CN106117120A - A kind of rectification water vapour penetration coupled method reclaims technique and the device of pyridine - Google Patents
A kind of rectification water vapour penetration coupled method reclaims technique and the device of pyridine Download PDFInfo
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- CN106117120A CN106117120A CN201610722685.XA CN201610722685A CN106117120A CN 106117120 A CN106117120 A CN 106117120A CN 201610722685 A CN201610722685 A CN 201610722685A CN 106117120 A CN106117120 A CN 106117120A
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- pyridine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
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Abstract
The present invention relates to a kind of rectification water vapour penetration coupled method and reclaim technique and the device of pyridine, it specifically comprises the following steps that and aqueous pyridine is entered rectifying column, and obtaining anhydrous pyridine or other heavy constituents at the bottom of tower, tower top obtains the azeotropic mixture of pyridine and water.An azeotropic mixture part refluxes, a part of overheated rear entrance vapor permeable membrane dewatering system, obtains anhydrous pyridine after film multiple stage separation.Film separation system per-meate side is connected with vacuum system, and prime penetrating fluid directly discharges, and the rear class penetrating fluid containing pyridine enters above rectifying column and recycles.Present invention process process is simple, and energy consumption is low, and no third component adds, and the response rate is high.
Description
Technical field
The present invention relates to technique and device that a kind of pyridine reclaims, particularly relate to a kind of rectification-vapor permeable membrane coupled method
Reclaim technique and the device of pyridine, belong to vapor permeable membrane application.
Background technology
Pyridine is important pesticide, medical material, is again good organic solvent and organic catalyst compound.Pyridine waste water
If directly discharging, not only environment being caused serious harm, and great economic loss can be caused.Pyridine and water can be formed
Low azeotropic mixture, uses common rectificating method to separate.Pyridine is dissolved in water, ethanol, ether equal solvent, and pyridine is formed with water and contains
Water 43%(mass percent) azeotropic mixture.Produce pyridine, aqueous mixtures residual liquid the most sometimes, the most also for
The requirement of environmental protection, needs to reclaim the pyridine in pyridine aqueous mixtures.
Tradition separates the method that pyridine aqueous mixtures uses the azeotropic distillation with benzene as entrainer, i.e. tower top obtains benzene water azeotropic
Thing, obtains pyridine at the bottom of tower.In order to improve the purity of pyridine further, can be to the row distillation again of the pyridine at the bottom of tower.Benzene in benzene water azeotropic mixture
Content reaches 91.17% (mass percent), and substantial amounts of benzene is both needed to steam from tower top, there is energy consumption relatively big, and operation is strict, and benzene may
The shortcomings such as pollution are brought to pyridine.Salt easily blocks and etching apparatus, and saline extraction is applied seldom in actual industrial.Transformation essence
Evaporate flow process to be formed by 2 the rectifying column connections operating pressure different, make azeotropic composition change by changing pressure, thus across
The most former azeotropic composition realizes separating, and this technique can avoid the use of entrainer, but energy consumption is bigger than normal.
Summary of the invention
It is an object of the invention to propose the method that a kind of rectification-vapor permeable membrane coupled method carries out pyridine dehydration.Steam
Permeable membrane technology utilizes is dissolved (absorption) character different from diffusion rate in film by component each in separating mixture and reaches point
From purpose, separation process is not limited by component VLE, it is possible to realizes distilling with low energy consumption, extract, the tradition such as absorption
The separation task that has been difficult to of method, substitute tradition pyridine dehydration technique and there is the biggest advantage.The method has technique mistake
Journey is simple, and safety coefficient is high, and the response rate is high, and energy consumption is low, the feature of cleanliness without any pollution.
A kind of rectification-vapor permeation reclaims the technique of pyridine, comprises the steps:
1st step, carries out preliminary purification by the way of rectification by aqueous pyridine, and tower top obtains the azeotropic mixture of pyridine and water, at the bottom of tower
Obtain pyridine and other heavy constituent;
The azeotropic mixture part backflow of the 2nd step, pyridine and water, enters vapor permeable membrane dewatering system and carries out after another part is overheated
Dehydration, retains side at vapor permeable membrane and is recycled pyridine, obtain 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;Oozing of the first order
Transparent liquid is directly discharged, and the penetrating fluid of the second level is back to rectifying column recycling.
In 1st step, the operation pressure of rectifying column is 0~0.5Mpa.Feed liquid so can be made to enter steam in vapour form
Permeable membrane separation unit, improves mass transfer force, saves energy consumption.
In 2nd step, after overheated, the azeotropic mixture of pyridine and water is warming up to 90~150 DEG C.So can make feed liquid 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 100~8000Pa by evacuation.
In 2nd step, vapor permeable membrane is to be made up of 1~100 membrance separation unit series, parallel or series-parallel connection.If film divides
Too small from area, then can not reach separation accuracy, if membrance separation area is excessive, then the energy consumption that can cause system is too high, passes through
Adjust series connection and number in parallel, it is possible to achieve different disposal requires and production capacity.
In 2nd step, the material of vapor permeable membrane is polyvinyl alcohol film, polyimides, chitosan or molecular screen membrane.
Described aqueous pyridine refers to the acid waste water containing pyridine produced in pyrethrin production process, and wherein pyridine contains
Amount about 15~20%, pH about 4.2~5.3;Need to add alkali regulation pH to neutral before carrying out rectification.
A kind of rectification-vapor permeation reclaims the device of pyridine, includes: rectifying column, and the tower top of rectifying column is provided with tower
Top fractional condenser, be provided with reboiler at the bottom of tower, the liquid-phase outlet of dephlegmator of top of the tower by superheater again with water vapour penetration membrane separator
The side entrance that retains of group connects, and the side outlet that retains of water vapour penetration membrane separator group is connected with condenser, water vapour penetration membrance separation
The per-meate side of unit connects penetrating fluid condenser and vacuum pump.
Described penetrating fluid condenser is by the one-level penetrating fluid condenser being sequentially connected with 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, in parallel or mixed
Connection is constituted.
Water vapour penetration membrane material in water vapour penetration membrane separator is polyvinyl alcohol film, polyimides, chitosan or divides
Sub-sieve membrane.
Described device also includes the pH value for regulating aqueous pyridine to neutral pH regulator portion.
Beneficial effect
The pyridine recovery method that the present invention provides can carry out pyridine recovery effectively so that it is moisture is reduced to 0.01%(w/
W) below.Simultaneously, it is ensured that the infiltration water containing pyridine that water vapour penetration membrane separator group produces can reclaim profit further
With, technical process is lost almost without pyridine, directly the content of organics in the waste water of discharge is the lowest.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the pyridine retracting device that the present invention provides.
1, rectifying column;2, dephlegmator of top of the tower;3, reboiler;4, superheater;5, water vapour penetration membrane separator group;6, condensation
Device;7, one-level penetrating fluid condenser;8, two grades of penetrating fluid condensers;9, vacuum pump.
Detailed description of the invention
Below by detailed description of the invention, the present invention is described in further detail.But those skilled in the art will manage
Solving, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Unreceipted concrete skill in embodiment
Art or condition person, according to the technology described by the document in this area or condition or carried out according to product description.Examination used
Agent or instrument unreceipted production firm person, be can by city available from conventional products.
The value expressed using range format should be interpreted as in a flexible way not only including clearly listing as scope
The numerical value of limit value, but also include containing all single numerical value within the range or subinterval, just as each numerical value and Zi Qu
Between be expressly recited out.Such as, the concentration range of " about 0.1% to about 5% " should be understood to not only to include clearly to list
The concentration of about 0.1% to about 5%, also includes the single concentration (e.g., 1%, 2%, 3% and 4%) in the range of indication and subinterval (example
As, 0.1% to 0.5%, 1% to 2.2%, 3.3% to 4.4%).Heretofore described percentage ratio without special instruction in the case of,
Refer to percentage by weight.
" embodiment ", " another embodiment ", " embodiment " addressed in this manual etc., refer to
In conjunction with this embodiment describe specific features, structure or be included in the application generality describe at least one embodiment in.
The most multiple local appearance statement of the same race is not necessarily to refer to same embodiment.Furthermore, it is understood that combine arbitrary
When embodiment describes a specific features, structure or feature, to be advocated is to combine other embodiments to realize this spy
Levy, structure or feature also fall in the application scope of the claimed.
Process in following example is the acid waste water containing pyridine produced in pyrethrin production process, wherein pyridine
Content about 15~20%, pH about 4.2~5.3.
The present invention uses rectification-water vapour penetration membrane separation process to separate aqueous pyridine solution, and film retains side tower reactor
Can obtain water content low-down pyridine product, the direct gas phase of tower top material of rectifying column enters water vapour penetration membranous system, simultaneously
Rear class penetrating fluid entrance rectifying column with pyridine reclaims further.Whole process energy consumption is low, and technique is simple, it is achieved that pyridine
The maximum response rate and zero-emission.
Embodiment 1
1000kg/h pyridine waste water containing pyridine 20% is sent into rectifying column, and rectifying column operation pressure is 0.1MPa, and reflux ratio is
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 membranes (every grade of membrane module face
Amass as 30m2) permeable membrane separation unit 5 in series.Membranous system osmotic lateral pressure controls at 1000Pa.Water in feed liquid is saturating
Crossing vapor permeable membrane to condense through one-level penetrating fluid condenser 7 and two grades of penetrating fluid condensers 8, one-level penetrating fluid directly discharges, and two
Level penetrating fluid is directly entered rectifying column 1 and carries out the circulation and stress of pyridine.
Embodiment 2
1000kg/h pyridine waste water containing pyridine 20% is sent into rectifying column, and rectifying column operation 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 NaA molecular sieve vapor permeable membranes (every
Level membrane module area is 10m2) permeable membrane separation unit 5 in series.Membranous system osmotic lateral pressure controls at 700Pa.Feed liquid
In water condense through one-level penetrating fluid condenser 7 and two grades of penetrating fluid condensers 8 through vapor permeable membrane, one-level penetrating fluid is direct
Discharge, two grades of penetrating fluids are directly entered rectifying column 1 and carry out the circulation and stress of pyridine.
Embodiment 3
1000kg/h pyridine waste water containing pyridine 20% is sent into rectifying column, and rectifying column operation pressure is 0.20MPa.Tower top obtains
The pyridine of water content about 41.8%, is superheated to 130 DEG C and enters into by 10 NaA molecular sieve vapor permeable membranes (every grade of membrane module area
For 7m2) permeable membrane separation unit 5 in series.Membranous system osmotic lateral pressure controls at 2000Pa.Water in feed liquid is through steaming
Vapour permeable membrane condenses through one-level penetrating fluid condenser 7 and two grades of penetrating fluid condensers 8, and one-level penetrating fluid directly discharges, and two grades ooze
Transparent liquid is directly entered rectifying column 1 and carries out the circulation and stress of pyridine.
Embodiment 4
1000kg/h pyridine waste water containing pyridine 20% is added alkali regulation pH to neutrality, sends into rectifying column, rectifying column operation pressure
For 0.15MPa, 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 and divided by 4 NaA
(every grade of membrane module area is 10m to son sieve vapor permeable membrane2) permeable membrane separation unit 5 in series.Membranous system infiltration side pressure
Power controls at 700Pa.Water in feed liquid passes through vapor permeable membrane through one-level penetrating fluid condenser 7 and two grades of penetrating fluid condensers 8
Condensation, one-level penetrating fluid directly discharges, and two grades of penetrating fluids are directly entered rectifying column 1 and carry out the circulation and stress of pyridine.
Claims (10)
1. the technique that rectification-vapor permeation reclaims pyridine, it is characterised in that comprise the steps: the 1st step, by aqueous
Pyridine carries out preliminary purification by the way of rectification, and tower top obtains the azeotropic mixture of pyridine and water, obtains pyridine and other is heavy at the bottom of tower
Component;The azeotropic mixture part backflow of the 2nd step, pyridine and water, enters vapor permeable membrane dewatering system and enters after another part is overheated
Row dehydration, retains side at vapor permeable membrane and is recycled pyridine, obtain water in per-meate side.
The technique that rectification the most according to claim 1-vapor permeation reclaims pyridine, it is characterised in that the 2nd described step
In, in vapor permeable membrane dehydration, the steam of per-meate side is through condensed in two stages;The penetrating fluid of the first order directly discharges, the second level
Penetrating fluid be back to rectifying column recycling.
The technique that rectification the most according to claim 1-vapor permeation reclaims pyridine, it is characterised in that in the 1st step, essence
The operation pressure evaporating tower is 0~0.5Mpa;In 2nd step, after overheated, the azeotropic mixture of pyridine and water is warming up to 90~150
℃;In 2nd step, the per-meate side of vapor permeable membrane keeps pressure 100~8000Pa by evacuation.
The technique that rectification the most according to claim 1-vapor permeation reclaims pyridine, it is characterised in that in the 2nd step, steams
Vapour permeable membrane is to be made up of 1~100 membrance separation unit series, parallel or series-parallel connection.
The technique that rectification the most according to claim 1-vapor permeation reclaims pyridine, it is characterised in that in the 2nd step, steams
The material of vapour permeable membrane is polyvinyl alcohol film, polyimides, chitosan or molecular screen membrane.
The technique that rectification the most according to claim 1-vapor permeation reclaims pyridine, it is characterised in that described is aqueous
Pyridine refers to the acid waste water containing pyridine produced in pyrethrin production process, and wherein pyridine content about 15~20%, pH is about
4.2~5.3;Need to add alkali regulation pH to neutral before carrying out rectification.
7. the device of rectification-vapor permeation recovery 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), be provided with reboiler (3) at the bottom of tower, the liquid-phase outlet of dephlegmator of top of the tower (2) is by overheated
Device (4) side entrance that retains with water vapour penetration membrane separator group (5) again is connected, water vapour penetration membrane separator group (5) retain side
Outlet is connected with condenser (6), and the per-meate side of water vapour penetration membrane separator group (5) connects penetrating fluid condenser and vacuum pump
(9).
Rectification the most according to claim 7-vapor permeation reclaims the device of pyridine, it is characterised in that described infiltration
Liquid condensing device is made up of one-level penetrating fluid condenser (7) being sequentially connected with and two grades of penetrating fluid condensers (8), two grades of infiltrations
Liquid condensing device (8) is connected with rectifying column (1).
Rectification the most according to claim 7-vapor permeation reclaims the device of pyridine, it is characterised in that described steam
Permeable membrane separation unit (5) 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, chitosan or molecular screen membrane.
Rectification the most according to claim 7-vapor permeation reclaims the device of pyridine, it is characterised in that described device
In also include pH value for regulating aqueous pyridine to neutral pH regulator portion.
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Cited By (4)
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CN107185265A (en) * | 2017-06-21 | 2017-09-22 | 武汉智宏思博化工科技有限公司 | The dehydration of organic solvent equipment that a kind of rectifying column is coupled with seepage slope membranous system |
CN112121453A (en) * | 2020-09-10 | 2020-12-25 | 天津大学 | In-tower reactive distillation and membrane coupling process method and device for producing ethyl levulinate |
CN114212941A (en) * | 2021-12-21 | 2022-03-22 | 江苏三吉利化工股份有限公司 | System and method for recovering MOE (metal oxide organic ether) in ethylene glycol monomethyl ether wastewater |
CN116332836A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Method for recovering pyridine waste solvent |
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CN107185265A (en) * | 2017-06-21 | 2017-09-22 | 武汉智宏思博化工科技有限公司 | The dehydration of organic solvent equipment that a kind of rectifying column is coupled with seepage slope membranous system |
CN112121453A (en) * | 2020-09-10 | 2020-12-25 | 天津大学 | In-tower reactive distillation and membrane coupling process method and device for producing ethyl levulinate |
CN112121453B (en) * | 2020-09-10 | 2023-12-05 | 天津大学 | In-tower reactive distillation and membrane coupling process method and device for producing ethyl levulinate |
CN114212941A (en) * | 2021-12-21 | 2022-03-22 | 江苏三吉利化工股份有限公司 | System and method for recovering MOE (metal oxide organic ether) in ethylene glycol monomethyl ether wastewater |
CN116332836A (en) * | 2022-07-28 | 2023-06-27 | 四川熔增环保科技有限公司 | Method for recovering pyridine waste solvent |
CN116332836B (en) * | 2022-07-28 | 2024-03-26 | 四川熔增环保科技有限公司 | Method for recovering pyridine waste solvent |
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