CN109316965A - Organic phosphonate permeates the application for drawing solute and positive permeability apparatus as positive - Google Patents
Organic phosphonate permeates the application for drawing solute and positive permeability apparatus as positive Download PDFInfo
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- CN109316965A CN109316965A CN201811227206.2A CN201811227206A CN109316965A CN 109316965 A CN109316965 A CN 109316965A CN 201811227206 A CN201811227206 A CN 201811227206A CN 109316965 A CN109316965 A CN 109316965A
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
- C02F5/14—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances containing phosphorus
Abstract
The invention discloses organic phosphonates as the application for drawing solute and positive permeability apparatus is just permeated, and belongs to positive infiltration technology field.The organic phosphonate compound chemical structural formula are as follows:Wherein R1、R2、R3、R4、R5、R6、R7And R8At least one is Na or K, and others are H, n 1,2 or 3.The positive infiltration is drawn to the diluted liquid that draws obtained after solute just permeates applied to antisludging agent.The application is solute is drawn in positive infiltration to be configured to the solution for containing the organic phosphonate compound that mass fraction is 5%-35% as just permeating to draw liquid, it is preferred that the mass fraction of organic phosphonate compound is 15%-30%, the pH value that liquid is drawn in positive infiltration is 5-10.Positive infiltration in the present invention draws solute and acts on water flux height in positive process of osmosis, and reversed Solute flux is small；With good forward osmosis membrane scale inhibition effect, and the liquid that draws after dilution directly applies to scale inhibition.
Description
Technical field
The invention belongs to positive infiltration technology fields, draw more particularly, to organic phosphonate compound as positive infiltration
The application of solute and positive permeability apparatus.
Background technique
Under the background that freshwater resources are increasingly in short supply and non-renewable energy resources reserves gradually decrease, countries in the world are all energetically
Develop the water treatment technology of low energy consumption.Membrane Separation for Water Treatment is excellent since its treatment effeciency is high, occupied area is small, is easy to amplify etc.
Point plays important role in water treatment field.Traditional Membrane Separation for Water Treatment such as nanofiltration, reverse osmosis etc. are usually with pump
The pressure of generation makes hydrone through film as driving force, and the solutes such as salt, small organic molecule are trapped, to obtain pure
Water.But these membrane technologies are commonly present the problems such as energy consumption height and serious fouling membrane in application process.Positive infiltration is used as 21st century one
The new Membrane Separation for Water Treatment of kind, causes the attention of more and more researchers.Positive infiltration is a spontaneous process, it be with
Draw the transmitting that the osmotic pressure gradient of liquid and feed liquid two sides is driving force to realize hydrone.Compared with traditional membrane technology, just
Infiltration have the advantages that low energy consumption, solute rejection is high, fouling membrane be inclined to it is low, sea water desalination, wastewater treatment, food processing,
The fields such as drug concentration show huge application potential.
The key element that liquid is positive process of osmosis is drawn in positive infiltration, and the height of osmotic pressure determines the water of positive process of osmosis
Flux height, and the size of its molecular dimension decides the size of its reversed Solute flux.The water of feed liquid side in positive process of osmosis
Molecule, which constantly enters, draws liquid side, will cause the dilution for drawing liquid, reduces its osmotic pressure so as to cause flux decline, therefore
It needs to ensure that positive process of osmosis has continual and steady water flux output to drawing liquid and be concentrated.Draw the regenerative process one of liquid
As need to consume more energy, therefore find the recovery method of low energy consumption, or drawing liquid and can be directly applied to after dilution
It is very significant in actual production life process.
It can be encountered and traditional film when handling easy fouling water sample such as seawater and brackish water, mineral waste water etc. with positive process of osmosis
The same problem of process, film surface are easy to happen mineral scale.Mineral scale is a kind of fouling membrane phenomenon, is referred in film
Surface forms mineral solids substance, increases the transport resistance of hydrone and flux is caused to decline, will form cake layer when serious
Flux degradation even flux is caused to be reduced to zero.Film surface fouling can reduce membrane separation efficiency, increase cleaning frequency, increase
The replacement cost of film.Chemical cleaning and physical cleaning are the common methods for removing film surface minerals dirt, and these methods are to one
A little hard, adhesive force are strong and the effect of the minerals dirt such as minerals dirt such as calcium sulfate, barium sulfate of acid-soluble difference is poor and right
Film be easy to cause irreversible breaking.Another kind alleviate film surface mineral scale method be in preprocessing process into feed liquid
It is added a certain amount of antisludging agent, and the type of antisludging agent, addition concentration, addition period propose very high want to practical operation
It asks.Therefore, the method meaning weight of film scaling fouling problem a kind of easy to operate and being effectively relieved in positive process of osmosis is found
Greatly.
Summary of the invention
The present invention solves that water flux in positive process of osmosis in the prior art is low, reversed Solute flux is big, forward osmosis membrane knot
Dirt pollution and dilution after draw liquid cannot directly using etc. technical problems.
To achieve the above object, according to one aspect of the present invention, a kind of organic phosphonate compound is provided as just
The application of solute is drawn in infiltration, and the organic phosphonate compound has chemical structural formula shown in formula I；
In the Formulas I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and others are H；Or R1、R2、R3、
R4、R5、R6、R7And R8At least one is K, and others are H；
In the Formulas I, n 1,2 or 3.
Preferably, the diluted liquid that draws that solute is used to obtain after just permeating is drawn into the positive infiltration and is applied to scale inhibition
Agent.
Preferably, by it is described it is positive infiltration draw solute be used for just permeate after obtain it is diluted draw liquid applied to boiler it is cold
But the antisludging agent of recirculated water or oil field reinjection water.
Preferably, the positive infiltration is drawn into solute to be configured to the organic phospho acid for being 5%-35% containing mass fraction
The solution of salt compound draws liquid as positive infiltration.
Preferably, the mass fraction of the organic phosphonate compound is 15%-30%.
Preferably, using it is described it is positive infiltration draw solute be configured to pH value be 5-10 solution as just permeate draw liquid.
It is another aspect of this invention to provide that providing a kind of positive permeability apparatus, the liquid that draws of the positive permeability apparatus is organic
Phosphonic acids salting liquid, the organic phosphonate have chemical structural formula shown in formula I；
In the Formulas I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and others are H；Or R1、R2、R3、
R4、R5、R6、R7And R8At least one is K, and others are H；
In the Formulas I, n 1,2 or 3.
Preferably, the mass fraction of organic phosphonate is 5%-35% in the organic phospho acid salting liquid；The organic phosphine
The pH value of acid salt solution is 5-10；
Preferably, the mass fraction of organic phosphonate is 15%-30% in the organic phospho acid salting liquid.
Preferably, the permeable membrane of the positive permeability apparatus is plate membrane or hollow-fibre membrane.
Preferably, the permeable membrane of the positive permeability apparatus is polysulfones base forward osmosis membrane, polyvinylidene fluoride forward osmosis membrane or poly-
Ether sulfone base forward osmosis membrane.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, can obtain down and show
Beneficial effect:
(1) present invention uses molecular weight to draw solute as positive infiltration for the organic phosphonate of 400Da-800Da, due to it
Molecular volume is significantly greater than common NaCl and draws solute, and the organic phospho acid salt anionic after dissociation has more negative electricity
Lotus can form stronger electrostatic repulsion with the forward osmosis membrane of belt surface negative electricity, it is made to cannot easily penetrate forward osmosis membrane, thus
Efficiently solve the problems, such as that reversed Solute flux is big.
(2) liquid sodium ethylenediamine tetramethylenephosphonate salt (EDTMPA-Na) solution is drawn in positive infiltration provided by the invention, when
It is suitable with the water flux that 1M NaCl draws solution generation when mass concentration is 30%, and its reversed Solute flux is only 1M
NaCl draws the one third of liquid.
(3) organic phosphonate that the present invention uses is a kind of excellent antisludging agent, and solute is drawn in positive process of osmosis leakage
The mineral scale pollution on forward osmosis membrane surface can be slowed down, and have excellent control to the calcium sulfate scaling pollution of infiltration film surface
Effect processed.
(4) present invention draws solute by the organic phosphonate leaked in positive process of osmosis to slow down the minerals of film surface
Scaling fouling has more near the interface of feed liquid and film compared with the organic phosphonate that equal quality is added directly into feed liquid
The organic phosphonate of high concentration, to have better scale inhibition effect.
(5) sodium ethylenediamine tetramethylenephosphonate salt (EDTMPA-Na) of the present invention draws solute as positive infiltration,
There is better scale inhibition effect than disodium edta (EDTA-Na).
(6) organic phosphonate of the present invention draws solute as positive infiltration, after dilution draw liquid do not need into
Row regeneration, may be directly applied to boiler cooling water recirculation system and oil field reinjection water, inhibit boiler or oil field stratum pipeline knot
Dirt can save the diluted energy for drawing and consuming needed for liquid regenerative process.
Detailed description of the invention
Fig. 1 is positive osmotic water flux test result figure.
Fig. 2 is just to permeate reversed Solute flux test result figure.
Fig. 3 is positive process of osmosis film scaling fouling control test result figure.
Fig. 4 is the electron microscope of positive process of osmosis film scaling fouling control test caudacoria.
It is to draw liquid that Fig. 5, which is with 1M NaCl, by the sodium ethylenediamine tetramethylenephosphonate salt (EDTMPA-Na) of certain mass
It is added directly into the calcium sulfate saturated solution feed liquid that saturation index is 1.6 and is tested, and drawn with 30wt%EDTMPA-Na
Take the test result comparison diagram of liquid.
Fig. 6 is positive process of osmosis film scaling fouling control test, sodium ethylenediamine tetramethylenephosphonate salt (EDTMPA-Na)
With disodium edta (EDTA-Na) comparing result figure.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
The present invention provides a kind of positive infiltrations to draw liquid, and the pH value that liquid is drawn in the positive infiltration is 5-10, mass concentration model
Enclose the application that the organic phosphonate for 5%-35% (preferably 15%-30%) draws liquid as positive infiltration, the organic phospho acid
Salt compound has chemical structural formula shown in formula I；
In the Formulas I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and others are H；Or R1、R2、R3、
R4、R5、R6、R7And R8At least one is K, and others are H.
In the Formulas I, n 1,2 or 3.
Embodiment 1
(1) ethylenediamine tetramethylene phosphonic acid of commercialization (EDTMPA) is dissolved in deionized water, with NaOH adjust pH to
7, sodium ethylenediamine tetramethylenephosphonate salting liquid is obtained, is then purified 72 hours with the bag filter that molecular cut off is 100Da, is obtained
Obtain pure substance completely.
(2) the sodium ethylenediamine tetramethylenephosphonate solution that will be obtained in step (1), vacuum distillation, then 75 DEG C of vacuum are dry
Dry 12 hours, obtain the EDTMPA-Na solid.
Embodiment 2
(1) ethylenediamine tetramethylene phosphonic acid of commercialization (EDTMPA) is dissolved in deionized water, adjusts pH to 7 with KOH,
Ethylenediamine tetramethylene phosphonic acid potassium salt soln is obtained, is then purified 72 hours with the bag filter that molecular cut off is 100Da, is obtained
Clean pure substance.
(2) the ethylenediamine tetramethylene phosphonic acid potassium solution that will be obtained in step (1), vacuum distillation, then 75 DEG C of vacuum are dry
Dry 12 hours, obtain the EDTMPA-K solid.
Embodiment 3
(1) ethylenediamine tetra-acetic acid of commercialization (EDTA) is dissolved in deionized water, adjusts pH to 7 with NaOH, obtains second
Then ethylenediamine tetraacetic acid (EDTA) sodium salt solution is purified 72 hours with the bag filter that molecular cut off is 100Da, obtain clean pure
Object.
(2) the sodium ethylene diamine tetracetate solution that will be obtained in step (1), vacuum distillation, then 75 DEG C of vacuum drying 12 are small
When, obtain the EDTA-Na solid.
Interpretation of result:
Solid in the embodiment 1 is dissolved in deionized water, preparation mass fraction be 10wt%, 15wt%,
20wt%, 25wt%, 30wt%'s draws liquid, using deionized water as feed liquid, with the Aquaporin Inside of commercializationTMIt is positive to seep
Permeable membrane carries out positive penetration testing.Test condition is 25 ± 1 DEG C of solution temperature, effective membrane area 3.87cm2, water velocity 0.3L/
Min, each concentration determination 1.5 hours are averaged with the completely new film of three pieces retest under the same conditions 3 times.
Positive osmotic water flux result is as shown in Figure 1, just to permeate reversed Solute mass result as shown in Figure 2: the result shows that real
It applies sodium ethylenediamine tetramethylenephosphonate described in example 1 (EDTMPA-Na) water flux with higher and lower reversed solute is logical
Amount；Under the concentration of 30wt%, the active layer of film is towards drawing under liquid mode, and the water flux of embodiment 1 is up to 45.0L m-2h-1, reversed Solute flux is about 3.4g m-2h-1。
Using 30wt%EDTMPA-Na or 1M NaCl as drawing liquid, the calcium sulfate saturated solution for being 1.6 with saturation index
As feed liquid, sodium chloride in calcium sulfate saturated solution, sodium sulphate, calcium sulfate concentration be respectively 24mM, 25mM, 44mM, select
The Aquaporin Inside of commercializationTMForward osmosis membrane is the long-time test that forward osmosis membrane carries out 24 hours, investigates film fouling
The difference of pollution condition.
After test 24 hours, as shown in figure 3, being about using the rate of descent of 30wt%EDTMPA-Na as flux when drawing liquid
15%；It is when drawing liquid with 1M NaCl, water flux rate of descent is about 40%, hence it is evident that be higher than the former, it is known that being with NaCl
Scale formation is serious when drawing liquid, and lighter using EDTMPA-Na as forward osmosis membrane surface scale phenomenon when drawing liquid.Test
Film afterwards is characterized with scanning electron microscope, as shown in figure 4, occurring more using 1M NaCl as the film surface for drawing liquid
Grain object, and be that particulate matter on the film for draw liquid is less with 30wt%EDTMPA-Na is proved herein using EDTMPA-Na as drawing
Forward osmosis membrane surface scale phenomenon is lighter when taking liquid.This is because EDTMPA-Na is a kind of excellent antisludging agent, to CaSO4、
BaSO4The equal dirty inhibitory effect of minerals dirt is obvious.In positive process of osmosis, the EDTMPA-Na reversely spread draws solute can
With Ca in feed liquid2+Chelating, reduce feed liquid in Ca2+Concentration；EDTMPA-Na can also be adsorbed in mineral crystals, be prevented
Its further growth, to alleviate the scaling fouling on forward osmosis membrane surface.
The EDTMPA-Na of certain mass is added directly into the calcium sulfate saturated solution feed liquid that saturation index is 1.6, with
1M NaCl is to draw liquid test within 24 hours, investigates the pollution condition of film, and in being with the EDTMPA-Na solution of 30wt%
The test result for drawing liquid compares.
As shown in figure 5, water flux rate of descent increases with the increase of EDTMPA-Na additional amount in feed liquid, show
EDTMPA-Na is a kind of excellent antisludging agent, and the scaling fouling on forward osmosis membrane surface can be effectively relieved.After test 24 hours,
With 30wt%EDTMPA-Na be water flux rate of descent when drawing liquid lower than the EDTMPA-Na that 3mg is added directly into feed liquid when
Flux rate of descent.In positive process of osmosis, forward osmosis membrane can be passed through and spread to feed liquid, meeting by drawing the EDTMPA-Na in liquid
There is higher concentration near the interface that feed liquid and film are formed, so as to play good scale inhibition effect.Conventional control film knot
Dirt pollution needs intermittently to be added the antisludging agent of certain mass into feed liquid, and additional amount needs accurately calculate, and otherwise will cause
The waste of medicament, and with organic phosphonate compound be draw liquid control forward osmosis membrane surface scale pollution operating method letter
It is single and efficient.
In addition, the effect of common antisludging agent EDTA-Na in this experiment is also provided a comparison of, with same substance amount concentration
For EDTMPA-Na or EDTA-Na as liquid is drawn, concentration is set as 0.5M, is made with the calcium sulfate saturated solution that saturation index is 1.6
For feed liquid, the Aquaporin Inside of commercialization is selectedTMForward osmosis membrane is the long-time test that forward osmosis membrane carries out 24 hours,
Investigate the difference of film scaling fouling situation.
Water flux keep result as shown in fig. 6, with 0.5M EDTMPA-Na be draw liquid when, water flux conservation rate be higher than with
For 0.5M EDTA-Na as water flux conservation rate when drawing liquid, this illustrates that EDTMPA-Na ratio EDTA-Na draws solute just
There are superior scale-inhibiting properties in process of osmosis.Organic phosphonate compound after dilution draws solution and may be directly applied to
Boiler cooling water recirculation system or oil field reinjection water can inhibit boiler or oil field stratum pipeline scaling.Draw the direct benefit of liquid
With eliminating the diluted energy for drawing and consuming required for liquid regenerative process.
In conclusion organic phosphonate compound provided by the invention is just permeating and is drawing liquid and can produce higher water flux
With lower reversed Solute flux.In the mineral scale Contamination measurement of film, the organic phosphonate compound reversely spread is drawn
The mineral scale for taking solute that can inhibit film surface pollutes.Liquid phase ratio is drawn with common antisludging agent edetate,
Ethylenediamine tetramethylene phosphonic acid salt draws liquid has more excellent scale-inhibiting properties in positive process of osmosis.Positive process of osmosis terminates
Afterwards, diluted organic phosphonate compound draws liquid and does not need to be regenerated, and may be directly applied to boiler cooling water recirculation system
Or oil field reinjection water, inhibit boiler or oil field stratum pipeline scaling, eliminates the energy consumed required for drawing liquid regenerative process.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (10)
1. the application that organic phosphonate compound draws solute as positive infiltration, which is characterized in that the organic phosphonate chemical combination
Object has chemical structural formula shown in formula I；
In the Formulas I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and others are H；Or R1、R2、R3、R4、R5、
R6、R7And R8At least one is K, and others are H；
In the Formulas I, n 1,2 or 3.
2. application as described in claim 1, which is characterized in that the positive infiltration is drawn what solute was used to obtain after just permeating
The diluted liquid that draws is applied to antisludging agent.
3. application as claimed in claim 2, which is characterized in that the positive infiltration is drawn what solute was used to obtain after just permeating
The diluted liquid that draws is applied to boiler cooling circulating water or the antisludging agent of oil field reinjection water.
4. application as described in claim 1, which is characterized in that solute is drawn in the positive infiltration and is configured to containing mass fraction
Solution for the organic phosphonate compound of 5%-35% draws liquid as positive infiltration.
5. application as claimed in claim 4, which is characterized in that the mass fraction of the organic phosphonate compound is 15%-
30%.
6. application as described in claim 1, which is characterized in that drawing solute to be configured to pH value by the positive infiltration is 5-10's
Solution draws liquid as positive infiltration.
7. a kind of positive permeability apparatus, which is characterized in that the liquid that draws of the positive permeability apparatus is organic phospho acid salting liquid, described organic
Phosphonate has chemical structural formula shown in formula I；
In the Formulas I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and others are H；Or R1、R2、R3、R4、R5、
R6、R7And R8At least one is K, and others are H；
In the Formulas I, n 1,2 or 3.
8. positive permeability apparatus as claimed in claim 7, which is characterized in that organic phosphonate in the organic phospho acid salting liquid
Mass fraction is 5%-35%；The pH value of the organic phospho acid salting liquid is 5-10；
Preferably, the mass fraction of organic phosphonate is 15%-30% in the organic phospho acid salting liquid.
9. positive permeability apparatus as claimed in claim 7 or 8, which is characterized in that the permeable membrane of the positive permeability apparatus is plate membrane
Or hollow-fibre membrane.
10. positive permeability apparatus as claimed in claim 7 or 8, which is characterized in that the permeable membrane of the positive permeability apparatus is polysulfones base
Forward osmosis membrane, polyvinylidene fluoride forward osmosis membrane or polyethers sulfuryl forward osmosis membrane.
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