CN109053424A - System and method of the field of new materials from multiple types acetic acid devil liquor recovery purification acetic acid - Google Patents
System and method of the field of new materials from multiple types acetic acid devil liquor recovery purification acetic acid Download PDFInfo
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- CN109053424A CN109053424A CN201811282614.8A CN201811282614A CN109053424A CN 109053424 A CN109053424 A CN 109053424A CN 201811282614 A CN201811282614 A CN 201811282614A CN 109053424 A CN109053424 A CN 109053424A
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- acetic acid
- evaporator
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- effect
- rectifying column
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 title claims abstract description 369
- 239000000463 material Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000000746 purification Methods 0.000 title claims abstract description 25
- 238000011084 recovery Methods 0.000 title claims abstract description 22
- 230000000694 effects Effects 0.000 claims abstract description 110
- 238000000605 extraction Methods 0.000 claims abstract description 89
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000012141 concentrate Substances 0.000 claims abstract description 13
- 238000009833 condensation Methods 0.000 claims abstract 3
- 230000005494 condensation Effects 0.000 claims abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 64
- 239000012071 phase Substances 0.000 claims description 50
- 238000004821 distillation Methods 0.000 claims description 27
- 238000009834 vaporization Methods 0.000 claims description 24
- 230000008016 vaporization Effects 0.000 claims description 24
- 150000003839 salts Chemical class 0.000 claims description 18
- 238000004064 recycling Methods 0.000 claims description 16
- DKPFZGUDAPQIHT-UHFFFAOYSA-N butyl acetate Chemical compound CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 11
- 239000007792 gaseous phase Substances 0.000 claims description 10
- 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
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 235000011056 potassium acetate Nutrition 0.000 claims description 5
- 239000001632 sodium acetate Substances 0.000 claims description 5
- 235000017281 sodium 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
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 2
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 claims description 2
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 claims description 2
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 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
- 159000000000 sodium salts Chemical class 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 19
- 239000007788 liquid Substances 0.000 abstract description 14
- 239000002699 waste material Substances 0.000 abstract description 13
- 229960000583 acetic acid Drugs 0.000 description 107
- 239000000052 vinegar Substances 0.000 description 26
- 235000021419 vinegar Nutrition 0.000 description 26
- 238000000926 separation method Methods 0.000 description 18
- 239000002351 wastewater Substances 0.000 description 14
- 229920005610 lignin Polymers 0.000 description 11
- 238000001704 evaporation Methods 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 8
- 239000002253 acid Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- -1 Dichlorodiphenyl Acetate Chemical compound 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- ZDGGJQMSELMHLK-UHFFFAOYSA-N m-Trifluoromethylhippuric acid Chemical compound OC(=O)CNC(=O)C1=CC=CC(C(F)(F)F)=C1 ZDGGJQMSELMHLK-UHFFFAOYSA-N 0.000 description 3
- 238000010025 steaming Methods 0.000 description 3
- 238000002207 thermal evaporation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- 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
Abstract
The present invention provides field of new materials from the system and method for multiple types acetic acid devil liquor recovery purification acetic acid, system includes 1st effective evaporator, 2nd effect evaporator, extraction tower and rectifying column, 1st effective evaporator concentrated solution outlet is connect with 2nd effect evaporator entrance, the outlet of 1st effective evaporator secondary steam is connect with 2nd effect evaporator heat transfer medium inlet, 2nd effect evaporator heat transfer medium outlet and the outlet of 2nd effect evaporator secondary steam are connect with rectifying column feed inlet, and the outlet of extraction tower extraction phase is connect with rectifying column feed inlet.Method includes sending the raw material containing the miscellaneous component of weight to 1st effective evaporator to be evaporated, and concentrate is sent to 2nd effect evaporator, and secondary steam is as 2nd effect evaporator heat source；The secondary steam of condensation is sent into azeotropic distillation in rectifying column；Raw material a part without containing the miscellaneous component of weight is extracted；Another part raw material and extraction phase are sent into azeotropic distillation in rectifying column, the system and method can from variety classes acetic acid waste liquid recovery of acetic acid, system equipment small investment, low energy consumption.
Description
Technical field
The invention belongs to acetic acid recovery technical field of refinement, return more particularly, to field of new materials from multiple types acetic acid waste liquid
Receive the system and method for purification acetic acid.
Background technique
It is also a kind of excellent organic solvent that acetic acid, which is important industrial chemicals, is widely used in chemical industry, light textile, medicine etc.
The fields such as industry.And acetic acid wastewater can be generated in many Chemical Manufacture links, the source of acetic acid wastewater is different, and composition is different,
What some production links generated is the acetic acid wastewater containing the boiling point weight miscellaneous component higher than acetic acid, and what some were generated is dilute vinegar
Acid wants recovery of acetic acid to need to remove moisture for spirit of vinegar, and the acetic acid wastewater containing the miscellaneous component of weight is also needed to take off
Except heavy miscellaneous component therein.
The boiling point of acetic acid is higher than water, but close with water, and relative volatility is little, therefore generally requires the method by rectifying
Water is removed, acetic acid dehydration generallys use conventional distillation or azeotropic distillation, the acetic acid of high-purity is obtained according to conventional distillation, needs
The more number of plates and biggish reflux ratio are wanted, equipment investment is high, and generates very big energy consumption, and azeotropic distillation is by making entrainer
Azeotropic mixture is formed with water, changes the relative volatility of water and acetic acid, makes the reduction of the number of plates needed for rectifying, reflux ratio reduces, and saves
Part energy consumption, but it is lower for acetate concentration in raw material when, the dosage of required entrainer increases, and rectifying column load increases, and is
Energy consumption of uniting is still very big.In addition, the process of the miscellaneous component of separation weight can also generate biggish for the acetic acid wastewater containing the miscellaneous component of weight
Energy consumption.
It is whole therefore, it is necessary to the system and method that one kind can separate and recover purification acetic acid from variety classes acetic acid waste liquid
The equipment investment of a acetic acid recovery refining system is few, and recycling subtractive process system energy consumption is low.
Summary of the invention
The problem to be solved in the present invention is to provide the systems that field of new materials refines acetic acid from multiple types acetic acid devil liquor recovery
And method, purification acetic acid can be separated and recovered from variety classes acetic acid waste liquid, the entire equipment investment for recycling refining system is few, is
Low energy consumption for system.
It is returned in order to solve the above technical problems, it is an object of the present invention to provide field of new materials from multiple types acetic acid waste liquid
The system for receiving purification acetic acid, including 1st effective evaporator, 2nd effect evaporator, extraction tower and first rectifying column, 1st effective evaporator are equipped with
Dense material feed inlet, the concentrated solution outlet of 1st effective evaporator and the material inlet of 2nd effect evaporator connect, and the two of 1st effective evaporator
The connection of the heat transfer medium inlet of secondary steam (vapor) outlet and 2nd effect evaporator, the heat transfer medium outlet and 2nd effect evaporator of 2nd effect evaporator
Secondary steam outlet connect with the feed inlet of first rectifying column, equipped with dilute material entrance, the extraction phase of extraction tower goes out extraction tower
It mouthful is connect with the feed inlet of first rectifying column, it is preferred that 1st effective evaporator is falling film evaporator, it is preferred that 2nd effect evaporator is
Forced-circulation evaporator.
In technical solution, it is preferred that further include phase-splitter and return tank, the top gaseous phase of first rectifying column produces mouth and divides
The entrance of phase device connects, and mutually outlet is connect the oil of phase-splitter with return tank, the reflux inlet and extraction of return tank and first rectifying column
The feed inlet of tower is taken to connect.
In technical solution, it is preferred that further include Second distillation column, the charging of the water phase outlet and Second distillation column of phase-splitter
Mouth connection, the top gaseous phase extraction mouth of Second distillation column and the entrance of phase-splitter connect.
In technical solution, it is preferred that 1st effective evaporator includes an effect heat exchanger and an effect vaporization chamber, and 2nd effect evaporator includes
Two effect heat exchangers, two effect vaporization chambers and condenser, an effect heat exchanger are connected to an effect vaporization chamber, the secondary steam of an effect vaporization chamber
Outlet with two effect heat exchangers be connected to, two effect heat exchangers with two imitate vaporization chambers is connected to, two imitate vaporization chambers secondary steams export with it is cold
The entrance of condenser connects, and the outlet of concentrated solution outlet and condenser of an effect vaporization chamber and the feed inlet of first rectifying column connect.
It is a further object of the present invention to provide field of new materials from the method for multiple types acetic acid devil liquor recovery purification acetic acid, wraps
It includes:
The first step will be sent to 1st effective evaporator containing the raw material of the miscellaneous component of weight and be evaporated, and the concentrate of generation is sent to two
Effect evaporator is evaporated, and the secondary steam that 1st effective evaporator is generated is as the heat source of 2nd effect evaporator；
Second step will be added in the secondary steam of condensed 1st effective evaporator and 2nd effect evaporator feeding first rectifying column
Entrainer carries out azeotropic distillation operation；
Raw material a part without containing the miscellaneous component of weight is sent into extraction tower by third step, carries out counter-current extraction operation；
The extraction phase of 4th step, the raw material by another part without containing the miscellaneous component of weight and extraction tower is sent into first rectifying column
Carry out azeotropic distillation operation；
5th step, in first rectifying column side take-off acetate products；
The sequence of the first step and third step can be interchanged.
In this method, due to acetic acid wastewater source difference, impurities ingredient is different in the acetic acid wastewater of generation, for containing
There is boiling point to be higher than the acetic acid wastewater of the miscellaneous component of weight of acetic acid, be sent in double effect evaporator, is evaporated operation, separation is wherein
The miscellaneous component of weight, be first evaporated separation through 1st effective evaporator, the concentrate containing a small amount of acetic acid of generation is sent into two effect evaporations
Continue to separate in device, the acetic acid for then isolating 1st effective evaporator and 2nd effect evaporator is sent into rectifying column after condensing, and is added
Enter entrainer and carry out azeotropic distillation operation, 2nd effect evaporator bottom is the miscellaneous component of weight of concentration；And for without containing the miscellaneous component of weight
Spirit of vinegar waste water, a part is pumped to the top of extraction tower by charging, and extractant enters from the bottom of extraction tower, carries out inverse
Stream contact extracting operation, raffinate phase waste water are discharged by tower reactor, and extraction phase contains acetic acid, extractant and part water, by the tower of extraction tower
Top extraction, which is sent into rectifying column, carries out azeotropic distillation operation, and another part is fed directly to rectifying column, carries out azeotropic distillation operation, most
Afterwards in rectifying column side take-off acetate products.The processing of processing and spirit of vinegar to the acetic acid wastewater of the miscellaneous component containing weight can simultaneously into
Row can also be handled respectively, and rectifying part carries out azeotropic distillation in same rectifying column.
This method can recycle purification acetic acid from different types of acetic acid waste liquid, and handle the miscellaneous component of weight in acetic acid waste liquid
Shi Caiyong double effect evaporator, heat source of the secondary steam that 1st effective evaporator generates as 2nd effect evaporator, on the one hand efficiently uses
Waste heat in product reduces system energy consumption, and it is cooling required cold on the other hand to also eliminate Dichlorodiphenyl Acetate product after 1st effective evaporator
But equipment and energy consumption；And in distillation operation, spirit of vinegar raw material is divided into two parts, and a part is first sent into extraction tower and isolates major part
Water, then give together with another part raw material to rectifying column and carry out azeotropic operation, greatly reduce the treating capacity and rectifying of rectifying column
Water content in tower in material makes the reduction of entrainer dosage, and rectifying column operational load reduces, and rectifying column energy consumption substantially reduces.
In technical solution, it is preferred that further include being sent into phase-splitter to carry out after condensing the top gaseous phase of first rectifying column
Split-phase, and oily phase a part that split-phase is obtained is back in first rectifying column, another part is sent to be extracted into extraction tower
Operation.Rectifying tower top gaseous phase is mainly water, extractant, there are also part acetic acid for entrainer, and after phase-splitter split-phase, oil is mutually main
It for extractant, entrainer and acetic acid, is back in rectifying column and extraction tower, further separates acetic acid therein.
In technical solution, it is preferred that further include that the water phase that phase-splitter split-phase obtains is sent into Second distillation column to progress essence
Operation is evaporated, and the overhead extraction of Second distillation column is mutually sent and carries out split-phase into phase-splitter.In the water phase that phase-splitter split-phase obtains
Predominantly water also contains partial extraction agent and entrainer, water phase is sent to recovery tower after distillation operation, part is isolated
Moisture, then by water phase extractant and entrainer be recycled to phase-splitter and utilize again, extractant and entrainer can be greatlyd save
Dosage, reduce extractant, entrainer waste.
In technical solution, it is preferred that extractant used in extracting operation is the extractant for adding salt；Usually extraction vinegar
For acid using extractant n-butyl acetate etc., the solvability of general extractant Dichlorodiphenyl Acetate is lower, and also bigger than normal to the solubility of water,
Therefore Extraction of Acetic Acid can be gone out by needing larger amount of extractant just in extraction, expend a large amount of extractants and extraction tower load very
Greatly, energy consumption is high, and extractant used in extracting operation is the extractant for adding salt, the addition of salt in this acetic acid recovery method
The activity coefficient of each component makes acetic acid in extractant to change the solubility of each component in extractant in changeable solution
Middle solubility improves, and the solubility of water reduces, and so as to reduce the dosage of extractant in extracting operation, reduces extraction tower operation
Load reduces energy consumption.
Preferably, salt is the combination of one or both of sylvite and sodium salt；
It is furthermore preferred that salt is one of potassium acetate, sodium acetate, sodium nitrate, potassium nitrate, sodium sulphate and potassium sulfate or a variety of
Combination；
It is furthermore preferred that salt is one of potassium acetate, sodium acetate, sodium nitrate and potassium nitrate or a variety of combinations；
Preferably, extractant is acetic ester compounds；
It is furthermore preferred that extractant is one of n-butyl acetate, isobutyl acetate, methyl acetate or a variety of mixed
It closes；
It is furthermore preferred that extractant is n-butyl acetate.
In technical solution, it is preferred that the concentration of salt is 30-300kg/m in extractant3, it is preferred that the concentration of salt is 80-
150kg/m3。
In technical solution, it is preferred that the temperature of 1st effective evaporator is 90-115 DEG C, and the temperature of 2nd effect evaporator is 50-80
DEG C, operating pressure 40-60kpa.
Wherein, the mass ratio of extractant and raw material is chosen as 1-10, it is preferred that the mass ratio of extractant and raw material is 5-8.
Wherein, be chosen as 0.5-3 into the mass ratio of extraction tower and the raw material of rectifying column, it is preferred that enter extraction tower with
The mass ratio of the raw material of rectifying column is 1.
Wherein, the extracting operation temperature of extraction tower is 20-80 DEG C, pressure 100-130kPa, theoretical cam curve 30-
70。
Wherein, the theoretical cam curve of rectifying column is 50-80, reflux ratio 0.5-0.8.
The advantages and positive effects of the present invention are:
1. the system and method for recycling purification acetic acid can be handled different types of acetic acid waste liquid, recycling purification
Acetic acid therein, and low energy consumption for system entirety；
2. removing miscellaneous group of timesharing of weight in acetic acid waste liquid uses double effect evaporator, the secondary steam that 1st effective evaporator is generated is made
For the heat source of 2nd effect evaporator, waste heat in product is efficiently used, reduces evaporator total energy consumption, and save secondary in 1st effective evaporator
The condensing plant and energy consumption of steam；
3. the higher a part of material of spirit of vinegar material of pair water content is first carried out through moisture in extracting operation removal material again
Azeotropic distillation operation, substantially reduces the treating capacity of rectifying column, reduces the dosage of entrainer in distillation operation, drops rectifying column load
Low, distillation operation energy consumption reduces, although extraction tower more than independent azeotropic distillation, rectifying column tower diameter, tower height are reduced, whole
Body equipment investment is high unlike independent azeotropic distillation；
4. adding salt in extractant used in extracting operation, changes the solubility of acetic acid and water in extractant, make vinegar
Solubility of the acid in extractant improves, and the solubility of water reduces, so that the dosage for extracting required extractant is substantially reduced,
Extraction tower load reduction, system energy consumption reduce；
5. also the extractant and entrainer isolated are recycled and recycled, disappearing for extractant and entrainer is reduced
Consumption.
Detailed description of the invention
Fig. 1 is the structure that the field of new materials of the embodiment of the present invention refines the system of acetic acid from a variety of acetic acid devil liquor recoveries
Schematic diagram.
In figure:
1,1st effective evaporator 2,2nd effect evaporator 3, extraction tower
4, rectifying column 5, dense material feed inlet 6, dilute material entrance
7, phase-splitter 8, return tank 9, rectifying column
10, surge tank 11, one imitates heat exchanger 12, one and imitates vaporization chamber
13, feed pump 21, two imitates heat exchanger 22, two and imitates vaporization chamber
23, condenser 24, forced circulation pump
Specific embodiment
Inventive embodiments are described further with reference to the accompanying drawing:
As shown in Figure 1, system of the field of new materials described in the present embodiment from multiple types acetic acid devil liquor recovery purification acetic acid,
Including 1st effective evaporator 1,2nd effect evaporator 2, extraction tower 3 and rectifying column 4,1st effective evaporator 1 is equipped with dense material feed inlet 5, dense
Feed pump is connected with before material feed inlet 5, the concentrated solution outlet of 1st effective evaporator 1 is connect with the material inlet of 2nd effect evaporator 2,
The secondary steam outlet of 1st effective evaporator 1 is connect with the heat transfer medium inlet of 2nd effect evaporator 2, and the heat transfer of 2nd effect evaporator 2 is situated between
Matter outlet and the secondary steam outlet of 2nd effect evaporator 2 are connect with the feed inlet of rectifying column 4, and extraction tower 3 is equipped with dilute material entrance
6, the extraction phase outlet of extraction tower 3 is connect with the feed inlet of rectifying column 4.
In acetic acid waste liquid to be processed, it is higher than the material of the miscellaneous component of weight of acetic acid through dense on 1st effective evaporator 1 containing boiling point
Material feed inlet 5 enters 1st effective evaporator 1, carries out preliminary evaporation separation, generates at the top of 1st effective evaporator 1 by acetic acid and water group
At secondary steam, bottom generates the concentration material containing the miscellaneous component of weight, and bottom concentration material, which enters in 2nd effect evaporator 2, to be continued
Evaporation separation, and the secondary steam that 1st effective evaporator 1 generates is passed through heat source of the shell side as 2nd effect evaporator of 2nd effect evaporator
For 2nd effect evaporator heat supply, 2nd effect evaporator evaporation separation generates the secondary steam containing acetic acid and water at top, raw in bottom
The enriched product of the miscellaneous component of Cheng Hanchong, collects and discharges, and the secondary steam generated by 1st effective evaporator evaporation is in 2nd effect evaporator 2
In be condensed into liquid, be pumped to rectifying through charging jointly with through the isolated secondary steam of the condensed 2nd effect evaporator 2 of condenser
In tower 4, entrainer is added and carries out azeotropic distillation, in rectifying column side take-off acetate products；And dilute vinegar without containing the miscellaneous component of weight
Sour material a part is sent through dilute material entrance 6 to 3 top of extraction tower through feed pump, and extractant entrance, extraction is arranged in 3 bottom of extraction tower
Take agent from extraction tower bottom be sent into, carry out counter current contacting extracting operation, remove material in moisture, then with remaining a part
Spirit of vinegar material is sent into progress azeotropic distillation operation in rectifying column 4 together, in tower bottom side take-off acetate products.
The system of recycling purification acetic acid can handle different types of acetic acid waste liquid, therefrom recycle and refine acetic acid；To containing
There is the acetic acid waste liquid of the miscellaneous component of weight to remove the miscellaneous component of weight using double effect evaporator, the secondary steam that 1st effective evaporator generates is as two
The heat source for imitating evaporator, the heat for the secondary steam for making full use of 1st effective evaporator to generate reduce energy consumption, and 1st effective evaporator generates
Secondary steam be condensed in 2nd effect evaporator shell side, the condenser after also eliminating 1st effective evaporator；To contain more water
Point spirit of vinegar carry out extraction plus azeotropic distillation operation, a part of spirit of vinegar first through extraction remove most of moisture after again with it is another
Partial material carries out azeotropic distillation jointly, and rectifying column treating capacity reduces, and entrainer dosage is low, rectifying column load reduction, rectifying behaviour
Make energy consumption reduction, it is whole although an extraction tower, tower diameter, the tower height of rectifying column reduce more than independent azeotropic distillation
Height of the equipment investment unlike independent azeotropic distillation.
Surge tank 10 and feed pump 13, surge tank 10 and 2nd effect evaporator are additionally provided between 2nd effect evaporator 2 and rectifying column 4
The outlet of 2 condenser 23 is connected with the outlet of two effect heat exchangers 21 of 2nd effect evaporator 2, the outlet of surge tank 10 and feed pump
13 connections, feed pump 13 are connect with the feed inlet of rectifying column 4.
In technical solution, it is preferred that further include phase-splitter 7 and return tank 8, the top gaseous phase of rectifying column 4 produces mouth and divides
The entrance of phase device 7 connects, and mutually outlet is connect the oil of phase-splitter 7 with return tank 8, the reflux inlet and extraction of return tank 8 and rectifying column 4
The feed inlet of tower 3 is taken to connect.Rectifying tower top gaseous phase is mainly water, extractant, there are also part acetic acid for entrainer, through phase-splitter 7
After split-phase, oil is mainly mutually extractant, entrainer and acetic acid, is back in rectifying column 4 and extraction tower 3, is further separated
Acetic acid therein.
In technical solution, it is preferred that further include rectifying column 9, the water phase outlet of phase-splitter 7 and the feed inlet of rectifying column 9 connect
It connects, the top gaseous phase extraction mouth of rectifying column 9 is connect with the entrance of phase-splitter 7.Extraction is mainly contained in water phase after 7 split-phase of phase-splitter
Agent, entrainer and water are taken, water phase is sent into rectifying column 9 and carries out distillation operation, water and extractant and entrainer are separated, can will be extracted
It takes agent and entrainer to recycle and reuse, reduces the consumption of extractant and entrainer.
Wherein, 1st effective evaporator 1 includes an effect heat exchanger 11 and an effect vaporization chamber 12, and 2nd effect evaporator 2 includes that two effects are changed
Hot device 21, two imitates vaporization chamber 22 and condenser 23, and an effect heat exchanger 11 is connected to an effect vaporization chamber 12, and the two of an effect vaporization chamber 12
Secondary steam (vapor) outlet is connected to two effect heat exchangers 21, and two effect heat exchangers 21 are connected to two effect vaporization chambers 22, and the two of two effect vaporization chambers 22
Secondary steam (vapor) outlet is connect with the entrance of condenser 23, the outlet and rectifying of the concentrated solution outlet and condenser 23 of an effect vaporization chamber 12
The feed inlet of tower 4 connects.
Preferably, it is additionally provided with forced circulation pump 24 between two effect heat exchangers 21 and two effect vaporization chambers 22, due to two effect evaporations
The material viscosity of the initial concentration handled in device 2 increased, and make relatively to glue in 2nd effect evaporator 2 by the way that forced circulation pump 24 is arranged
Thick material forced circulation, promotes circulating for material, prevents material sticks in evaporator, improves evaporation efficiency.
Preferably, 1st effective evaporator 1 is falling film evaporator, since falling film evaporator internal feed liquid is under the effect of gravity along pipe
The decline of wall film-like, heat transfer coefficient is high, and evaporation efficiency is higher.
Field of new materials provided by the invention refines the specific embodiment of the method for acetic acid from multiple types acetic acid devil liquor recovery
It is as follows:
Embodiment one
The method of recycling purification acetic acid in the present embodiment includes the following steps:
Treating material are as follows: dense acetic acid material comprises about acetic acid 62%, water 23%, sugar 8%, lignin 7%, spirit of vinegar
Material includes acetic acid 50%, water 50%.
1. dense acetic acid material is conveyed into 1st effective evaporator by feed pump, added in 1st effective evaporator by falling film evaporator
Thermal evaporation makes sugar and lignin separation in wherein acetic acid and water and material, and 1st effective evaporator temperature is 105 DEG C, operating pressure
For normal pressure, top produces the secondary steam containing acetic acid and water, and extraction initial concentration in lower part contains sugar, lignin and a small amount of vinegar
The concentrate of acid, water, secondary steam are passed through the shell side of 2nd effect evaporator as heat source, and cold in the shell side of 2nd effect evaporator
Solidifying, 2nd effect evaporator temperature is 80 DEG C, operating pressure 50kpa, and concentrate, which is sent into 2nd effect evaporator, carries out forced circulation steaming
Hair separation produces the acetic acid and water isolated, concentrate of the bottom extraction containing sugar and lignin on top；
2. being contained only after condensing through the secondary steam of 1st effective evaporator separation and the secondary steam of 2nd effect evaporator separation
Acetic acid and water are sent to the middle and lower part for being delivered to rectifying column after surge tank by pump, carry out azeotropic distillation operation；
3. the 23% of spirit of vinegar material is delivered at the top of extraction tower by feed pump, extractant enters from extraction tower bottom
Normal pressure and temperature counter current contacting extracting operation is carried out, extractant is the n-butyl acetate solvent for adding potassium acetate, extractant and raw material
Mass ratio be 2:1, the concentration of salt is 100kg/h in extractant, and extraction tower tower diameter is 300mm, theoretical cam curve 50；
4. the overhead extraction of extraction tower is acetic acid and extractant, it is delivered in rectifying column through feed pump as charging, and it is another
A part of spirit of vinegar material and got in step 2 acetic acid and aqueous mixtures carry out azeotropic distillation operation together, and entrainer is vinegar
Sour N-butyl, the additional amount of entrainer are 800kg/h, the top of the distillation column 800mm, and theoretical pedal number is 30-40, minimum reflux
Than for 0.5-0.8, steam consumption 1.1t/h, after azeotropic distillation operates, rectifying side take-off acetic acid, concentration is
99.5%；
5. the top of the distillation column extraction gas phase is mainly water, extractant, entrainer and a small amount of acetic acid, by it through condenser cooling
It is sent into split-phase in phase-splitter afterwards, gained oil is mutually mainly extractant, entrainer and acetic acid, and oil is mutually sent into return tank, a part
It is back in rectifying column through reflux pump, another part is pumped into extraction tower and reuses, and water phase is mainly water, also contains portion
Divide extractant and entrainer；
6. sending water phase obtained by split-phase into recovery tower, distillation operation is carried out, extractant and entrainer is obtained in tower top, send
The further split-phase into phase-splitter, the storage of tower reactor extracted waste water or discharge of recovery tower.
Embodiment two
The method of recycling purification acetic acid in the present embodiment includes the following steps:
Treating material are as follows: dense acetic acid material comprises about acetic acid 70%, water 15%, sugar 9%, lignin 6%, spirit of vinegar
Material includes acetic acid 35%, water 65%.
1. dense acetic acid material is conveyed into 1st effective evaporator by feed pump, added in 1st effective evaporator by falling film evaporator
Thermal evaporation, 1st effective evaporator temperature are 107 DEG C, and operating pressure is normal pressure, make wherein acetic acid and water with it is sugared and wooden in material
Element separation, top produce the secondary steam containing acetic acid and water, and extraction initial concentration in lower part contains sugar, lignin and a small amount of vinegar
The concentrate of acid, water, secondary steam are passed through the shell side of 2nd effect evaporator as heat source, and cold in the shell side of 2nd effect evaporator
Solidifying, 2nd effect evaporator temperature is 83 DEG C, operating pressure 50kpa, and concentrate, which is sent into 2nd effect evaporator, carries out forced circulation steaming
Hair separation produces the acetic acid and water isolated, concentrate of the bottom extraction containing sugar and lignin on top；
2. being contained only after condensing through the secondary steam of 1st effective evaporator separation and the secondary steam of 2nd effect evaporator separation
Acetic acid and water are sent to the middle and lower part for being delivered to rectifying column after surge tank by pump, carry out azeotropic distillation operation；
3. in spirit of vinegar material 40% is delivered at the top of extraction tower by feed pump, extractant enters from extraction tower bottom
Normal pressure and temperature counter current contacting extracting operation is carried out, extractant is the i-butyl ester solvent for adding sodium acetate, extractant and raw material
Mass ratio be 8:1, the concentration of salt is 120kg/h in extractant, and extraction tower tower diameter is 300mm, theoretical cam curve 50；
4. the overhead extraction of extraction tower is acetic acid and extractant, it is delivered in rectifying column through feed pump as charging, and it is another
A part of spirit of vinegar material and got in step 2 acetic acid and aqueous mixtures carry out azeotropic distillation operation together, and entrainer is vinegar
Sour isobutyl ester, the additional amount of entrainer are 1000kg/h, the top of the distillation column 800mm, and theoretical pedal number is 30-40, and minimum is returned
Stream is than being 0.5-0.8, steam consumption 1.1t/h, and after azeotropic distillation operates, rectifying side take-off acetic acid, concentration is
99.5%；
5. the top of the distillation column extraction gas phase is mainly water, extractant, entrainer and a small amount of acetic acid, by it through condenser cooling
It is sent into split-phase in phase-splitter afterwards, gained oil is mutually mainly extractant, entrainer and acetic acid, and oil is mutually sent into return tank, a part
It is back in rectifying column through reflux pump, another part is pumped into extraction tower and reuses, and water phase is mainly water, also contains portion
Divide extractant and entrainer；
6. sending water phase obtained by split-phase into recovery tower, distillation operation is carried out, extractant and entrainer is obtained in tower top, send
The further split-phase into phase-splitter, the storage of tower reactor extracted waste water or discharge of recovery tower.
Embodiment three
The method of recycling purification acetic acid in the present embodiment includes the following steps:
Treating material are as follows: dense acetic acid material comprises about acetic acid 45%, water 42%, sugar 8%, lignin 5%, spirit of vinegar
Material includes acetic acid 23%, water 77%.
1. dense acetic acid material is conveyed into 1st effective evaporator by feed pump, added in 1st effective evaporator by falling film evaporator
Thermal evaporation makes sugar and lignin separation in wherein acetic acid and water and material, and 1st effective evaporator temperature is 102 DEG C, operating pressure
For normal pressure, top produces the secondary steam containing acetic acid and water, and extraction initial concentration in lower part contains sugar, lignin and a small amount of vinegar
The concentrate of acid, water, secondary steam are passed through the shell side of 2nd effect evaporator as heat source, and cold in the shell side of 2nd effect evaporator
Solidifying, 2nd effect evaporator temperature is 75 DEG C, operating pressure 50kpa, and concentrate, which is sent into 2nd effect evaporator, carries out forced circulation steaming
Hair separation produces the acetic acid and water isolated, concentrate of the bottom extraction containing sugar and lignin on top；
2. being contained only after condensing through the secondary steam of 1st effective evaporator separation and the secondary steam of 2nd effect evaporator separation
Acetic acid and water are sent to the middle and lower part for being delivered to rectifying column after surge tank by pump, carry out azeotropic distillation operation；
3. the 50% of spirit of vinegar material is delivered at the top of extraction tower by feed pump, extractant enters from extraction tower bottom
Normal pressure and temperature counter current contacting extracting operation is carried out, extractant be the methyl acetate solvent of addition sodium nitrate, extractant and raw material
Mass ratio is 9:1, and the concentration of salt is 150kg/h in extractant, and extraction tower tower diameter is 300mm, theoretical cam curve 50；
4. the overhead extraction of extraction tower is acetic acid and extractant, it is delivered in rectifying column through feed pump as charging, and it is another
A part of spirit of vinegar material and got in step 2 acetic acid and aqueous mixtures carry out azeotropic distillation operation together, and entrainer is vinegar
Sour methyl esters, the additional amount of entrainer are 1000kg/h, the top of the distillation column 800mm, and theoretical pedal number is 30-40, minimum reflux
Than for 0.5-0.8, steam consumption 1.1t/h, after azeotropic distillation operates, rectifying side take-off acetic acid, concentration is
99.5%；
5. the top of the distillation column extraction gas phase is mainly water, extractant, entrainer and a small amount of acetic acid, by it through condenser cooling
It is sent into split-phase in phase-splitter afterwards, gained oil is mutually mainly extractant, entrainer and acetic acid, and oil is mutually sent into return tank, a part
It is back in rectifying column through reflux pump, another part is pumped into extraction tower and reuses, and water phase is mainly water, also contains portion
Divide extractant and entrainer；
6. sending water phase obtained by split-phase into recovery tower, distillation operation is carried out, extractant and entrainer is obtained in tower top, send
The further split-phase into phase-splitter, the storage of tower reactor extracted waste water or discharge of recovery tower.
Several embodiments of the present invention are described in detail above, but the content is only preferable implementation of the invention
Example, should not be considered as limiting the scope of the invention.It is all according to all the changes and improvements made by the present patent application range
Deng should still be within the scope of the patent of the present invention.
Claims (10)
1. field of new materials from multiple types acetic acid devil liquor recovery purification acetic acid system, it is characterised in that: including 1st effective evaporator,
2nd effect evaporator, extraction tower and first rectifying column, the 1st effective evaporator are equipped with dense material feed inlet, the 1st effective evaporator
Concentrated solution outlet is connect with the material inlet of the 2nd effect evaporator, the secondary steam outlet and described two of the 1st effective evaporator
Imitate the heat transfer medium inlet connection of evaporator, the heat transfer medium outlet of the 2nd effect evaporator and the 2nd effect evaporator it is secondary
Steam (vapor) outlet is connect with the feed inlet of the first rectifying column, and the extraction tower is equipped with dilute material entrance, the extraction of the extraction tower
Mutually outlet is taken to connect with the feed inlet of the first rectifying column, it is preferred that the 1st effective evaporator is falling film evaporator, preferably
, the 2nd effect evaporator is forced-circulation evaporator.
2. the system of recycling purification acetic acid according to claim 1, it is characterised in that: it further include phase-splitter and return tank,
The top gaseous phase extraction mouth of the first rectifying column is connect with the entrance of the phase-splitter, and the oil of the phase-splitter mutually exports and institute
Return tank connection is stated, the return tank is connect with the feed inlet of the reflux inlet of the first rectifying column and the extraction tower.
3. the system of recycling purification acetic acid according to claim 2, it is characterised in that: it further include Second distillation column, it is described
The water phase outlet of phase-splitter connect with the feed inlet of the Second distillation column, the top gaseous phase of the Second distillation column produce mouth and
The entrance of the phase-splitter connects.
4. the system of recycling purification acetic acid according to claim 1 to 3, it is characterised in that: the 1st effective evaporator packet
An effect heat exchanger and an effect vaporization chamber are included, the 2nd effect evaporator includes two effect heat exchangers, two effect vaporization chambers and condenser, described
One effect heat exchanger is connected to the effect vaporization chamber, and the secondary steam outlet of the effect vaporization chamber connects with the two effects heat exchanger
Logical, the two effect heat exchanger is connected to the two effects vaporization chamber, the secondary steam outlet and the condensation of the two effects vaporization chamber
The entrance of device connects, the outlet of the concentrated solution outlet and the condenser of the effect vaporization chamber and the first rectifying column into
Material mouth connection.
5. the method that field of new materials refines acetic acid from multiple types acetic acid devil liquor recovery, it is characterised in that: include:
The first step will be sent to 1st effective evaporator containing the raw material of the miscellaneous component of weight and be evaporated, and the concentrate of generation, which is sent to two effects, to be steamed
The secondary steam that hair device is evaporated, and the 1st effective evaporator is generated is as the heat source of 2nd effect evaporator；
Azeotropic will be added in the secondary steam of condensed 1st effective evaporator and 2nd effect evaporator feeding first rectifying column in second step
Agent carries out azeotropic distillation operation；
Raw material a part without containing the miscellaneous component of weight is sent into extraction tower by third step, carries out counter-current extraction operation；
The extraction phase of 4th step, the raw material by another part without containing the miscellaneous component of weight and the extraction tower is sent into first rectifying
Azeotropic distillation operation is carried out in tower；
5th step, in the first rectifying column side take-off acetate products；
The sequence of the first step and the third step can be interchanged.
6. the method for recycling purification acetic acid according to claim 5, it is characterised in that: further include by the first rectifying column
Top gaseous phase condensation after be sent into phase-splitter and carry out split-phase, and oily phase a part that split-phase is obtained is back to first essence
It evaporates in tower, another part, which is sent, carries out extracting operation into the extraction tower.
7. the method for recycling purification acetic acid according to claim 6, it is characterised in that: further include by the phase-splitter split-phase
Obtained water phase, which is sent into Second distillation column, carries out distillation operation, and the overhead extraction of the Second distillation column is mutually sent to described
Split-phase is carried out in phase-splitter.
8. according to the method for any recycling purification acetic acid of claim 5-7, it is characterised in that: used in extracting operation
Extractant is the extractant for adding salt,
Preferably, the salt is combination one or more in sylvite and sodium salt；
It is furthermore preferred that the salt is one of potassium acetate, sodium acetate, sodium nitrate, potassium nitrate, sodium sulphate and potassium sulfate or a variety of
Combination；
It is furthermore preferred that the salt is one of potassium acetate, sodium acetate, sodium nitrate and potassium nitrate or a variety of combinations；
Preferably, the extractant is acetic ester compounds；
It is furthermore preferred that the extractant is one of n-butyl acetate, isobutyl acetate, methyl acetate or a variety of mixed
It closes；
It is furthermore preferred that the extractant is n-butyl acetate.
9. it is according to claim 8 recycling purification acetic acid method, it is characterised in that: salt described in the extractant it is dense
Degree is 30-300kg/m3, it is preferred that the concentration of the salt is 80-150kg/m3。
10. according to the method for any recycling purification acetic acid of claim 5-9, it is characterised in that: the 1st effective evaporator
Temperature be 90-115 DEG C, the temperature of the 2nd effect evaporator is 50-80 DEG C, operating pressure 40-60kpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811282614.8A CN109053424B (en) | 2018-10-31 | System and method for recycling refined acetic acid from various acetic acid waste liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811282614.8A CN109053424B (en) | 2018-10-31 | System and method for recycling refined acetic acid from various acetic acid waste liquid |
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| Publication Number | Publication Date |
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| CN109053424A true CN109053424A (en) | 2018-12-21 |
| CN109053424B CN109053424B (en) | 2024-04-19 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591752A (en) * | 2019-09-24 | 2019-12-20 | 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 |
| CN111762920A (en) * | 2020-07-21 | 2020-10-13 | 河南城建学院 | Method for reducing concentration of potassium ions in acetic acid waste liquid |
| CN111847716A (en) * | 2020-07-21 | 2020-10-30 | 河南城建学院 | Purification device for acetic acid waste liquid |
| CN115557470A (en) * | 2022-10-31 | 2023-01-03 | 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 |
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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110591752A (en) * | 2019-09-24 | 2019-12-20 | 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 |
| 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 |
| CN111762920A (en) * | 2020-07-21 | 2020-10-13 | 河南城建学院 | Method for reducing concentration of potassium ions in acetic acid waste liquid |
| CN111847716A (en) * | 2020-07-21 | 2020-10-30 | 河南城建学院 | Purification device for acetic acid waste liquid |
| CN115557470A (en) * | 2022-10-31 | 2023-01-03 | 湖南双阳高科化工有限公司 | Production method and production device of electronic-grade hydrogen peroxide |
| 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 |
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