CN106698574A - Continuous emulsion liquid membrane extraction device and recovery process of epichlorohydrin wastewater - Google Patents
Continuous emulsion liquid membrane extraction device and recovery process of epichlorohydrin wastewater Download PDFInfo
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- CN106698574A CN106698574A CN201611247081.0A CN201611247081A CN106698574A CN 106698574 A CN106698574 A CN 106698574A CN 201611247081 A CN201611247081 A CN 201611247081A CN 106698574 A CN106698574 A CN 106698574A
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- emulsion
- waste water
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
Abstract
The invention relates to a continuous emulsion liquid membrane extraction device and a recovery process of epichlorohydrin wastewater, and belongs to the technical field of water treatment. An integrated treatment process is adopted, the epichlorohydrin wastewater is treated, pre-extraction is mainly carried out through an emulsion liquid membrane, micropores of a porous ceramic filter penetrate through a chloride solution to obtain a purified salt solution, and the extracted emulsion is subjected to vacuum distillation after being demulsified to obtain a solvent. The solvent can be recycled to prepare an emulsion and the continuity of the whole process is achieved.
Description
Technical field
The present invention relates to a kind of continous way emulsion liquid film extraction equipment and the recovery process of epoxychloropropane waste water, belong to
Water-treatment technology field.
Background technology
Epoxychloropropane is a kind of important Organic Chemicals and fine chemical product, and purposes is quite varied, main to use
In production epoxy resin, synthetic glycerine, chlorohydrin rubber, nitroglycerine, fiberglass, electric insulation product.Additionally, epoxy chloropropionate
Alkane can be additionally used in synthesis nitroglycerine, fiberglass, electric insulation product, surfactant, medicine, agricultural chemicals, coating, sizing material, from
The multiple products such as sub-exchange resin, plasticizer, glycidyl derivatives, chlorohydrin rubber, as cellulose esters, resin, cellulose
The solvent of ether, for producing chemical stabilizer, chemical dyestuff and water treatment agent etc..
Glycerine legal system epoxychloropropane technology is long-standing, is in the past to be limited not obtain significant progress by cost, closely
Because crude oil price skyrockets high over year, various countries greatly develop Biodiesel, and a large amount of biological glycerols of by-product (are accounted for therewith
Biodiesel amount 1/10), cause glycerol market superfluous, price drops all the way；And the global epoxychloropropane of another aspect is very
In short supply, under this background, glycerine legal system epoxychloropropane just obtains new life.Glycerine method primary raw material is glycerine, chlorine
Change hydrogen, catalyst and quick lime.Technical process mainly includes following two reaction members：One hydrochlorination unit, two
Milk of lime saponification unit, other also have lime slaking, intermediate and product purification unit.
The characteristics of glycerine method is flexible production process, reacting balance, safe operation stabilization, low in raw material price, reduced investment；
Have the disadvantage because development time is shorter, be not also technically highly developed, be still significantly improved space.With the requirement of environmental protection
Increasingly stricter, it is imperative to strictly regulate treatment waste water, glycerine method saponification waste-water saliferous is high, containing organic matter is more miscellaneous, COD compared with
High, biodegradability is poor, is very difficult to direct biochemistry, and what is had goes biochemical treatment, it is necessary to waste substantial amounts of clear water, economy through dilution
It is poor.Some use multiple-effect evaporations produce calcium chloride, and the waste water for distilling out goes biochemical treatment.It is difficult that above method all has treatment
The big problem of degree.
The content of the invention
Present invention employs a kind of handling process of integrated form, epoxychloropropane waste water is processed, mainly passed through
Emulsion liquid film carries out pre-extracted, and during extraction is carried out, the micropore using porous ceramic filter is molten by chloride therein
Liquid is passed through, and obtains salting liquid after purification, and the emulsion after extracting is again by after demulsification, solvent being obtained by vacuum distillation, molten
Agent can be back to preparation emulsion, realize the continuity of overall process.
The recovery process of epoxychloropropane waste water, comprises the following steps：
1st step, prepares emulsion liquid film：Surfactant is dissolved in membrane solvent, and adds carrier, film auxiliary agent and salting liquid
Interior phase liquid, high-speed stirred emulsification is obtained WO emulsion film after mixing；
2nd step, extraction：By WO emulsion film and epoxychloropropane waste water according to volume ratio 1：10~20 feed to tubular type
In the passage of porous ceramic filter, after cross-flow filtration, saline solns ooze out from tube wall, and organic impurities enters liquid film；
3rd step, the WO emulsion film of multichannel opposite side discharge carries out demulsification treatment；
4th step, is layered in the feed liquid feeding layering tank after demulsification treatment, obtains water phase and oil phase；
5th step, vacuum distillation is carried out by oil phase feeding vacuum distillation kettle, steams octanol and kerosene, is back to emulsifying kettle reuse.
In the 1st described step, surfactant be selected from Span40, Span60, Span65 or Span80 in one kind or
Several mixing；Described membrane solvent is kerosene；Carrier is tri-n-octyl amine；Described film auxiliary agent is selected from octanol；Phase in salting liquid
Liquid refers to NaCl or KCl solution of the concentration in 15~35wt%, more preferably 25~30wt%；High-speed stirred refers to speed of agitator
In 2000~2500rpm.
In the 1st described step, the weight ratio in surfactant, membrane solvent, carrier, film auxiliary agent, salting liquid between phase liquid
Scope is 1：100~120：80~90：6~12：10~15.
In the 2nd described step, flow velocity of the mixed liquor in the passage of tubular porous ceramic filter 2 is 0.1~0.5m/
S, feed pressure is 0.1~0.5bar.
The material of described tubular ceramic filter is the one kind in aluminum oxide, zirconium oxide or titanium oxide；Tubular ceramic
The surface of filter is processed by silane coupler；The average pore size scope of tubular ceramic filter is 20~50 μm.
In the 3rd described step, described demulsification refers to the demulsification of high-pressure electrostatic method, and voltage range is 150~300V.
In the 4th described step, water is mutually back to emulsifying kettle.
In the 5th described step, the pressure limit of vacuum distillation is absolute pressure 100pa~200pa, and temperature is 50~65 DEG C.
A kind of continous way emulsion liquid film extraction equipment, includes：
Emulsifying kettle, for preparing WO emulsion film；
Waste water tank, for storing epoxychloropropane waste water；
Emulsifying kettle and waste water tank are all connected with one end passage of tubular ceramic filter；
The per-meate side of tubular ceramic filter is connected with purification brine tank；
The other end passage of tubular ceramic filter is connected with emulsion breaker, and emulsion breaker is processed for demulsification；
Emulsion breaker is connected with layering tank, and the oil phase outlet for being layered tank is connected with vacuum distillation kettle；
The top exit of vacuum distillation kettle is connected with emulsifying kettle.
Surfactant is additionally provided with emulsifying kettle and carrier adds tank.
Described emulsion breaker refers to high-voltage electrostatic demulsifying device.
Layering tank water is mutually exported and is connected with emulsifying kettle.
The material of described tubular ceramic filter is the one kind in aluminum oxide, zirconium oxide or titanium oxide；Tubular ceramic
The surface of filter is processed by silane coupler；The average pore size scope of tubular ceramic filter is 20~50 μm.
Brief description of the drawings
Fig. 1 is the structure chart that the continous way that the present invention is provided processes epoxychloropropane waste plant；
Wherein, 1, emulsifying kettle；2nd, tubular ceramic filter；3rd, emulsion breaker；4th, it is layered tank；5th, surfactant and carrier are added
Tank；6th, waste water tank；7th, brine tank is purified；8th, vacuum distillation kettle.
Specific embodiment
The manageable waste water of method provided by the present invention is suitable for the waste water produced by saponifying process glycerine method.It is useless
Main composition in water is：Inorganic salt content（Mainly NaCl and/or CaCl2）1500~8000mg/L of 15~25%, COD, gives up
The ester generated containing more glycerine, chlorine-containing compound and by alcohols and organic acid in water；More than chlorine-containing compound can be with
It is glycerin chlorohydrin alcohol, dichlorohydrin, epoxychloropropane and trichloropropane etc., the concentration of salt is high in the waste water of the method, COD contents
It is high.
Present invention employs a kind of handling process of integrated form, epoxychloropropane waste water is processed, mainly passed through
Emulsion liquid film carries out pre-extracted, and during extraction is carried out, the micropore using porous ceramic filter is molten by chloride therein
Liquid is passed through, and obtains salting liquid after purification, and the emulsion after extracting is again by after demulsification, solvent being obtained by vacuum distillation, molten
Agent can be back to preparation emulsion, realize the continuity of overall process.
In addition, key problem in technology of the invention is the mass concentration of phase liquid in salting liquid, it is necessary to using the chlorination of high concentration
Thing salt, and under a high concentration condition, prevent the salinity in epoxychloropropane waste water from penetrating emulsion film layer, and keep film
The integrality of layer.Because the oil droplet of emulsion is smaller, it is necessary to pass through the ethanol solution of Silane coupling agent KH550, KH570 etc. to table
Face carries out silicic acid anhydride, prevents oil droplet from entering to per-meate side through porous ceramic filter.Its processing method can be contained
There is the ethanol solution of 5~10% silane couplers by more than porous ceramic filter immersion treatment 20h, then dry after cleaning.
Handled wastewater source is in glycerine method production process in following examples, wherein containing CaCl2About 13%, COD models
About 9963 mg/L are enclosed, a certain amount of fixed sediment is also contained in waste water, appearance color is faint yellow.
The detection method of composition is in waste water：
COD：Hash DR900 type COD multi-parameters.
CaCl2Content：Using titration measuring.
Embodiment 1
1st step, prepares emulsion liquid film：Surfactant Span65 is dissolved in membrane solvent, and adds carrier tri-n-octyl amine, film
The NaCl of phase liquid 25wt% in auxiliary agent kerosene and salting liquid, the emulsification of 2000~2500rpm high-speed stirreds is obtained Water-In-Oil after mixing
Type emulsion liquid film, wherein, the weight in surfactant, membrane solvent, carrier, film auxiliary agent, salting liquid between phase liquid is than scope
1：100：80：6：10；
2nd step, extraction：By WO emulsion film and epoxychloropropane waste water according to volume ratio 1：10 feed to tubular porous
In the passage of ceramic filter 2, flow velocity of the mixed liquor in the passage of tubular porous ceramic filter 2 is 0.1m/s, feed liquid
Pressure is 0.1bar, and after cross-flow filtration, saline solns ooze out from tube wall, and organic impurities enters liquid film；Described tubular type
The material of ceramic filter 2 is zirconium oxide；The surface of tubular ceramic filter 2 is processed by silane coupler, and step is：To contain
There is the ethanol solution of 5% silane coupler by porous ceramic filter immersion treatment 20h, then dry after cleaning；Tubular ceramic
The average pore size scope of filter 2 is 20 μm；
3rd step, the WO emulsion film of multichannel opposite side discharge carries out 150V high-pressure electrostatic methods demulsification treatment；
4th step, is layered in the feed liquid feeding layering tank after demulsification treatment, obtains water phase and oil phase；
5th step, vacuum distillation is carried out by oil phase feeding vacuum distillation kettle, and the pressure of vacuum distillation is absolute pressure 100pa, and temperature is 50
DEG C, octanol and kerosene are steamed, it is back to emulsifying kettle reuse.
Embodiment 2
1st step, prepares emulsion liquid film：Surfactant Span65 is dissolved in membrane solvent, and adds carrier tri-n-octyl amine, film
The NaCl of phase liquid 25wt% in auxiliary agent kerosene and salting liquid, the emulsification of 2500rpm high-speed stirreds is obtained water-in-oil type emulsus after mixing
Liquid film, wherein, the weight in surfactant, membrane solvent, carrier, film auxiliary agent, salting liquid between phase liquid is 1 than scope： 120：
90： 12： 15；
2nd step, extraction：By WO emulsion film and epoxychloropropane waste water according to volume ratio 1：20 chargings are more to tubular type
In the passage of hole ceramic filter 2, flow velocity of the mixed liquor in the passage of tubular porous ceramic filter 2 is 0.5m/s, material
Hydraulic coupling is 0.5bar, and after cross-flow filtration, saline solns ooze out from tube wall, and organic impurities enters liquid film；Described pipe
The material of formula ceramic filter 2 is zirconium oxide；The surface of tubular ceramic filter 2 is processed by silane coupler, and step is：Will
Ethanol solution containing 10% silane coupler is dried by porous ceramic filter immersion treatment 20h, then after cleaning；Tubular type
The average pore size scope of ceramic filter 2 is 50 μm；
3rd step, the WO emulsion film of multichannel opposite side discharge carries out 300V high-pressure electrostatic methods demulsification treatment；
4th step, is layered in the feed liquid feeding layering tank after demulsification treatment, obtains water phase and oil phase；
5th step, vacuum distillation is carried out by oil phase feeding vacuum distillation kettle, and the pressure of vacuum distillation is absolute pressure 200pa, and temperature is 65
DEG C, octanol and kerosene are steamed, it is back to emulsifying kettle reuse.
Embodiment 3
1st step, prepares emulsion liquid film：Surfactant Span65 is dissolved in membrane solvent, and adds carrier tri-n-octyl amine, film
The NaCl of phase liquid 25wt% in auxiliary agent kerosene and salting liquid, the emulsification of 2200rpm high-speed stirreds is obtained water-in-oil type emulsus after mixing
Liquid film, wherein, the weight in surfactant, membrane solvent, carrier, film auxiliary agent, salting liquid between phase liquid is 1 than scope：110：
85：7：12；
2nd step, extraction：By WO emulsion film and epoxychloropropane waste water according to volume ratio 1：15 feed to tubular porous
In the passage of ceramic filter 2, flow velocity of the mixed liquor in the passage of tubular porous ceramic filter 2 is 0.3m/s, feed liquid
Pressure is 0.3bar, and after cross-flow filtration, saline solns ooze out from tube wall, and organic impurities enters liquid film；Described tubular type
The material of ceramic filter 2 is zirconium oxide；The surface of tubular ceramic filter 2 is processed by silane coupler, and step is：To contain
There is the ethanol solution of 7% silane coupler by porous ceramic filter immersion treatment 20h, then dry after cleaning；Tubular ceramic
The average pore size scope of filter 2 is 30 μm；
3rd step, the WO emulsion film of multichannel opposite side discharge carries out 200V high-pressure electrostatic methods demulsification treatment；
4th step, is layered in the feed liquid feeding layering tank after demulsification treatment, obtains water phase and oil phase；
5th step, vacuum distillation is carried out by oil phase feeding vacuum distillation kettle, and the pressure of vacuum distillation is absolute pressure 150pa, and temperature is 55
DEG C, octanol and kerosene are steamed, it is back to emulsifying kettle reuse.
Embodiment 4
Difference with embodiment 3 is：Porous ceramic filter is without surface hydrophobicity modification.
1st step, prepares emulsion liquid film：Surfactant Span65 is dissolved in membrane solvent, and adds carrier three just pungent
Amine, film auxiliary agent kerosene and in salting liquid phase liquid 25wt% NaCl, after mixing 2200rpm high-speed stirreds emulsification be obtained Water-In-Oil
Type emulsion liquid film, wherein, the weight in surfactant, membrane solvent, carrier, film auxiliary agent, salting liquid between phase liquid is than scope
1：110：85：7：12；
2nd step, extraction：By WO emulsion film and epoxychloropropane waste water according to volume ratio 1：15 feed to tubular porous
In the passage of ceramic filter 2, flow velocity of the mixed liquor in the passage of tubular porous ceramic filter 2 is 0.3m/s, feed liquid
Pressure is 0.3bar, and after cross-flow filtration, saline solns ooze out from tube wall, and organic impurities enters liquid film；Described tubular type
The material of ceramic filter 2 is zirconium oxide；The average pore size scope of tubular ceramic filter 2 is 30 μm；
3rd step, the WO emulsion film of multichannel opposite side discharge carries out 200V high-pressure electrostatic methods demulsification treatment；
4th step, is layered in the feed liquid feeding layering tank after demulsification treatment, obtains water phase and oil phase；
5th step, vacuum distillation is carried out by oil phase feeding vacuum distillation kettle, and the pressure of vacuum distillation is absolute pressure 150pa, and temperature is 55
DEG C, octanol and kerosene are steamed, it is back to emulsifying kettle reuse.
Reference examples 1
Difference with embodiment 3 is：The mass concentration of phase liquid is 5% in salting liquid.
Reference examples 2
Difference with embodiment 3 is：The mass concentration of phase liquid is 35% in salting liquid.
The purified water that the per-meate side of porous ceramic filter is obtained carries out water analysis, as a result as follows：
COD contents are low in the waste water after present invention treatment as can be seen from the table, and major part is absorbed by liquid film, can obtain purer
CaCl2Solution.Embodiment 3 is compared with embodiment 4 as can be seen that carrying out hydrophobic changing by the surface to porous ceramic filter
Property treatment, can prevent emulsus drip enter ceramic filter per-meate side, improve effluent quality；By reference examples and embodiment 3
Can effectively prevent CaCl2 from entering in drop compared to as can be seen that controlling the content of interior phase salting liquid, and prevent emulsion from breaking
Split.
Claims (10)
1. the recovery process of epoxychloropropane waste water, it is characterised in that comprise the following steps：
1st step, prepares emulsion liquid film：Surfactant is dissolved in membrane solvent, and adds carrier, film auxiliary agent and salting liquid
Interior phase liquid, high-speed stirred emulsification is obtained WO emulsion film after mixing；
2nd step, extraction：By WO emulsion film and epoxychloropropane waste water according to volume ratio 1：10~20 feed to tubular type
Porous ceramic filter（2）Passage in, after cross-flow filtration, saline solns ooze out from tube wall, and organic impurities enters liquid
Film；
3rd step, the WO emulsion film of multichannel opposite side discharge carries out demulsification treatment；
4th step, is layered in the feed liquid feeding layering tank after demulsification treatment, obtains water phase and oil phase；
5th step, vacuum distillation is carried out by oil phase feeding vacuum distillation kettle, steams octanol and kerosene, is back to emulsifying kettle reuse.
2. the recovery process of epoxychloropropane waste water according to claim 1, it is characterised in that in the 1st described step, table
Face activating agent is selected from the mixing of one or more in Span40, Span60, Span65 or Span80；Described membrane solvent is
Kerosene；Carrier is tri-n-octyl amine；Described film auxiliary agent is selected from octanol；Phase liquid refers to concentration 15~35wt%'s in salting liquid
NaCl or KCl solution, more preferably 25~30wt%；High-speed stirred refers to speed of agitator in 2000~2500rpm.
3. the recovery process of epoxychloropropane waste water according to claim 1, it is characterised in that in the 1st described step, table
Weight in face activating agent, membrane solvent, carrier, film auxiliary agent, salting liquid between phase liquid is 1 than scope：100~120：80~90：6
~12：10~15.
4. the recovery process of epoxychloropropane waste water according to claim 1, it is characterised in that in the 2nd described step, mixes
Feed liquid is closed in tubular porous ceramic filter（2）Passage in flow velocity be 0.1~0.5m/s, feed pressure is 0.1~
0.5bar。
5. the recovery process of epoxychloropropane waste water according to claim 1, it is characterised in that described tubular ceramic mistake
Filter（2）Material be one kind in aluminum oxide, zirconium oxide or titanium oxide；Tubular ceramic filter（2）Surface by silicon
Alkane coupling agent treatment；Tubular ceramic filter（2）Average pore size scope be 20~50 μm.
6. the recovery process of epoxychloropropane waste water according to claim 1, it is characterised in that in the 3rd described step, institute
The demulsification stated refers to the demulsification of high-pressure electrostatic method, and voltage range is 150~300V.
7. the recovery process of epoxychloropropane waste water according to claim 1, it is characterised in that in the 4th described step, water
Mutually it is back to emulsifying kettle；In the 5th described step, the pressure limit of vacuum distillation is absolute pressure 100pa~200pa, temperature is 50~
65℃。
8. a kind of continous way emulsion liquid film extraction equipment, it is characterised in that include：
Emulsifying kettle（1）, for preparing WO emulsion film；
Waste water tank（6）, for storing epoxychloropropane waste water；
Emulsifying kettle（1）With waste water tank（6）All with tubular ceramic filter（2）The connection of one end passage；
Tubular ceramic filter（2）Per-meate side with purification brine tank（7）Connection；
Tubular ceramic filter（2）Other end passage and emulsion breaker（3）Connection, emulsion breaker（3）For demulsification treatment；
Emulsion breaker（3）With layering tank（4）Connection, is layered tank（4）Oil phase outlet with vacuum distillation kettle（8）Connection；
Vacuum distillation kettle（8）Top exit and emulsifying kettle（1）Connection.
9. continous way emulsion liquid film extraction equipment according to claim 8, it is characterised in that emulsifying kettle（1）On also set up
There are surfactant and carrier to add tank（5）；Described emulsion breaker（3）It refer to high-voltage electrostatic demulsifying device；Layering tank（4）Water mutually goes out
Mouth and emulsifying kettle（1）Connection.
10. continous way emulsion liquid film extraction equipment according to claim 8, it is characterised in that described tubular ceramic mistake
Filter（2）Material be one kind in aluminum oxide, zirconium oxide or titanium oxide；Tubular ceramic filter（2）Surface by silicon
Alkane coupling agent treatment；Tubular ceramic filter（2）Average pore size scope be 20~50 μm.
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|---|---|---|---|
| CN201611247081.0A CN106698574B (en) | 2016-12-29 | 2016-12-29 | A kind of recovery process of continous way emulsion liquid film extraction equipment and epoxychloropropane waste water |
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|---|---|---|---|
| CN201611247081.0A CN106698574B (en) | 2016-12-29 | 2016-12-29 | A kind of recovery process of continous way emulsion liquid film extraction equipment and epoxychloropropane waste water |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058541A (en) * | 2014-07-15 | 2014-09-24 | 潍坊滨海石油化工有限公司 | Method for treating waste water produced in production of EDTA (ethylene diamine tetraacetic acid) |
| CN105858810A (en) * | 2016-04-12 | 2016-08-17 | 浙江丝科院轻纺材料有限公司 | Method for capturing dyes in dyeing wastewater through supported liquid membrane technology |
-
2016
- 2016-12-29 CN CN201611247081.0A patent/CN106698574B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104058541A (en) * | 2014-07-15 | 2014-09-24 | 潍坊滨海石油化工有限公司 | Method for treating waste water produced in production of EDTA (ethylene diamine tetraacetic acid) |
| CN105858810A (en) * | 2016-04-12 | 2016-08-17 | 浙江丝科院轻纺材料有限公司 | Method for capturing dyes in dyeing wastewater through supported liquid membrane technology |
Non-Patent Citations (1)
| Title |
|---|
| IWONA CICHOWSKA-KOPCZYNSKA等: "PREPARATION AND PHYSICOCHEMICAL CHARACTERISATION OF CERAMIC SUPPORTS FOR SUPORTED LIQUID MEMBRANES", 《PHYSICOCHEM. PROBL. MINER. PROCESS》 * |
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