CN206033629U - Rectification device of pyridine is retrieved to vapor permeation coupling method - Google Patents
Rectification device of pyridine is retrieved to vapor permeation coupling method Download PDFInfo
- Publication number
- CN206033629U CN206033629U CN201620940264.XU CN201620940264U CN206033629U CN 206033629 U CN206033629 U CN 206033629U CN 201620940264 U CN201620940264 U CN 201620940264U CN 206033629 U CN206033629 U CN 206033629U
- Authority
- CN
- China
- Prior art keywords
- pyridine
- vapor permeation
- water vapour
- rectifying column
- membrane separator
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The utility model relates to a rectification device of pyridine is retrieved to vapor permeation coupling method, including: rectifying column (1), the top of the tower of rectifying column (1) is provided with top of the tower partial condenser (2), is provided with reboiler (3) at the bottom of the tower, and the liquid phase export of top of the tower partial condenser (2) is connected with vapor permeation membrane separation unit's (5) the side entrance of holding back through over heater (4) again, and vapor permeation membrane separation unit's (5) the side export of holding back is connected with condenser (6), and vapor permeation membrane separation unit's (5) infiltration side is connected with penetrant condenser and vacuum pump (9). The utility model discloses process is simple, and the energy consumption is low, and no third component is added, and the rate of recovery is high.
Description
Technical field
This utility model is related to the device that a kind of rectification-water vapour penetration coupled method reclaims pyridine, belongs to vapor permeable membrane application
Field.
Background technology
Pyridine is important pesticide, medical material, is good organic solvent and organic catalyst compound again.Pyridine waste water
If directly discharged, serious harm is not only caused to environment, and can cause great economic loss.Pyridine can be formed most with water
Low azeotropic mixture, cannot be separated using common rectificating method.Pyridine is dissolved in water, ethanol, ether equal solvent, and pyridine is formed with water and contained
Water 43%（Mass percent）Azeotropic mixture.In the industrial production sometimes produce pyridine, aqueous mixtures residual liquid, while also for
The requirement of environmental protection, needs to reclaim the pyridine in pyridine aqueous mixtures.
Tradition separates the method that pyridine aqueous mixtures adopt the azeotropic distillation with benzene as entrainer, i.e. tower top obtains benzene water azeotropic
Thing, bottom of towe obtain pyridine.In order to further improve the purity of pyridine, can be to the row distillation again of the pyridine of bottom of towe.Benzene in benzene water azeotropic mixture
Content is both needed to from tower top steam up to 91.17% (mass percent), substantial amounts of benzene, and it is larger to there is energy consumption, and operation is strict, and benzene may
The shortcomings of pollution is brought to pyridine.Salt easily blocking and etching apparatus, saline extraction is in actual industrial using few.Transformation essence
Evaporate flow process and be coupled by 2 different rectifying columns of operating pressure and form, changed by changing pressure and constituting azeotropic, so as to across
More former azeotropic composition is realized separating, and the technique can avoid the use of entrainer, but energy consumption is also bigger than normal.
The content of the invention
The purpose of this utility model is to propose that a kind of rectification-vapor permeable membrane coupled method carries out the device of pyridine dehydration.
Water vapour penetration membrane technology is reached using being dissolved (adsorb) properties different from diffusion rate in film by each component in separating mixture
To detached purpose, separation process is not limited by component VLE, can realize distillation, extraction, absorption etc. with low energy consumption
Traditional method is difficult to the separation task for completing, and substitutes traditional pyridine dehydration technique and has very big advantage.The method has work
Skill process is simple, and safety coefficient is high, and the response rate is high, and energy consumption is low, the characteristics of cleanliness without any pollution.
A kind of rectification-vapor permeation reclaims the technique of pyridine, comprises the steps：
1st step, aqueous pyridine is carried out by way of rectification preliminary purification, and tower top obtains the azeotropic mixture of pyridine and water,
Bottom of towe obtains pyridine and other heavy constituents；
The azeotropic mixture part backflow of the 2nd step, pyridine and water, enters vapor permeable membrane dewatering system after another part is overheated
Be dehydrated, pyridine is recycled in vapor permeable membrane retention side, obtains water in per-meate side.
In the 2nd described step, in vapor permeable membrane dehydration, the steam of per-meate side is through condensed in two stages；The first order is oozed
Transparent liquid is directly discharged, and the penetrating fluid of the second level is back to rectifying column recycling.
In 1st step, the operating pressure of rectifying column is 0～0.5Mpa.Feed liquid can be so made to enter steam in vapour form
Infiltration membrane separator group, improves mass transfer force, saves energy consumption.
In 2nd step, by the azeotropic mixture of pyridine and water is warming up to 90～150 DEG C after overheated.Feed liquid can so be made with
Vapor form enters water vapour penetration membrane separator group, improves mass transfer force, and can reduce the water content in product.
In 2nd step, the per-meate side of vapor permeable membrane keeps pressure in 100～8000Pa by evacuation.
In 2nd step, vapor permeable membrane is made up of 1～100 membrance separation unit series, parallel or series-parallel connection.If film point
It is too small from area, then separation accuracy can not be reached, if membrance separation area is excessive, the energy consumption of system can be caused too high, passed through
Adjustment series connection and number in parallel, it is possible to achieve different disposal is required and production capacity.
In 2nd step, the material of vapor permeable membrane is polyvinyl alcohol film, polyimides, shitosan or molecular screen membrane.
The acid waste water containing pyridine that described aqueous pyridine is produced in referring to pyrethrin production process, wherein pyridine contain
Amount about 15～20%, pH about 4.2～5.3；Need before rectification is carried out plus alkali adjusts pH to neutrality.
A kind of rectification-vapor permeation reclaims the device of pyridine, includes：Rectifying column, the tower top of rectifying column are provided with tower
Top fractional condenser, bottom of towe are provided with reboiler, the liquid-phase outlet of dephlegmator of top of the tower by superheater again with water vapour penetration membrane separator
The retention side entrance connection of group, the retention side outlet of water vapour penetration membrane separator group are connected with condenser, water vapour penetration membrance separation
The per-meate side of unit is connected with penetrating fluid condenser and vacuum pump.
Described penetrating fluid condenser is by the one-level penetrating fluid condenser being sequentially connected and two grades of penetrating fluid condenser institutes
Composition, two grades of penetrating fluid condensers are connected with rectifying column.
Described water vapour penetration membrane separator group be serially connected by 1～100 water vapour penetration membrane separator, it is in parallel or mixed
Connection is constituted.
Water vapour penetration membrane material in water vapour penetration membrane separator is polyvinyl alcohol film, polyimides, shitosan or divides
Sub- sieve membrane.
PH value for adjust aqueous pyridine is included in described device also to neutral pH regulator portion.
Beneficial effect
The pyridine recovery method that this utility model is provided can effectively carry out pyridine recovery so as to which moisture is reduced to
0.01%（w/w）Below.Simultaneously, it is ensured that the infiltration water energy containing pyridine that water vapour penetration membrane separator group is produced enough enters one
Step is recycled, almost no pyridine loss in technical process, and directly the content of organics in the waste water of discharge is very low.
Description of the drawings
Fig. 1 is the schematic flow sheet of the pyridine retracting device that this utility model is provided.
1st, rectifying column；2nd, dephlegmator of top of the tower；3rd, reboiler；4th, superheater；5th, water vapour penetration membrane separator group；6th, condense
Device；7th, one-level penetrating fluid condenser；8th, two grades of penetrating fluid condensers；9th, vacuum pump.
Specific embodiment
This utility model is described in further detail below by specific embodiment.But those skilled in the art will
Understand, the following example is merely to illustrate this utility model, and should not be regarded as limiting scope of the present utility model.In embodiment not
Dated particular technique or condition person, enter according to the technology or condition described by document in the art or according to product description
OK.Agents useful for same or the unreceipted production firm person of instrument, be can by city available from conventional products.
Using range format expression value should be interpreted as in a flexible way not only include clearly include as scope
The numerical value of limit value, but also including all single numbers or subinterval for covering within the range, just as each numerical value and sub-district
Between be expressly recited out.For example, the concentration range of " about 0.1% to about 5% " should be understood to not only include what is clearly included
The concentration of about 0.1% to about 5%, also including the single concentration in the range of alluding to（Such as, 1%, 2%, 3% and 4%）And subinterval（Example
Such as, 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%）.Percentage ratio described in this utility model is in the situation without special instruction
Under, refer to percentage by weight.
It is addressed in this manual to " one embodiment ", " another embodiment ", " embodiment " etc., refer to
Specific features, structure with reference to embodiment description are included at least one embodiment of the application generality description.
It is not necessarily to refer to same embodiment that statement of the same race occur in multiple places in the description.Furthermore, it is understood that combining arbitrary
When embodiment describes specific features, structure or a feature, to be advocated is realizing this spy with reference to other embodiment
Levy, structure or feature also fall in the application scope of the claimed.
What is processed in following examples is the acid waste water containing pyridine produced in pyrethrin production process, wherein pyridine
Content about 15～20%, pH about 4.2～5.3.
This utility model is separated to aqueous pyridine solution using rectification-water vapour penetration membrane separation process, film retention side
Tower reactor can obtain the low-down pyridine product of water content, and the direct gas phase of tower top material of rectifying column enters water vapour penetration membranous system,
Further reclaim into rectifying column simultaneous with the rear class penetrating fluid of pyridine.Whole process energy consumption is low, and process is simple realizes pyrrole
The response rate of the maximum of pyridine and zero-emission.
Embodiment 1
Will containing pyridine 20% 1000kg/h pyridines waste water send into rectifying column, rectifying column operating pressure be 0.1MPa, reflux ratio
For 0.5.Tower top obtains the pyridine of water content about 42.5%, is superheated to 120 DEG C and enters into by 6 vapor permeable membrane (every grade of membrane modules
Area is 30m2) infiltration membrane separator group 5 in series.Membranous system osmotic lateral pressure is controlled in 1000Pa.Water in feed liquid
Condense through vapor permeable membrane Jing one-level penetrating fluids condenser 7 and two grades of penetrating fluid condensers 8, one-level penetrating fluid is directly discharged,
Two grades of penetrating fluids are directly entered rectifying column 1 carries out the circulation and stress of pyridine.
Embodiment 2
1000kg/h pyridines waste water containing pyridine 20% is sent into into rectifying column, rectifying column operating pressure is 0.15MPa, is flowed back
Than for 0.9.Tower top obtains the pyridine of water content about 42.1%, is superheated to 140 DEG C and enters into by 4 NaA molecular sieve vapor permeable membranes
(every grade of membrane module area is 10m2) infiltration membrane separator group 5 in series.Membranous system osmotic lateral pressure is controlled in 700Pa.
Water in feed liquid passes through vapor permeable membrane Jing one-level penetrating fluids condenser 7 and two grades of penetrating fluid condensers 8 are condensed, one-level penetrating fluid
Directly discharge, two grades of penetrating fluids are directly entered rectifying column 1 carries out the circulation and stress of pyridine.
Embodiment 3
1000kg/h pyridines waste water containing pyridine 20% is sent into into rectifying column, rectifying column operating pressure is 0.20MPa.Tower top
The pyridine of water content about 41.8% is obtained, 130 DEG C is superheated to and is entered into by 10 NaA molecular sieve vapor permeable membrane (every grade of membrane modules
Area is 7m2) infiltration membrane separator group 5 in series.Membranous system osmotic lateral pressure is controlled in 2000Pa.Water in feed liquid is saturating
Cross vapor permeable membrane Jing one-level penetrating fluids condenser 7 and two grades of penetrating fluid condensers 8 are condensed, one-level penetrating fluid is directly discharged, two
Level penetrating fluid is directly entered rectifying column 1 carries out the circulation and stress of pyridine.
Embodiment 4
Add alkali to adjust pH the 1000kg/h pyridine waste water containing pyridine 20% and send into rectifying column, rectifying column operation to neutrality
Pressure is 0.15MPa, and reflux ratio is 0.9.Tower top obtains the pyridine of water content about 42.1%, is superheated to 140 DEG C and enters into by 4
(every grade of membrane module area is 10m to NaA molecular sieve vapor permeable membrane2) infiltration membrane separator group 5 in series.Membranous system permeates
Lateral pressure is controlled in 700Pa.Water in feed liquid passes through vapor permeable membrane Jing one-level penetrating fluids condenser 7 and two grades of infiltration liquid condensings
Device 8 is condensed, and one-level penetrating fluid is directly discharged, and two grades of penetrating fluids are directly entered rectifying column 1 carries out the circulation and stress of pyridine.
Claims (4)
1. a kind of rectification-vapor permeation reclaims the device of pyridine, it is characterised in that include：Rectifying column（1）, rectifying column（1）
Tower top be provided with dephlegmator of top of the tower（2）, bottom of towe is provided with reboiler（3）, dephlegmator of top of the tower（2）Liquid-phase outlet by overheated
Device（4）Again with water vapour penetration membrane separator group（5）Retention side entrance connection, water vapour penetration membrane separator group（5）Retention side
Outlet and condenser（6）Connection, water vapour penetration membrane separator group（5）Per-meate side be connected with penetrating fluid condenser and vacuum pump
（9）.
2. rectification according to claim 1-vapor permeation reclaims the device of pyridine, it is characterised in that described infiltration
Liquid condensing device is by the one-level penetrating fluid condenser being sequentially connected（7）With two grades of penetrating fluid condensers（8）Constituted, two grades of infiltrations
Liquid condensing device（8）With rectifying column（1）Connection.
3. rectification according to claim 1-vapor permeation reclaims the device of pyridine, it is characterised in that described steam
Infiltration membrane separator group（5）Be be serially connected by 1～100 water vapour penetration membrane separator, in parallel or series-parallel connection is constituted；Water vapour penetration
Water vapour penetration membrane material in membrane separator is polyvinyl alcohol film, polyimides, shitosan or molecular screen membrane.
4. rectification according to claim 1-vapor permeation reclaims the device of pyridine, it is characterised in that described device
In also include for adjusting the pH value of aqueous pyridine to neutral pH regulator portion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620940264.XU CN206033629U (en) | 2016-08-25 | 2016-08-25 | Rectification device of pyridine is retrieved to vapor permeation coupling method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620940264.XU CN206033629U (en) | 2016-08-25 | 2016-08-25 | Rectification device of pyridine is retrieved to vapor permeation coupling method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN206033629U true CN206033629U (en) | 2017-03-22 |
Family
ID=58305441
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201620940264.XU Active CN206033629U (en) | 2016-08-25 | 2016-08-25 | Rectification device of pyridine is retrieved to vapor permeation coupling method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN206033629U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113698371A (en) * | 2020-05-20 | 2021-11-26 | 中国石油化工集团公司 | Method and device for recovering tetrahydrofuran by rectification-membrane separation coupling method |
-
2016
- 2016-08-25 CN CN201620940264.XU patent/CN206033629U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113698371A (en) * | 2020-05-20 | 2021-11-26 | 中国石油化工集团公司 | Method and device for recovering tetrahydrofuran by rectification-membrane separation coupling method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103224456B (en) | Process and device for refining acetonitrile with a pervaporation method | |
| CN103408514B (en) | Technique and device for recovering tetrahydrofuran by pervaporation method | |
| CN101143803B (en) | Method for separating dimethyl carbonate and methanol azeotrope | |
| US20090057128A1 (en) | Liquid separation by membrane assisted vapor stripping process | |
| CN106117120B (en) | A kind of technique and device of rectifying-Steam soak coupled method recycling pyridine | |
| CN107253901A (en) | A kind of separation of high-purity isopropanol and purification method | |
| KR20160104716A (en) | System and method for organic solvent purification | |
| CN104027996A (en) | A pervaporation rectification coupled system and a use thereof | |
| JP6196807B2 (en) | Water-soluble organic substance concentration method and water-soluble organic substance concentration apparatus | |
| CN104557529A (en) | Refining method and device for n-propyl acetate esterification synthesis | |
| CN104109078B (en) | A kind of method that in Sulpyrine production, ethanol reclaims | |
| CN106045872B (en) | The pervaporation method recovery system and method for a kind of Dimethylformamide Residue | |
| CN103709022A (en) | Process and device for recovering butanone by pervaporation method | |
| CN105218317A (en) | A kind of method that in hexanitrobibenzyl production, ethanol reclaims and device | |
| CN110234620B (en) | Method for producing high-concentration alcohol | |
| CN206033629U (en) | Rectification device of pyridine is retrieved to vapor permeation coupling method | |
| JP5604677B2 (en) | Separation apparatus for azeotropic mixture and method for separating azeotropic mixture | |
| CN104193651A (en) | Refining method and device for synthesizing acetonitrile from acetic acid by ammoniation | |
| CN108424350A (en) | A kind of technique of purification medicinal ethyl alcohol | |
| CN103613480A (en) | Device and method for recycling low-concentration organic solvent | |
| CN103772144B (en) | A kind of method utilizing osmotic gasification-rectification integrated separation acetone-butanol alcohol fermentation liquid | |
| JP2011218321A (en) | Apparatus and method for distilling volatile organic compound | |
| CN106986769B (en) | Separation and integration system and separation and integration method of ethyl acetate-water system | |
| CN107206286A (en) | The method and apparatus that dimethyl carbonate is purified using pervaporation | |
| JPH01107805A (en) | Method of recovering by refining used solvent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |