CN109053424B - System and method for recycling refined acetic acid from various acetic acid waste liquid - Google Patents
System and method for recycling refined acetic acid from various acetic acid waste liquid Download PDFInfo
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- CN109053424B CN109053424B CN201811282614.8A CN201811282614A CN109053424B CN 109053424 B CN109053424 B CN 109053424B CN 201811282614 A CN201811282614 A CN 201811282614A CN 109053424 B CN109053424 B CN 109053424B
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 485
- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000002699 waste material Substances 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 title claims abstract description 24
- 238000004064 recycling Methods 0.000 title description 8
- 238000000605 extraction Methods 0.000 claims abstract description 90
- 238000001704 evaporation Methods 0.000 claims abstract description 37
- 230000008020 evaporation Effects 0.000 claims abstract description 37
- 239000012535 impurity Substances 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 68
- 239000000463 material Substances 0.000 claims description 44
- 238000010992 reflux Methods 0.000 claims description 27
- 238000005191 phase separation Methods 0.000 claims description 21
- 150000003839 salts Chemical class 0.000 claims description 17
- 238000007670 refining Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 12
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- 239000011552 falling film Substances 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 5
- 235000011056 potassium acetate Nutrition 0.000 claims description 5
- 239000004317 sodium nitrate Substances 0.000 claims description 5
- 235000010344 sodium nitrate Nutrition 0.000 claims description 5
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 4
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 4
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 claims description 4
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 claims description 4
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 2
- 235000011151 potassium sulphates Nutrition 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 16
- 239000003795 chemical substances by application Substances 0.000 description 28
- 239000002351 wastewater Substances 0.000 description 19
- 239000007789 gas Substances 0.000 description 14
- 229920005610 lignin Polymers 0.000 description 12
- 238000011084 recovery Methods 0.000 description 12
- 238000010533 azeotropic distillation Methods 0.000 description 10
- 238000004821 distillation Methods 0.000 description 8
- 238000000926 separation method Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- -1 acetate compound Chemical class 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011345 viscous material Substances 0.000 description 1
Classifications
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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
-
- 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
-
- 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
- C07C51/46—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by azeotropic distillation
-
- 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
- C07C51/48—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a system and a method for recovering refined acetic acid from various acetic acid waste liquid, wherein the system comprises a first-effect evaporator, a second-effect evaporator, an extraction tower and a rectifying tower, a concentrated solution outlet of the first-effect evaporator is connected with an inlet of the second-effect evaporator, a secondary steam outlet of the first-effect evaporator is connected with a heat transfer medium inlet of the second-effect evaporator, a heat transfer medium outlet of the second-effect evaporator and a secondary steam outlet of the second-effect evaporator are connected with a feed inlet of the rectifying tower, and an extraction phase outlet of the extraction tower is connected with a feed inlet of the rectifying tower. The method comprises the steps of delivering raw materials containing heavy impurity components to a first-effect evaporator for evaporation, delivering concentrated solution to a second-effect evaporator, and taking secondary steam as a heat source of the second-effect evaporator; feeding the condensed secondary steam into a rectifying tower for azeotropic rectification; extracting a part of the raw materials without heavy impurity components; the other part of raw materials and the extraction phase are sent into a rectifying tower for azeotropic rectification, and the system and the method can recover acetic acid from different kinds of acetic acid waste liquid, and have the advantages of low system equipment investment and low energy consumption.
Description
Technical Field
The invention belongs to the technical field of acetic acid recovery and refining, and particularly relates to a system and a method for recovering and refining acetic acid from various acetic acid waste liquid.
Background
Acetic acid is an important chemical raw material and is an excellent organic solvent, and is widely applied to the fields of chemical industry, light spinning, medicine industry and the like. While acetic acid wastewater is produced in many chemical production links, the sources of the acetic acid wastewater are different, the compositions of the acetic acid wastewater are different, acetic acid wastewater containing heavy impurity components with boiling points higher than those of acetic acid is produced in some production links, dilute acetic acid is produced, the water is required to be removed for recycling the acetic acid, and the heavy impurity components are required to be removed for the acetic acid wastewater containing the heavy impurity components.
The boiling point of acetic acid is higher than that of water, but is close to that of water, and the relative volatility is low, so that water is generally required to be removed by a rectification method, the acetic acid is usually subjected to ordinary rectification or azeotropic rectification, if the acetic acid with high purity is obtained by ordinary rectification, more tower plates and larger reflux ratio are required, the equipment investment is high, and great energy consumption is generated. In addition, the process of separating heavy impurity components also generates larger energy consumption for the acetic acid wastewater containing the heavy impurity components.
Therefore, a system and a method for separating and recovering the refined acetic acid from different types of acetic acid waste liquid are needed, the equipment investment of the whole acetic acid recovery refining system is low, and the energy consumption of the recovery refining process system is low.
Disclosure of Invention
The invention aims to solve the problem of providing a system and a method for recovering and refining acetic acid from various acetic acid waste liquid, which can separate and recover the refined acetic acid from the various acetic acid waste liquid, and the whole recovery and refining system has less equipment investment and low system energy consumption.
In order to solve the technical problems, an object of the present invention is to provide a system for recovering refined acetic acid from various acetic acid waste liquid, which comprises a first-effect evaporator, a second-effect evaporator, an extraction tower and a first rectifying tower, wherein the first-effect evaporator is provided with a concentrated material inlet, a concentrated solution outlet of the first-effect evaporator is connected with a material inlet of the second-effect evaporator, a secondary steam outlet of the first-effect evaporator is connected with a heat transfer medium inlet of the second-effect evaporator, a heat transfer medium outlet of the second-effect evaporator and a secondary steam outlet of the second-effect evaporator are connected with a material inlet of the first rectifying tower, the extraction tower is provided with a dilute material inlet, an extraction phase outlet of the extraction tower is connected with a material inlet of the first rectifying tower, preferably, the first-effect evaporator is a falling film evaporator, and preferably, the second-effect evaporator is a forced circulation evaporator.
In the technical scheme, the device preferably further comprises a phase separator and a reflux tank, wherein the gas phase extraction outlet at the top of the first rectifying tower is connected with the inlet of the phase separator, the oil phase outlet of the phase separator is connected with the reflux tank, and the reflux tank is connected with the reflux inlet of the first rectifying tower and the feed inlet of the extraction tower.
In the technical scheme, the method preferably further comprises a second rectifying tower, wherein the water phase outlet of the phase separator is connected with the feed inlet of the second rectifying tower, and the gas phase extraction outlet at the top of the second rectifying tower is connected with the inlet of the phase separator.
In the technical scheme, preferably, the first-effect evaporator comprises a first-effect heat exchanger and a first-effect evaporation chamber, the second-effect evaporator comprises a second-effect heat exchanger, a second-effect evaporation chamber and a condenser, the first-effect heat exchanger is communicated with the first-effect evaporation chamber, a secondary steam outlet of the first-effect evaporation chamber is communicated with the second-effect heat exchanger, the second-effect heat exchanger is communicated with the second-effect evaporation chamber, a secondary steam outlet of the second-effect evaporation chamber is connected with an inlet of the condenser, and a concentrated solution outlet of the first-effect evaporation chamber and an outlet of the condenser are connected with a feed inlet of the first rectifying tower.
It is another object of the present invention to provide a method for recovering purified acetic acid from various types of acetic acid waste solutions, comprising:
Firstly, delivering raw materials containing heavy impurity components to a first-effect evaporator for evaporation, delivering the generated concentrated solution to a second-effect evaporator for evaporation, and taking secondary steam generated by the first-effect evaporator as a heat source of the second-effect evaporator;
secondly, sending the secondary steam of the first-effect evaporator and the second-effect evaporator after condensation into a first rectifying tower, and adding an entrainer to carry out azeotropic rectification operation;
Thirdly, sending a part of raw materials which do not contain heavy impurity components into an extraction tower for countercurrent extraction operation;
fourthly, sending the other part of raw materials without heavy impurity components and the extract phase of the extraction tower into a first rectifying tower for azeotropic rectification;
Fifthly, extracting acetic acid products from the side line of the first rectifying tower;
the order of the first step and the third step may be interchanged.
In the method, because the sources of acetic acid wastewater are different, the impurity components contained in the generated acetic acid wastewater are different, acetic acid wastewater containing heavy impurity components with boiling points higher than that of acetic acid is sent into a double-effect evaporator to be evaporated, the heavy impurity components in the acetic acid wastewater are separated, the acetic acid wastewater is firstly evaporated and separated by a first-effect evaporator, the generated concentrated solution containing a small amount of acetic acid is sent into a second-effect evaporator to be continuously separated, then acetic acid separated by the first-effect evaporator and the second-effect evaporator is sent into a rectifying tower after being condensed, an entrainer is added to be subjected to azeotropic rectification, and the bottom of the second-effect evaporator is the concentrated heavy impurity component; and for dilute acetic acid wastewater which does not contain heavy impurity components, a part of the dilute acetic acid wastewater is pumped to the top of an extraction tower through a feed pump, an extracting agent enters from the bottom of the extraction tower and is subjected to countercurrent contact extraction operation, raffinate phase wastewater is discharged from a tower kettle, an extracting phase contains acetic acid, the extracting agent and part of water and is extracted from the top of the extraction tower and is sent to a rectifying tower for azeotropic distillation operation, the other part of the extracting phase is directly sent to the rectifying tower for azeotropic distillation operation, and finally an acetic acid product is extracted from the side line of the rectifying tower. The treatment of the acetic acid wastewater containing heavy impurity components and the treatment of dilute acetic acid can be carried out simultaneously or respectively, and the rectification part of the acetic acid wastewater can carry out azeotropic rectification in the same rectification tower.
According to the method, the refined acetic acid can be recovered from different types of acetic acid waste liquid, and when heavy and impurity components in the acetic acid waste liquid are treated, the double-effect evaporator is adopted, and secondary steam generated by the first-effect evaporator is used as a heat source of the second-effect evaporator, so that on one hand, waste heat in a product is effectively utilized, the energy consumption of a system is reduced, and on the other hand, cooling equipment and energy consumption required for cooling the acetic acid product after the first-effect evaporator are omitted; in the rectification operation, the dilute acetic acid raw material is divided into two parts, one part is firstly sent to an extraction tower to separate most of water, and then is sent to a rectification tower together with the other part of raw material for azeotropic operation, so that the treatment capacity of the rectification tower and the water content in the materials in the rectification tower are greatly reduced, the consumption of an entrainer is reduced, the operation load of the rectification tower is reduced, and the energy consumption of the rectification tower is greatly reduced.
In the technical scheme, the method preferably further comprises the steps of condensing the gas phase at the top of the first rectifying tower, sending the condensed gas phase into a phase separator for phase separation, and refluxing one part of the oil phase obtained by phase separation into the first rectifying tower, and sending the other part of the oil phase into an extraction tower for extraction operation. The gas phase at the top of the rectifying tower is mainly water, extractant, entrainer and partial acetic acid, and after phase separation by a phase separator, the oil phase is mainly extractant, entrainer and acetic acid, and the oil phase is refluxed to the rectifying tower and the extracting tower to further separate the acetic acid.
In the technical scheme, the method preferably further comprises the steps of sending the water phase obtained by phase separation of the phase separator to a second rectifying tower for rectification operation, and sending the top extracted phase of the second rectifying tower to the phase separator for phase separation. The water phase obtained by phase separation of the phase separator is mainly water, and also contains partial extractant and entrainer, after the water phase is sent to a recovery tower to be rectified, partial water is separated, and then the extractant and entrainer in the water phase are recovered to the phase separator for reuse, so that the consumption of the extractant and entrainer can be greatly reduced, and the waste of the extractant and entrainer is reduced.
In the technical scheme, preferably, the extractant used in the extraction operation is an extraction solvent added with salt; the extraction solvent used in the extraction operation in the acetic acid recovery method is an extraction solvent added with salt, and the addition of the salt can change the activity coefficient of each component in the solution, so that the solubility of each component in the extraction solvent is changed, the solubility of acetic acid in the extraction solvent is improved, and the solubility of water is reduced, so that the consumption of the extraction agent in the extraction operation can be reduced, the operation load of the extraction tower is reduced, and the energy consumption is reduced.
Preferably, the salt is one or a combination of potassium and sodium salts;
more preferably, the salt is one or more of potassium acetate, sodium nitrate, potassium nitrate, sodium sulfate and potassium sulfate;
more preferably, the salt is one or more of potassium acetate, sodium nitrate and potassium nitrate;
Preferably, the extraction solvent is an acetate compound;
more preferably, the extraction solvent is one or more of n-butyl acetate, isobutyl acetate and methyl acetate;
more preferably, the extraction solvent is n-butyl acetate.
In the technical scheme, the concentration of salt in the extracting agent is preferably 30-300kg/m 3, and the concentration of salt is preferably 80-150kg/m 3.
In the technical scheme, the temperature of the first-effect evaporator is preferably 90-115 ℃, the temperature of the second-effect evaporator is preferably 50-80 ℃, and the operating pressure is preferably 40-60kpa.
Wherein the mass ratio of the extractant to the raw materials is 1-10, preferably 5-8.
Wherein the mass ratio of the raw materials entering the extraction tower to the rectifying tower is 0.5-3, and preferably, the mass ratio of the raw materials entering the extraction tower to the rectifying tower is 1.
Wherein the extraction operation temperature of the extraction tower is 20-80 ℃, the pressure is 100-130kPa, and the theoretical plate number is 30-70.
Wherein the theoretical plate number of the rectifying tower is 50-80, and the reflux ratio is 0.5-0.8.
The invention has the advantages and positive effects that:
1. The system and the method for recycling and refining the acetic acid can treat different types of acetic acid waste liquid, recycle and refine the acetic acid in the acetic acid waste liquid, and have low energy consumption of the whole system;
2. When heavy and impurity components in the acetic acid waste liquid are removed, the double-effect evaporator is used, secondary steam generated by the first-effect evaporator is used as a heat source of the second-effect evaporator, waste heat in the product is effectively utilized, the total energy consumption of the evaporator is reduced, and condensing equipment and energy consumption of the secondary steam in the first-effect evaporator are omitted;
3. The method comprises the steps of firstly removing water in a part of dilute acetic acid materials with higher water content through extraction operation, then carrying out azeotropic distillation operation, greatly reducing the treatment capacity of a distillation tower, reducing the consumption of entrainer in the distillation operation, reducing the load of the distillation tower, reducing the energy consumption of the distillation operation, and reducing the diameter and the height of the distillation tower although one more extraction tower is used than single azeotropic distillation, so that the overall equipment investment is not higher than single azeotropic distillation;
4. The salt is added into the extractant used in the extraction operation, so that the solubility of acetic acid and water in the extractant is changed, the solubility of acetic acid in the extractant is improved, and the solubility of water is reduced, thereby greatly reducing the consumption of the extractant required by extraction, reducing the load of an extraction tower and reducing the energy consumption of a system;
5. The separated extractant and entrainer are also recovered and recycled, so that the consumption of the extractant and the entrainer is reduced.
Drawings
FIG. 1 is a schematic diagram of a system for recovering purified acetic acid from various acetic acid waste streams according to an embodiment of the present invention.
In the figure:
1. first-effect evaporator 2, second-effect evaporator 3 and extraction tower
4. Rectifying tower 5, dense material feed inlet 6 and dilute material inlet
7. Phase separator 8, reflux drum 9, rectifying column
10. Buffer tank 11, first-effect heat exchanger 12 and first-effect evaporation chamber
13. Feed pump 21, two-effect heat exchanger 22 and two-effect evaporation chamber
23. Condenser 24, forced circulation pump
Detailed Description
Embodiments of the invention are further described below with reference to the accompanying drawings:
As shown in fig. 1, the system for recovering refined acetic acid from various acetic acid waste liquid according to the embodiment comprises a first-effect evaporator 1, a second-effect evaporator 2, an extraction tower 3 and a rectifying tower 4, wherein the first-effect evaporator 1 is provided with a concentrated material feed inlet 5, a feed pump is connected in front of the concentrated material feed inlet 5, a concentrated solution outlet of the first-effect evaporator 1 is connected with a material inlet of the second-effect evaporator 2, a secondary steam outlet of the first-effect evaporator 1 is connected with a heat transfer medium inlet of the second-effect evaporator 2, a heat transfer medium outlet of the second-effect evaporator 2 and a secondary steam outlet of the second-effect evaporator 2 are connected with a feed inlet of the rectifying tower 4, the extraction tower 3 is provided with a dilute material inlet 6, and an extract phase outlet of the extraction tower 3 is connected with a feed inlet of the rectifying tower 4.
In the acetic acid waste liquid to be treated, a material containing heavy impurity components with boiling point higher than that of acetic acid enters the first-effect evaporator 1 through a concentrated material feed port 5 on the first-effect evaporator 1 for preliminary evaporation separation, secondary steam consisting of acetic acid and water is generated at the top of the first-effect evaporator 1, a concentrated material containing heavy impurity components is generated at the bottom of the first-effect evaporator, the concentrated material at the bottom enters the second-effect evaporator 2 for continuous evaporation separation, the secondary steam generated by the first-effect evaporator 1 is introduced into a shell side of the second-effect evaporator as a heat source of the second-effect evaporator for supplying heat to the second-effect evaporator, the second-effect evaporator for evaporation separation generates secondary steam containing acetic acid and water at the top of the second-effect evaporator, a concentrated product containing heavy impurity components is generated at the bottom of the second-effect evaporator, the secondary steam generated by evaporation of the first-effect evaporator is condensed into a liquid state in the second-effect evaporator 2, the secondary steam separated by the second-effect evaporator 2 is pumped into a rectifying tower 4 together through feeding, an entrainer is added for azeotropic distillation, and an acetic acid product is extracted at a side line of the rectifying tower; and a part of the dilute acetic acid material without heavy impurity components is sent to the top of the extraction tower 3 through a dilute material inlet 6 by a feed pump, an extractant inlet is arranged at the bottom of the extraction tower 3, the extractant is sent from the bottom of the extraction tower to carry out countercurrent contact extraction operation, the moisture in the material is removed, and then the dilute acetic acid material and the rest part of the dilute acetic acid material are sent into a rectifying tower 4 together to carry out azeotropic rectification operation, and acetic acid products are extracted from the side line of the bottom of the tower.
The system for recycling and refining acetic acid can treat different types of acetic acid waste liquid, and recycle and refine acetic acid from the waste liquid; the acetic acid waste liquid containing heavy impurity components is removed by using a double-effect evaporator, the secondary steam generated by the first-effect evaporator is used as a heat source of the second-effect evaporator, the heat of the secondary steam generated by the first-effect evaporator is fully utilized, the energy consumption is reduced, the secondary steam generated by the first-effect evaporator is condensed in the shell pass of the second-effect evaporator, and a condenser behind the first-effect evaporator is also omitted; the method is characterized in that the operation of extraction and azeotropic distillation is carried out on the dilute acetic acid containing more water, a part of dilute acetic acid is subjected to azeotropic distillation together with another part of materials after most of water is removed by extraction, the treatment capacity of a distillation column is reduced, the consumption of an entrainer is low, the load of the distillation column is reduced, the energy consumption of distillation operation is reduced, and the whole equipment investment is not higher than that of the single azeotropic distillation although one more extraction column is used than that of the single azeotropic distillation.
A buffer tank 10 and a feed pump 13 are further arranged between the two-effect evaporator 2 and the rectifying tower 4, the buffer tank 10 is connected with the outlet of a condenser 23 of the two-effect evaporator 2 and the outlet of a two-effect heat exchanger 21 of the two-effect evaporator 2, the outlet of the buffer tank 10 is connected with the feed pump 13, and the feed pump 13 is connected with the feed inlet of the rectifying tower 4.
In the technical scheme, the device preferably further comprises a phase separator 7 and a reflux tank 8, wherein a gas phase extraction outlet at the top of the rectifying tower 4 is connected with an inlet of the phase separator 7, an oil phase outlet of the phase separator 7 is connected with the reflux tank 8, and the reflux tank 8 is connected with a reflux inlet of the rectifying tower 4 and a feed inlet of the extraction tower 3. The gas phase at the top of the rectifying tower is mainly water, extractant, entrainer and partial acetic acid, and after phase separation by the phase separator 7, the oil phase is mainly extractant, entrainer and acetic acid, and the oil phase is refluxed to the rectifying tower 4 and the extracting tower 3 to further separate the acetic acid therein.
In the technical scheme, the method preferably further comprises a rectifying tower 9, wherein the water phase outlet of the phase separator 7 is connected with the feeding port of the rectifying tower 9, and the gas phase extraction port at the top of the rectifying tower 9 is connected with the inlet of the phase separator 7. The water phase after phase separation by the phase separator 7 mainly contains extractant, entrainer and water, the water phase is sent into the rectifying tower 9 for rectifying operation, the water is separated from the extractant and the entrainer, the extractant and the entrainer can be recycled, and the consumption of the extractant and the entrainer is reduced.
The first-effect evaporator 1 comprises a first-effect heat exchanger 11 and a first-effect evaporation chamber 12, the second-effect evaporator 2 comprises a second-effect heat exchanger 21, a second-effect evaporation chamber 22 and a condenser 23, the first-effect heat exchanger 11 is communicated with the first-effect evaporation chamber 12, a secondary steam outlet of the first-effect evaporation chamber 12 is communicated with the second-effect heat exchanger 21, the second-effect heat exchanger 21 is communicated with the second-effect evaporation chamber 22, a secondary steam outlet of the second-effect evaporation chamber 22 is connected with an inlet of the condenser 23, and a concentrated solution outlet of the first-effect evaporation chamber 12 and an outlet of the condenser 23 are connected with a feed inlet of the rectifying tower 4.
Preferably, a forced circulation pump 24 is further arranged between the two-effect heat exchanger 21 and the two-effect evaporation chamber 22, and the viscosity of the primarily concentrated material processed in the two-effect evaporator 2 is increased, so that the more viscous material in the two-effect evaporator 2 is forced to circulate by arranging the forced circulation pump 24, the circulating flow of the material is promoted, the adhesion of the material in the evaporator is prevented, and the evaporation efficiency is improved.
Preferably, the first-effect evaporator 1 is a falling film evaporator, and the feed liquid in the falling film evaporator falls in a film shape along the pipe wall under the action of gravity, so that the heat transfer coefficient is high, and the evaporation efficiency is higher.
The specific examples of the method for recovering and refining acetic acid from various acetic acid waste liquid provided by the invention are as follows:
example 1
The method for recovering and refining acetic acid in the embodiment comprises the following steps:
the materials to be treated are as follows: the concentrated acetic acid feed included approximately 62% acetic acid, 23% water, 8% sugar, 7% lignin, and the dilute acetic acid feed included 50% acetic acid, 50% water.
1. The concentrated acetic acid material is conveyed into a first-effect evaporator through a feed pump, the first-effect evaporator is heated and evaporated by a falling film evaporator, so that acetic acid and water are separated from sugar and lignin in the material, the temperature of the first-effect evaporator is 105 ℃, the operating pressure is normal pressure, secondary steam containing acetic acid and water is extracted from the upper part, primarily concentrated solution containing sugar, lignin and a small amount of acetic acid and water is extracted from the lower part, the secondary steam is taken as a heat source to be introduced into the shell side of the second-effect evaporator, and is condensed in the shell side of the second-effect evaporator, the temperature of the second-effect evaporator is 80 ℃, the operating pressure is 50kpa, the concentrated solution is conveyed into the second-effect evaporator for forced circulation evaporation separation, the separated acetic acid and water are extracted from the upper part, and the concentrated solution containing sugar and lignin is extracted from the bottom;
2. after the secondary steam separated by the first-effect evaporator and the secondary steam separated by the second-effect evaporator are condensed, only acetic acid and water are contained, and the secondary steam is sent into a buffer tank and then is sent to the middle lower part of a rectifying tower by a pump for azeotropic rectification operation;
3. 23% of dilute acetic acid material is conveyed to the top of an extraction tower through a feed pump, an extracting agent enters from the bottom of the extraction tower to perform normal pressure normal temperature countercurrent contact extraction operation, the extracting agent is n-butyl acetate solvent added with potassium acetate, the mass ratio of the extracting agent to raw materials is 2:1, the concentration of salt in the extracting agent is 100kg/h, the diameter of the extraction tower is 300mm, and the theoretical plate number is 50;
4. Acetic acid and an extracting agent are extracted from the top of the extraction tower and are conveyed into a rectifying tower through a feed pump to serve as feed, azeotropic rectification operation is carried out together with the other part of dilute acetic acid material and the acetic acid and water mixture obtained in the step 2, the entrainer is n-butyl acetate, the adding amount of the entrainer is 800kg/h, the top of the rectifying tower is 800mm, the theoretical pedal number is 30-40, the minimum reflux ratio is 0.5-0.8, the steam consumption is 1.1t/h, and acetic acid is extracted from a rectifying side line after azeotropic rectification operation, and the concentration is 99.5%;
5. The gas phase extracted from the top of the rectifying tower is mainly water, an extracting agent, an entrainer and a small amount of acetic acid, the gas phase is cooled by a condenser and then is sent into a phase separator for phase separation, the obtained oil phase is mainly the extracting agent, the entrainer and the acetic acid, the oil phase is sent into a reflux tank, one part of the oil phase is refluxed into the rectifying tower by a reflux pump, the other part of the oil phase is pumped into the extracting tower for recycling, the water phase is mainly water, and the oil phase also contains part of the extracting agent and the entrainer;
6. and (3) sending the water phase obtained by phase separation into a recovery tower for rectification operation, obtaining an extractant and an entrainer at the top of the tower, sending the extractant and the entrainer into a phase separator for further phase separation, and storing or discharging waste water extracted from the tower bottom of the recovery tower.
Example two
The method for recovering and refining acetic acid in the embodiment comprises the following steps:
The materials to be treated are as follows: the concentrated acetic acid feed included approximately 70% acetic acid, 15% water, 9% sugar, 6% lignin, and the dilute acetic acid feed included 35% acetic acid, 65% water.
1. The concentrated acetic acid material is conveyed into a first-effect evaporator through a feed pump, the first-effect evaporator is heated and evaporated by a falling film evaporator, the temperature of the first-effect evaporator is 107 ℃, the operating pressure is normal pressure, acetic acid and water in the first-effect evaporator are separated from sugar and lignin in the material, secondary steam containing acetic acid and water is extracted from the upper part, primarily concentrated solution containing sugar, lignin and a small amount of acetic acid and water is extracted from the lower part, the secondary steam is taken as a heat source to be introduced into the shell side of the second-effect evaporator, and is condensed in the shell side of the second-effect evaporator, the temperature of the second-effect evaporator is 83 ℃, the operating pressure is 50kpa, the concentrated solution is conveyed into the second-effect evaporator for forced circulation evaporation separation, the separated acetic acid and water are extracted from the upper part, and the concentrated solution containing sugar and lignin is extracted from the bottom;
2. after the secondary steam separated by the first-effect evaporator and the secondary steam separated by the second-effect evaporator are condensed, only acetic acid and water are contained, and the secondary steam is sent into a buffer tank and then is sent to the middle lower part of a rectifying tower by a pump for azeotropic rectification operation;
3. Conveying 40% of dilute acetic acid material to the top of an extraction tower through a feed pump, enabling an extracting agent to enter from the bottom of the extraction tower to perform normal-pressure normal-temperature countercurrent contact extraction operation, wherein the extracting agent is isobutyl acetate solvent added with sodium acetate, the mass ratio of the extracting agent to raw materials is 8:1, the concentration of salt in the extracting agent is 120kg/h, the diameter of the extraction tower is 300mm, and the theoretical plate number is 50;
4. Acetic acid and an extracting agent are extracted from the top of the extraction tower and are conveyed into a rectifying tower through a feed pump to serve as feed, azeotropic rectification operation is carried out together with the other part of dilute acetic acid material and the acetic acid and water mixture obtained in the step 2, the entrainer is isobutyl acetate, the adding amount of the entrainer is 1000kg/h, the top of the rectifying tower is 800mm, the theoretical pedal number is 30-40, the minimum reflux ratio is 0.5-0.8, the steam consumption is 1.1t/h, and the concentration of acetic acid is 99.5% from a rectifying side line after azeotropic rectification operation;
5. The gas phase extracted from the top of the rectifying tower is mainly water, an extracting agent, an entrainer and a small amount of acetic acid, the gas phase is cooled by a condenser and then is sent into a phase separator for phase separation, the obtained oil phase is mainly the extracting agent, the entrainer and the acetic acid, the oil phase is sent into a reflux tank, one part of the oil phase is refluxed into the rectifying tower by a reflux pump, the other part of the oil phase is pumped into the extracting tower for recycling, the water phase is mainly water, and the oil phase also contains part of the extracting agent and the entrainer;
6. and (3) sending the water phase obtained by phase separation into a recovery tower for rectification operation, obtaining an extractant and an entrainer at the top of the tower, sending the extractant and the entrainer into a phase separator for further phase separation, and storing or discharging waste water extracted from the tower bottom of the recovery tower.
Example III
The method for recovering and refining acetic acid in the embodiment comprises the following steps:
The materials to be treated are as follows: the concentrated acetic acid feed included approximately 45% acetic acid, 42% water, 8% sugar, 5% lignin, and the dilute acetic acid feed included 23% acetic acid, 77% water.
1. The concentrated acetic acid material is conveyed into a first-effect evaporator through a feed pump, the first-effect evaporator is heated and evaporated by a falling film evaporator, so that acetic acid and water are separated from sugar and lignin in the material, the temperature of the first-effect evaporator is 102 ℃, the operating pressure is normal pressure, secondary steam containing acetic acid and water is extracted from the upper part, primary concentrated solution containing sugar, lignin and a small amount of acetic acid and water is extracted from the lower part, the secondary steam is taken as a heat source to be introduced into the shell side of the second-effect evaporator, and is condensed in the shell side of the second-effect evaporator, the temperature of the second-effect evaporator is 75 ℃, the operating pressure is 50kpa, the concentrated solution is conveyed into the second-effect evaporator for forced circulation evaporation separation, the separated acetic acid and water are extracted from the upper part, and the concentrated solution containing sugar and lignin is extracted from the bottom;
2. after the secondary steam separated by the first-effect evaporator and the secondary steam separated by the second-effect evaporator are condensed, only acetic acid and water are contained, and the secondary steam is sent into a buffer tank and then is sent to the middle lower part of a rectifying tower by a pump for azeotropic rectification operation;
3. 50% of dilute acetic acid material is conveyed to the top of an extraction tower through a feed pump, an extracting agent enters from the bottom of the extraction tower to perform normal pressure normal temperature countercurrent contact extraction operation, the extracting agent is methyl acetate solvent added with sodium nitrate, the mass ratio of the extracting agent to raw materials is 9:1, the concentration of salt in the extracting agent is 150kg/h, the diameter of the extraction tower is 300mm, and the theoretical plate number is 50;
4. Acetic acid and an extracting agent are extracted from the top of the extraction tower and are conveyed into a rectifying tower through a feed pump to serve as feed, azeotropic rectification operation is carried out together with the other part of dilute acetic acid material and the acetic acid and water mixture obtained in the step 2, the entrainer is methyl acetate, the adding amount of the entrainer is 1000kg/h, the top of the rectifying tower is 800mm, the theoretical pedal number is 30-40, the minimum reflux ratio is 0.5-0.8, the steam consumption is 1.1t/h, and the concentration of the acetic acid is 99.5% from a rectifying side line after azeotropic rectification operation;
5. The gas phase extracted from the top of the rectifying tower is mainly water, an extracting agent, an entrainer and a small amount of acetic acid, the gas phase is cooled by a condenser and then is sent into a phase separator for phase separation, the obtained oil phase is mainly the extracting agent, the entrainer and the acetic acid, the oil phase is sent into a reflux tank, one part of the oil phase is refluxed into the rectifying tower by a reflux pump, the other part of the oil phase is pumped into the extracting tower for recycling, the water phase is mainly water, and the oil phase also contains part of the extracting agent and the entrainer;
6. and (3) sending the water phase obtained by phase separation into a recovery tower for rectification operation, obtaining an extractant and an entrainer at the top of the tower, sending the extractant and the entrainer into a phase separator for further phase separation, and storing or discharging waste water extracted from the tower bottom of the recovery tower.
The foregoing describes several embodiments of the present invention in detail, but the description is merely a preferred embodiment of the invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (11)
1. System for retrieve refined acetic acid from multiple class acetic acid waste liquid, its characterized in that: the device comprises a first effect evaporator, a second effect evaporator, an extraction tower and a first rectifying tower, wherein a concentrated material feed inlet is formed in the first effect evaporator, a concentrated solution outlet of the first effect evaporator is connected with a material inlet of the second effect evaporator, a secondary steam outlet of the first effect evaporator is connected with a heat transfer medium inlet of the second effect evaporator, a heat transfer medium outlet of the second effect evaporator and a secondary steam outlet of the second effect evaporator are connected with a feed inlet of the first rectifying tower, a dilute material inlet is formed in the extraction tower, an extraction phase outlet of the extraction tower is connected with a feed inlet of the first rectifying tower, the first effect evaporator is a falling film evaporator, and the second effect evaporator is a forced circulation evaporator.
2. The system for recovering and purifying acetic acid according to claim 1, wherein: the device comprises a first rectifying tower, a phase separator, a reflux tank, an oil phase outlet, a reflux inlet and a feed inlet, wherein the gas phase extraction outlet at the top of the first rectifying tower is connected with the inlet of the phase separator, the oil phase outlet of the phase separator is connected with the reflux tank, and the reflux tank is connected with the reflux inlet of the first rectifying tower and the feed inlet of the extraction tower.
3. The system for recovering and purifying acetic acid according to claim 2, wherein: the device also comprises a second rectifying tower, wherein the water phase outlet of the phase separator is connected with the feed inlet of the second rectifying tower, and the gas phase extraction outlet at the top of the second rectifying tower is connected with the inlet of the phase separator.
4. A system for recovering and refining acetic acid according to any one of claims 1-3, wherein: the first-effect evaporator comprises a first-effect heat exchanger and a first-effect evaporation chamber, the second-effect evaporator comprises a second-effect heat exchanger, a second-effect evaporation chamber and a condenser, the first-effect heat exchanger is communicated with the first-effect evaporation chamber, a secondary steam outlet of the first-effect evaporation chamber is communicated with the second-effect heat exchanger, the second-effect heat exchanger is communicated with the second-effect evaporation chamber, a secondary steam outlet of the second-effect evaporation chamber is connected with an inlet of the condenser, and a heat transfer medium outlet of the second-effect evaporator and an outlet of the condenser are connected with a feed inlet of the first rectifying tower.
5. The method for recovering and refining acetic acid from various acetic acid waste liquid is characterized in that: comprising the following steps:
Firstly, delivering a raw material containing heavy impurity components with boiling points higher than those of acetic acid to a first-effect evaporator for evaporation, delivering the generated concentrated solution to a second-effect evaporator for evaporation, and taking secondary steam generated by the first-effect evaporator as a heat source of the second-effect evaporator;
secondly, sending the secondary steam of the first-effect evaporator and the second-effect evaporator after condensation into a first rectifying tower, and adding an entrainer to carry out azeotropic rectification operation;
Thirdly, sending a part of raw materials which do not contain heavy impurity components into an extraction tower for countercurrent extraction operation; the extractant used in the extraction operation is an extraction solvent added with salt, wherein the salt is one or a combination of more of potassium acetate, sodium nitrate, potassium nitrate, sodium sulfate and potassium sulfate; the extraction solvent is one or more of n-butyl acetate, isobutyl acetate and methyl acetate;
fourthly, sending the other part of raw materials which do not contain heavy impurity components and the extraction phase of the extraction tower into the first rectifying tower for azeotropic rectification;
fifthly, extracting acetic acid products from the side line of the first rectifying tower;
The order of the first step and the third step may be interchanged.
6. The method for recovering and purifying acetic acid according to claim 5, wherein: the method also comprises the steps of condensing the gas phase at the top of the first rectifying tower, sending the condensed gas phase into a phase separator for phase separation, and refluxing part of the oil phase obtained by phase separation into the first rectifying tower, and sending the other part of the oil phase into the extraction tower for extraction operation.
7. The method for recovering and purifying acetic acid according to claim 6, wherein: the method also comprises the steps of sending the water phase obtained by phase separation of the phase separator to a second rectifying tower for rectification operation, and sending the top extracted phase of the second rectifying tower to the phase separator for phase separation.
8. The method for recovering and purifying acetic acid according to claim 5, wherein: in the extraction operation, the salt is one or a combination of more of potassium acetate, sodium nitrate and potassium nitrate; the extraction solvent is n-butyl acetate.
9. The method for recovering and purifying acetic acid according to claim 8, wherein: the concentration of the salt in the extractant is 30-300kg/m 3.
10. The method for recovering and purifying acetic acid according to claim 9, wherein: the salt concentration is 80-150kg/m 3.
11. The method for recovering and purifying acetic acid according to any one of claims 5 to 10, wherein: the temperature of the first-effect evaporator is 90-115 ℃, the temperature of the second-effect evaporator is 50-80 ℃, and the operating pressure is 40-60kpa.
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| CN110591752B (en) * | 2019-09-24 | 2021-04-27 | 青岛华世洁环保科技有限公司 | Method and device for recovering and purifying dichloromethane-white oil mixed solution |
| CN111762920B (en) * | 2020-07-21 | 2023-04-18 | 河南城建学院 | Method for reducing concentration of potassium ions in acetic acid waste liquid |
| CN111847716B (en) * | 2020-07-21 | 2023-08-18 | 河南城建学院 | Purification device for acetic acid waste liquid |
| CN115557470B (en) * | 2022-10-31 | 2023-10-17 | 湖南双阳高科化工有限公司 | Production method and production device of electronic grade hydrogen peroxide |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09151158A (en) * | 1995-09-29 | 1997-06-10 | Showa Denko Kk | Purification of acetic acid |
| CN101306989A (en) * | 2007-05-16 | 2008-11-19 | 中国石油化工股份有限公司 | Process for separating acetic acid from water by salt-containing extracting, rectifying and separating |
| CN102153458A (en) * | 2011-02-28 | 2011-08-17 | 福州大学 | Method for recovering dilute acetic acid by virtue of extraction-azeotropic distillation of sec-butyl acetate |
| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
| CN102432453A (en) * | 2011-10-31 | 2012-05-02 | 安丘市鲁安药业有限责任公司 | Process and equipment for purifying dilute acetic acid solution |
| CN107459449A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of acetic acid is separated from water method |
| CN107459448A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of acetic acid is separated from water method |
| CN206799475U (en) * | 2017-06-06 | 2017-12-26 | 南昌金轩科技有限公司 | A kind of purifying plant of the recovery of acetic acid from acetic acid wastewater |
-
2018
- 2018-10-31 CN CN201811282614.8A patent/CN109053424B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09151158A (en) * | 1995-09-29 | 1997-06-10 | Showa Denko Kk | Purification of acetic acid |
| CN101306989A (en) * | 2007-05-16 | 2008-11-19 | 中国石油化工股份有限公司 | Process for separating acetic acid from water by salt-containing extracting, rectifying and separating |
| CN102153458A (en) * | 2011-02-28 | 2011-08-17 | 福州大学 | Method for recovering dilute acetic acid by virtue of extraction-azeotropic distillation of sec-butyl acetate |
| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
| CN102432453A (en) * | 2011-10-31 | 2012-05-02 | 安丘市鲁安药业有限责任公司 | Process and equipment for purifying dilute acetic acid solution |
| CN107459449A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of acetic acid is separated from water method |
| CN107459448A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of acetic acid is separated from water method |
| CN206799475U (en) * | 2017-06-06 | 2017-12-26 | 南昌金轩科技有限公司 | A kind of purifying plant of the recovery of acetic acid from acetic acid wastewater |
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