tower 3 through the first reboiler 7 of tower reactor, again waste acid water is transported to mixing tank 2, by the middle and upper part charging of atmospheric distillation tower 3 after mixing with the feed liquid from the second phase splitter 10, 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 DEG C, in the first reboiler 7, heat exchange is carried out with the feed liquid from tower reactor, steam after heat exchange is cooled to 90 DEG C through the first water cooler 6, be transported to the first phase splitter 5 and carry out phase-splitting, heavy phase water backflow after phase-splitting, light is N-BUTYL ACETATE mutually, the mixture of fourth alcohol and water, be transported to vacuum rectification tower 8 and carry out enrichment purification, when tower top temperature is 97.8 DEG C, when bottom temperature is 101.4 DEG C, tower reactor obtains the water that purity is 99.99%, vacuum rectification tower 8 number of theoretical plate is 14, working pressure is 15kPa, overhead vapours is cooled to 30 DEG C through the second water cooler 9, be transported to the second phase splitter 10 and carry out phase-splitting, gently reflux mutually after phase-splitting, heavy phase is transported to mixing tank 2, enrichment purification is carried out with from being transported to atmospheric distillation tower 3 after the waste acid water mixing of First Heat Exchanger 1, the steam of compression rectification tower 14 tower top is as the thermal source of the second reboiler 11 of vacuum rectification tower 8, tower top temperature is 55.7 DEG C, when bottom temperature is 67.7 DEG C, tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate being 0.67, vacuum rectification tower 8 distillate is transported to pump 12 and is pressurized to 10atm, and through the second interchanger 13, heat exchange is to 130 DEG C, its heat transferring medium is compression rectification tower 14 tower reactor distillate, then feed liquid is transported to compression rectification tower 14, compression rectification tower 14 number of theoretical plate is 35, and working pressure is 5atm, tower reactor adopts reboiler heating, through conventional rectification, tower top temperature is 172.1 DEG C, when bottom temperature is 194.3 DEG C, 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 reactor adopts reboiler heating to need power consumption 755.26kw, 0.3MPa steam saving to be 1.26 tons/hour, by steam per ton 130 yuan calculating, year steam saving 10080 tons, nearly 1,310,000 yuan of economic benefit; Vacuum rectification 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, vacuum rectification tower 8 reboiler institute heat requirement can be provided by compression rectification tower tower 14 overhead vapours, only need consume compression rectification tower 14 reboiler institute heat requirement 64.95kw, realizing energy-conservation is 40.1%.
Embodiment 2:
Will 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 DEG C, heat transferring medium is the distillate of atmospheric distillation tower 3 through the first reboiler 7 of tower reactor, again waste acid water is transported to mixing tank 2, by the middle and upper part charging of atmospheric distillation tower 3 after mixing with the feed liquid from the second phase splitter 10, 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 DEG C, in the first reboiler 7, heat exchange is carried out with the feed liquid from tower reactor, steam after heat exchange is cooled to 75 DEG C through the first water cooler 6, be transported to the first phase splitter 5 and carry out phase-splitting, heavy phase water backflow after phase-splitting, light is N-BUTYL ACETATE mutually, the mixture of fourth alcohol and water, be transported to vacuum rectification tower 8 and carry out enrichment purification, when tower top temperature is 96.8 DEG C, when bottom temperature is 102.9 DEG C, tower reactor obtains the water that purity is 99.99%, vacuum rectification tower 8 number of theoretical plate is 11, working pressure is 10kPa, overhead vapours is cooled to 30 DEG C through the second water cooler 9, be transported to the second phase splitter 10 and carry out phase-splitting, gently reflux mutually after phase-splitting, heavy phase is transported to mixing tank 2, enrichment purification is carried out with from being transported to atmospheric distillation tower 3 after the waste acid water mixing of First Heat Exchanger 1, the steam of compression rectification tower 14 tower top is as the thermal source of the second reboiler 11 of vacuum rectification tower 8, tower top temperature is 49.1 DEG C, when bottom temperature is 59 DEG C, tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate being 0.38, vacuum rectification tower 8 distillate is transported to pump 12 and is pressurized to 11atm, and through the second interchanger 13, heat exchange is to 135 DEG C, its heat transferring medium is compression rectification tower 14 tower reactor distillate, then feed liquid is transported to compression rectification tower 14, compression rectification tower 14 number of theoretical plate is 39, and working pressure is 4.5atm, tower reactor adopts reboiler heating, through conventional rectification, tower top temperature is 167.9 DEG C, when bottom temperature is 189.3 DEG C, 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 reactor adopts reboiler heating to need power consumption 1211.28kw, 0.3MPa steam saving to be 2.01 tons/hour, by steam per ton 130 yuan calculating, year steam saving 16090 tons, nearly 2,090,000 yuan of economic benefit; Vacuum rectification 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, vacuum rectification tower 8 reboiler institute heat requirement can be provided by compression rectification tower 14 overhead vapours, only need consume compression rectification tower 14 reboiler institute heat requirement 85.60kw, realizing energy-conservation is 40.3%.
Embodiment 3
Will 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 DEG C, heat transferring medium is the distillate of atmospheric distillation tower 3 through the first reboiler 7 of tower reactor, again waste acid water is transported to mixing tank 2, by the middle and upper part charging of atmospheric distillation tower 3 after mixing with the feed liquid from the second phase splitter 10, 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 DEG C, in the first reboiler 7, heat exchange is carried out with the feed liquid from tower reactor, steam after heat exchange is cooled to 80 DEG C through the first water cooler 6, be transported to the first phase splitter 5 and carry out phase-splitting, heavy phase water backflow after phase-splitting, light is N-BUTYL ACETATE mutually, the mixture of fourth alcohol and water, be transported to vacuum rectification tower 8 and carry out enrichment purification, when tower top temperature is 95.2 DEG C, when bottom temperature is 100.1 DEG C, tower reactor obtains the water that purity is 99.99%, vacuum rectification tower 8 number of theoretical plate is 12, working pressure is 10kPa, overhead vapours is cooled to 36.8 DEG C through the second water cooler 9, be transported to the second phase splitter 10 and carry out phase-splitting, gently reflux mutually after phase-splitting, heavy phase is transported to mixing tank 2, enrichment purification is carried out with from being transported to atmospheric distillation tower 3 after the waste acid water mixing of First Heat Exchanger 1, the steam of compression rectification tower 14 tower top is as the thermal source of the second reboiler 11 of vacuum rectification tower 8, tower top temperature is 53.8 DEG C, when bottom temperature is 65.2 DEG C, tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate being 0.59, vacuum rectification tower 8 distillate is transported to pump 12 and is pressurized to 11atm, and through the second interchanger 13, heat exchange is to 135 DEG C, its heat transferring medium is compression rectification tower 14 tower reactor distillate, then feed liquid is transported to compression rectification tower 14, and compression rectification tower 14 number of theoretical plate is 37, working pressure is 4.5atm, tower reactor adopts reboiler heating, and through conventional rectification, tower top temperature is 170.6 DEG C, when bottom temperature is 192.5 DEG C, 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 reactor adopts reboiler heating to need power consumption 885.56kw, 0.3MPa steam saving to be 1.47 tons/hour, by steam per ton 130 yuan calculating, year steam saving 11760 tons, nearly 1,530,000 yuan of economic benefit; Vacuum rectification 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, vacuum rectification tower 8 reboiler institute heat requirement can be provided by compression rectification tower 14 overhead vapours, only need consume compression rectification tower 14 reboiler institute heat requirement 70.85kw, realizing energy-conservation is 40.1%.
Applicant states, 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 namely 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 equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within 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 characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, 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 (13)
1. the energy-saving reclaiming process of N-BUTYL ACETATE and butanols in waste acid water, it is characterized in that, described technique comprises the steps:
1) by waste acid water and the atmospheric distillation tower (3) containing N-BUTYL ACETATE, butanols through the distillate of first reboiler (7) of tower reactor in the middle heat exchange of First Heat Exchanger (1), then be transported in mixing tank (2), mix with the feed liquid from the second phase splitter (10), 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, heavy phase water backflow after phase-splitting, be gently the mixture of N-BUTYL ACETATE, fourth alcohol and water mutually, enter vacuum rectification tower (8) and carry out enrichment purification, atmospheric distillation tower (3) tower reactor obtains pure water;
3) vacuum rectification tower (8) overhead vapours is after the second water cooler (9) cooling, be transported to the second phase splitter (10) and carry out phase-splitting, gently reflux mutually after phase-splitting, 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 vacuum rectification tower (8) tower reactor, and tower reactor obtains the distillate only containing N-BUTYL ACETATE and butanols;
4) vacuum rectification tower (8) distillate is transported to pump (12) pressurization, again 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;
Step 2) in atmospheric distillation tower (3) tower top gas mixture through compressor (4) compression after gaseous tension be 2.5 ~ 3atm, temperature is 200 ~ 222 DEG C;
Step 3) in vacuum rectification tower (8) tower reactor obtain the distillate only containing N-BUTYL ACETATE and butanols;
Step 5) in compression rectification tower (14) tower top obtain finished product butanols, tower reactor obtains finished product N-BUTYL ACETATE;
The separate mode that described technique adopts azeotropic distillation and conventional rectification to combine.
2. technique as claimed in claim 1, is characterized in that, step 1) in the temperature of waste acid water be 20 ~ 30 DEG C.
3. technique as claimed in claim 1, is characterized in that, step 1) described in waste acid water temperature after First Heat Exchanger (1) be 70 ~ 75 DEG C.
4. technique as claimed in claim 1, is characterized in that, step 2) in gas after compression with the feed liquid from tower reactor through the first reboiler (7) heat exchange, after heat exchange, steam is cooled to 75 ~ 90 DEG C through the first water cooler (6).
5. technique as claimed in claim 1, is characterized in that, step 2) in atmospheric distillation tower (3) tower top temperature be 95 ~ 98 DEG C, when bottom temperature is 100 ~ 103 DEG C, tower reactor obtains pure water.
6. technique as claimed in claim 1, is characterized in that, step 3) in the working pressure of vacuum rectification tower (8) be 10 ~ 15kPa.
7. technique as claimed in claim 1, is characterized in that, step 3) in vacuum rectification tower (8) overhead vapours be cooled to 30 ~ 37 DEG C through the second water cooler (9).
8. technique as claimed in claim 1, is characterized in that, step 3) in vacuum rectification tower (8) tower top temperature be 49 ~ 56 DEG C, when bottom temperature is 59 DEG C ~ 68 DEG C, tower reactor obtains the distillate only containing N-BUTYL ACETATE and butanols.
9. technique as claimed in claim 1, is characterized in that, step 4) in vacuum rectification tower (8) distillate be transported to pump (12) and be pressurized to 10 ~ 11atm.
10. technique as claimed in claim 1, is characterized in that, step 4) in after the pressurization of vacuum rectification tower (8) distillate through the second interchanger (13) heat exchange to 130 ~ 135 DEG C.
11. techniques as claimed in claim 1, is characterized in that, step 5) in compression rectification tower (14) working pressure be 4.5 ~ 5atm.
12. techniques as claimed in claim 1, is characterized in that, step 5) in compression rectification tower (14) tower top temperature be 168 ~ 172 DEG C, when bottom temperature is 189 ~ 194 DEG C, tower top obtains finished product butanols, and tower reactor obtains finished product N-BUTYL ACETATE.
13. techniques as described in any one of claim 1-12, it is characterized in that, described technique comprises the following steps:
1) by waste acid water and the atmospheric distillation tower (3) containing N-BUTYL ACETATE, butanols through the distillate of first reboiler (7) of tower reactor in middle heat exchange to 70 ~ 75 DEG C of First Heat Exchanger (1), then be transported in mixing tank (2), mix with the feed liquid from the second phase splitter (10), 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 DEG C, 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 DEG C through the first water cooler (6), be transported to the first phase splitter (5) and carry out phase-splitting, heavy phase water backflow after phase-splitting, be gently the mixture of N-BUTYL ACETATE, fourth alcohol and water mutually, enter vacuum rectification tower (8) and carry out enrichment purification; Tower top temperature is 95 ~ 98 DEG C, and when bottom temperature is 100 ~ 103 DEG C, atmospheric distillation tower (3) tower reactor obtains the pure water that purity is greater than 99.99%;
3) working pressure of vacuum rectification tower (8) is 10 ~ 15kPa, overhead vapours is after the second water cooler (9) is cooled to 30 ~ 37 DEG C, be transported to the second phase splitter (10) and carry out phase-splitting, gently reflux mutually after phase-splitting, 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 vacuum rectification tower (8) tower reactor; Tower top temperature is 49 ~ 56 DEG C, and when bottom temperature is 59 ~ 68 DEG C, vacuum rectification tower (8) tower reactor obtains only containing N-BUTYL ACETATE and butanols, and alcohol ester is than the distillate being 0.38 ~ 0.67;
4) vacuum rectification 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 DEG C, 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 DEG C, and when bottom temperature is 189 ~ 194 DEG C, tower top obtains butanols, wherein biodiversity percentage concentration <0.5%, ester mass percentage concentration <5%, tower reactor obtains N-BUTYL ACETATE, its mass percentage concentration >99%.
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| CN106916050B (en) * | 2017-04-27 | 2023-11-07 | 太原理工大学 | Separation device for low-carbon mixed alcohol and application method thereof |
| CN109876485A (en) * | 2019-03-11 | 2019-06-14 | 天津乐科节能科技有限公司 | Acetic acid recovery is from backheat rectifier unit and method |
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| CN116271906B (en) * | 2023-03-14 | 2023-09-22 | 安徽瑞柏新材料有限公司 | Environment-friendly low-energy-consumption continuous butyl acetate preparation equipment |
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