CN103304005A - Method for removing phenol in phenol contained wastewater by using hollow fiber membrane - Google Patents
Method for removing phenol in phenol contained wastewater by using hollow fiber membrane Download PDFInfo
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Abstract
The invention discloses a method for removing phenol in phenol contained wastewater by using a hollow fiber membrane. The method comprises the following steps of: mixing a carrier and a diluent to prepare an extractant, wherein the adopted extractant carrier is tributyl phosphate, and the adopted diluent is coal oil or benzene; stirring and fully mixing the extractant and a stripping agent to prepare treating fluid; removing the phenol out of the phenol contained wastewater by using a hollow fiber membrane device; and after pretreating the hollow fiber membrane device, injecting the treating fluid into a tube pass of a membrane component, and injecting the phenol contained wastewater into a shell pass of the hollow fiber membrane component, wherein the wastewater can be treated through the same membrane component or a plurality of serial membrane components in a circular manner for many times; after the wastewater is subjected to two-stage treatment, the phenol concentration is less than 100mg/L; and after the wastewater is subjected to five-stage treatment, the phenol concentration is less than 5mg/L, the removal rate reaches up to 99.8 percent, and the wastewater reaches the national emission standard.
Description
Technical field
The present invention relates to a kind of Treatment of Phenol Containing Water, be specifically related to adopt the tubular fibre embrane method to remove the method for phenol in wastewater, belong to field of environment protection.
Background technology
Coke-oven plant, refinery, producer gas plant and in the phenol production process, all can discharge a large amount of phenolic wastewater.Phenolic wastewater harm is very large, and it can be invaded in the human body by contact, suction and the oral administration of skin, mucous membrane.Phenol and other phenols can produce supersensitivity to skin.The water that long-term drinking is polluted by aldehydes matter can cause dizziness, anaemia and various nervous system disorders.Phenolic wastewater can cause that the water fish class is dead and suppress the microorganism self-sow, with the direct irrigated farmland of undressed phenolic wastewater, can make the withered and underproduction of farm crop, the havoc ecotope.Therefore, China's industrial wastewater discharge standard code Phenols In Industrial Liquid Waste content must not be higher than 0.5mg/L.The harmless treatment of phenolic wastewater is one of indispensable process procedure of above-mentioned related industries.
The main methods of phenolic wastewater is as follows at present:
1. Physical: mainly comprise absorption method, steaming process and extraction process.Absorption method be utilize sorbent material porous character with the absorption of the aldehydes matter in the waste water, adsorb saturated after, recycle alkali lye, steam or organic solvent and separate adsorption desorption.This method shortcoming is that cost is high, the secondary pollution that the poor and easy generation of dephenolization effect the 3rd component is brought.Steaming process claims again vaporizing extract process, and when phenolic wastewater and the strong convection current of steam, phenol namely changes in the water vapour, thereby waste water is purified, and contains the steam of phenol to reclaim phenol with the sodium hydroxide washing again.This method dephenolize efficient is lower, and unstable, is eliminated gradually in recent years.Extraction process is widely used in the processing of phenolic wastewater and the recovery of phenol, and its shortcoming is easily to cause solvent loss, thereby makes solvent-oil ratio large, and causes secondary pollution.
2. chemical method: mainly contain chemical oxidization method, Wet Catalytic Oxidation Method and burning method etc.Chemical oxidization method is to add chemical oxidizing agent in water, and the phenolic compound in the waste water is oxidized to CO
2And water.Main drawback is that the little processing requirements that do not reach of oxygenant consumption, consumption greatly then consume greatly, and be uneconomical, therefore multiplex phenolic wastewater in processing lower concentration.Wet Catalytic Oxidation Method is to pass into air under high temperature, high pressure, makes the organism direct oxidation degraded in the waste water.This method is high to equipment requirements, and the loss of catalyzer is large.Burning method is that phenolic wastewater burns by oil fuel or mixed gas in incinerator.The method thermal losses is large, and aldehydes matter can not reclaim, and the consume of refractory masonry is large in the incinerator.
3. biological process: mainly comprise biomembrance process, activated sludge process etc.Biomembrance process is to utilize to be attached to the lip-deep microorganism mucous membrane of filtration medium in the biological filter and to process phenolic compound in the waste water.This method is had relatively high expectations to condition of water quality and the pre-treatment of water inlet, and because phenol organic matter is poisonous and the antibiont degradation property is arranged, treatment effect is undesirable.Activated sludge process is to utilize aerobic bacteria and other protozoon in the active sludge that phenolic compound in the water is carried out the adsorption and oxidation decomposition, and objectionable impurities is changed into stable innoxious substance.Main drawback is that water quality and the pre-treatment of intaking required height, and the operation spending is larger, and degradation time is long, and clearance is undesirable.
Above-mentioned various traditional treatment method is owing to being subject to the restriction of know-why, exist secondary pollution, waste water can't reuse or processing cost cross high defective.In recent years, the liquid film technology that combines solvent extraction and solid film partition method grows up gradually, has become one of effective way of processing this type of waste water.
Patent US4420643 provides a kind of method of extraction water Phenol in Aqueous Solution, and it selects the linear alkylbenzene that contains trioctyl phosphine oxide as extraction agent, can make the extracting phenols upper limit of concentration increase by 30% (massfraction).This invention adopt respectively the aqueous solution and organic phase one way and circulation, and stream and adverse current carry out, the ratio of water and oil phase is selected in 1: 30-30: 1, the result shows, trioctyl phosphine oxide so that the raising of straight chain type alkylbenzene effect of extracting.Alkylbenzene, isopropyl naphthalene, diisobutyl naphthalene are 0.5 in water-oil ratio, and trioctyl phosphine oxide exists in the situation effect of extracting very effective, and in addition, trioctyl phosphine oxide and straight chain type alkylbenzene steam than phenol boiling point Gao Kexian, and substantially water insoluble.Aqueous-phase concentration was 1.58% (containing trioctyl phosphine oxide 325g/L), and water-oil ratio is 7.5, under three stage countercurrent conditions phenol concentration was reduced to below the 5ppm.Phenol recovery is the method by straight run distillation from the straight chain type alkylbenzene.The advantage of this law is that extraction agent can be recycled.Shortcoming is that Distillation recovery phenol energy consumption is higher.
Patent CN200610018774.2 provides a kind of microemulsion that adopts to process the method that contains in the phenol trade effluent.This invention is mixed by oil phase and interior water, wherein oil phase is comprised of two-(2-ethylhexyl) phosphoric acid ester, sorbitan monooleate, kerosene 1: 0.5 in mass ratio～1.5: 4～6, interior water is basic solution, and the volume ratio of oil phase and interior water is 5: 2～3.Use the turntable extracting tower counter-current extraction, the one-level percentage extraction can reach more than 97%.If the employing multiple-stage treatment then needs the emulsion clarification, and 3 times system is newborn again to adopt the hydrochloric acid back extraction.There is the shortcoming that condensate film stability is poor, swelling ratio is higher except in the phenol process, is difficult to form stable microemulsion.
Document Amini.Study on a new surfactant for removal of phenol from wastewater by emulsion liquid membrane[J] .Journal of Hazardous Materials 2008, the people such as 582-588 report Hamid R.Mortaheb adopt gasoline, paraffin and toluene etc. as extraction agent, adopt Span80 as tensio-active agent, use the emulsion liquid membrane technology Phenol-Containing Wastewater Treatment, investigated operational condition, successful.But there are the problems such as swelling, liquid-sheet disintegration in the emulsion liquid membrane process, easily causes the separating effect forfeiture, and follow-up demulsification technology is complicated, is difficult to large-scale promotion.
In sum, adopt at present extracting process to remove the technology of phenol in the water all not satisfactory, need a kind of novel Treatment of Phenol Containing Water of exploitation badly, promote the realization of phenolic wastewater green treatment process.
Summary of the invention
The present invention proposes to adopt tubular fibre embrane method Phenol-Containing Wastewater Treatment in order to overcome the shortcoming of above-mentioned phenolic wastewater treatment process, this be a kind of more economically, the treatment process of environmental protection.
The method concrete steps are as follows:
A. with extraction agent carrier and mixing diluents preparation extraction agent, wherein the carrier bulk mark is 10～50%; The extraction agent carrier adopts tributyl phosphate, and thinner adopts kerosene or benzene; Extraction agent and reverse-extraction agent are fully stirred again and be mixed with treatment solution, wherein the volume fraction of extraction agent is 1-10%; Described reverse-extraction agent is that concentration is NaOH or the KOH aqueous solution of 0.1-1mol/L.
B. adopt hollow fiber membrane device that the phenol in the phenolic wastewater is removed, idiographic flow is: hollow fiber membrane device is carried out pre-treatment, extraction agent is filled with the tube side of membrane module, infiltrate half an hour, be full of extraction agent in the fenestra; The treatment solution of steps A preparation is injected the tube side of membrane module, phenolic wastewater is injected the shell side of membrane module, tube side, shell side volume flow ratio are 50: 1-1: 50, be preferably 10: 1-1: 20; Described tubular fibre mould material is hydrophobic class, such as polyvinylidene difluoride (PVDF), polyethylene, polypropylene; The hollow-fibre membrane internal diameter is 0.5～3.0mm, and external diameter is 0.6～4.0mm, and porosity is 30～80%, and the hollow fiber membrane device load factor is 0.1-0.6;
Pending phenolic wastewater phenol concentration is 500-5000mg/L, is 1.0-7.0 with the sulphur acid for adjusting pH value before entering hollow fiber membrane device, is preferably 4.0-6.0.
The used device schematic diagram of step B as shown in Figure 1, its core component is hollow fiber film assembly (1), membrane module (1) is comprised of hollow-fibre membrane and the housing of some amount, be tube side in the hollow fiber film tube, pipe is shell side outward; (7), (8) are respectively the tube side interface; (5), (6) are respectively the shell side interface.From Preparation tank (3), treatment solution is pumped into the membrane module tube side by interface (7) with pump (2), flow through behind the membrane module, flow out from interface (8), get back to Preparation tank (3), use simultaneously pump (2) that waste water is pumped into the membrane module shell side from interface (5), flow through behind the membrane module, flow out from interface (6), get back to storage tank (4).
Two strands of materials among the step B in tube side and the shell side can be taked adverse current, and stream or the operating method of cross-flow, phenol in the waste water is extracted in the treatment solution by the extraction agent in the fenestra, further with treatment solution in the alkali lye generation phenates that reacts, realize simultaneously the regeneration of extraction agent carrier.
In order to satisfy the processing requirements of different levels of emissions, phenolic wastewater can pass through multiple-stage treatment, and namely the mode by circulation makes the same membrane module of waste water Multiple through then out or processes by the membrane module of a plurality of series connection.Waste water through 2 grades of processing after phenol concentration be lower than 100mg/L, be lower than 5mg/L after 5 grades of processing, clearance is up to 99.8%, simultaneously enrichment phenol in the alkali lye.
Treatment solution is through behind the clarified separation, extraction agent and reverse-extraction agent phase-splitting, and extraction agent can recycle, and phenol is enriched in the back extraction mutually with the form of phenates, but the Pyrogentisinic Acid recycles.
Know-why of the present invention is: by add the organic phase extraction agent in a side liquid of film, make the film surface form one deck liquid film, utilize the characteristics of liquid film selective migration, the phenol in the waste water is constantly transmitted in treatment solution, thereby reach the purpose of removing phenol in wastewater.According to the characteristic of liquid film non-equilibrium mass transfer, phenol can be realized contrary concentration gradient migration: liquid film one side, and the phenol content continuous decrease in the waste water, ultimate density can reach actual requirement; Opposite side, phenol content continues to rise in the reverse-extraction agent, and ultimate density can be up to 40000mg/L.
Advantage of the present invention is: the extraction agent small droplets in (1) treatment solution can be constantly and the liquid film renewal that collides, and improved stability and the mass-transfer efficiency of liquid film process.When (2) adopting hollow-fibre membrane, can provide huge mass transfer area, and turndown ratio is large, the fluid flow rate of hollow-fibre membrane both sides can independently be regulated.(3) facility compact, volume is little, and is easy to amplify, and required function unit and interconnecting piece are few, and postprocessing working procedures is simple, so investment cost and process cost all can significantly reduce.(4) technical process is simple, non-secondary pollution, obvious environment benefit.(5) waste water after treatment, water resources can be used as diluting water and reclaim to use, and reclaims the recycling that liquid can be realized phenol after treatment.
Description of drawings
Fig. 1 is tubular fibre membrane water treatment device schematic diagram, wherein each sequence number representative: (1) hollow fiber film assembly; (2) reaching (2 ') is infusion pump; (3) treatment solution Preparation tank; (4) phenolic wastewater storage tank; (5) shell side interface; (6) shell side interface; (7) tube side interface; (8) tube side interface
Fig. 2 is embodiment 1 phenol in wastewater content and the graph of a relation of processing progression
Fig. 3 is embodiment 4 phenol in wastewater content and the graph of a relation in treatment time
Embodiment:
Below describe implementation process of the present invention and effect in detail by specific embodiment, but protection domain is not subjected to the restriction of embodiment.Adopt mutually middle phenol content of 4-AA Water by Ultraviolet Spectrophotometry among the embodiment.
Adopt device shown in Figure 1, wherein the useful length of used membrane contactor is 300mm, and internal diameter 10mm, tubular fibre mould material are PP, and inside and outside footpath is respectively 0.35mm, 0.45mm, and loading level is 100.
A. take tbp as carrier, take kerosene as mixing diluents the preparation extraction agent, wherein the volume fraction of carrier is 10%; NaOH solution 400ml take concentration as 1mol/L is reverse-extraction agent, is 1: 20 by extraction agent in the treatment solution and reverse-extraction agent volume ratio, and extraction agent and reverse-extraction agent two-phase are stirred.
B. treatment solution is inputted in the membrane module from tube side, the ingress flow is 50ml/min.With the phenolic wastewater 970mL simulation phenolic wastewater of about 400mg/L, use H
2SO
4Solution is regulated waste water acidity and is about pH4.5, and phenolic wastewater is inputted membrane module from shell side, and flow is 65ml/min.Two strands of logistics counter-current operations.
Phenol content changed as shown in Figure 2 with the processing time in the phenolic wastewater.As can be seen from Figure 2, the treatment time, approximately behind the 300min, clearance reached more than 90%, and the average mass transfer flux of whole treating processes is 1557mg/m
2H.
Adopt 1 condition among the embodiment, with two strands of logistics cocurrent cooling operations.
With the phenolic wastewater 1000mL simulation phenolic wastewater of about 500mg/L, use H
2SO
4Solution is regulated waste water acidity and is about pH4.5.Treatment time, approximately behind the 300min, clearance reached more than 90%, and the average mass transfer flux of whole treating processes is 1443mg/m
2H.
Adopt device among the embodiment 1, the material condition is constant, simulates phenolic wastewater with the about phenolic wastewater 1000mL of 400mg/L, uses H
2SO
4Solution is regulated waste water acidity and is about pH4.5.Change mass flow in tube side and the shell side, wherein treatment solution is in tube side input membrane module, and the ingress flow is 50ml/min; Phenolic wastewater is inputted membrane module from shell side, and flow is 100ml/min.Two strands of logistics counter-current operations.
Treatment time, approximately behind the 300min, clearance was 94%, and the average mass transfer flux of whole treating processes is 1898mg/m
2H.
Adopt the form of hollow fiber membrane device series connection, the membrane module useful length is 300mm in the hollow fiber membrane device that adopts, internal diameter 25mm; Mould material is polypropylene, and inside and outside footpath is respectively 0.35mm, 0.45mm, and loading level is 1000.
A. take tbp as carrier, take kerosene as mixing diluents the preparation extraction agent, wherein the volume fraction of carrier is 30%; NaOH solution 400ml take concentration as 2mol/L is reverse-extraction agent, is 1: 20 by extraction agent in the treatment solution and reverse-extraction agent volume ratio, extraction agent and reverse-extraction agent two-phase is made into treatment solution stirs.
B. adopt the mode of cascade extraction.In tube side input membrane module, the exit flow is 20ml/min with treatment solution.With the phenolic wastewater 2L simulation phenolic wastewater of about 2000mg/L, use H
2SO
4Solution is regulated waste water acidity and is about pH4.5, and phenolic wastewater is inputted membrane module from shell side, and realizes operate continuously, and flow is 100ml/min, and tube side, shell side throughput ratio are 1: 5.
Phenol content with the variation relation of processing progression as shown in Figure 2 in the phenolic wastewater.As seen from Figure 2, after 3 grades, feed liquid residence time in the film device only is about 3min, clearance can reach 99%, after 5 grades, phenol in wastewater concentration reaches standards for industrial water usage less than 5mg/L, and the waste water after 1 grade or 2 grades of processing just can be used for other technological process in the actual industrial treating processes, and the average mass transfer flux of whole treating processes is 4400mg/m
2H.
Claims (8)
1. method that adopts hollow-fibre membrane to remove phenol in the phenolic wastewater, concrete steps are as follows:
A. with extraction agent carrier and mixing diluents preparation extraction agent, wherein the carrier bulk mark is 10～50%; The extraction agent carrier adopts tbp, and thinner adopts kerosene or benzene; Extraction agent and reverse-extraction agent are fully stirred again and be mixed with treatment solution, wherein the volume fraction of extraction agent is 1-10%; Described reverse-extraction agent is that concentration is NaOH or the KOH aqueous solution of 0.1-1mol/L;
B. adopt hollow fiber membrane device that the phenol in the phenolic wastewater is removed, idiographic flow is: the tube side of tributyl phosphate being filled with membrane module, infiltrate half an hour, make to be full of tributyl phosphate in the fenestra, again the treatment solution of steps A preparation is injected the tube side of membrane module; Phenolic wastewater is injected the shell side of membrane module, tube side, shell side volume flow ratio are 50: 1-1: 50; Phenol in the waste water is extracted in the treatment solution by the tributyl phosphate in the fenestra, further with treatment solution in the alkali lye generation phenates that reacts, realize the regeneration of tributyl phosphate;
Described tubular fibre mould material is for being polyvinylidene difluoride (PVDF), polyethylene, polypropylene; The hollow-fibre membrane internal diameter is 0.5～3.0mm, and external diameter is 0.6～4.0mm, and porosity is 30～80%, and the load factor of hollow-fibre membrane in device is 0.1-0.6.
2. remove the method for phenol in the phenolic wastewater according to employing hollow-fibre membrane claimed in claim 1, the used device schematic diagram of step B as shown in Figure 1, its core component is hollow fiber film assembly (1), membrane module (1) is comprised of hollow-fibre membrane and the housing of some amount, be tube side in the hollow fiber film tube, pipe is outer to be shell side; (7), (8) are respectively the tube side interface; (5), (6) are respectively the shell side interface; Its technical process is from Preparation tank (3) treatment solution to be pumped into the membrane module tube side by interface (7) with pump (2), flow through behind the membrane module, flow out from interface (8), get back to Preparation tank (3), use simultaneously pump (2) that waste water is pumped into the membrane module shell side from interface (5), flow through behind the membrane module, flow out from interface (6), get back to storage tank (4).
3. employing hollow-fibre membrane according to claim 1 removes the method for phenol in the phenolic wastewater, it is characterized in that for pending phenolic wastewater phenol concentration is 500-5000ppm, before entering hollow fiber membrane device, will use first the sulphur acid for adjusting pH value to 1.0-7.0.
4. employing hollow-fibre membrane according to claim 1 removes the method for phenol in the phenolic wastewater, it is characterized in that tube side, shell side volume flow ratio are 10: 1-1: 20.
5. employing hollow-fibre membrane according to claim 1 removes the method for phenol in the phenolic wastewater, it is characterized in that pending phenolic wastewater phenol before entering hollow fiber membrane device with the sulphur acid for adjusting pH value to 4.0-6.0.
6. employing hollow-fibre membrane according to claim 1 removes the method for phenol in the phenolic wastewater, it is characterized in that step B treatment solution and the flow pattern of pending phenolic wastewater in contactor can for and stream, adverse current or cross-flow passes.
7. employing hollow-fibre membrane according to claim 1 removes the method for phenol in the phenolic wastewater, it is characterized in that present method can adopt single-pass operation to realize the batch processing of phenolic wastewater; Also can adopt operate continuously to process, namely by regular taking-up high density contain phenol treatment solution and processed waste water, and constantly replenish fresh treatment solution, waste water, realize operate continuously.
8. employing hollow-fibre membrane according to claim 1 removes the method for phenol in the phenolic wastewater, it is characterized in that adopting single film device to process, and also can process by a plurality of membrane contactor series and parallels.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106007199A (en) * | 2016-07-01 | 2016-10-12 | 博天环境工程（北京）有限公司 | Method for treating wastewater of rifampicin antibiotic washing section |
| CN106745443A (en) * | 2017-01-18 | 2017-05-31 | 赵俊博 | A kind of extracting process of low concentration of water sample extraction device to phenol in water quality |
| RU2680394C2 (en) * | 2017-06-07 | 2019-02-20 | Федеральное государственное казенное военное образовательное учреждение высшего образования "Военный учебно-научный центр Военно-воздушных сил "Военно-воздушная академия имени профессора Н.Е. Жуковского и Ю.А. Гагарина" (г. Воронеж) Министерства обороны Российской Федерации | Method for concentrating phloroglucine from aqueous solutions |
| CN109943482A (en) * | 2019-03-06 | 2019-06-28 | 泰州市惠利生物科技有限公司 | A method of extraction preparation r-4- chloro-3-hydroxyl ethyl butyrate is coupled using enzyme mebrane reactor |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106007199A (en) * | 2016-07-01 | 2016-10-12 | 博天环境工程（北京）有限公司 | Method for treating wastewater of rifampicin antibiotic washing section |
| CN106745443A (en) * | 2017-01-18 | 2017-05-31 | 赵俊博 | A kind of extracting process of low concentration of water sample extraction device to phenol in water quality |
| CN106745443B (en) * | 2017-01-18 | 2018-02-06 | 赵俊博 | A kind of extracting process of low concentration of water sample extraction device to phenol in water quality |
| RU2680394C2 (en) * | 2017-06-07 | 2019-02-20 | Федеральное государственное казенное военное образовательное учреждение высшего образования "Военный учебно-научный центр Военно-воздушных сил "Военно-воздушная академия имени профессора Н.Е. Жуковского и Ю.А. Гагарина" (г. Воронеж) Министерства обороны Российской Федерации | Method for concentrating phloroglucine from aqueous solutions |
| CN109943482A (en) * | 2019-03-06 | 2019-06-28 | 泰州市惠利生物科技有限公司 | A method of extraction preparation r-4- chloro-3-hydroxyl ethyl butyrate is coupled using enzyme mebrane reactor |
| CN109943482B (en) * | 2019-03-06 | 2022-03-29 | 江苏惠利生物科技有限公司 | Method for preparing ethyl r-4-chloro-3-hydroxybutyrate by coupling extraction of enzyme membrane reactor |
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Application publication date: 20130918 |