CN1919821A - Method of recovery acetic acid from acetic acid containing waste water - Google Patents
Method of recovery acetic acid from acetic acid containing waste water Download PDFInfo
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- CN1919821A CN1919821A CN 200610021835 CN200610021835A CN1919821A CN 1919821 A CN1919821 A CN 1919821A CN 200610021835 CN200610021835 CN 200610021835 CN 200610021835 A CN200610021835 A CN 200610021835A CN 1919821 A CN1919821 A CN 1919821A
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Abstract
The invention discloses a recycling method of acetate from waste water with acetate, which is characterized by the following: adopting multi-effect distilling system to recycle acetate; making last tower steam as heat source of next tower to boil; or making the next tower steam as heat source of last tower to boil.
Description
Technical field
The present invention relates to from the waste water that contains acetic acid, reclaim the method for acetic acid.
Background technology
Acetic acid is a kind of important industrial chemicals commonly used or product, and many chemical processes all relate to the utilization and the recovery of acetic acid.Be to adopt the conventional distillation method to divide dried up-vinegar stock to reclaim acetic acid the earliest, the column plate that this method needs is many, and reflux ratio is big, and the rate of recovery is low, the energy consumption height; The oldest power-economizing method is to add the close material of acetic ester or physical properties and acetic acid to carry out azeotropic distillation, and its operational condition is difficult to be grasped, and still contains entrainer and little acetic acid in the water after separating, and needs to reclaim again, and energy-conservation amplitude is little.In recent years, some investigators have carried out dividing dried up and research acetic acid with the method for liquid-liquid extraction rectifying, utilize a kind of and water not dissolve each other and boiling point be significantly higher than acetic acid and with acetic acid have strong avidity solvent, as dimethyl formamide, N-methylacetamide, N-N-formyl morpholine N-, tetramethylene sulfone, alkyl ethanol amine etc., acetic acid is transferred to from water in the solvent of adding, utilize rectificating method with solvent and acetic acid separated again, reach the purpose of extracting and separating water-acetic acid; This method always has certain solubleness owing to selected solvent in water, the pollution that often brings the third material, and need to adopt at least two rectifying tower, and investment is big, and complex process is compared with conventional distillation, and energy-saving effect is also not obvious.
Summary of the invention
The purpose of this invention is to provide a kind of novel method that reclaims acetic acid from contain acetic acid containing waste water, this method also can cut down the consumption of energy when guaranteeing to obtain high purity acetic acid greatly.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method that reclaims acetic acid from contain acetic acid containing waste water, adopt the multiple-effect distillation system to reclaim acetic acid.
The above-mentioned multiple-effect distillation system different rectifying tower of at least two pressure of serving as reasons constitute, and according to pressure from high to low or order from low to high, the high-pressure tower overhead vapours of adjacent two towers is made the thermal source of lower pressure column reboiler.The number of rectifying tower (promptly imitating number) is preferably by 2-5 the different rectifying tower of pressure and constitutes.Used rectifying tower can be a packing tower, also can be tray column; The preferred less high efficiency packing tower of resistance that adopts.
The used different rectifying tower of pressure in the above-mentioned multiple-effect distillation system can be selected compression rectification tower, atmospheric distillation tower and the rectification under vacuum tower of different pressures for use.The operational condition of each rectifying tower is: have the 15-80 theoretical plate number, reflux ratio (trim the top of column is gone into the amount of liquid of tower and the ratio of overhead product amount) 1.0-7, the compression rectification pressure tower is that 0.20-0.50MPa (absolute pressure, down together), atmospheric distillation pressure tower are that 0.1-0.15MPa, rectification under vacuum pressure tower are 0.01-0.06MPa.
The principle of multiple-effect rectifying is: raw material is transported in each tower equably by approximate.The working pressure of tower is imitated last one by the 1st and is imitated step by step and reduce, and makes the tower still temperature that the tower top temperature of last effect is imitated a little more than back one.The 1st tower still of imitating tower is by the water vapor heat supply, and its overhead vapours heats the 2nd tower still of imitating as thermal source, and being condensed simultaneously obtains product.By that analogy, last effect overhead vapours one is imitated the tower still heat is provided backward as thermal source, simultaneously back one imitate tower bottoms as heat-eliminating medium with its condensation.Carry out so repeatedly.To the last one imitate, after an effect overhead vapours heating on its tower still quilt, overhead vapours is by extraneous heat-eliminating medium condensation.Like this, in whole flow process, just imitate the adding live steam the 1st, in the end one imitate the adding heat-eliminating medium, middle each tower then no longer needs to add steam and heat-eliminating medium, reaches energy-conservation purpose thus.Certainly, if also contain other impurity in the raw material, can according to circumstances increase cooling medium etc. at other tower.
In rectifying, the separating power of rectifying tower, depend primarily on rectifying tower suitable number of theoretical plate and the size of reflux ratio.The size of reflux ratio is to the separating effect and the economy important influence of rectifying.Increase reflux ratio, just can improve product purity, but also increase energy consumption.Therefore, when rectifying designed, reflux ratio was the conscientiously selected parameters of need.
On the other hand, the energy-saving effect of most rectifying decides with its effect number.Theoretically, compare with single tower, the energy-saving effect of the double-effect rectification of being made up of double tower is 50%, and the energy-saving effect of three-effect rectification is 67%, and the energy-saving effect of quadruple effect rectifying is 75%.By that analogy, imitate rectifying for N, its energy-saving effect can represent with a formula, that is:
Wherein η is an energy-saving effect, and N is the effect number of multiple-effect rectifying.But above-mentioned energy-saving effect is theoretical value, then can hang down when practical application.But also to consider relation between the facility investment of the energy of saving and increase.Can determine that it imitates number according to situations such as the temperature of the concentration of acetic acid in the waste water, thermal source and other economic principles.Imitate the increase of number, investment can increase certainly to some extent, but is not proportional, and because of the treatment capacity of each tower is inversely proportional to imitating number, it is many more promptly to imitate number, and the diameter of tower is more little, and each heat exchanger area also reduces.
Compared with prior art, the invention has the beneficial effects as follows: the present invention adopts the multiple-effect distillation system to reclaim acetic acid, order according to the pressure height, the high-pressure tower overhead vapours of adjacent two towers is made the thermal source of lower pressure column reboiler, that is to say that except that last tower, the condensation latent heat of all the other each the column overhead steam system self that all is distillated recycles, thereby the energy consumption of whole rectifying process is reduced greatly, and consumption of calorie is imitated number near 1/ of conventional distillation; And the acetic acid purity height of recovery gained, the rate of recovery is also high.In addition, the inventive method reclaims acetic acid need not add other solvent, and technology is simple, can not bring the pollution of other material.
Description of drawings
Fig. 1 is the double-effect rectification schema of the embodiment of the invention 2;
Fig. 2 is the double-effect rectification countercurrent flow figure of the embodiment of the invention 3;
Fig. 3 is the three-effect rectification schema of the embodiment of the invention 5;
Fig. 4 is the quadruple effect distillation process figure of the embodiment of the invention 7;
Fig. 5 is the quadruple effect distillation process figure of the embodiment of the invention 9.
Wherein, 1 is preheater, and 2 is the compression rectification tower, and 3 is reboiler, and 4 is the atmospheric distillation tower, and 5 are the rectification under vacuum tower, and 6 is condenser, and 7 is vacuum pump.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Embodiment 1
Present embodiment is a conventional distillation, as the reference examples of embodiment 2 and 3: adopt prior art conventional distillation (single tower) method to reclaim acetic acid from the waste water that contains acetic acid.Single tower is the atmospheric distillation tower, ripple packing, number of theoretical plate 50.
Operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| Single tower | 0.105 | 3.0 | 101.0 | 119.4 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | |
| Water | Acetic acid | ||
| Raw material | 570 | 66 | 34 |
| Product | 192.54 | 0.28 | 99.72 |
| Waste water | 377.46 | 99.52 | 0.48 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is 9.148t/t (acetic acid); The acetic acid rate of recovery is 99.07%.(" raw material " in the table be meant to reclaim and contain the acetic acid containing waste water raw material before the acetic acid, and " product " is meant the high purity acetic acid that reclaims the back gained through rectifying tower, and " waste water " is meant and reclaims the aqueous solution that is left behind the acetic acid; Pressure is absolute pressure; Down together.)
Present embodiment is a double-effect rectification: adopt the inventive method (double-effect rectification) to reclaim acetic acid from the waste water that contains acetic acid, flow process is seen Fig. 1, and two towers respectively are compression rectification tower and atmospheric distillation tower, are ripple packing, and number of theoretical plate is 50.
Each tower operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| The compression rectification tower | 0.308 | 3.2 | 134.5 | 137.0 |
| The atmospheric distillation tower | 0.105 | 2.85 | 101.1 | 119.5 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | |
| Water | Acetic acid | ||
| Raw material | 570 | 66 | 34 |
| Product | 191.2 | 0.25 | 99.75 |
| Waste water | 378.8 | 99.18 | 0.82 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is 4.465t/t (acetic acid), compares energy efficient 51.19% with embodiment 1; The acetic acid rate of recovery is 98.41%.
Present embodiment is double-effect rectification (adverse current): adopt the inventive method (double-effect rectification, adverse current) reclaim acetic acid from the waste water that contains acetic acid, flow process is seen Fig. 2, and two towers respectively are atmospheric distillation tower and compression rectification tower, be ripple packing, number of theoretical plate is 50.
Each tower operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| The atmospheric distillation tower | 0.105 | 2.90 | 101.0 | 103.7 |
| The compression rectification tower | 0.191 | 3.82 | 118.9 | 140.5 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | |
| Water | Acetic acid | ||
| Raw material | 570 | 66 | 34 |
| Product | 192.7 | 0.11 | 99.89 |
| Waste water | 377.3 | 99.66 | 0.34 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is 4.70t/t (acetic acid), compares energy efficient 48.62% with embodiment 1; The acetic acid rate of recovery is 99.32%.
Present embodiment is a conventional distillation, as the reference examples of embodiment 5: adopt prior art conventional distillation (single tower) method to reclaim acetic acid from the acetic acid containing waste water that contains light impurity.Single tower is the atmospheric distillation tower, floating valve tray, number of theoretical plate 50, tray efficiency 65%.
Operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| Single tower | 0.110 | 3.7 | 102.4 | 130.0 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | ||
| The ethyl ester methyl esters | Water | Acetic acid | ||
| Raw material | 2238.7 | 0.99 | 72.18 | 26.83 |
| Product | 587.1 | 0 | 0.39 | 99.61 |
| Waste water | 1651.6 | 1.35 | 97.7 | 0.95 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is 15.731t/t (acetic acid); The acetic acid rate of recovery is 97.36%.
Present embodiment is a three-effect rectification: adopt the inventive method (three-effect rectification) to reclaim acetic acid from the acetic acid containing waste water that contains light impurity, flow process is seen Fig. 3, and three towers respectively are compression rectification tower, atmospheric distillation tower and rectification under vacuum tower; Preceding two compression rectification towers are the floating valve tray tower, each tower number of theoretical plate 50, tray efficiency 65%; The rectification under vacuum tower is a ripple packing, number of theoretical plate 40.Because of a small amount of light impurity is arranged in the raw material, the condensation of compression rectification column overhead vapor portion, vapour phase is drawn light impurity.
Each tower operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| The compression rectification tower | 0.355 | 4.0 | 131.3 | 144.2 |
| The atmospheric distillation tower | 0.126 | 3.51 | 106.1 | 116.5 |
| The rectification under vacuum tower | 0.040 | 3.73 | 75.9 | 91.0 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | ||
| Methyl acetate | Water | Acetic acid | ||
| Raw material | 2238.7 | 0.99 | 72.18 | 26.83 |
| Product | 589.7 | 0 | 0.16 | 99.84 |
| Lighting end | 13.3 | 51.53 | 48.23 | 0.24 |
| Waste water | 1635.7 | 0.94 | 98.35 | 0.72 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is 5.588t/t (acetic acid), compares energy efficient 64.48% with embodiment 4; The acetic acid rate of recovery is 98.02%.
Present embodiment is a conventional distillation, as the reference examples of embodiment 7: adopt prior art conventional distillation (single tower) method to reclaim acetic acid from the waste water that contains acetic acid.Single tower is the atmospheric distillation tower, ripple packing, number of theoretical plate 50.
Operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| Single tower | 0.110 | 2.7 | 102.4 | 121.2 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | |
| Water | Acetic acid | ||
| Raw material | 4643 | 85.07 | 14.93 |
| Product | 671 | 0.14 | 99.86 |
| Waste water | 3972 | 99.43 | 0.57 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is 25.47t/t (acetic acid); The acetic acid rate of recovery is 96.66%.
Embodiment 7
Present embodiment is quadruple effect rectifying: adopt the inventive method (quadruple effect rectifying) to reclaim acetic acid from the waste water that contains acetic acid, flow process is seen Fig. 4, and four towers are respectively No. 1 tower, No. 2 towers, No. 3 towers and No. 4 towers.No. 1 tower and No. 2 towers are the compression rectification tower, and No. 2 tower internal pressures are less than No. 1 tower internal pressure, and No. 3 towers are the atmospheric distillation tower, and No. 4 towers are the rectification under vacuum tower; Four towers are ripple packing, and number of theoretical plate is 50.
Each tower operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| No. 1 tower | 0.290 | 3.00 | 132.4 | 133.3 |
| No. 2 towers | 0.193 | 3.03 | 119.1 | 120.3 |
| No. 3 towers | 0.121 | 3.09 | 104.9 | 107.1 |
| No. 4 towers | 0.040 | 3.04 | 75.9 | 92.9 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | |
| Water | Acetic acid | ||
| Raw material | 4643 | 85.07 | 14.93 |
| Product | 673.3 | 0.21 | 99.79 |
| Waste water | 3969.7 | 99.47 | 0.53 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is 6.85t/t (acetic acid), compares energy efficient 73.11% with embodiment 6; The acetic acid rate of recovery is 96.93%.
Embodiment 8
Present embodiment is a conventional distillation, reference examples as embodiment 9: adopt prior art conventional distillation method separating acetic acid from the acetic acid containing waste water that contains light impurity and heavy seeds, because in the raw material except that containing water and light impurity, also contain heavy seeds, so need with 2 towers, the 1st tower is dehydration tower, ripple packing, number of theoretical plate 50, cat head steams waste water; Second tower is a weight-removing column, and cat head steams pure acetic acid.The reboiler of two towers is used steam heating respectively.
Operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| Lightness-removing column | 0.11 | 2.70 | 101.8 | 121.1 |
| Weight-removing column | 0.11 | 1.00 | 120.6 | 132.0 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | |||
| Light impurity | Water | Acetic acid | Heavy seeds | ||
| Raw material | 571.43 | 4.00 | 61.00 | 35.00 | 0.09 |
| Product | 195.37 | 0.00 | 0.19 | 99.81 | 0.00 |
| Waste water | 374.08 | 6.11 | 93.08 | 0.81 | 0.00 |
| Heavy seeds | 1.98 | 0.00 | 0.00 | 75.00 | 25.00 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is: lightness-removing column 7.86t/t (acetic acid), and weight-removing column 0.51t/t (acetic acid) amounts to 8.37t/t (acetic acid); The acetic acid rate of recovery is 97.50%.
Embodiment 9
Present embodiment is quadruple effect rectifying: adopt the inventive method (quadruple effect rectifying) separating acetic acid from the acetic acid containing waste water that contains light impurity and heavy seeds, flow process is seen Fig. 5, and four towers are respectively No. 1 tower, No. 2 towers, No. 3 towers and No. 4 towers.No. 1 tower and No. 2 towers are the compression rectification tower, and No. 2 tower internal pressures are less than No. 1 tower internal pressure, and No. 3 towers and No. 4 towers are the rectification under vacuum tower, and No. 4 tower internal pressures are less than No. 3 tower internal pressures; Four towers are ripple packing, and first three tower number of theoretical plate is tower theoretical plate number 10 50, No. 4.Because of a small amount of light, heavy seeds is arranged in the raw material, in the condensation of No. 1 column overhead vapor portion, vapour phase is drawn light impurity.As separating heavy seeds usefulness, do not need higher reflux ratio with No. 4 towers because of separating heavy seeds, No. 3 column overhead steam only part for No. 4 tower reboilers heating, the condensation in No. 3 tower condensers of unnecessary steam.
Each tower operational condition sees the following form:
| Equipment | Tower top pressure MPa (a) | Reflux ratio | Tower top temperature ℃ | Tower still temperature ℃ |
| No. 1 tower | 0.435 | 3.20 | 130.2 | 149.0 |
| No. 2 towers | 0.164 | 3.26 | 114.0 | 117.9 |
| No. 3 towers | 0.085 | 3.38 | 85.2 | 102.0 |
| No. 4 towers | 0.020 | 1.00 | 71.7 | 73.2 |
Material balance sees the following form:
| Material | Flow kg/h | Form % (mass) | |||
| Light impurity | Water | Acetic acid | Heavy seeds | ||
| Raw material | 571.43 | 4.00 | 61.00 | 35.00 | 0.09 |
| Product | 196.26 | 0.00 | 0.09 | 99.91 | 0.00 |
| Waste water | 353.64 | 2.65 | 96.81 | 0.54 | 0.00 |
| Light impurity | 19.55 | 69.80 | 30.07 | 0.12 | 0.00 |
| Heavy seeds | 1.98 | 0.00 | 0.00 | 75.00 | 25.00 |
Per hour heating steam of present embodiment method (0.6MPaf) consumption is 3.17t/t (acetic acid), compares energy efficient 62.13% with embodiment 8; The acetic acid rate of recovery is 98.04%.
By above each embodiment as seen, acetic acid recovery method of the present invention can cut down the consumption of energy greatly, and consumption of calorie is imitated number near 1/ of conventional distillation, and the acetic acid purity of acquisition is higher, and the rate of recovery of acetic acid is also high; And technology is simple, does not have the pollution of other material.
Claims (7)
1. a method that reclaims acetic acid from contain acetic acid containing waste water is characterized in that: adopt the multiple-effect distillation system to reclaim acetic acid.
2. the method that from contain acetic acid containing waste water, reclaims acetic acid according to claim 1, it is characterized in that: the described multiple-effect distillation system different rectifying tower of at least two pressure of serving as reasons constitute, and according to pressure from high to low or order from low to high, the high-pressure tower overhead vapours of adjacent two towers is made the thermal source of lower pressure column reboiler.
3. the method that reclaims acetic acid from contain acetic acid containing waste water according to claim 2, it is characterized in that: described multiple-effect distillation system is for to be made of 2-5 the different rectifying tower of pressure.
4. the method that reclaims acetic acid from contain acetic acid containing waste water according to claim 2, it is characterized in that: described rectifying tower is packing tower or tray column.
5. the method that reclaims acetic acid from contain acetic acid containing waste water according to claim 4, it is characterized in that: described rectifying tower is the less high efficiency packing tower of resistance.
6. according to each described method that reclaims acetic acid from contain acetic acid containing waste water among the claim 2-5, it is characterized in that: the different rectifying tower of described pressure comprises compression rectification tower, atmospheric distillation tower and rectification under vacuum tower.
7. the method that from contain acetic acid containing waste water, reclaims acetic acid according to claim 6, it is characterized in that: the operational condition of described each rectifying tower is: have the 15-80 theoretical plate number, reflux ratio 1.0-7, compression rectification pressure tower are that 0.20-0.50MPa, atmospheric distillation pressure tower are that 0.1-0.15MPa, rectification under vacuum pressure tower are 0.01-0.06MPa.
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| CN107501085A (en) * | 2017-09-25 | 2017-12-22 | 华东理工大学 | A kind of method that economic benefits and social benefits are thermally integrated separation of extractive distillation acetic acid and aqueous mixtures |
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