CN108993145A - A kind of processing method of coking wastewater - Google Patents
A kind of processing method of coking wastewater Download PDFInfo
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- CN108993145A CN108993145A CN201810754366.6A CN201810754366A CN108993145A CN 108993145 A CN108993145 A CN 108993145A CN 201810754366 A CN201810754366 A CN 201810754366A CN 108993145 A CN108993145 A CN 108993145A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/002—Forward osmosis or direct osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/002—Forward osmosis or direct osmosis
- B01D61/005—Osmotic agents; Draw solutions
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/445—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by forward osmosis
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Abstract
A kind of processing method of coking wastewater of the present invention, carries out infiltration processing for coking wastewater.The forward osmosis membrane that osmosis process uses is Hydration Technology Innovations HTI (CTA) permeable membrane produced or the Poten forward osmosis membrane of Bo Tian Environmental Protection Technology Co., Ltd production.In the present invention, using permeating method, the harmful organic substance in coking wastewater can be efficiently retained；Compared to existing processing method, energy consumption is lower, and fouling membrane is smaller, and treatment effect is more preferable.To the rejections of the toxic small molecules such as pyridine, indoles up to 70% or more." water quality pollutant emission limit " is fully achieved in water outlet after processing.
Description
Technical field
The present invention relates to environmental project technical field of waste water processing, and in particular to a kind of novel, efficient processing coking is useless
The intensifying method of water intoxication small molecule.
Background technique
It currently, the coking wastewater that coking industry generates is one of environmental pollution industry the most serious, while being also the whole nation
One of every maximum industrial wastewater of annual emissions, is listed in the emphasis monitoring object of environmental monitoring.According to incompletely statistics, state of China
Interior coke-oven plant, steel plant and gasworks etc., annual coking wastewater discharge amount is up to 100,000,000 tons or more.Not with plant layout
Disconnected to expand, enterprise's production capacity gradually increases, and the increase year by year of coke output, the industrial wastewater of generation is also being continuously increased how
Effectively administering industrial coking wastewater, oneself becomes China or even one of important environmental problem that the world faces.Industrial coking wastewater contains
There are tens kinds even to reach hundreds of organic matter, including phenol and its derivative, amino benzenes compounds, quinolines, pyrrole
The aromatics and heterocyclic compound containing phenyl ring such as pyridine.Phenol, aniline, quinoline in the composition of coking wastewater, indoles, based on pyridine etc.
It is difficult to biodegradable organic substance.And pyridine is endocrine disruption hardly degraded organic substance, their strong toxicities, molecular weight
Small, removal difficulty is big.
According to the different characteristics of major pollutants in coking wastewater, the domestic and international widely applied processing technique of industry, mainly
Including bioanalysis, chemical method, physical-chemical process.But the big multiple process routes of these methods are cumbersome, it is at high cost, or even by processing
National emission standard cannot still be reached afterwards.Membrane bioreactor (MBR) technique is by bioanalysis and microfiltration membranes or ultrafiltration membrane at present
It is combined into together, it can be used to handle coking wastewater as a kind of novel process.But tradition MBR process flow is pretreated
First through Biochemical method, primary water outlet that treated due to microfiltration membranes and surpasses coking wastewater using micro-filtration or ultrafiltration membrance filter
Filter sizes are relatively large, therefore secondary water outlet still remains toxic small molecule content height, the defective workmanships such as complicated component, after giving
Continuous advanced treating brings many difficulties.
Summary of the invention
For the difficulty for solving existing Treatment of Coking Effluent, the purpose of the present invention is to provide one kind for handling coking wastewater
The intensifying method of Poisoning small molecule.
In order to solve these defects of the prior art, the present inventor good can overcome the prior art by numerous studies
Existing defect, the technical solution of the present invention is as follows:
Coking wastewater is carried out infiltration processing by a kind of processing method of coking wastewater, and water penetrates permeable membrane in coking wastewater,
Into drawing in liquid.
The present inventor is had found by numerous studies, and using permeating method, the nocuousness that can efficiently retain in coking wastewater is organic
Object；Compared to existing processing method, energy consumption is lower, and fouling membrane is smaller, and treatment effect is more preferable.
Preferably, the forward osmosis membrane that osmosis process uses is Hydration Technology Innovations
HTI (CTA) permeable membrane of production or the Poten forward osmosis membrane of Bo Tian Environmental Protection Technology Co., Ltd production.By the study found that adopting
With the preferred permeable membrane, the retention of the harmful organic substance in coking wastewater can be obviously improved.
Further preferably, the permeable membrane is HTI (CTA).It is more preferable using the water treatment effect of the permeable membrane.
The present invention also passes through the study found that HTI (CTA) permeable membrane or Poten permeable membrane are impregnated progress in water in advance
Pretreatment.So pretreatment, can promote the initial flux of film, early period rejection.
In the present invention, the coking wastewater is the waste water including at least at least one of indoles, pyridine.
The method of the present invention particularly suitable for it is mild, efficiently at low cost the processing prior art be difficult to handle containing indoles, pyrrole
The waste water of pyridine.
The method of the present invention can be suitble to the indoles of any concentration content, pyridine waste water processing.It is particularly suitable for the dense of indoles
Degree is less than or equal to 50mg/L；The concentration of pyridine is less than or equal to 50mg/L；NH3The concentration of-N is less than or equal to 100mg/L's
The processing of coking wastewater.Coking wastewater under the concentration range, treatment effeciency is high, and the rejection of organic matter is high, process stabilizing,
Technique can guarantee permanently effective.
In the present invention, process of osmosis is used as using inorganic salt solution and draws liquid.
Preferably, process of osmosis draws the aqueous solution that liquid is at least one of sodium chloride, sodium sulphate, magnesium chloride.
Preferably, the molar concentration of the solute for drawing liquid of starting is 0.5~4mol/L.
The method of the present invention, it can be achieved that coking wastewater continuous treatment, for example, to two separate chambers separated by permeable membrane
It is continuously injected into feed liquid (present invention is also referred to as coking wastewater) in any one chamber in room, injects and draws into another chamber
Liquid.The study found that feed liquid and the flow velocity for drawing liquid have a great impact to membrane flux and reversed flux salt.
Preferably, coking wastewater and the velocity ratio for drawing liquid are 1~12: 1~12.
Still more preferably, coking wastewater and the velocity ratio for drawing liquid are 1~8: 1~8.Of the invention has been surprisingly found that, control
System under the ratio, can biggish raisings film average water flux, the reversed flux salt of film is effectively reduced, with respect to there is a lower energy
Consumption.
Preferably, the flow velocity of coking wastewater is that 10~120L/h (is equivalent to 2.2cm/s~26.4cm/ in infiltration processing
s)；Drawing flow velocity is 10~120L/h (being equivalent to 2.2cm/s~26.4cm/s)；Select flow velocity appropriate that can effectively improve film
Water flux reduces reversed flux salt.
Preferably, the flow velocity of coking wastewater is 80L/h in infiltration processing；Drawing flow velocity is 10~80L/h.This hair
Bright people's discovery, under the flow, treatment effect is more preferable, film Js (the reversed flux salt of film)/Jw (film average water flux Jw) ratio is more
Low, treatment effect is more excellent.
Preferably, in infiltration processing, coking wastewater with draw that liquid is reverse and the operation of parallel film surface.Help to improve film water
Fouling membrane is effectively reduced in flux.
Preferably, the molar concentration for drawing liquid in control osmosis process is 0.5~4mol/L.With infiltration
Constantly carrying out, the water in coking wastewater constantly penetrates permeable membrane, into drawing in liquid, the osmotic pressure drawn in liquid is reduced, into
And slow down infiltration process；In the present invention, maintaining the molar concentration for drawing liquid in heat exchanger chambers is 0.5~4mol/L, can be with
Stablize film rejection and maintain higher level, and water flux is made to be stably maintained at higher level, reversed flux salt maintains
Lower level.
Preferably, by selecting different film directions to draw liquid level to support by feed liquid surface to the active layer of HTI film
Layer (FO mode)；Or feed liquid is drawn liquid level to active layer (PRO mode), select suitable film direction that can have towards supporting layer
Effect improves membrane flux, reduces fouling membrane, reduces the reversed flux salt of film.
Further preferably, the permeable membrane is HTI (CTA) permeable membrane, wherein the work of described HTI (CTA) permeable membrane
Property level is to liquid level (active layer is contacted with liquid is drawn) is drawn, and supporting layer is towards coking wastewater (supporting layer is contacted with coking wastewater)
(PRO mode).Compared to forward osmosis membrane active layer towards coking wastewater, supporting layer is towards drawing liquid (FO mode), PRO operation
Under mode, film J can be further decreaseds(the reversed flux salt of film)/Jw(film average water flux Jw) ratio, make the comprehensive permeability of film
It can be more excellent.
As further preferred, long-term effect tests are carried out to two kinds of forward osmosis membranes, Poten and HTI (CTA) forward osmosis membrane exist
Under FO mode, coking wastewater is as feed liquid, 1mol/L Na2SO4As liquid is drawn, it is carried out continuously positive infiltration in 15 days respectively and surveys
Examination, feed liquid and to draw flow velocity be 24L/h, research has been surprisingly found that HTI (CTA) film properties are best, and rejection, which is stablized, to exist
70% or more, and water flux and reversed flux salt fluctuate very little, water flux Jw stablizes in 5.5Kg/m2H, reversed flux salt Js
Stablize in 4.5g/m2.h, HTI (CTA) film does not find apparent fouling membrane phenomenon.
Preferably, during dialysis, every continuous operation 4~8 days rinses permeable membrane two sides using deionized water.Research
It was found that through this process, the flux of permeable membrane can be obviously improved, improve treatment effect.
Further preferably, in deionization flushing process, the flow of the deionized water of two sides is 60~100L/h, washing time
Preferably 20~40min.
For example, in order to maintain the long-term high-throughput performance of Poten film, in long-term effect test, can periodically carry out to film
Physical cleaning keeps the comprehensive permeance property of film more excellent to eliminate fouling membrane.
It, can also will treated draws liquid and carry out reverse osmosis place except constantly in addition to drawing and supplementing solute in liquid in the present invention
Reason, then will draw liquid recycled into osmosis process after concentration.
Implement the processing system of the processing method, including a container, container intracavity room are separated into independence by permeable membrane
Two heat exchanger chambers, respectively feed compartment (coking wastewater room) and draw liquid chamber；The feed compartment and the appearance for drawing liquid chamber
Entrance and exit is provided on wall, the entrance of the feed compartment is connected by the outlet of feed liquid circulation pump and feed liquid storage tank
It connects, the outlet of feed compartment is connect with the entrance of feed liquid storage tank；
The entrance for drawing liquid chamber is connected by drawing liquid circulating pump with the outlet for drawing liquid storage tank, draws liquid chamber
Export and draw the entrance connection of liquid storage tank.
In the present invention, feed liquid is transferred to feed compartment by feed liquid storage tank；It draws liquid and is transferred to by drawing liquid storage tank and draw liquid chamber；
Feed liquid in feed compartment is under the driving of film two sides permeable pressure head, and water therein enters through permeable membrane to be drawn in liquid, after infiltration
Feed liquid be back in feed liquid storage tank, circular treatment；Treated draw liquid (drawing liquid after dilution) be back to draw liquid storage
In tank, recycle；With infiltration processing continuous progress, can incessantly to draw in liquid supplement solute (sodium chloride, sulfuric acid
The water-soluble electrolytes such as sodium, magnesium chloride)；The molar concentration for maintaining to draw the solute in liquid chamber is 0.5~4mol/L, makes osmotic pressure
Maintain a maintenance level.
Drawing liquid and can also carry out reverse osmosis treatment after dilution of the invention carries out concentration to liquid is drawn, after concentration
Draw liquid recycling apply；In this way, can be without constantly adding solute in liquid to drawing.
A kind of processing method of preferred coking wastewater of the present invention, includes the following steps:
It is 20~50mg/L that step A., which is configured to indoles concentration in laboratory, and pyridine concentration is 20~50mg/L, NH3- N is dense
Degree is the simulation coking wastewater of 50~100mg/L；
Step B. is just permeating the preparation for drawing liquid: being configured to molar concentration in laboratory is that drawing for 0.5~4mol/L is molten
Liquid, wherein solute can be one of sodium chloride, sodium sulphate, magnesium chloride etc.；
Step C. by HTI (CTA) forward osmosis membrane or Poten forward osmosis membrane impregnate in water for 24 hours more than, pre-processed,
Permeable membrane must be pre-processed.
Step D. feed liquid (simulation coking wastewater) flow rate set is that 10~120L/h (is equivalent to 2.2cm/s~26.4cm/
S), it draws flow velocity to be set as 10~120L/h (being equivalent to 2.2cm/s~26.4cm/s), feed liquid and draws all each free magnetic of liquid
Power pump is squeezed into, and wherein feed liquid turns again to material liquid tank after flowing through magnetic drive pump, fluid flowmeter, forward osmosis membrane from material liquid tank, entirely
Process is closed cycle.Liquid is drawn equally to draw from drawing to turn again to after flow container flows through magnetic drive pump, fluid flowmeter, forward osmosis membrane
Flow container is taken, process is also closed cycle；
Step E. is in membrane separating process, since the hydrone in feed liquid is under the action of the permeable pressure head driving force of film two sides
Constantly entered across fenestra and draw liquid side, in osmosis process, preferably every 0.5~1h to draw supplemented in liquid it is a certain amount of
Solute controls the molar concentration of solute in 0.5~4mol/L；
Step F. continuous work from feed liquid and draws the total of indoles and pyridine in the separately sampled measurement two sides solution of liquid after for 24 hours
Organic Carbon TOC content.
When step G.Poten and HTI (CTA) film carries out long-term effect test, FO mode is chosen, film two sides flow velocity is 24L/
H is carried out continuously 15 days positive penetration testing, the data of record water flux, reversed flux salt and rejection.
Beneficial effect
The present invention can efficiently retain indoles, pyridine toxic small molecule in coking wastewater, one section of rejection up to 70% or more,
Water outlet is set to can achieve national emission standard.
Detailed description of the invention
Fig. 1 be the present invention use forward osmosis membrane SEM figure, middle and upper part be divided into two surfaces of Poten forward osmosis membrane with
And sectional view；Lower part is divided into two surfaces and sectional view of HTI (CTA) forward osmosis membrane；In Fig. 1, the surface A represents active layer；B table
Face represents supporting layer；
Fig. 2 is flow diagram of the invention；Wherein, 1. feed liquids fill 2. conductivity meter, 3. magnetic drive pump, 4. spinner
It counts 5. membrane module, 6. pressure gauge 7. and draws liquid filling；
Fig. 3 is HTI (CTA) forward osmosis membrane active layer AFM test chart；
Fig. 4 is Poten forward osmosis membrane active layer AFM test chart；
Fig. 5 is that 1 different feed liquid flow velocity of embodiment (feed liquid is 1~8: 8 with flow velocity ratio is drawn) influences Poten film properties
Trend (FO mode)；
Fig. 6 is that 2 difference of embodiment draws flow velocity (feed liquid is 8: 1~8 with flow velocity ratio is drawn) to Poten film properties
Effect tendency (FO mode)；
Fig. 7 is that 3 different feed liquid flow velocity of embodiment (feed liquid is 1~8: 8 with flow velocity ratio is drawn) influences on HTI film properties
Gesture (FO mode)
Fig. 8 is that 4 difference of embodiment draws flow velocity (feed liquid is 8: 1~8 with flow velocity ratio is drawn) to the shadow of HTI film properties
It rings trend (FO mode)；
Fig. 9 is that 5 different feed liquid flow velocity of embodiment (feed liquid is 1~8: 8 with flow velocity ratio is drawn) influences on HTI film properties
Gesture (PRO mode)；
Figure 10 is that 6 difference of embodiment draws flow velocity (feed liquid is 8: 1~8 with flow velocity ratio is drawn) to HTI film properties
Effect tendency (PRO mode)；
Figure 11 is embodiment 7Poten forward osmosis membrane in long-term effect test in 15 days, and water flux and reversed flux salt are at any time
Between variation tendency (FO mode, film two sides flow velocity is 24L/h)；
Figure 12 is embodiment 7Poten forward osmosis membrane in long-term effect test in 15 days, to the rejection of indoles, pyridine with
The variation tendency of time；
Figure 13 is embodiment 8HTI (CTA) forward osmosis membrane in long-term effect test in 15 days, water flux and reversed flux salt
(FO mode, film two sides flow velocity is 24L/h to the trend that changes with time；
Figure 14 is embodiment 8HTI (CTA) forward osmosis membrane in long-term effect test in 15 days, to the rejection of indoles, pyridine
Change with time trend.
Specific embodiment
Embodiment 1
The present embodiment is inquired into, using Poten forward osmosis membrane, Treatment of Coking Effluent effect under different feed liquid flow velocity, and tool
Body is as follows:
Step (1): the preparation of simulation coking wastewater (feed liquid):
Being configured to indoles, pyridine, ammonia nitrogen concentration in laboratory is respectively 50mg/L, the simulation coking of 50mg/L, 80mg/L
Waste water 1L；
Step (2): the preparation of liquid is drawn in positive infiltration:
Molar concentration is prepared in laboratory and draws solution 1.5L for 1mol/L, and wherein solute selects sodium sulphate.
Step (3): the selection and pretreatment of business forward osmosis membrane:
Taking Poten forward osmosis membrane, (SEM figure is shown in Fig. 1, upper part；PA；62.53 ° of contact angle) effective dimensions be 4.5*
2.5cm is first dipped into deionized water before experiment and is pre-processed 24 hours, it is primary to change water halfway；
Feed velocity is successively set as 10,20,40,80L/h, draws flow velocity and is set as 80L/h, studies feed velocity pair
The influence of membrane permeability energy is to determine optimized operation condition.Wherein feed liquid is drawn liquid level and is supported to film towards Poten film activity layer
Layer (FO mode), feed liquid and draws all each free magnetic drive pump of liquid and squeezes into, and wherein feed liquid flows through magnetic drive pump, fluid flow from material liquid tank
Material liquid tank is turned again to after meter, forward osmosis membrane, whole process is closed cycle (schematic diagram is shown in Fig. 3).Liquid is drawn equally from drawing
Flow container, which flows through to turn again to after magnetic drive pump, fluid flowmeter, forward osmosis membrane, draws flow container, and process is also closed cycle；
Feed liquid balance registration of each hour record, records a feed liquid conductivity registration, to calculate film water per hour
Flux and reversed salt (sodium sulphate) flux.System continuous operation 10 hours.
In continuous osmosis process, every 0.5h supplements a certain amount of sodium sulphate to drawing in liquid, liquid conductance is drawn in control
Rate precision is ± 0.15ms/cm.
After the completion of infiltration processing, the indoles in liquid and feed liquid is drawn to treated, the TOC of pyridine is measured, it is quantitative
Test method calculates the rejection of indoles, pyridine toxic small molecule, with material flow referring to " water and Monitoring And Analysis of The Quality method "
The increase of speed, Poten film rejection are basically unchanged, and are greater than 60%, film average water flux JwRespectively 6.8,8.2,11.9,
14.7kg/m2H, the reversed flux salt J of filmsRespectively 84.1,67.1,48.7,14.9g/m2h。
Test result shows the increase with feed velocity, film average water flux JwFrom 6.8kg/m2H increases to 14.7kg/
m2H, the reversed flux salt J of filmsFrom 84.1g/m2H drops to 14.9g/m2H selects 80L/h (being equivalent to 17.6cm/s) in feed velocity
When, Js/JwIt is worth minimum 1.01, film properties are best.
Embodiment 2
The present embodiment is inquired into, and using Poten forward osmosis membrane, draws the Treatment of Coking Effluent effect under flow velocity in difference,
It is specific as follows:
Step (1): the preparation of coking wastewater is simulated:
Being configured to indoles, pyridine, ammonia nitrogen concentration in laboratory is respectively 50mg/L, the simulation coking of 50mg/L, 80mg/L
Waste water 1L；
Step (2): the preparation of liquid is drawn in positive infiltration:
Preparing molar concentration in laboratory is that 1mol/L draws solution 1.5L, and wherein solute selects sodium sulphate, because its at
This is relatively low, and osmotic pressure is also relatively high, and ionic hydration radius is big.
Step (3): the selection and pretreatment of the positive infiltration plate membrane of business:
The effective dimensions for taking Poten forward osmosis membrane (with embodiment 1) is 4.5*2.5cm, needs to be dipped into before experiment
It is pre-processed 24 hours in deionized water, it is primary to change water halfway；
It draws flow velocity and is successively set as 10,20,40,80L/h, feed velocity is set as 80L/h, and flow velocity is drawn in research
Influence to membrane permeability energy is to determine optimized operation condition.Wherein feed liquid draws liquid level to film branch towards Poten film activity layer
It supports layer (FO mode), feed liquid and draws all each free magnetic drive pump of liquid and squeeze into, wherein feed liquid flows through magnetic drive pump, liquid flow from material liquid tank
Material liquid tank is turned again to after meter, forward osmosis membrane, whole process is closed cycle.It draws liquid and equally flows through magnetic force from drawing flow container
It is turned again to after pump, fluid flowmeter, forward osmosis membrane and draws flow container, process is also closed cycle；
Feed liquid balance registration of each hour record, records a feed liquid conductivity registration, to calculate film water per hour
Flux and reversed salt (sodium sulphate) flux.System continuous operation 10 hours.
In continuous osmosis process, every 0.5h supplements a certain amount of sodium sulphate to drawing in liquid, liquid conductance is drawn in control
Rate precision is ± 0.15ms/cm.
After the completion of infiltration processing, the indoles in liquid and feed liquid is drawn to treated, the TOC of pyridine is measured, it is quantitative
Test method calculates the rejection of indoles, pyridine toxic small molecule referring to " water and Monitoring And Analysis of The Quality method ", with drawing liquid
The increase of flow velocity, Poten film rejection are basically unchanged, and are greater than 60%, film average water flux Jw is respectively 9.1,12.9,
13.2、14.7kg/m2H, the reversed flux salt J of filmsRespectively 8.6,9.7,12.4,14.9g/m2h。
Test result show feed velocity be 20L/h (being equivalent to 4.4cm/s) when, Js/JwIt is worth minimum 0.75, film property
It can be best.
Embodiment 3
The present embodiment is inquired into, using HTI (CTA) forward osmosis membrane, Treatment of Coking Effluent effect under different feed liquid flow velocity,
It is specific as follows:
Step (1): the preparation of coking wastewater is simulated:
Being configured to indoles, pyridine, ammonia nitrogen concentration in laboratory is respectively 50mg/L, the simulation coking of 50mg/L, 80mg/L
Waste water 1L；
Step (2): the preparation of liquid is drawn in positive infiltration:
Preparing molar concentration in laboratory is that 1mal/L draws solution 1.5L, and wherein solute selects sodium sulphate, because its at
This is relatively low, and osmotic pressure is also relatively high, and ionic hydration radius is big.
Step (3): the selection and pretreatment of the positive infiltration plate membrane of business:
Taking HTI (CTA) forward osmosis membrane, (SEM figure is shown in Fig. 1, lower part；CTA；49.25 ° of contact angle) effective dimensions be
4.5*2.5cm, needs to be dipped into deionized water before experiment and pre-processes 24 hours, and it is primary to change water halfway；
Feed velocity is successively set as 10,20,40,80L/h, draws flow velocity and is set as 80L/h, studies feed velocity pair
The influence of membrane permeability energy is to determine optimized operation condition.Wherein feed liquid draws liquid level to film supporting layer towards HTI film activity layer
(FO mode), feed liquid and draws all each free magnetic drive pump of liquid and squeezes into, and wherein feed liquid flows through magnetic drive pump, fluid flow from material liquid tank
Material liquid tank is turned again to after meter, forward osmosis membrane, whole process is closed cycle.It draws liquid and equally flows through magnetic force from drawing flow container
It is turned again to after pump, fluid flowmeter, forward osmosis membrane and draws flow container, process is also closed cycle；
Feed liquid balance registration of each hour record, records a feed liquid conductivity registration, to calculate film water per hour
Flux and reversed salt (sodium sulphate) flux.System continuous operation 10 hours.
In continuous osmosis process, every 0.5h supplements a certain amount of sodium sulphate to drawing in liquid, liquid conductance is drawn in control
Rate precision is ± 0.15ms/cm.
After the completion of infiltration processing, the indoles in liquid and feed liquid is drawn to treated, the TOC of pyridine is measured, it is quantitative
Test method calculates the rejection of indoles, pyridine toxic small molecule, the retention of HTI film referring to " water and Monitoring And Analysis of The Quality method "
Rate is basically unchanged, and is greater than 70%, film average water flux JwRespectively 3.1,3.9,5.8,7.1kg/m2H, the reversed flux salt J of films
Respectively 7.4,5.6,5.3,4.1g/m2h。
Test result shows the increase with feed velocity, and film average water flux Jw is from 3.1kg/m2H increases to 7.1kg/
m2H, the reversed flux salt J of filmsFrom 7.4g/m2H drops to 4.1g/m2H selects 80L/h (being equivalent to 17.6cm/s) in feed velocity
When, Js/JwIt is worth minimum 0.58, film properties are best.
Embodiment 4
The present embodiment is inquired into, and using HTI (CTA) forward osmosis membrane, draws the effect of the Treatment of Coking Effluent under flow velocity in difference
Fruit, specific as follows:
Step (1): the preparation of coking wastewater is simulated:
Being configured to indoles, pyridine, ammonia nitrogen concentration in laboratory is respectively 50mg/L, the simulation coking of 50mg/L, 80mg/L
Waste water 1L；
Step (2): the preparation of liquid is drawn in positive infiltration:
Preparing molar concentration in laboratory is that 1mol/L draws solution 1.5L, and wherein solute selects sodium sulphate, because its at
This is relatively low, and osmotic pressure is also relatively high, and ionic hydration radius is big.
Step (3): the selection and pretreatment of the positive infiltration plate membrane of business:
The effective dimensions for taking HTI (CTA) forward osmosis membrane is 4.5*2.5cm, needs to be dipped into deionized water before experiment
Middle pretreatment 24 hours, it is primary to change water halfway；
It draws flow velocity and is successively set as 10,20,40,80L/h, feed velocity is set as 80L/h, and flow velocity is drawn in research
Influence to membrane permeability energy is to determine optimized operation condition.Wherein feed liquid is drawn liquid level and is supported to film towards HTI film activity layer
Layer (FO mode), feed liquid and draws all each free magnetic drive pump of liquid and squeezes into, and wherein feed liquid flows through magnetic drive pump, fluid flow from material liquid tank
Material liquid tank is turned again to after meter, forward osmosis membrane, whole process is closed cycle.It draws liquid and equally flows through magnetic force from drawing flow container
It is turned again to after pump, fluid flowmeter, forward osmosis membrane and draws flow container, process is also closed cycle；
Feed liquid balance registration of each hour record, records a feed liquid conductivity registration, to calculate film water per hour
Flux and reversed salt (sodium sulphate) flux.System continuous operation 10 hours.
In continuous osmosis process, every 0.5h supplements a certain amount of sodium sulphate to drawing in liquid, control is drawn liquid and dropped to
Rate precision is ± 0.15ms/cm.
After the completion of infiltration processing, the indoles in liquid and feed liquid is drawn to treated, the TOC of pyridine is measured, it is quantitative
Test method calculates the rejection of indoles, pyridine toxic small molecule referring to " water and Monitoring And Analysis of The Quality method ", with drawing liquid
The increase of flow velocity, HTI film rejection are basically unchanged, and are greater than 70%, film average water flux JwRespectively 4.3,4.9,5.3,
7.1kg/m2H, the reversed flux salt J of filmsRespectively 3.6,3.2,3.9,4.1g/m2h.Drawing flow velocity selection 80L/h (quite
In 17.6cm/s) when, Js/JwIt is worth minimum 0.58, film properties are best.
Embodiment 5
It is compared with embodiment 3, difference is, the direction of HTI (CTA) forward osmosis membrane is different, specific as follows:
Step (1): the preparation of coking wastewater is simulated:
Being configured to indoles, pyridine, ammonia nitrogen concentration in laboratory is respectively 50mg/L, the simulation coking of 50mg/L, 80mg/L
Waste water 1L；
Step (2): the preparation of liquid is drawn in positive infiltration:
Preparing molar concentration in laboratory is that 1mol/L draws solution 1.5L, and wherein solute selects sodium sulphate, because its at
This is relatively low, and osmotic pressure is also relatively high, and ionic hydration radius is big.
Step (3): the selection and pretreatment of the positive infiltration plate membrane of business:
The effective dimensions for taking HTI (CTA) forward osmosis membrane is 4.5*2.5cm, needs to be dipped into deionized water before experiment
Middle pretreatment 24 hours, it is primary to change water halfway；
Feed velocity is successively set as 10,20,40,80L/h, draws flow velocity and is set as 80L/h, studies feed velocity pair
The influence of membrane permeability energy is to determine optimized operation condition.Wherein feed liquid draws liquid level to film activity layer towards HTI film supporting layer
(PRO mode), feed liquid and draws all each free magnetic drive pump of liquid and squeezes into, and wherein feed liquid flows through magnetic drive pump, fluid flow from material liquid tank
Material liquid tank is turned again to after meter, forward osmosis membrane, whole process is closed cycle.It draws liquid and equally flows through magnetic force from drawing flow container
It is turned again to after pump, fluid flowmeter, forward osmosis membrane and draws flow container, process is also closed cycle；
Feed liquid balance registration of each hour record, records a feed liquid conductivity registration, to calculate film water per hour
Flux and reversed salt (sodium sulphate) flux.System continuous operation 10 hours.
In continuous osmosis process, every 0.5h supplements a certain amount of sodium sulphate to drawing in liquid, liquid conductance is drawn in control
Rate precision is ± 0.15ms/cm.
After the completion of infiltration processing, the indoles in liquid and feed liquid is drawn to treated, the TOC of pyridine is measured, it is quantitative
Test method calculates the rejection of indoles, pyridine toxic small molecule, with material flow referring to " water and Monitoring And Analysis of The Quality method "
The increase of speed, HTI film rejection is basically unchanged, and is greater than 70%, film average water flux Jw is respectively 7.5,6.5,8.9,
5.2kg/m2H, the reversed flux salt J of filmsRespectively 11.3,13.5,14.8,12.2g/m2h.10L/h (phase is selected in feed velocity
When in 2.2cm/s) when, Js/JwIt is worth minimum 1.5, film properties are best.
Embodiment 6
It is compared with embodiment 4, difference is, the direction of HTI (CTA) forward osmosis membrane is different, specific as follows:
Step (1): the preparation of coking wastewater is simulated:
Being configured to indoles, pyridine, ammonia nitrogen concentration in laboratory is respectively 50mg/L, the simulation coking of 50mg/L, 80mg/L
Waste water 1L；
Step (2): the preparation of liquid is drawn in positive infiltration:
Preparing molar concentration in laboratory is that 1mol/L draws solution 1.5L, and wherein solute selects sodium sulphate, because its at
This is relatively low, and osmotic pressure is also relatively high, and ionic hydration radius is big.
Step (3): the selection and pretreatment of the positive infiltration plate membrane of business:
The effective dimensions for taking HTI (CTA) forward osmosis membrane is 4.5*2.5cm, needs to be dipped into deionized water before experiment
Middle pretreatment 24 hours, it is primary to change water halfway；
It draws flow velocity and is successively set as 10,20,40,80L/h, feed velocity is set as 80L/h, and flow velocity is drawn in research
Influence to membrane permeability energy is to determine optimized operation condition.Wherein feed liquid draws liquid level to film activity layer towards HTI supporting layer
(PRO mode), feed liquid and draws all each free magnetic drive pump of liquid and squeezes into, and wherein feed liquid flows through magnetic drive pump, fluid flow from material liquid tank
Material liquid tank is turned again to after meter, forward osmosis membrane, whole process is closed cycle.It draws liquid and equally flows through magnetic force from drawing flow container
It is turned again to after pump, fluid flowmeter, forward osmosis membrane and draws flow container, process is also closed cycle；
Feed liquid balance registration of each hour record, records a feed liquid conductivity registration, to calculate film water per hour
Flux and reversed salt (sodium sulphate) flux.System continuous operation 10 hours.
In continuous osmosis process, every 0.5h supplements a certain amount of sodium sulphate to drawing in liquid, liquid conductance is drawn in control
Rate precision is soil 0.15ms/cm.
After the completion of infiltration processing, the indoles in liquid and feed liquid is drawn to treated, the TOC of pyridine is measured, it is quantitative
Test method calculates the rejection of indoles, pyridine toxic small molecule referring to " water and Monitoring And Analysis of The Quality method ", with drawing liquid
The increase of flow velocity, HTI film rejection are basically unchanged, and are greater than 70%, film average water flux JwRespectively 8.4,8.0,6.8,
5.2kg/m2H, the reversed flux salt J of filmsRespectively 0.42,0.44,0.68,2.33g/m2h.Drawing flow velocity selection 10L/h
When (being equivalent to 2.2cm/s), Js/JwIt is worth minimum 0.42, film properties are best.
Embodiment 7
The present embodiment is inquired into, using Poten forward osmosis membrane, feed liquid and to draw flow velocity be all 24L/h, and water flux and reversed
Flux salt changes with time trend.It is specific as follows:
Step (1): the preparation of coking wastewater is simulated:
Being configured to indoles, pyridine, ammonia nitrogen concentration in laboratory is respectively 50mg/L, the simulation coking of 50mg/L, 80mg/L
Waste water 1L；
Step (2): the preparation of liquid is drawn in positive infiltration:
Preparing molar concentration in laboratory is that 1mol/L draws solution 1.5L, and wherein solute selects sodium sulphate, because its at
This is relatively low, and osmotic pressure is also relatively high, and ionic hydration radius is big.
Step (3): the selection and pretreatment of the positive infiltration plate membrane of business:
The effective dimensions for taking Poten forward osmosis membrane (with embodiment 1) is 4.5*2.5cm, needs to be dipped into before experiment
It is pre-processed 24 hours in deionized water, it is primary to change water halfway；
Wherein feed liquid is towards Poten film activity layer, draws liquid level to film supporting layer (FO mode), feed liquid and to draw liquid all each
Free magnetic drive pump is squeezed into, and wherein feed liquid turns again to feed liquid after flowing through magnetic drive pump, fluid flowmeter, forward osmosis membrane from material liquid tank
Tank, whole process are closed cycle.Liquid is drawn equally from drawing after flow container flows through magnetic drive pump, fluid flowmeter, forward osmosis membrane again
Secondary return to draws flow container, and process is also closed cycle；
Feed liquid balance registration of each hour record, records a feed liquid conductivity registration, to calculate film water per hour
Flux and reversed salt (sodium sulphate) flux, system are run 10 hours daily, and continuous operation 15 days.
In continuous osmosis process, every 0.5h supplements a certain amount of sodium sulphate to drawing in liquid, liquid conductance is drawn in control
Rate precision is ± 0.15ms/cm.
After the completion of daily infiltration processing, the indoles in liquid and feed liquid is drawn to treated, the TOC of pyridine is surveyed
It is fixed, calculate the rejection of indoles, pyridine toxic small molecule.The water flux fluctuation in 15 days of Poten film is larger as the result is shown, preceding
In 7 day time, water flux is most tall and big to reach 18kg/m2.h, after running to the 7th day, discovery water flux starts to reduce, from 16kg/
m2.h 7kg/m is dropped to2.h, mainly as caused by fouling membrane.Reversed flux salt is stablized in first 7 days in 13g/m2.h, from
After 7 days, reversed flux salt starts to reduce, and drops to 7g/m always2.h.Have been surprisingly found that film rejection is relatively stable in 15 days, and
50% or so can be maintained, illustrates that this body structure does not impact fouling membrane to film.
Embodiment 8
The present embodiment is inquired into, using HTI (CTA) forward osmosis membrane, feed liquid and to draw flow velocity be all 24L/h, water flux and
Reversed flux salt changes with time trend.It is specific as follows:
Step (1): the preparation of coking wastewater is simulated:
Being configured to indoles, pyridine, ammonia nitrogen concentration in laboratory is respectively 50mg/L, the simulation coking of 50mg/L, 80mg/L
Waste water 1L；
Step (2): the preparation of liquid is drawn in positive infiltration:
Preparing molar concentration in laboratory is that 1mol/L draws solution 1.5L, and wherein solute selects sodium sulphate, because its at
This is relatively low, and osmotic pressure is also relatively high, and ionic hydration radius is big.
Step (3): the selection and pretreatment of the positive infiltration plate membrane of business:
The effective dimensions for taking Poten forward osmosis membrane (with embodiment 1) is 4.5*2.5cm, needs to be dipped into before experiment
It is pre-processed 24 hours in deionized water, it is primary to change water halfway；
Wherein feed liquid is towards HTI (CTA) film activity layer, draws liquid level to film supporting layer (FO mode), feed liquid and draws liquid
All each free magnetic drive pump is squeezed into, and wherein feed liquid turns again to material after flowing through magnetic drive pump, fluid flowmeter, forward osmosis membrane from material liquid tank
Flow container, whole process are closed cycle.Liquid is drawn equally from drawing after flow container flows through magnetic drive pump, fluid flowmeter, forward osmosis membrane
It turns again to and draws flow container, process is also closed cycle；
Feed liquid balance registration of each hour record, records a feed liquid conductivity registration, to calculate film water per hour
Flux and reversed salt (sodium sulphate) flux, system are run 10 hours daily, and continuous operation 15 days.
In continuous osmosis process, every 0.5h supplements a certain amount of sodium sulphate to drawing in liquid, liquid conductance is drawn in control
Rate precision is ± 0.15ms/cm.
After the completion of daily infiltration processing, the indoles in liquid and feed liquid is drawn to treated, the TOC of pyridine is surveyed
It is fixed, calculate the rejection of indoles, pyridine toxic small molecule.Have been surprisingly found that HTI (CTA) film water flux in 15 days it is highly stable and
Maintain 5.6kg/m2.h, illustrate that the film contamination resistance is very strong, indoles, pyridine pollutant will not cause dirt to the film substantially
Dye.Within 15 day time, reversed flux salt is very low to be also stably maintained at 4.5g/m very much2.h.Within 15 day time, film is had been surprisingly found that
Rejection is up to very stable to 70% or more, and always, illustrates that film structural stability itself is fine.Resultant effect is substantially better than biography
System MBR technique.
Comparative example 1
In above-described embodiment 3, solute is not supplemented in liquid periodically to drawing in continuous osmosis process, keep other
Just the same in operating condition and embodiment 3, after the completion of infiltration processing, as the result is shown due to the reduction of permeable pressure head, film is average
Water flux is compared with embodiment 3 and is decreased, reversed salt (sodium sulphate) flux and indoles, the rejection of pyridine and embodiment 3
It is essentially identical.The result shows that timing helps to improve film average water flux to supplement solute in liquid is drawn.
Comparative example 2
In above-described embodiment 4, HTI (CTA) is not pre-processed, keeps complete in other operating conditions and embodiment 4
Exactly the same, after the completion of infiltration processing, as the result is shown since film needs to soak early period, initial membrane flux is dropped compared with embodiment 4
It is low, cause film average water flux to decrease.The reversed salt of film (sodium sulphate) flux and rejection and implementation to indoles, pyridine
Example 4 is essentially identical.The result shows that carrying out pretreatment operation to film helps to improve film average water flux.
Comparative example 3
In order to compare with ultrafiltration membrane used in traditional MBR, company is reached using HTI of the present invention (CTA) film and three respectively
The ultrafiltration membrane of production is filtered processing to above-mentioned simulation coking wastewater, the results show that three reach ultrafiltration membrane to small molecule indole, pyrrole
Piperidinyl does not originally have any retention, and HTI (CTA) the forward osmosis membrane filter effect for showing that the present invention uses is substantially better than in traditional MBR
The ultrafiltration membrane used.
By obtaining to analysis of experimental data, the comprehensive permeance property of HTI (CTA) forward osmosis membrane is substantially better than Poten and just seeps
Permeable membrane, two kinds of forward osmosis membranes are all tested under FO mode, the J of HTI (CTA) forward osmosis membranes/JwLower value is 0.58, i.e., in feed liquid
With when drawing flow velocity and being 80L/h (being equivalent to 17.6cm/s), HTI (CTA) film has superior permeance property.Work as HTI
(CTA) when forward osmosis membrane is under PRO operation mode, the J of films/JwIt is worth minimum 0.42, i.e., is 80L/h (suitable in feed velocity
In 17.6cm/s), draw flow velocity be 10L/h (being equivalent to 2.2cm/s) when, HTI (CTA) film have optimal permeance property.
The rejection of HTI film is up to 70% or more, hence it is evident that better than Poten forward osmosis membrane.
Embodiment 9
If above-described embodiment 7 has the advantages that initial water flux height etc. because Poten film is in long-term effect test, for
Poten film contamination resistance difference improves, and by carrying out physical cleaning every other week, film two sides cleaning agent is all cheap goes
Ionized water, two sides flow velocity are 80L/h, clean 30min every time.Have been surprisingly found that cleaning caudacoria flux recovery rate be up to 90% with
On, in 15 days periods, membrane flux can maintain higher 12Kg/m substantially2.h.As a result illustrate that simple physics is clear
Wash the average water flux that Poten film can be improved.
Claims (10)
1. a kind of processing method of coking wastewater, which is characterized in that coking wastewater is carried out infiltration processing, water is saturating in coking wastewater
Permeable membrane is crossed, into drawing in liquid.
2. the processing method of coking wastewater as described in claim 1, which is characterized in that the permeable membrane be by
HTI (CTA) permeable membrane of Hydration Technology Innovations or the Poten of Bo Tian Environmental Protection Technology Co., Ltd
Permeable membrane.
3. the processing method of coking wastewater as claimed in claim 2, which is characterized in that the permeable membrane is HTI (CTA) infiltration
Permeable membrane, wherein the active layer of described HTI (CTA) permeable membrane is towards liquid level is drawn, and supporting layer is towards coking wastewater.
4. the processing method of coking wastewater as described in claim 1, which is characterized in that in advance by HTI (CTA) permeable membrane or
Poten permeable membrane impregnates in water, is pre-processed.
5. the processing method of coking wastewater as described in claim 1, which is characterized in that the coking wastewater be including at least
The waste water of at least one of indoles, pyridine；
Preferably, in the coking wastewater, the concentration of indoles is less than or equal to 50mg/L；The concentration of pyridine is less than or equal to
50mg/L；NH3The concentration of-N is less than or equal to 100mg/L；
Process of osmosis draws the aqueous solution that liquid is at least one of sodium chloride, sodium sulphate, magnesium chloride；Liquid is drawn in starting
The molar concentration of solute is 0.5~4mol/L.
6. the processing method of coking wastewater as claimed in claim 5, which is characterized in that drawing in control osmosis process
The molar concentration of liquid is 0.5~4mol/L.
7. the processing method of coking wastewater as claimed in claim 6, which is characterized in that drawn to treated in liquid add it is molten
Matter, maintaining the molar concentration of the solute in osmosis process is 0.5~4mol/L.
8. the processing method of the coking wastewater as described in claim 1,5,6 or 7, which is characterized in that coking wastewater and draw liquid
Velocity ratio be 1~12: 1~12；Preferably 1~8: 1~8.
9. the processing method of coking wastewater as claimed in claim 8, which is characterized in that in infiltration processing, the stream of coking wastewater
Speed is 10~120L/h.
10. the processing method of coking wastewater as described in claim 1, which is characterized in that will treated draw liquid carry out it is anti-
Infiltration processing, will draw liquid recycled into osmosis process after concentration；
Preferably, during dialysis, every continuous operation 4~8 days rinses permeable membrane two sides using deionized water.
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