CN106380393B - A kind of method of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater - Google Patents
A kind of method of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater Download PDFInfo
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- CN106380393B CN106380393B CN201610783238.5A CN201610783238A CN106380393B CN 106380393 B CN106380393 B CN 106380393B CN 201610783238 A CN201610783238 A CN 201610783238A CN 106380393 B CN106380393 B CN 106380393B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
- Y02B30/52—Heat recovery pumps, i.e. heat pump based systems or units able to transfer the thermal energy from one area of the premises or part of the facilities to a different one, improving the overall efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The present invention relates to a kind of methods of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater, belong to acetic acid recovery technical field.The present invention uses heat pump-multi-effect distillation combined system recovery of acetic acid, heat pump column overhead steam after compression, can be used not only as heat pump tower tower bottom heat, moreover it is possible to preheat to waste water, and the heat source as next rectifying tower reboiler, it is lower relative to individually multi-effect distillation system energy consumption.In addition, the recycling of the method for the present invention acetic acid suitable for low-concentration acetic acid wastewater, resulting acetic acid purity is high, the rate of recovery are also high.Meanwhile acetic acid recovery of the present invention is not required to that other solvents are added, simple process will not bring the pollution of other materials.The present invention be it is a kind of it is easy to operate, at low cost, energy consumption is small, the method for acetic acid purity and the high recovery of acetic acid from low-concentration acetic acid wastewater of the rate of recovery.
Description
Technical field
The invention belongs to acetic acid recovery technical field, specially a kind of heat pump-multi-effect distillation is from low-concentration acetic acid wastewater
The method of recovery of acetic acid.
Background technique
Acetic acid is a kind of important common industrial chemicals or product, and many chemical processes all refer to the utilization of acetic acid and return
It receives.It is to use conventional distillation method separation water-vinegar stock with recovery of acetic acid earliest, the column plate which needs is more, and reflux ratio is big,
The rate of recovery is low, and energy consumption is high；Oldest power-economizing method is that substance similar in acetate or physical property and acetic acid is added to carry out azeotropic essence
It evaporates, the more difficult grasp of operating condition, and still contains entrainer and a small amount of acetic acid in the water after separation, need recycling, energy conservation
Amplitude it is little.In recent years, some researchers have carried out with the research of method the separation water and acetic acid of liquid-liquid extraction rectifying, benefit
Be significantly higher than acetic acid with a kind of immiscible with water and boiling point and have the solvent of strong affinity with acetic acid, as dimethylformamide,
N- methylacetamide, N- N-formyl morpholine N, sulfolane, alkylethanolamine etc., by acetic acid from the solvent for being transferred to addition in water, then
Using rectificating method by solvent and acetic acid separated, achieve the purpose that extraction and separation water-acetic acid, the method due to selected solvent in water
There is certain solubility, often brings the pollution of the third substance.
Summary of the invention
The purpose of the present invention is to provide a kind of heat pump-multi-effect distillation system recovery of acetic acid from low-concentration acetic acid wastewater
Method, the present invention can also substantially reduce energy consumption while guaranteeing to obtain high-purity acetic acid.
The technical solution adopted by the present invention to solve the technical problems is: a kind of heat pump-multi-effect distillation is from low-concentration acetic acid
The method of recovery of acetic acid in waste water, using heat pump-multi-effect distillation combined system recovery of acetic acid.
Preferably as one kind of the invention, the heat pump-multi-effect distillation combined system is made of heat pump tower and purifying column, heat
Pump column overhead steam a part supplies after compressor compresses to heat pump tower reboiler for purifying tower reboiler heat supply, another part
Heat, then to heat pump column overhead is returned after spirit of vinegar feeding preheating, after the purified tower rectifying of heat pump tower materials at bottom of tower, tower bottom obtains vinegar
Acid product.
Preferably as one kind of the invention, the heat pump-multi-effect distillation combined system is made of heat pump tower and purifying column, heat
Column overhead steam is pumped all after compressor compresses, elder generation is to heat pump tower reboiler heat supply, then to spirit of vinegar feeding preheating, finally to
Tower reboiler heat supply is purified, after the purified tower rectifying of heat pump tower materials at bottom of tower, tower bottom obtains acetate products.
Preferably as one kind of the invention, the heat pump tower and purifying column are selected from compression rectification tower, the normal pressure of different pressures
Rectifying column and vacuum rectification tower.
Preferably as one kind of the invention, the heat pump tower can be packed tower, is also possible to plate column, preferably more passes through
The plate column of Ji.The purifying column can be packed tower, be also possible to plate column, preferably packed tower.
Preferably as one kind of the invention, the theoretical cam curve of the heat pump tower is 15-120, reflux ratio 1.0-7.0,
Pressure is 0.10-0.50MPa.
Preferably as one kind of the invention, the theoretical cam curve of the purifying column is 15-120, reflux ratio 1.0-7.0,
Pressure is 0.01-0.06MPa.Further, when heat pump pressure tower is greater than 0.3MPa, purifying column is atmospheric distillation tower.
The principle of heat pump distillation are as follows: by heat pump column overhead steam all through compressor compresses, and heat is provided to reboiler,
Only need a tower, it is no longer necessary to which outside provides steam heating, is equivalent to the multi-effect distillation of unlimited multistage.If compressed steam is used to
As the heat source of next rectifying tower reboiler, it is formed heat pump-multi-effect distillation combined system rectifying mode.In this way,
In whole flow process, in addition to needing to heat steam when driving, heat enough heat pump of the heat pump column overhead steam after compressor compresses
Tower and purification tower reboiler heat supply, entire distillation process no longer need external steam, and energy consumption substantially reduces.Since process is short, make
Equipment investment it is low, device is easy to operate.Certainly, if also containing other impurity in raw material, can according to circumstances increase in other towers
Add cooling medium etc..
In distillation process, the separating capacity of rectifying column depends primarily on the comparable number of theoretical plate of rectifying column institute and reflux
The size of ratio.The size of reflux ratio has an important influence the separating effect and economy of distillation process.Increase reflux ratio, just
Product purity can be improved, but also increase energy consumption.Therefore, in distillation design, reflux ratio is the parameter that need to conscientiously select.
Beneficial effects of the present invention: the present invention uses heat pump-multi-effect distillation combined system recovery of acetic acid, and heat pump column overhead is steamed
Vapour after compression, can be used not only as heat pump tower tower bottom heat, moreover it is possible to preheat to waste water, and as purification tower reboiler
Heat source is lower relative to individual multi-effect distillation system energy consumption.In addition, the method for the present invention vinegar suitable for low-concentration acetic acid wastewater
The recycling of acid, resulting acetic acid purity is high, the rate of recovery are also high.Meanwhile recovery of acetic acid is not required to be added other solvents, simple process,
The pollution of other materials will not be brought.
Detailed description of the invention
Fig. 1 is the quadruple effect distillation process figure of the embodiment of the present invention 1；
Fig. 2 is that heat pump-multi-effect distillation of the embodiment of the present invention 2 combines distillation process figure；
Heat pump-multi-effect distillation that Fig. 3 is 3-5 of the embodiment of the present invention combines distillation process figure.
Appended drawing reference: 1- preheater, 2- compressor, 3- reboiler, 4- condenser, 5- vacuum pump, 6- compression rectification tower, 7-
Atmospheric distillation tower, 8- vacuum rectification tower.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.All features disclosed in this specification or disclosed all methods or in the process
Step can combine in any way other than mutually exclusive feature and/or step.
Any feature disclosed in this specification (including any accessory claim, abstract), unless specifically stated,
It is replaced by other equivalent or with similar purpose alternative features.That is, unless specifically stated, each feature is a series of
An example in equivalent or similar characteristics.
Embodiment 1:
The present embodiment is quadruple effect rectifying, as the comparative example of embodiment 2~5, using quadruple effect disclosed in patent CN1919821
The method of rectifying recovery of acetic acid from low-concentration acetic acid wastewater, detailed process are as shown in Figure 1.Four towers are respectively No. 1 tower, No. 2
Tower, No. 3 towers and No. 4 towers.No. 1 tower and No. 2 towers are compression rectification tower, less than No. 1 tower pressure interior force of No. 2 tower pressure interior forces, and No. 3 towers are
Atmospheric distillation tower, No. 4 towers are vacuum rectification tower；Four towers are ripple packing, number of theoretical plate 52.
Each tower operating condition see the table below:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature (DEG C) | Bottom temperature (DEG C) |
| No. 1 tower | 0.430 | 3.20 | 111.8 | 112.3 |
| No. 2 towers | 0.153 | 3.13 | 99.0 | 99.7 |
| No. 3 towers | 0.099 | 3.27 | 84.9 | 86.0 |
| No. 4 towers | 0.059 | 3.24 | 64.1 | 74.2 |
Material balance see the table below:
Consumption of calorie is 5643.13kW, recovery rate 99.15% to the present embodiment method per hour.It is (" former in table
Material " refers to that the waste water raw material before recovery of acetic acid, " product " refer to the resulting high-purity acetic acid after rectifying column recycles,
" waste water " refers to remaining aqueous solution after recovery of acetic acid；Pressure is absolute pressure, similarly hereinafter.)
Embodiment 2
The present embodiment is combination rectifying, using the method for the present invention heat pump-multi-effect distillation combined system method from low concentration
Recovery of acetic acid in acetic acid wastewater, process are shown in that Fig. 2, two towers are respectively No. 1 tower, No. 2 towers.No. 1 tower is compression rectification tower, No. 2 towers
For vacuum rectification tower；No. 1 tower is plate column, and 72, No. 2 towers of number of theoretical plate are ripple packing, number of theoretical plate 52.
Each tower operating condition see the table below:
Material balance see the table below:
The present embodiment heat pump column overhead steam a part for purifying 3 heat supply of tower reboiler, press through compressor 2 by another part
3 heat supply of heat pump tower reboiler is given after contracting, then to heat pump column overhead is returned after spirit of vinegar feeding preheating, heat pump tower materials at bottom of tower is through mentioning
After pure tower rectifying, tower bottom obtains acetate products.
It is 1379.86kW (compressor efficiency 80%, similarly hereinafter) that the present embodiment method consumes energy per hour, compared with Example 1,
Energy saving 75.55%；Recovery rate is 99.59%.
Embodiment 3
The present embodiment is combination rectifying, using the method for the present invention heat pump-multi-effect distillation combined system method from low concentration
Recovery of acetic acid in acetic acid wastewater, process are shown in that Fig. 3, two towers are respectively No. 1 tower, No. 2 towers.No. 1 tower is compression rectification tower, No. 2 towers
For vacuum rectification tower；No. 1 tower is plate column, and 102, No. 2 towers of number of theoretical plate are ripple packing, number of theoretical plate 62.
Each tower operating condition see the table below:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature (DEG C) | Bottom temperature (DEG C) |
| No. 1 tower | 0.120 | 2.85 | 104.8 | 111.0 |
| No. 2 towers | 0.025 | 1.80 | 65.3 | 78.2 |
Material balance see the table below:
The present embodiment heat pump column overhead steam is all after the compression of compressor 2, first to 3 heat supply of heat pump tower reboiler, then it is right
Spirit of vinegar feeding preheating, finally to 3 heat supply of purifying column reboiler, after the purified tower rectifying of heat pump tower materials at bottom of tower, tower bottom is obtained
Acetate products.
The present embodiment method is consumed energy per hour for 1205.72kW, compared with Example 1, energy saving 78.63%；Acetic acid
The rate of recovery is 99.60%.
Embodiment 4
The present embodiment is combination rectifying, using the method for the present invention heat pump-multi-effect distillation combined system method from low concentration
Recovery of acetic acid in acetic acid wastewater, process are shown in that Fig. 3, two towers are respectively No. 1 tower, No. 2 towers.No. 1 tower is compression rectification tower, No. 2 towers
For vacuum rectification tower；No. 1 tower is plate column, and 102, No. 2 towers of number of theoretical plate are ripple packing, number of theoretical plate 62.
Each tower operating condition see the table below:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature (DEG C) | Bottom temperature (DEG C) |
| No. 1 tower | 0.200 | 3.30 | 120.2 | 125.1 |
| No. 2 towers | 0.025 | 1.80 | 65.3 | 78.2 |
Material balance see the table below:
The present embodiment heat pump column overhead steam is all after the compression of compressor 2, first to 3 heat supply of heat pump tower reboiler, then it is right
Spirit of vinegar feeding preheating, finally to 3 heat supply of purifying column reboiler, after the purified tower rectifying of heat pump tower materials at bottom of tower, tower bottom is obtained
Acetate products.
The present embodiment method is consumed energy per hour for 1151.99kW, compared with Example 1, energy saving 79.59%；Acetic acid
The rate of recovery is 99.59%.
Embodiment 5
The present embodiment is combination rectifying, using the method for the present invention heat pump-multi-effect distillation combined system method from low concentration
Recovery of acetic acid in acetic acid wastewater, process are shown in that Fig. 3, two towers are respectively No. 1 tower, No. 2 towers.No. 1 tower is compression rectification tower (heat pump
Tower), No. 2 towers are vacuum rectification tower；No. 1 tower is plate column, and 102, No. 2 towers of number of theoretical plate are ripple packing, and number of theoretical plate is
62。
Each tower operating condition see the table below:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature (DEG C) | Bottom temperature (DEG C) |
| No. 1 tower | 0.300 | 3.70 | 133.5 | 137.7 |
| No. 2 towers | 0.025 | 1.90 | 65.2 | 78.6 |
Material balance see the table below:
The present embodiment heat pump column overhead steam is all after the compression of compressor 2, first to 3 heat supply of heat pump tower reboiler, then it is right
Spirit of vinegar feeding preheating, finally to 3 heat supply of purifying column reboiler, after the purified tower rectifying of heat pump tower materials at bottom of tower, tower bottom is obtained
Acetate products.
The present embodiment method is consumed energy per hour for 1137.63kW, compared with Example 1, energy saving 79.84%；Acetic acid
The rate of recovery is 99.76%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of method of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater, which is characterized in that the method is adopted
With heat pump-multi-effect distillation combined system recovery of acetic acid:
The heat pump-multi-effect distillation combined system is made of heat pump tower and purifying column, and heat pump column overhead steam a part is for mentioning
Pure tower reboiler heat supply, another part after compressor compresses give the heat supply of heat pump tower reboiler, then to spirit of vinegar feeding preheating after
Heat pump column overhead is returned to, after the purified tower rectifying of heat pump tower materials at bottom of tower, tower bottom obtains acetate products；
The heat pump-multi-effect distillation combined system is made of heat pump tower and purifying column, and heat pump column overhead steam is all through compressor
After compression, first to heat pump tower reboiler heat supply, then to spirit of vinegar feeding preheating, finally to purifying column reboiler heat supply, heat pump tower
After the purified tower rectifying of materials at bottom of tower, tower bottom obtains acetate products.
2. a kind of method of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater as described in claim 1, feature
It is, the heat pump tower and purifying column compression rectification tower, atmospheric distillation tower and vacuum rectification tower selected from different pressures.
3. a kind of method of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater as described in claim 1, feature
It is, the heat pump tower is packed tower or plate column, and the purifying column is packed tower or plate column.
4. a kind of method of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater as described in claim 1, feature
It is, the theoretical cam curve of the heat pump tower is 15-120, reflux ratio 1.0-7.0, pressure 0.10-0.50MPa.
5. a kind of method of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater as described in claim 1, feature
It is, the theoretical cam curve of the purifying column is 15-120, reflux ratio 1.0-7.0, pressure 0.01-0.06MPa.
6. a kind of method of heat pump-multi-effect distillation recovery of acetic acid from low-concentration acetic acid wastewater as claimed in claim 5, feature
It is, when heat pump pressure tower is greater than 0.3MPa, purifying column is atmospheric distillation tower.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1919821A (en) * | 2006-09-13 | 2007-02-28 | 西南化工研究设计院 | Method of recovery acetic acid from acetic acid containing waste water |
| US20070102276A1 (en) * | 2005-11-09 | 2007-05-10 | Honeywell International, Inc. | Apparatus and methods for water regeneration from waste |
| CN102153092A (en) * | 2011-04-27 | 2011-08-17 | 天津大学 | Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane |
-
2016
- 2016-08-30 CN CN201610783238.5A patent/CN106380393B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070102276A1 (en) * | 2005-11-09 | 2007-05-10 | Honeywell International, Inc. | Apparatus and methods for water regeneration from waste |
| CN1919821A (en) * | 2006-09-13 | 2007-02-28 | 西南化工研究设计院 | Method of recovery acetic acid from acetic acid containing waste water |
| CN102153092A (en) * | 2011-04-27 | 2011-08-17 | 天津大学 | Heat pump distillation and multi-effect distillation integrated device and process for purifying trichlorosilane |
Non-Patent Citations (1)
| Title |
|---|
| 低浓度DMF废水的热集成回收新工艺;孙钦鹤等;《计算机与应用化学》;20120428;第29卷(第4期);第413-418页 |
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