CN208898768U - The equipment of mixed acid waste water during a kind of extraction-partition wall rectification process Carboxylic Acid Fibre is plain - Google Patents
The equipment of mixed acid waste water during a kind of extraction-partition wall rectification process Carboxylic Acid Fibre is plain Download PDFInfo
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Abstract
The utility model relates to the equipment of mixed acid waste water in a kind of extraction-partition wall rectification process Carboxylic Acid Fibre element, the equipment includes extraction tower, extractant recycling rectifying column, extractant recycling rectifying column condenser, divided-wall distillation column, divided-wall distillation column king-tower condenser, divided-wall distillation column secondary tower condenser and divided-wall distillation column cooler.Pass through the acetic acid extracted by mixed acid waste water in extraction tower and propionic acid (or butyric acid) is separated from water phase, extraction phase containing extractant, acetic acid and propionic acid (or butyric acid) enters divided-wall distillation column and is separated, the separation of extractant, acetic acid and propionic acid (or butyric acid) is integrated into the same divided-wall distillation column and is carried out, significantly reduce energy consumption and equipment investment, and realize the separation of acetic acid, propionic acid (or butyric acid) and water ternary component containing azeotropic system, and extractant recycling rectifying column can recycle extractant.
Description
Technical field
The utility model belongs to field of waste water treatment, and in particular to a kind of extraction-partition wall rectification process Carboxylic Acid Fibre element
The equipment of middle mixed acid waste water.
Background technique
Cellulose esters is a kind of important cellulose derivative, and also referred to as Carboxylic Acid Fibre element, common Carboxylic Acid Fibre is known as
Cellulose acetate, cellulose acetate propionate or acetylbutyrylcellulose etc., wherein cellulose acetate yield is maximum, is widely used in
Coating additive, plastics, perforated membrane etc..Cellulose acetate has excellent flame resistance, toughness, fusing point and clarity etc., however by
In its dissolubility, water-resistance, flexibility, weatherability and mouldability defect and limit it and further apply.Exactly this need
It asks, is developed cellulose mixed esters, the advantages of it inherits cellulose acetate overcomes its disadvantage, and has and tree
Lipid phase capacitive is good, light resistance and cold resistance are had excellent performance, and has been widely used in superior automobile coating and printing ink etc..Currently,
The cellulose mixed esters for having formed large-scale production includes cellulose acetate propionate and acetylbutyrylcellulose.
The preparation method of cellulose acetate propionate (or acetylbutyrylcellulose) is: using sulfuric acid as catalyst, acetic acid, propionic acid
(or butyric acid) is solvent, is raw material using native cellulose, and carrying out esterification with aceticanhydride and the third acid anhydride (or butanoic anhydride) can be obtained
Crude product, using finished product cellulose acetate propionate after the operation of the units such as hydrolysis, neutralization, precipitating, washing, boiling and drying
(or acetylbutyrylcellulose).A large amount of low concentration mixed acid can be generated in this esterification and subsequent product subtractive process
Waste water, wherein acetic acid content is about 25%, and propionic acid (or butyric acid) content is about 25%, remaining is water.Although acetic acid is not deposited with water
In azeotropic, but the two relative volatility very little, conventional distillation are difficult to separate, and propionic acid and water, butyric acid and water have binary and is total to
Boiling.Propionic acid and water binary system, propionic acid content is 17.8% in azeotropic composition, and azeotropic temperature is 99.1 DEG C；Butyric acid and water binary
System, azeotropic composition in butyric acid content be 18.5%, azeotropic temperature be 99.4 DEG C.Therefore, in cellulose acetate propionate (or acetic acid
Cellulose butyrate) the mixed acid waste water that generates in production process is difficult to realize the recycling of organic acid in waste water by conventional distillation.
Patent CN102153458A discloses a kind of method of sec-butyl acetate extraction-azeotropic distillation recycling spirit of vinegar, should
The entrainer of extractant and azeotropy rectification column of the method using sec-butyl acetate as extraction tower；A part of spirit of vinegar is sent into extraction tower
The overhead reflux liquid at top, azeotropy rectification column divides a small gangs of to send as extractant to the bottom of extraction tower；Extraction column overhead obtains
Extraction phase containing sec-butyl acetate, acetic acid and a small amount of water；It is the water containing acetate in minute that tower reactor, which obtains raffinate phase, and raffinate phase enters molten
Agent recovery tower；The upper half that the extraction phase of extraction tower is sent into azeotropy rectification column carries out further concentrate, the recycling of this method Dichlorodiphenyl Acetate
Rate is higher than 95%, and acetic acid content is below 0.5% in waste water.Although the method overcome directly adopt reflux caused by rectification method
Than the disadvantages of big, energy consumption is high, increase the production capacity of spirit of vinegar recycling, but due to using high boiling extractant, diluted acid is useless
Water only has part to enter extraction tower, and it is secondary de- that the aqueous diluted acid of another part needs to enter azeotropy rectification column progress azeotropic distillation
Water, process is complicated and waste water in acid content it is higher, it is real since the enthalpy of vaporization of water is very big and in azeotropic distillation dehydration
The energy consumption or higher of border operation, in addition, the technique can only separate acetic acid and water binary composition, is not directed to answering containing azeotropic system
The separation of heteropolyacids aqueous solution.
Utility model content
In view of this, the purpose of this utility model is to propose that a kind of extraction-partition wall rectification process Carboxylic Acid Fibre mixes in plain
The equipment for closing sour waste water, the separation of the acetic acid, propionic acid (or butyric acid) and water ternary component of azeotropic system is able to achieve using the equipment,
It is effectively reduced energy consumption and equipment investment.
Technical solution one)
The equipment of mixed acid waste water during a kind of extraction-partition wall rectification process Carboxylic Acid Fibre is plain, including extraction tower, extractant
It recycles rectifying column, extractant recycling rectifying column condenser, extractant and recycles rectifying tower reboiler, divided-wall distillation column, partition wall
Rectifying column king-tower condenser, divided-wall distillation column secondary tower condenser, divided-wall distillation column reboiler and divided-wall distillation column are cold
But device；
Middle and upper part in the divided-wall distillation column is equipped with a partition being vertically arranged, the top of the partition and the separation
Connection at the top of wall rectifying column, so that being divided into three regions inside the divided-wall distillation column: being located at divided-wall distillation column middle and upper part
The partition being vertically arranged side king-tower rectifying section, positioned at the another of the partition being vertically arranged described in divided-wall distillation column middle and upper part
The secondary tower rectifying section of side and public stripping section positioned at divided-wall distillation column lower part；
The tower top of the extraction tower is equipped with extraction phase discharge port, and the top of the extraction tower is equipped with mixing acid waste liquid charging
Mouthful, the tower bottom of the extraction tower is equipped with raffinate phase discharge port, and the lower part of the extraction tower is equipped with extractant feed mouth；The extraction
It takes and is equipped with extractant recovery port at the top of agent recycling rectifying column, the extractant recycling rectifier is equipped with raffinate phase feed inlet
Rectifier column reflux mouth is recycled with extractant, the extractant recycling rectifier bottoms are equipped with waste water discharge opening；The partition wall
Rectifier bottoms correspond to public stripping section and produce mouth, corresponding king-tower essence at the top of the divided-wall distillation column equipped with divided-wall distillation column
It evaporates section and produces mouth equipped with overhead, the divided-wall distillation column top corresponds to king-tower rectifying section equipped with extraction phase feed inlet and master
Tower refluxing opening, the corresponding secondary tower rectifying section in divided-wall distillation column top are equipped with secondary tower overhead extraction mouth, the partition wall rectifying
Tower top corresponds to secondary tower rectifying section equipped with secondary tower refluxing opening；
The raffinate phase of the raffinate phase discharge port of the extraction tower tower bottom and described extractant recycling rectifier into
Material mouth is connected by extraction tower raffinate phase discharge nozzle, the extraction phase discharge port and the divided-wall distillation column of the extraction column overhead
The extraction phase feed inlet on top is connected by extraction tower extraction phase discharge nozzle, the extraction at the top of the extractant recycling rectifying column
Agent recovery port recycles rectifying column condenser by sequentially connected extractant, extractant recycles the top of the distillation column extraction pipe, separates
Wall rectifying column cooler, extractant circulation pipe and extractant feed pipe are connected on the extractant feed mouth of the lower part of extraction tower,
The extractant recycling rectifier column reflux mouth of the extractant recycling rectifier is connect with the outlet of recovery tower condenser；Institute
Overhead extraction mouth at the top of the divided-wall distillation column stated passes through sequentially connected divided-wall distillation column king-tower condenser, separation
Wall rectifying column overhead extraction pipe, divided-wall distillation column cooler, extractant circulation pipe and extractant feed pipe are connected to extraction
It takes on the extractant feed mouth of tower lower part, the king-tower refluxing opening and divided-wall distillation column king-tower on the divided-wall distillation column top
The outlet of condenser connects；The mixing acid waste liquid feed inlet on the extraction tower top is equipped with mixed acid wastewater feed pipe, institute
The feed end and extractant storage device for the extractant feed pipe stated, the waste water discharge of the extractant recycling rectifier bottoms
Mouth is equipped with extractant recycling tower bottom of rectifying tower waste water extraction pipe；Secondary tower overhead extraction mouth at the top of the divided-wall distillation column
It is connect by divided-wall distillation column secondary tower condenser with divided-wall distillation column secondary tower overhead extraction pipe, the divided-wall distillation column
The divided-wall distillation column extraction mouth of bottom is equipped with divided-wall distillation column tower reactor extraction pipe, the pair on the divided-wall distillation column top
Tower refluxing opening is connect with the outlet of divided-wall distillation column secondary tower condenser；
Circulation is additionally provided with outside the extractant recycling rectifying column and boils pipeline one again, and circulation is boiled again is connected with extraction on pipeline one
Agent is taken to recycle rectifying tower reboiler, the import that circulation boils pipeline one again is connect with the bottom of extractant recycling rectifying column, and circulation is again
The outlet for boiling pipeline one is connect with the lower part of extractant recycling rectifying column；
It is additionally provided with circulation outside the public stripping section of the divided-wall distillation column lower part and boils pipeline two again, circulation boils pipeline again
Divided-wall distillation column reboiler is connected on two, circulation boils the import of pipeline two again and the bottom of divided-wall distillation column connects, and follows
Ring boils the outlet of pipeline two again and the lower part of divided-wall distillation column connects.
Further, the partition being vertically arranged eccentric setting in the divided-wall distillation column, so that the secondary tower rectifying
The cross-sectional area ratio of section and king-tower rectifying section is more than or equal to 0.25 and less than 1.0.The product produced due to king-tower and secondary tower
Difference is measured to select the cross-sectional area of king-tower rectifying section and secondary tower rectifying section ratio.
Further, the tower internals type of the divided-wall distillation column includes the group of column plate or filler or column plate and filler
It closes, wherein king-tower theoretical number of plates of rectifying section is 12-38, and secondary tower theoretical number of plates of rectifying section is 12-36, public stripping section number of theoretical plate
For 6-40.
Further, the tower internals type of the extraction tower is column plate or filler, number of theoretical plate 12-18.
Further, the extractant recycling rectifying column is by being located at the rectifying section of raffinate phase feed inlet or more and being located at raffinate
Phase feed inlet stripping section composition below, tower internals type is column plate or filler, theoretical number of plates of rectifying section 10-20, stripping section
Number of theoretical plate is 12-30.
Technical solution two)
The method for handling mixed acid waste water in Carboxylic Acid Fibre element, sequentially includes the following steps:
Step S1: the mixed acid waste water generated in Carboxylic Acid Fibre element production process is through mixed acid wastewater feed pipe from mixed acid
Waste liquid feed inlet enters extraction tower top, and extractant enters extraction tower lower part from extractant feed pipe；
Step S2: the raffinate phase of extraction tower tower bottom by extraction tower raffinate phase discharge nozzle enter extractant recycle rectifying column into
Row rectifying, the steam that extractant recycles the top of the distillation column rising realize phase transformation through condenser, and the material for condensing acquisition is extractant,
A part passes back into tower from the extractant recycling rectifier column reflux mouth of extractant recycling rectifier, and another part is through cooling
The extractant feed mouth that device is cooled and returned to extraction tower lower part is recycled, and extractant recycles the waste water in rectifying column from tower bottom
Waste water discharge opening by extractant recycling tower bottom of rectifying tower waste water produce pipe discharge system；
Step S3: the extraction phase for extracting column overhead enters the king-tower essence of divided-wall distillation column through extraction tower extraction phase discharge nozzle
It evaporates section and carries out rectifying, gas-liquid carries out mass transfer in tower, and the steam risen at the top of king-tower rectifying section realizes phase transformation through king-tower condenser, cold
The solidifying material obtained is extractant, and a part passes back into tower, and another part is after cooler is cooling from the extractant of extraction tower
Feed inlet is back in extraction tower and is recycled；It is mentioned from the material one that king-tower rectifying section declines into the public of divided-wall distillation column
Section is evaporated, public stripping section bottom produces material two；Material after producing material two is separating again through divided-wall distillation column reboiler
Gas-liquid mass transfer exchange is carried out in the secondary tower rectifying section of wall rectifying column, the steam risen at the top of secondary tower rectifying section is real through secondary tower condenser
Existing phase transformation, condenses the material three of acquisition, produces from secondary tower overhead extraction mouth, and another part passes back into tower from secondary tower refluxing opening.
Material one includes acetic acid and propionic acid or acetic acid and butyric acid, and material two is propionic acid or butyric acid, and material three is acetic acid.
Further, the extractant is the chlorohydrocarbon or alkane that boiling spread is 36~70 DEG C.Such as methylene chloride and ring
Hexane etc..Low-boiling chlorohydrocarbon or alkane dissolve each other with acetic acid and propionic acid (or butyric acid), but not soluble in water, later period and acetic acid and third
Sour (or butyric acid) separation is also easy.
Preferably, the operating condition setting in the extraction tower are as follows: tower top operating pressure is normal pressure, and operation temperature is normal
Temperature, the volume ratio from the extractant and the mixed acid waste water entered from mixed acid wastewater feed pipe of the entrance of extractant feed pipe are
1.0-2.5。
Preferably, the operating condition setting in the extractant recycling rectifying column are as follows: tower top operating pressure is normal pressure, tower top
Temperature is 36-70 DEG C, and the column bottom temperature is 99-101 DEG C, and the overhead reflux ratio is 0.8-5.5.
Preferably, the operating condition setting in the divided-wall distillation column are as follows: the tower top temperature of king-tower rectifying section is 36-70
DEG C, the overhead reflux ratio of king-tower rectifying section is 0.8-2.0；The tower top temperature of secondary tower rectifying section is 115-118 DEG C, secondary tower rectifying section
Overhead reflux ratio be 1.5-4.2；The column bottom temperature of the public stripping section is 140-164 DEG C.
In use, periodically discharge part extractant is regenerated, and supplement a small amount of fresh extractant.
The remarkable advantage of the utility model is:
(1) pass through the acetic acid extracted by mixed acid waste water and propionic acid (or butyric acid) in extraction tower (T1) to divide from water phase
Separate out and, the extraction phase containing extractant, acetic acid and propionic acid (or butyric acid) enters divided-wall distillation column and is separated, by extractant,
The separation of acetic acid and propionic acid (or butyric acid) is integrated into the same divided-wall distillation column and carries out, and significantly reduces energy consumption and equipment
Investment, and realize the separation of acetic acid, propionic acid (or butyric acid) and water ternary component containing azeotropic system, and extractant recycles rectifying
Tower can recycle extractant.
(2) select low-boiling chlorohydrocarbon or alkane for extractant, by extracting the acetic acid and third in mixed acid waste water
Sour (or butyric acid) is all separated from water phase, and acid content is down to 0.05% hereinafter, solving acid content in waste water in waste water
High technical problem；And it also can be easily separated in later period low-boiling chlorohydrocarbon or alkane with acetic acid and propionic acid (or butyric acid).
(3) by divided-wall distillation column, realize the separation of extractant, acetic acid and propionic acid (or butyric acid) is integrated into it is same
It is carried out in a tower, significantly reduces energy consumption and equipment investment, and realize acetic acid, propionic acid (or butyric acid) and water containing azeotropic system
The separation of ternary component, compared with traditional azeotropic distillation technique, mixed acid is useless in extraction-partition wall rectification process Carboxylic Acid Fibre element
The technique of water can save energy consumption 16-39%, save equipment investment 20-32%.
(4) it under the conditions of the utility model Processes and apparatus, is separated by divided-wall distillation column, divided-wall distillation column secondary tower
The acetic acid content of tower top is greater than 99.5%, and propionic acid (or butyric acid) content of divided-wall distillation column tower reactor is greater than 99.5%.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model embodiment.
In figure: T1 is extraction tower；T2 is that extractant recycles rectifying column；E1 is that extractant recycles rectifying column condenser；E2 is
Extractant recycles rectifying tower reboiler；T3 is divided-wall distillation column, and I is king-tower rectifying section, and II is secondary tower rectifying section, and III is public affairs
Stripping section altogether；E3 is divided-wall distillation column king-tower condenser；E4 is divided-wall distillation column secondary tower condenser；E5 is partition wall rectifying
Tower reboiler；E6 is divided-wall distillation column cooler；PL1 is mixed acid wastewater feed pipe, and PL2 is extractant storage device, PL3
For extraction tower raffinate phase discharge nozzle, PL4 is that extractant recycles the top of the distillation column extraction pipe, and PL5 is that extractant recycles rectifying tower
Kettle waste water extraction pipe, PL6 are extraction tower extraction phase discharge nozzle, and PL7 is divided-wall distillation column overhead extraction pipe, and PL8 is extraction
Agent circulation pipe is taken, PL9 is extractant feed pipe, and PL10 is divided-wall distillation column secondary tower overhead extraction pipe, and PL11 is partition wall essence
Tower tower reactor extraction pipe is evaporated, PL12 circulation boils pipeline one again, and PL13 circulation boils pipeline two again.
Specific embodiment
The utility model is described further with reference to the accompanying drawings and embodiments.
Embodiment 1
As shown in Figure 1, the present embodiment provides mixed acid waste water in a kind of extraction-partition wall rectification process Carboxylic Acid Fibre element
Equipment, it is characterised in that: including extraction tower T1, extractant recycling rectifying column T2, extractant recycling rectifying column condenser E1, extraction
Rectifying tower reboiler E2, divided-wall distillation column T3, divided-wall distillation column king-tower condenser E3, divided-wall distillation column secondary tower are recycled in agent
Condenser E4, divided-wall distillation column reboiler E5 and divided-wall distillation column cooler E6；
Middle and upper part in the divided-wall distillation column T3 is equipped with a partition being vertically arranged, the top of the partition with described point
Connection at the top of the rectifying column T3 of next door, so that being divided into three regions inside the divided-wall distillation column T3: being located at divided-wall distillation column
The king-tower rectifying section I of the side of the partition being vertically arranged of the middle and upper part T3, it is erected positioned at the described of the middle and upper part divided-wall distillation column T3
The secondary tower rectifying section II of the other side for the partition set and public stripping section III positioned at the lower part divided-wall distillation column T3；
The tower top of the extraction tower T1 is equipped with extraction phase discharge port, the top of the extraction tower T1 be equipped with mixing acid waste liquid into
Material mouth, the tower bottom of the extraction tower T1 are equipped with raffinate phase discharge port, and the lower part of the extraction tower T1 is equipped with extractant feed mouth；Institute
Extractant recovery port is equipped at the top of the extractant recycling rectifying column T2 stated, the extractant recycling top rectifying column T2 is equipped with extraction
Remaining phase feed inlet and extractant recycle rectifier column reflux mouth, and the extractant recycling bottom rectifying column T2 is discharged equipped with waste water
Mouthful；The bottom the divided-wall distillation column T3 corresponds to public stripping section III and produces mouth, the partition wall essence equipped with divided-wall distillation column
It evaporates corresponding king-tower rectifying section I at the top of tower T3 and is equipped with overhead extraction mouth, the top the divided-wall distillation column T3 corresponds to king-tower essence
Section I is evaporated equipped with extraction phase feed inlet and king-tower refluxing opening, and the corresponding secondary tower rectifying section II in the top divided-wall distillation column T3 is equipped with
Secondary tower overhead extraction mouth, the top the divided-wall distillation column T3 correspond to secondary tower rectifying section II equipped with secondary tower refluxing opening；
The raffinate of the raffinate phase discharge port of the extraction tower T1 tower bottom and the extractant recycling top rectifying column T2
Phase feed inlet is by extraction tower raffinate phase discharge nozzle PL3 connection, the extraction phase discharge port of the extraction tower T1 tower top and described point
The extraction phase feed inlet on the next door top rectifying column T3 passes through extraction tower extraction phase discharge nozzle PL6 connection, the extractant recycling
Extractant recovery port at the top of rectifying column T2 recycles rectifying column condenser E1, extractant recycling essence by sequentially connected extractant
Column overhead extraction pipe PL4, divided-wall distillation column cooler E6, extractant circulation pipe PL8 and extractant feed pipe PL9 is evaporated to be connected to
On the extractant feed mouth of the lower part of extraction tower T1, the extractant on the extractant recycling top rectifying column T2 recycles rectifying column
Refluxing opening is connect with the outlet of recovery tower condenser E1；Overhead extraction mouth at the top of the divided-wall distillation column T3 passes through
Sequentially connected divided-wall distillation column king-tower condenser E3, divided-wall distillation column overhead produce pipe PL7, divided-wall distillation column
Cooler E6, extractant circulation pipe PL8 and extractant feed pipe PL9 are connected on the extractant feed mouth of the lower part extraction tower T1,
The king-tower refluxing opening on the top divided-wall distillation column T3 is connect with the outlet of divided-wall distillation column king-tower condenser E3；It is described
The top extraction tower T1 mixing acid waste liquid feed inlet be equipped with mixed acid wastewater feed pipe PL1, the extractant feed pipe
The waste water discharge opening of the feed end and extractant storage device PL2 of PL9, the extractant recycling bottom rectifying column T2 is equipped with
Extractant recycles tower bottom of rectifying tower waste water and produces pipe PL5；Secondary tower overhead extraction mouth at the top of the divided-wall distillation column T3 is logical
It crosses divided-wall distillation column secondary tower condenser E4 to connect with divided-wall distillation column secondary tower overhead extraction pipe PL10, the partition wall essence
The divided-wall distillation column extraction mouth for evaporating the bottom tower T3 is equipped with divided-wall distillation column tower reactor and produces pipe PL11, the partition wall rectifying
The secondary tower refluxing opening on the top tower T3 is connect with the outlet of divided-wall distillation column secondary tower condenser E4；
Circulation is additionally provided with outside the extractant recycling rectifying column T2 and boils one PL12 of pipeline again, and circulation boils one PL12 of pipeline again
On be connected with extractant recycling rectifying tower reboiler E2, circulation boil again one PL12 of pipeline import and extractant recycle rectifying column T2
Bottom connection, circulation boils the outlet of one PL12 of pipeline again to be connect with the lower part that extractant recycles rectifying column T2；
It is additionally provided with circulation outside the public stripping section III of the lower part divided-wall distillation column T3 and boils two PL13 of pipeline again, follows
Ring boils again is connected with divided-wall distillation column reboiler E5 on two PL13 of pipeline, circulation boils import and the partition wall of two PL13 of pipeline again
The bottom of rectifying column T3 connects, and the outlet that circulation boils two PL13 of pipeline again is connect with the lower part of divided-wall distillation column T3.
The extraction tower T1 of the present embodiment is the packed tower of tower diameter 40mm, and tower body and filler material are 316L, wire feeding
ForThe θ ring filler of specification, raising 2.0m, number of theoretical plate are 16 pieces.It is tower diameter 40mm's that extractant, which recycles rectifying column T2,
Packed tower, tower body and filler material are 316L, and wire feeding isThe θ ring filler of specification, tower height 3m, the reason of rectifying section
It is 12 pieces by plate number, the number of theoretical plate of stripping section is 18.Divided-wall distillation column T3 is the packed tower of tower diameter 50mm, tower body and filler
Material is 2205, and wire feeding isThe θ ring filler of specification, tower height 4.5m, king-tower rectifying section I and secondary tower rectifying section II
Number of theoretical plate be 22, the number of theoretical plate of public stripping section III is 24 pieces, and secondary tower rectifying section II is transversal with king-tower rectifying section I's
Area ratio is 0.6.
Step S1: the mixed acid waste water generated in Carboxylic Acid Fibre element production process is through mixed acid wastewater feed pipe PL1 from mixed
It closes acid waste liquid feed inlet and enters the top extraction tower T1, extractant enters the lower part extraction tower T1 from extractant feed pipe PL9；
Step S2: the raffinate phase of extraction tower T1 tower bottom enters extractant recycling essence by extraction tower raffinate phase discharge nozzle PL3
It evaporates tower T2 and carries out rectifying, extractant recycles the steam that rectifying column T2 tower top rises and realizes phase transformation through condenser E1, condenses acquisition
Material is extractant, and a part passes back into tower from the extractant recycling rectifier column reflux mouth on the extractant recycling top rectifying column T2
Interior, the extractant feed mouth that another part is cooled and returned to the lower part extraction tower T1 through cooler E6 is recycled, and extractant returns
The waste water in rectifying column T2 is received from the waste water discharge opening of tower bottom by extractant recycling tower bottom of rectifying tower waste water extraction pipe PL5 discharge
System；
Step S3: the extraction phase of extraction tower T1 tower top enters divided-wall distillation column T3 through extraction tower extraction phase discharge nozzle PL6
King-tower rectifying section I carry out rectifying, gas-liquid carries out mass transfer in tower, and the steam risen at the top of king-tower rectifying section I is through king-tower condenser
E3 realizes phase transformation, and the material for condensing acquisition is extractant, and a part passes back into tower, another part after cooler E6 is cooling from
The extractant feed mouth of extraction tower T1 is back in extraction tower T1 and is recycled；The material one declined from king-tower rectifying section I enters
The public stripping section III of divided-wall distillation column T3, the bottom public stripping section III produce material two；Material after producing material two
Again through divided-wall distillation column reboiler E5, gas-liquid mass transfer exchange is carried out in the secondary tower rectifying section II of divided-wall distillation column T3, it is secondary
The steam risen at the top of tower rectifying section II realizes phase transformation through secondary tower condenser E4, condenses the material three of acquisition, adopts from secondary tower tower top
Outlet extraction, another part pass back into tower from secondary tower refluxing opening.Material one includes acetic acid and propionic acid or acetic acid and butyric acid,
Material two is propionic acid or butyric acid, and material three is acetic acid.
Mixed acid waste water is that 6g/min is fed from extraction tower top with flow, and acetic acid content is 24% (quality in mixed acid
Score, similarly hereinafter), propionic acid content 26%, remaining is water；Selection methylene chloride is extractant, flow 8g/min, from extraction
The charging of tower lower part.The operating condition of extraction tower T1: tower top pressure normal pressure, operation temperature are room temperature；Extractant recycles rectifying column T2
Operating condition: tower top pressure normal pressure, 36.2 DEG C of tower top temperature, 99.6 DEG C of bottom temperature, reflux ratio 4.5.Divided-wall distillation column
The operating condition of T3: tower top pressure normal pressure, 36.3 DEG C of overhead temperature, king-tower reflux ratio is 1.8, secondary tower tower top temperature
117.7 DEG C, secondary tower reflux ratio be 3.0,140.7 DEG C of bottom temperature.
Under the above conditions, acetic acid content is 195ppm, propionic acid content 20ppm, two in the raffinate phase of extraction tower tower reactor
Chloromethanes content is 1.4%, remaining is water.It is 94.0% that extractant, which recycles methylene chloride content in the extraction of the top of the distillation column,
Yu Weishui, is recycled, and tower reactor waste water enters waste water system.Methylene chloride content is in the extraction of divided-wall distillation column overhead
97.0%, acetic acid content 0.4%, propionic acid content 45ppm, remaining is water, is recycled, divided-wall distillation column secondary tower tower top
Acetic acid purity is 99.8% in extraction, and propionic acid purity is 99.8% in the extraction of divided-wall distillation column tower reactor.
Embodiment 2
Unlike the embodiments above, the extraction tower T1 of the present embodiment is the packed tower of tower diameter 40mm, tower body and filler
Material is 316L, and wire feeding isThe θ ring filler of specification, raising 2.0m, number of theoretical plate are 16 pieces.Extractant recycling
Rectifying column T2 is the packed tower of tower diameter 40mm, and tower body and filler material are 316L, and wire feeding isThe θ ring of specification is filled out
Material, tower height 3m, the number of theoretical plate of rectifying section are 12 pieces, and the number of theoretical plate of stripping section is 18.Divided-wall distillation column T3 is tower diameter
The packed tower of 50mm, tower body and filler material are 2205, and wire feeding isThe θ ring filler of specification, tower height 4.5m are main
The number of theoretical plate of tower rectifying section I and secondary tower rectifying section II are 22, and the number of theoretical plate of public stripping section III is 24 pieces, secondary tower rectifying
The cross-sectional area ratio of section II and king-tower rectifying section I is 0.6.
Mixed acid waste water is that 5g/min is fed from extraction tower top with flow, and acetic acid content is 25% (quality in mixed acid
Score, similarly hereinafter), butyric acid content is 25%, remaining is water；Selection n-hexane is extractant, flow 7.5g/min, from extraction
The charging of tower lower part.The operating condition of extraction tower T1: tower top pressure normal pressure, operation temperature are room temperature；Extractant recycles rectifying column T2
Operating condition: tower top pressure normal pressure, 69.0 DEG C of tower top temperature, 100.3 DEG C of bottom temperature, reflux ratio 3.6.Divided-wall distillation column
The operating condition of T3: tower top pressure normal pressure, 68.8 DEG C of overhead temperature, king-tower reflux ratio is 1.0, secondary tower tower top temperature
117.6 DEG C, secondary tower reflux ratio be 3.0,162.8 DEG C of bottom temperature.
Under the above conditions, acetic acid content is 282ppm in the raffinate phase of extraction tower tower reactor, and butyric acid content is 48ppm, just
Hexane content is 0.2%, remaining is water.It is 98.5% that extractant, which recycles n-hexane content in the extraction of the top of the distillation column, and circulation makes
With tower reactor waste water enters waste water system.N-hexane content is 99.1% in the extraction of divided-wall distillation column overhead, acetic acid content
For 234ppm, remaining is water, is recycled, and acetic acid purity is 99.6% in divided-wall distillation column secondary tower overhead extraction, partition wall
Butyric acid purity is 99.7% in tower bottom of rectifying tower extraction.
Embodiment 3
Unlike the embodiments above, the extraction tower T1 of the present embodiment is the packed tower of tower diameter 40mm, tower body and filler
Material is 316L, and wire feeding isThe θ ring filler of specification, raising 2.0m, number of theoretical plate are 16 pieces.Extractant recycling
Rectifying column T2 is the packed tower of tower diameter 40mm, and tower body and filler material are 316L, and wire feeding isThe θ ring of specification is filled out
Material, tower height 3m, the number of theoretical plate of rectifying section are 12 pieces, and the number of theoretical plate of stripping section is 18.Divided-wall distillation column T3 is tower diameter
The packed tower of 50mm, tower body and filler material are 2205, and wire feeding isThe θ ring filler of specification, tower height 4.5m are main
The number of theoretical plate of tower rectifying section I and secondary tower rectifying section II are 22, and the number of theoretical plate of public stripping section III is 24 pieces, secondary tower rectifying
The cross-sectional area ratio of section II and king-tower rectifying section I is 0.6.
Mixed acid waste water is that 6g/min is fed from extraction tower top with flow, and acetic acid content is 24% (quality in mixed acid
Score, similarly hereinafter), propionic acid content 26%, remaining is water；Selection methylene chloride is extractant, flow 6g/min, from extraction
The charging of tower lower part.The operating condition of extraction tower T1: tower top pressure normal pressure, operation temperature are room temperature；Extractant recycles rectifying column T2
Operating condition: tower top pressure normal pressure, 36.0 DEG C of tower top temperature, 99 DEG C of bottom temperature, reflux ratio 0.8.Divided-wall distillation column T3
Operating condition: tower top pressure normal pressure, 36.0 DEG C of overhead temperature, king-tower reflux ratio be 0.8,115 DEG C of secondary tower tower top temperature,
Secondary tower reflux ratio be 1.5,140 DEG C of bottom temperature.
Under the above conditions, acetic acid content is 256ppm, propionic acid content 40ppm, two in the raffinate phase of extraction tower tower reactor
Chloromethanes content is 1.5%, remaining is water.It is 96.9% that extractant, which recycles methylene chloride content in the extraction of the top of the distillation column,
Yu Weishui, is recycled, and tower reactor waste water enters waste water system.Methylene chloride content is in the extraction of divided-wall distillation column overhead
97.6%, acetic acid content 64ppm, remaining is water, is recycled, and acetic acid purity is in divided-wall distillation column secondary tower overhead extraction
99.7%, divided-wall distillation column tower reactor extraction in propionic acid purity be 99.6%.
Embodiment 4
Unlike the embodiments above, the extraction tower T1 of the present embodiment is the packed tower of tower diameter 40mm, tower body and filler
Material is 316L, and wire feeding isThe θ ring filler of specification, raising 2.0m, number of theoretical plate are 16 pieces.Extractant recycling
Rectifying column T2 is the packed tower of tower diameter 40mm, and tower body and filler material are 316L, and wire feeding isThe θ ring of specification is filled out
Material, tower height 3m, the number of theoretical plate of rectifying section are 12 pieces, and the number of theoretical plate of stripping section is 18.Divided-wall distillation column T3 is tower diameter
The packed tower of 50mm, tower body and filler material are 2205, and wire feeding isThe θ ring filler of specification, tower height 4.5m are main
The number of theoretical plate of tower rectifying section I and secondary tower rectifying section II are 22, and the number of theoretical plate of public stripping section III is 24 pieces, secondary tower rectifying
The cross-sectional area ratio of section II and king-tower rectifying section I is 0.6.
Mixed acid waste water is that 4g/min is fed from extraction tower top with flow, and acetic acid content is 25% (quality in mixed acid
Score, similarly hereinafter), butyric acid content is 25%, remaining is water；Selection n-hexane is extractant, flow 10g/min, from extraction
The charging of tower lower part.The operating condition of extraction tower T1: tower top pressure normal pressure, operation temperature are room temperature；Extractant recycles rectifying column T2
Operating condition: tower top pressure normal pressure, 70.0 DEG C of tower top temperature, 101 DEG C of bottom temperature, reflux ratio 5.5.Divided-wall distillation column T3
Operating condition: tower top pressure normal pressure, 70.0 DEG C of overhead temperature, king-tower reflux ratio be 2.0,118 DEG C of secondary tower tower top temperature,
Secondary tower reflux ratio be 4.2,164 DEG C of bottom temperature.
Under the above conditions, acetic acid content is 325ppm in the raffinate phase of extraction tower tower reactor, and butyric acid content is 83ppm, just
Hexane content is 0.3%, remaining is water.It is 98.6% that extractant, which recycles n-hexane content in the extraction of the top of the distillation column, and circulation makes
With tower reactor waste water enters waste water system.N-hexane content is 99.4% in the extraction of divided-wall distillation column overhead, acetic acid content
For 312ppm, remaining is water, is recycled, and acetic acid purity is 99.6% in divided-wall distillation column secondary tower overhead extraction, partition wall
Butyric acid purity is 99.8% in tower bottom of rectifying tower extraction.
The above is only the preferred embodiment of the present invention, it is all done according to present utility model application the scope of the patents it is equal
Deng variation and modification, it should all belong to the covering scope of the utility model.
Claims (5)
1. the equipment of mixed acid waste water in a kind of extraction-partition wall rectification process Carboxylic Acid Fibre element, it is characterised in that: including extraction
Tower (T1), extractant recycling rectifying column (T2), extractant recycling rectifying column condenser (E1), extractant recycle rectifying tower reboiler
(E2), divided-wall distillation column (T3), divided-wall distillation column king-tower condenser (E3), divided-wall distillation column secondary tower condenser (E4),
Divided-wall distillation column reboiler (E5) and divided-wall distillation column cooler (E6)；
Middle and upper part in the divided-wall distillation column (T3) is equipped with a partition being vertically arranged, the top of the partition and the separation
Connection at the top of wall rectifying column (T3), so that being divided into three regions inside the divided-wall distillation column (T3): being located at partition wall rectifying
The king-tower rectifying section (I) of the side of the partition being vertically arranged of the middle and upper part tower (T3) is located at the middle and upper part divided-wall distillation column (T3)
The partition being vertically arranged the other side secondary tower rectifying section (II) and be located at public the proposing of the lower part divided-wall distillation column (T3)
Evaporate section (III)；
The tower top of the extraction tower (T1) is equipped with extraction phase discharge port, the top of the extraction tower (T1) be equipped with mixing acid waste liquid into
Material mouth, the tower bottom of the extraction tower (T1) are equipped with raffinate phase discharge port, and the lower part of the extraction tower (T1) is equipped with extractant feed
Mouthful；Extractant recovery port is equipped at the top of extractant recycling rectifying column (T2), the extractant recycles rectifying column (T2)
Top is equipped with raffinate phase feed inlet and extractant recycles rectifier column reflux mouth, and described extractant recycling bottom rectifying column (T2) is set
There is waste water discharge opening；Divided-wall distillation column (T3) bottom corresponds to public stripping section (III) and produces equipped with divided-wall distillation column
Mouthful, corresponding king-tower rectifying section (I) is equipped with overhead and produces mouth, the partition wall rectifying at the top of the divided-wall distillation column (T3)
The top tower (T3) corresponds to king-tower rectifying section (I) equipped with extraction phase feed inlet and king-tower refluxing opening, the divided-wall distillation column (T3)
Top corresponds to secondary tower rectifying section (II) equipped with secondary tower overhead extraction mouth, and divided-wall distillation column (T3) top corresponds to secondary tower rectifying
Section (II) is equipped with secondary tower refluxing opening；
The raffinate of the raffinate phase discharge port of described extraction tower (T1) tower bottom and extractant recycling top rectifying column (T2)
Phase feed inlet is connected by extraction tower raffinate phase discharge nozzle (PL3), the extraction phase discharge port of extraction tower (T1) tower top and institute
The extraction phase feed inlet for stating the top divided-wall distillation column (T3) is connected by extraction tower extraction phase discharge nozzle (PL6), the extraction
Take agent recycling rectifying column (T2) at the top of extractant recovery port by sequentially connected extractant recycling rectifying column condenser (E1),
Extractant recycles the top of the distillation column extraction pipe (PL4), divided-wall distillation column cooler (E6), extractant circulation pipe (PL8) and extraction
Agent feed pipe (PL9) is taken to be connected on the extractant feed mouth of the lower part of extraction tower (T1), the extractant recycles rectifying column
(T2) the extractant recycling rectifier column reflux mouth on top is connect with the outlet of recovery tower condenser (E1)；The partition wall rectifying
Overhead extraction mouth at the top of tower (T3) passes through sequentially connected divided-wall distillation column king-tower condenser (E3), partition wall rectifying
Tower overhead extraction pipe (PL7), divided-wall distillation column cooler (E6), extractant circulation pipe (PL8) and extractant feed pipe
(PL9) it is connected on the extractant feed mouth of the lower part extraction tower (T1), the king-tower on the top the divided-wall distillation column (T3) returns
Head piece is connect with the outlet of divided-wall distillation column king-tower condenser (E3)；The mixing acid waste liquid on described top extraction tower (T1) into
Material mouth is equipped with mixed acid wastewater feed pipe (PL1), and feed end and the extractant storage of the extractant feed pipe (PL9) fill
It sets (PL2), the waste water discharge opening of described extractant recycling bottom rectifying column (T2) is equipped with extractant and recycles tower bottom of rectifying tower
Waste water extraction pipe (PL5)；Secondary tower overhead extraction mouth at the top of the divided-wall distillation column (T3) passes through divided-wall distillation column pair
Tower condenser (E4) is connect with divided-wall distillation column secondary tower overhead extraction pipe (PL10), the bottom the divided-wall distillation column (T3)
Divided-wall distillation column extraction mouth be equipped with divided-wall distillation column tower reactor extraction pipe (PL11), on the divided-wall distillation column (T3)
The secondary tower refluxing opening in portion is connect with the outlet of divided-wall distillation column secondary tower condenser (E4)；
It is additionally provided with circulation outside extractant recycling rectifying column (T2) to boil again pipeline one (PL12), circulation boils pipeline one again
(PL12) extractant recycling rectifying tower reboiler (E2) is connected on, circulation boils the import of pipeline one (PL12) again and extractant returns
The bottom connection of rectifying column (T2) is received, circulation boils the lower part of outlet and extractant recycling rectifying column (T2) of pipeline one (PL12) again
Connection；
It is additionally provided with circulation outside the public stripping section (III) of described lower part divided-wall distillation column (T3) and boils pipeline two (PL13) again,
Circulation is boiled again to be connected with divided-wall distillation column reboiler (E5) on pipeline two (PL13), and circulation boils the import of pipeline two (PL13) again
It is connect with the bottom of divided-wall distillation column (T3), circulation is boiled again under outlet and divided-wall distillation column (T3) of pipeline two (PL13)
Portion's connection.
2. the equipment of mixed acid waste water in a kind of extraction according to claim 1-partition wall rectification process Carboxylic Acid Fibre element,
It is characterized by: the partition being vertically arranged eccentric setting in the divided-wall distillation column (T3), so that the secondary tower rectifying section
It (II) is more than or equal to 0.25 and less than 1.0 with the cross-sectional area ratio of king-tower rectifying section (I).
3. the equipment of mixed acid waste water in a kind of extraction according to claim 1-partition wall rectification process Carboxylic Acid Fibre element,
It is characterized by: the tower internals type of the divided-wall distillation column (T3) includes the group of column plate or filler or column plate and filler
It closes, wherein king-tower rectifying section (I) number of theoretical plate is 12-38, and secondary tower rectifying section (II) number of theoretical plate is 12-36, public stripping section
(III) number of theoretical plate is 6-40.
4. the equipment of mixed acid waste water in a kind of extraction according to claim 1-partition wall rectification process Carboxylic Acid Fibre element,
It is characterized by: the tower internals type of the extraction tower (T1) is column plate or filler, number of theoretical plate 12-18.
5. the equipment of mixed acid waste water in a kind of extraction according to claim 1-partition wall rectification process Carboxylic Acid Fibre element,
It is characterized by: extractant recycling rectifying column (T2) is by being located at the rectifying section of raffinate phase feed inlet or more and being located at raffinate phase
Feed inlet stripping section composition below, tower internals type are column plate or filler, theoretical number of plates of rectifying section 10-20, stripping section reason
It is 12-30 by plate number.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111888792A (en) * | 2020-08-24 | 2020-11-06 | 大连理工大学 | Device and method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation |
| CN112225680A (en) * | 2019-07-15 | 2021-01-15 | 中国石油化工股份有限公司 | Organic solvent purification method and device |
| CN112221181A (en) * | 2019-07-15 | 2021-01-15 | 中国石油化工股份有限公司 | Organic solvent recovery processing device and processing method |
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2018
- 2018-09-18 CN CN201821521890.0U patent/CN208898768U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225680A (en) * | 2019-07-15 | 2021-01-15 | 中国石油化工股份有限公司 | Organic solvent purification method and device |
| CN112221181A (en) * | 2019-07-15 | 2021-01-15 | 中国石油化工股份有限公司 | Organic solvent recovery processing device and processing method |
| CN111888792A (en) * | 2020-08-24 | 2020-11-06 | 大连理工大学 | Device and method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation |
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