CN109096066A - A kind of method and device removed and recycle butyl glycol ether in coating waste-water - Google Patents
A kind of method and device removed and recycle butyl glycol ether in coating waste-water Download PDFInfo
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- CN109096066A CN109096066A CN201811152263.9A CN201811152263A CN109096066A CN 109096066 A CN109096066 A CN 109096066A CN 201811152263 A CN201811152263 A CN 201811152263A CN 109096066 A CN109096066 A CN 109096066A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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Abstract
The present invention provides a kind of method and devices removed and recycle butyl glycol ether in coating waste-water, include the following steps: step 1: waste water raw material carries out rectifying after preheating, the overhead fraction that rectifying obtains cools to 60-90 DEG C and obtains condensate liquid, obtained condensate liquid is stood, split-phase, temperature remains 60 DEG C or more in phase separation tank in phase process, and the recombination after rectifying is divided into the waste water without butyl glycol ether；Step 2: light phase component is high concentration butyl glycol ether, and heavy phase component returns to rectifying column and carries out rectifying.The present invention overcome in the prior art coating waste-water processing difficulty is big, less economical and processing when destroy butyl glycol ether structure, the problems such as solvent recovery purity and the rate of recovery is low, removed under conditions of relatively loose simple, low energy consumption and recycle butyl glycol ether in waste water.
Description
Technical field
The invention belongs to coating industry field of waste water treatment, more particularly, to a kind of removing and recycle second two in coating waste-water
The method and device of alcohol butyl ether.
Background technique
Butyl glycol ether, 171.1 DEG C of boiling point, colourless flammable liquid can be with arbitrary proportion and water, acetone, benzene, four chlorinations
Carbon, ethyl alcohol and normal heptane are miscible.Since it is with excellent solubility property, thus it is widely used in paint, ink, metal cleaning
Agent and dye dispersant field are mainly used as the solvent of nitrocellulose, spray painting, quick-drying paint, varnish, enamel and paint stripper and change
Into the secondary solvent of emulsifiability.
Often inevitably containing the butyl glycol ether of low concentration in the waste water that above-mentioned industry generates, waste water is directly arranged
Very big pollution can not only be caused to environment by putting, but also will cause the loss of butyl glycol ether material.Existing processing method is to add thereto
Selectable solvent azeotropic distillation, tower top obtain the azeotropic mixture of selective solvent and water, and tower reactor obtains high-purity butyl glycol ether.But
The method energy consumption is high, the butyl glycol ether amount of recycling is few, does not have economy.Chinese patent 201510427215.6 mentions utilization
Nitric acid waste water aoxidizes butyl glycol ether waste water, realizes low energy consumption degradation, but the method can break butyl glycol ether structure
It is bad, it causes loss of material, and the method is restricted very big, can show acid in treated waste water, cause new pollution.
Summary of the invention
In view of this, a kind of the present invention is directed to propose method and dress removed and recycle butyl glycol ether in coating waste-water
Set, with overcome in the prior art coating waste-water processing difficulty it is big, it is less economical and processing when destroy butyl glycol ether structure,
The problems such as solvent recovery purity and the low rate of recovery, removes under conditions of relatively loose simple, low energy consumption and recycles second two in waste water
Alcohol butyl ether.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A method of it removes and recycles butyl glycol ether in coating waste-water, include the following steps:
Step 1: waste water raw material carries out rectifying after preheating, and the overhead fraction that rectifying obtains cools to 60-90 DEG C and obtains
Condensate liquid is stood obtained condensate liquid, split-phase, and temperature remains 60 DEG C or more in phase separation tank in phase process, essence
Recombination after evaporating is divided into the waste water without butyl glycol ether；
Step 2: light phase component is high concentration butyl glycol ether, and heavy phase component returns to rectifying column and carries out rectifying.
Further, distillation process operates under normal pressure or micro-positive pressure.
Further, the concentration of butyl glycol ether is less than or equal to 10% in waste water raw material.
The present invention also provides a kind of removing and the device of butyl glycol ether in coating waste-water is recycled, including rectifying column, cold
Condenser and split-phase return tank, the tower top of rectifying column are tower discharge port, and tower body is provided with tower feed inlet and tower refluxing opening, in condenser
Including two pipelines, material is entered in rectifying column after the first pipeline of condenser by tower feed inlet, and tower discharge port connects
The second pipeline of condenser is connect, the tank import of split-phase return tank is then connected, split-phase return tank includes that tank import, heavy constituent tank go out
Mouth and the outlet of light component tank, the outlet of heavy constituent tank are connect with tower refluxing opening.Rectifying column can use plate column or packed tower.
Further, the both ends of the first pipeline of condenser are respectively the first condenser inlet and the first condensator outlet,
The both ends of second pipeline of condenser are respectively the second condenser inlet and the second condensator outlet, and raw material passes through the first condenser
Import enters condenser, enters rectifying column after then reaching tower feed inlet from the first condensator outlet；Tower discharge port and second cold
Condenser import is connected, and the second condensator outlet is connected with the tank import of split-phase return tank.
Further, tank import is located at the top of split-phase return tank, and the outlet of heavy constituent tank and the outlet of light component tank, which are located at, to be divided
The bottom of phase return tank, and it is provided with demarcation plate between the outlet of heavy constituent tank and the outlet of light component tank, the height of demarcation plate is lower than
Split-phase return tank vertical direction height, tank import be located in the vertical direction demarcation plate be provided with heavy constituent tank outlet one
Side.
Further, the tower bottom of rectifying column is provided with tower bottom outlet and tower bottom reboiler.Tower bottom reboiler can be pressure
Recycle reboiler or thermosiphon reboiler.
Further, reflux pump is provided between the outlet of heavy constituent tank and tower refluxing opening.Raw material is delivered to by feed pump
Condenser.Feed pump and reflux pump use peristaltic pump, and peristaltic pump is capable of providing the charging of regime flow, flowed fluctuation is avoided to make essence
Vapor liquid equilibrium in tower is evaporated to be destroyed.Tower body, pipeline and the split-phase return tank of rectifying column should be carried out using polyurethane thermal pipe
Heat preservation.
Further, tail condenser is provided between condenser and split-phase return tank.
Butyl glycol ether content in waste water raw material should be less than being equal to 10%, and waste water raw material passes through the cooling medium of condenser
Be pumped into rectifying column from the tower feed inlet in tower after the preheating of channel and carry out rectifying, the mixed fraction of overhead extraction through the second condenser into
Mouth enters condensation in condenser, and, to 60-90 DEG C, the condensate liquid obtained from the second condenser inlet is produced to split-phase return tank,
Split-phase is stood in split-phase return tank, temperature remains 60 DEG C or more in split-phase return tank in phase process, heavy phase group lease making
The outlet of heavy constituent tank, which is left, returns rectifying column through reflux pump after split-phase return tank and flows back, the butyl glycol ether containing high concentration it is light
Phase component is exported from light component tank and is produced, and rectifying column extraction is free of the waste water of butyl glycol ether.Rectifying column is in normal pressure or micro-positive pressure
Lower progress azeotropic distillation operation.
The heavy phase component that split-phase return tank obtains need to be all pumped into the tower feed inlet of rectifying column as phegma.Rectifying column
Tower bottom outlet waste water in butyl glycol ether content in 100ppm or less.It is produced in the light component tank outlet of split-phase return tank
The content of butyl glycol ether is 50-80% in light phase component.
Compared with the existing technology, the method and device of the present invention removed and recycle butyl glycol ether in coating waste-water
It has the advantage that
(1) present invention proposes the completely new removing of one kind and recycles the device of butyl glycol ether in coating waste-water, makes low concentration
The process that butyl glycol ether waste water takes off butyl glycol ether is simply loose, and easy to operate, low energy consumption, and solvent removal rate is high, zero-emission is useless
Evaporated quantity of water is small, being capable of long period continuous and stable production；
(2) there is the special of split-phase at 60 DEG C or more using the butyl glycol ether aqueous solution in azeotropic composition in the present invention
Property, ingehious design split-phase return tank make overhead fraction carry out split-phase in split-phase return tank, by the second two of low concentration in waste water
It recycles to obtain high concentration butyl glycol ether while alcohol butyl ether efficient removal；
(3) present invention preheats waste water raw material using condenser preheating technology, avoids because caused by raw material preheating
Heat consumption, the wastewater flow rate that in addition present invention is evaporated is small, and the mode of operation of heavy phase reflux avoids high concentration ethylene glycol monomethyl ether ginseng
The case where causing energy consumption to increase with reflux appearance.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for removing and recycling the device of butyl glycol ether in coating waste-water.
1- rectifying column；101- tower discharge port；102- tower feed inlet；103- tower refluxing opening；The outlet of 104- tower bottom；105- tower bottom
Reboiler；2- condenser；The first condenser inlet of 201-；The first condensator outlet of 202-；The second condenser inlet of 203-；204-
Second condensator outlet；3- split-phase return tank；301- tank import；The outlet of 302- heavy constituent tank；The outlet of 303- light component tank；304-
Demarcation plate；4- tail condenser.
Specific embodiment
In addition to being defined, technical term used in following embodiment has universal with those skilled in the art of the invention
The identical meanings of understanding.Test reagent used in following embodiment is unless otherwise specified conventional biochemical reagent；It is described
Experimental method is unless otherwise specified conventional method.
Below with reference to examples and drawings 1, the present invention will be described in detail.
A kind of device removed and recycle butyl glycol ether in coating waste-water, including rectifying column 1, condenser 2 and split-phase are returned
Flow tank 3, the tower top of rectifying column 1 is tower discharge port 101, and tower body is provided with tower feed inlet 102 and tower refluxing opening 103, in condenser 2
Including two pipelines, material is entered in rectifying column 1 after the first pipeline of condenser 2 by tower feed inlet 102, tower discharging
Mouthfuls 101 connect the second pipeline of condensers 2, then connect the tank import 301 of split-phase return tank 3, split-phase return tank 3 include tank into
Mouth 301, heavy constituent tank outlet 302 and light component tank outlet 303, heavy constituent tank outlet 302 are connect with tower refluxing opening 103.Condensation
The both ends of first pipeline of device 2 are respectively the first condenser inlet 201 and the first condensator outlet 202, the second pipe of condenser 2
The both ends on road are respectively the second condenser inlet 203 and the second condensator outlet 204, and raw material passes through the first condenser inlet 201
Into condenser 2, enter rectifying column 1 after then reaching tower feed inlet 102 from the first condensator outlet 202；Tower discharge port 101 with
Second condenser inlet 203 is connected, and the second condensator outlet 204 is connected with the tank import 301 of split-phase return tank 3.Tank import 301
Positioned at the top of split-phase return tank 3, heavy constituent tank outlet 302 and light component tank export 303 bottoms for being located at split-phase return tank 3,
And demarcation plate 304 is provided between heavy constituent tank outlet 302 and light component tank outlet 303, the height of demarcation plate 304 is lower than split-phase
Return tank 3 is in the height of vertical direction, and tank import 301 is in the vertical direction positioned at demarcation plate 304 provided with the outlet of heavy constituent tank
302 side.
Waste water raw material flows out after the first condenser inlet 201 of condenser 3 enters through the first condensator outlet 202 cold
Condenser 3, then by tower feed inlet 102 enter in rectifying column 1 to liquid level be rectifying column 1 the total liquid level of tower reactor 2/3 when stop
It only feeds, is passed through heat medium in reboiler 105, normal pressure azeotropic distillation, the material in rectifying column 1 after rectifying, adopt by tower top
Mixed fraction out is condensed through condenser 2 and the condensation of tail condenser 4 is to 60-90 DEG C, and condensate liquid is produced to split-phase return tank 3
Interior, temperature remains at 60 DEG C or more in split-phase return tank 3, and mixed fraction split-phase in split-phase return tank 3, heavy phase fraction passes through
Reflux pump is back in rectifying column 1, and light phase fraction exports 104 from tower bottom from the waste water after 303 extraction of light component tank outlet, precipitation
Extraction.
Tail condenser 4 is provided between above-mentioned condenser 2 and split-phase return tank 3.Since heat exchange occurring in condenser 2
In the process the cooling of the mixed fraction of overhead extraction is not enough to reach predetermined value, it is therefore desirable to enter split-phase return tank 3
Cool down again before.
Waste water raw material used by following embodiment and comparative example is all from Sichuan paint company, each group in waste water raw material
Point content (mass fraction) is respectively as follows: water 89.82%, butyl glycol ether 10.08%, other impurity 0.1%.Following embodiment is equal
Using the device of the present invention removed and recycle butyl glycol ether in coating waste-water.The inspection that raw material, fraction and kettle liquid use
Surveying device is FL9790II type gas chromatograph, and nonpolar 60m capillary column, measuring method is using internal standard method.
Comparative example 1
Diameter 30mm is selected, high 1.5m glass rectifying column 1 is tested, and 2L tower reactor is pumped into raw material 1500ml, tail condenser 4
Cooling medium channel in be passed through room temperature cycles water, heat medium, atmospheric distillation, the kettle temperature of rectifying column 1 are passed through in reboiler 105
It is 100.1 DEG C, 96.2 DEG C of tower top temperature, reflux ratio 50, split-phase return tank 3 produces fraction 48ml, and fraction is not stratified, detects light phase
The content of middle butyl glycol ether is 15.11%, after producing fraction 40%, detects butyl glycol ether in the kettle liquid of rectifying column and remains
6.56%.
Embodiment 1
Diameter 30mm is selected, high 1.5m glass rectifying column is tested, and 2L tower reactor is pumped into raw material 1500ml, tail condenser 4
Cooling medium channel in be passed through 60 DEG C of hot water, heat medium, atmospheric distillation, the tower reactor temperature of rectifying column 1 are passed through in reboiler 105
100.1 DEG C of degree, 96.2 DEG C of tower top temperature, fraction split-phase in split-phase return tank 3, heavy phase returns to 1 tower reactor of rectifying column, split-phase volume
Than light phase: heavy phase=1:3, the content for detecting butyl glycol ether in light phase is 58.6%, when producing light phase fraction about 20%, detection
Butyl glycol ether residual quantity 32ppm in kettle liquid.
Embodiment 2
Diameter 30mm is selected, high 1.5m glass rectifying column is tested, and 2L tower reactor is pumped into raw material 1500ml, tail condenser 4
Cooling medium channel in be passed through 80 DEG C of hot water, heat medium, atmospheric distillation, the tower reactor temperature of rectifying column 1 are passed through in reboiler 105
100.0 DEG C of degree, 96.1 DEG C of tower top temperature, fraction split-phase in split-phase return tank 3, heavy phase returns to 1 tower reactor of rectifying column, split-phase volume
Than light phase: heavy phase=1:3.5, the content for detecting butyl glycol ether in light phase is 66.8%, when producing light phase fraction about 15%, inspection
Survey butyl glycol ether residual quantity 47ppm in kettle liquid.
Embodiment 3
Diameter 30mm is selected, high 1.5m glass rectifying column is tested, and 2L tower reactor is pumped into raw material 1500ml, tail condenser 4
Cooling medium channel in be passed through 90 DEG C of hot water, heat medium, atmospheric distillation, the tower reactor temperature of rectifying column 1 are passed through in reboiler 105
100.0 DEG C of degree, 96.1 DEG C of tower top temperature, fraction split-phase in split-phase return tank 3, heavy phase returns to 1 tower reactor of rectifying column, split-phase volume
Than light phase: heavy phase=1:4, the content for detecting butyl glycol ether in light phase is 74.3%, when producing light phase fraction about 15%, detection
Butyl glycol ether residual quantity 13ppm in kettle liquid.
Embodiment 4
Diameter 80mm is selected, high 1.5m glass rectifying column is tested, and 2L tower reactor is pumped into raw material 1500ml, tail condenser 4
Cooling medium channel in be passed through 90 DEG C of hot water, heat medium, atmospheric distillation, the tower reactor temperature of rectifying column 1 are passed through in reboiler 105
100.0 DEG C of degree, 96.1 DEG C of tower top temperature, fraction split-phase in split-phase return tank 3, heavy phase returns to 1 tower reactor of rectifying column, split-phase volume
Than light phase: heavy phase=1:4, the content for detecting butyl glycol ether in light phase is 76.6%, when producing light phase fraction about 15%, detection
Butyl glycol ether residual quantity 11ppm in kettle liquid.
As can be seen from the above-described embodiment, by using atmospheric distillation, the method for split-phase extraction can will be in waste water raw material
Butyl glycol ether content is reduced to 100ppm level below, while tower top obtains the high concentration butyl glycol ether of 50-80% and evaporates
Point, not only solved the problems, such as because in waste water containing butyl glycol ether due to the pollution environment that occurs, but also can be efficient by butyl glycol ether
Recycling.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of removing and the method for recycling butyl glycol ether in coating waste-water, characterized by the following steps:
Step 1: waste water raw material carries out rectifying after preheating, and the overhead fraction that rectifying obtains cools to 60-90 DEG C and condensed
Liquid is stood obtained condensate liquid, split-phase, and temperature remains 60 DEG C or more, after rectifying in phase separation tank in phase process
Recombination be divided into the waste water without butyl glycol ether；
Step 2: light phase component is high concentration butyl glycol ether, and heavy phase component returns to rectifying column and carries out rectifying.
2. removing according to claim 1 and the method for recycling butyl glycol ether in coating waste-water, it is characterised in that: rectifying
Process operates under normal pressure or micro-positive pressure.
3. removing according to claim 1 and the method for recycling butyl glycol ether in coating waste-water, it is characterised in that: waste water
The concentration of butyl glycol ether is less than or equal to 10% in raw material.
4. a kind of removing and the device for recycling butyl glycol ether in coating waste-water, it is characterised in that: including rectifying column (1), condensation
Device (2) and split-phase return tank (3), the tower top of rectifying column (1) are tower discharge port (101), tower body be provided with tower feed inlet (102) and
Tower refluxing opening (103), interior condenser (2) includes two pipelines, and material passes through tower after the first pipeline of condenser (2) and feeds
Mouth (102) enters in rectifying column (1), and tower discharge port (101) connects second pipeline of condenser (2), then connects split-phase and returns
The tank import (301) of tank (3) is flowed, split-phase return tank (3) includes tank import (301), heavy constituent tank outlet (302) and light component tank
It exports (303), heavy constituent tank outlet (302) is connect with tower refluxing opening (103).
5. removing according to claim 4 and the device for recycling butyl glycol ether in coating waste-water, it is characterised in that: condensation
The both ends of first pipeline of device (2) are respectively the first condenser inlet (201) and the first condensator outlet (202), condenser (2)
The both ends of the second pipeline be respectively the second condenser inlet (203) and the second condensator outlet (204), raw material is cold by first
Condenser import (201) enters condenser (2), then reaches tower feed inlet (102) from the first condensator outlet (202) and enters essence afterwards
Evaporate tower (1)；Tower discharge port (101) is connected with the second condenser inlet (203), and the second condensator outlet (204) and split-phase flow back
The tank import (301) of tank (3) is connected.
6. removing according to claim 4 simultaneously recycles the device of butyl glycol ether in coating waste-water, it is characterised in that: tank into
Mouth (301) is located at the top of split-phase return tank (3), and heavy constituent tank exports (302) and light component tank outlet (303) is returned positioned at split-phase
The bottom of tank (3) is flowed, and is provided with demarcation plate (304) between heavy constituent tank outlet (302) and light component tank outlet (303), point
The height of partition (304) is lower than split-phase return tank (3) in the height of vertical direction, and tank import (301) is located in the vertical direction
Demarcation plate (304) is provided with the side of heavy constituent tank outlet (302).
7. removing according to claim 4 and the device for recycling butyl glycol ether in coating waste-water, it is characterised in that: rectifying
The tower bottom of tower (1) is provided with tower bottom outlet (104) and tower bottom reboiler (105).
8. removing according to claim 4 and the device for recycling butyl glycol ether in coating waste-water, it is characterised in that: recombination
Divide between tank outlet (302) and tower refluxing opening (103) and is provided with reflux pump.
9. removing according to claim 4 and the device for recycling butyl glycol ether in coating waste-water, it is characterised in that: condensation
Tail condenser (4) are provided between device (2) and split-phase return tank (3).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811152263.9A CN109096066B (en) | 2018-09-29 | 2018-09-29 | Method and device for removing and recycling ethylene glycol butyl ether in coating wastewater |
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|---|---|---|---|
| CN201811152263.9A CN109096066B (en) | 2018-09-29 | 2018-09-29 | Method and device for removing and recycling ethylene glycol butyl ether in coating wastewater |
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| CN109096066B CN109096066B (en) | 2021-07-30 |
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