CN109316965B - Application of organic phosphonate as forward osmosis drawing solute and forward osmosis device - Google Patents
Application of organic phosphonate as forward osmosis drawing solute and forward osmosis device Download PDFInfo
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- CN109316965B CN109316965B CN201811227206.2A CN201811227206A CN109316965B CN 109316965 B CN109316965 B CN 109316965B CN 201811227206 A CN201811227206 A CN 201811227206A CN 109316965 B CN109316965 B CN 109316965B
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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
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Abstract
The invention discloses application of organic phosphonate as a forward osmosis drawing solute and a forward osmosis device, belonging to the technical field of forward osmosis. The chemical structural formula of the organic phosphonate compound is as follows:
wherein R is1、R2、R3、R4、R5、R6、R7And R8At least one is Na or K, the others are H, and n is 1, 2 or 3. And applying the diluted draw solution obtained after the forward osmosis of the forward osmosis draw solute to the scale inhibitor. The application is that the forward osmosis draw solute is prepared into a solution containing 5-35% of the organic phosphonate compound by mass as a forward osmosis draw solution, preferably 15-30% of the organic phosphonate compound by mass, and the pH value of the forward osmosis draw solution is 5-10. The forward osmosis draw solute has high water flux and small reverse solute flux in the forward osmosis process; has good scale inhibition effect of the forward osmosis membrane, and the diluted draw solution is directly applied to scale inhibition.
Description
Technical Field
The invention belongs to the technical field of forward osmosis, and particularly relates to application of an organic phosphonate compound as a forward osmosis draw solute and a forward osmosis device.
Background
Under the background of the increasing shortage of fresh water resources and the gradual reduction of the reserves of non-renewable energy resources, water treatment technologies with low energy consumption are vigorously developed in all countries in the world. The membrane water treatment technology plays an important role in the field of water treatment due to the advantages of high treatment efficiency, small occupied area, easiness in amplification and the like. In the conventional membrane water treatment technologies such as nanofiltration and reverse osmosis, water molecules permeate through a membrane by using pressure generated by a pump as a driving force, and solutes such as salts and small-molecule organic matters are trapped, so that pure water is obtained. However, these membrane technologies often have problems of high energy consumption and serious membrane pollution during the application process. Forward osmosis is a new membrane water treatment technology in the 21 st century, and attracts more and more researchers' attention. Forward osmosis is a spontaneous process that uses the osmotic pressure gradient across the draw solution and feed solution as the driving force to effect the transfer of water molecules. Compared with the traditional membrane technology, the forward osmosis has the advantages of low energy consumption, high solute rejection rate, low membrane pollution tendency and the like, and shows great application potential in the fields of seawater desalination, wastewater treatment, food processing, drug concentration and the like.
The forward osmosis draw solution is a key element of the forward osmosis process, the water flux of the forward osmosis process is determined by the osmotic pressure, and the reverse solute flux of the forward osmosis process is determined by the molecular size of the forward osmosis draw solution. In the forward osmosis process, water molecules on the feed liquid side continuously enter the liquid drawing side, dilution of the drawing liquid is caused, the osmotic pressure of the drawing liquid is reduced, and accordingly flux is reduced, and therefore the drawing liquid needs to be concentrated to ensure continuous and stable water flux output in the forward osmosis process. The regeneration process of the drawing liquid generally needs to consume more energy, so that a recovery method with low energy consumption is found, or the diluted drawing liquid can be directly applied to the actual production and life process, which is very significant.
When a forward osmosis process is used for treating water samples which are easy to scale, such as seawater, brackish water, mineral wastewater and the like, the same problems as those of the traditional membrane process are encountered, and mineral scaling is easy to occur on the surface of the membrane. Mineral scale formation is a membrane pollution phenomenon, and means that mineral solid matters are formed on the surface of a membrane, the transmission resistance of water molecules is increased, so that flux is reduced, and a filter cake layer is formed in serious conditions, so that the flux is seriously reduced, even the flux is reduced to zero. Fouling on the membrane surface can reduce the separation efficiency of the membrane, increase the cleaning frequency, and increase the replacement cost of the membrane. Chemical cleaning and physical cleaning are common methods for removing mineral scale on the surface of the membrane, and these methods have poor effects on hard, strong adhesive force and poor acid solubility mineral scale such as calcium sulfate, barium sulfate and other mineral scale, and are easy to cause irreversible damage to the membrane. Another method for relieving the mineral scale on the surface of the membrane is to add a certain amount of scale inhibitor into the feed liquid in the pretreatment process, and the type, the addition concentration and the addition period of the scale inhibitor put high requirements on the actual operation. Therefore, the method which is simple and convenient to operate and can effectively relieve the membrane fouling pollution problem in the forward osmosis process is significant to find.
Disclosure of Invention
The invention solves the technical problems that the water flux is low, the reverse solute flux is large, the forward osmosis membrane is polluted by scale, and the diluted draw solution can not be directly applied in the forward osmosis process in the prior art.
To achieve the above objects, according to one aspect of the present invention, there is provided a use of an organic phosphonate compound as a forward osmosis draw solute, the organic phosphonate compound having a chemical structural formula as shown in formula I;
in the formula I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and the others are H; or R1、R2、R3、R4、R5、R6、R7And R8At least one is K, and the others are H;
in the formula I, n is 1, 2 or 3.
Preferably, the forward osmosis draw solute is applied to a diluted draw solution obtained after forward osmosis, and the diluted draw solution is applied to a scale inhibitor.
Preferably, the forward osmosis draw solute is used as a diluted draw solution obtained after forward osmosis, and the diluted draw solution is applied to the scale inhibitor of boiler cooling circulating water or oilfield reinjection water.
Preferably, the forward osmosis draw solute is prepared into a solution containing 5-35% by mass of the organic phosphonate compound as a forward osmosis draw solution.
Preferably, the mass fraction of the organic phosphonate compound is 15-30%.
Preferably, the forward osmosis draw solute is formulated as a solution having a pH of 5-10 as the forward osmosis draw solution.
According to another aspect of the invention, a forward osmosis device is provided, wherein a draw solution of the forward osmosis device is an organic phosphonate solution, and the organic phosphonate has a chemical structural formula shown as a formula I;
in the formula I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and the others are H; or R1、R2、R3、R4、R5、R6、R7And R8At least one is K, and the others are H;
in the formula I, n is 1, 2 or 3.
Preferably, the mass part of the organic phosphonate in the organic phosphonate solution is 5-35%; the pH value of the organic phosphonate solution is 5-10;
preferably, the mass fraction of the organic phosphonate in the organic phosphonate solution is 15-30%.
Preferably, the permeable membrane of the forward osmosis device is a flat sheet membrane or a hollow fiber membrane.
Preferably, the permeable membrane of the forward osmosis device is a polysulfone-based forward permeable membrane, a polyvinylidene fluoride-based forward permeable membrane or a polyethersulfone-based forward permeable membrane.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
(1) the invention adopts the organic phosphonate with the molecular weight of 400Da-800Da as the forward osmosis draw solute, and the molecular volume of the organic phosphonate is obviously larger than that of the common NaCl draw solute, and the dissociated organic phosphonate anion has more negative charges and can form stronger electrostatic repulsion with the forward osmosis membrane with negative surface charge, so that the organic phosphonate anion is difficult to permeate through the forward osmosis membrane, thereby effectively solving the problem of large reverse solute flux.
(2) When the mass concentration of the solution of the ethylene diamine tetra methylene phosphonic acid sodium salt (EDTMPA-Na) in the forward osmosis drawing solution is 30%, the water flux of the solution is equivalent to that of a 1M NaCl drawing solution, and the reverse solute flux of the solution is only one third of that of the 1M NaCl drawing solution.
(3) The organic phosphonate used in the invention is an excellent scale inhibitor, the absorption solute leaked in the forward osmosis process can slow down mineral scale pollution on the surface of the forward osmosis membrane, and the organic phosphonate has an excellent control effect on calcium sulfate scale pollution on the surface of the osmosis membrane.
(4) According to the invention, mineral scale pollution on the membrane surface is slowed down by drawing solute through organic phosphonate leaked in the forward osmosis process, and compared with the method of directly adding organic phosphonate with the same mass into feed liquid, organic phosphonate with higher concentration is arranged near the interface of the feed liquid and the membrane, so that the scale inhibition effect is better.
(5) The ethylene diamine tetraacetic acid disodium salt (EDTMPA-Na) adopted by the invention is used as a forward osmosis drawing solute and has better scale inhibition effect than ethylene diamine tetraacetic acid disodium salt (EDTA-Na).
(6) The organic phosphonate adopted by the invention is used as a forward osmosis drawing solute, and the diluted drawing solution does not need to be regenerated, and can be directly applied to a boiler cooling water circulation system and oilfield reinjection water to inhibit scaling of a boiler or an oilfield formation pipeline, so that the energy consumed in the regeneration process of the diluted drawing solution can be saved.
Drawings
Fig. 1 is a graph showing the results of a forward osmosis water flux test.
Figure 2 is a graph of forward osmosis reverse solute flux test results.
FIG. 3 is a graph of the results of a forward osmosis process membrane fouling control test.
FIG. 4 is an electron micrograph of the membrane after a membrane fouling control test in the forward osmosis process.
FIG. 5 is a graph obtained by directly adding a certain mass of ethylenediaminetetramethylenephosphonic acid sodium salt (EDTMPA-Na) to a calcium sulfate saturated solution having a saturation index of 1.6 with 1M NaCl as an extraction solution, and comparing the result with that of the extraction solution with 30 wt% EDTMPA-Na.
FIG. 6 is a graph showing the results of a membrane fouling control test in forward osmosis process comparing ethylenediaminetetramethylenephosphonic acid sodium salt (EDTMPA-Na) with ethylenediaminetetraacetic acid sodium salt (EDTA-Na).
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The invention provides a forward osmosis drawing liquid, wherein the pH value of the forward osmosis drawing liquid is 5-10, and an organic phosphonate with the mass concentration range of 5-35% (preferably 15-30%) is used as the forward osmosis drawing liquid, and the organic phosphonate compound has a chemical structural formula shown in a formula I;
in the formula I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and the others are H; or R1、R2、R3、R4、R5、R6、R7And R8At least one is K and the others are H.
In the formula I, n is 1, 2 or 3.
Example 1
(1) Commercial ethylenediamine tetramethylene phosphonic acid (EDTMPA) is dissolved in deionized water, the pH value is adjusted to 7 by NaOH to obtain an ethylenediamine tetramethylene phosphonic acid sodium salt solution, and then the solution is purified for 72 hours by a dialysis bag with the molecular weight cutoff of 100Da to obtain a clean pure substance.
(2) Distilling the solution of the ethylenediamine tetramethylene phosphonic acid sodium obtained in the step (1) under reduced pressure, and then drying for 12 hours under vacuum at 75 ℃ to obtain the EDTMPA-Na solid.
Example 2
(1) Commercial ethylenediamine tetramethylene phosphonic acid (EDTMPA) is dissolved in deionized water, the pH value is adjusted to 7 by KOH, an ethylenediamine tetramethylene phosphonic acid potassium salt solution is obtained, and then the solution is purified for 72 hours by a dialysis bag with the molecular weight cutoff of 100Da, so that a clean pure substance is obtained.
(2) Distilling the solution of the ethylene diamine tetra methylene phosphonic acid potassium obtained in the step (1) under reduced pressure, and then drying the solution for 12 hours under vacuum at 75 ℃ to obtain the EDTMPA-K solid.
Example 3
(1) Commercial Ethylene Diamine Tetraacetic Acid (EDTA) is dissolved in deionized water, the pH value is adjusted to 7 by NaOH to obtain ethylene diamine tetraacetic acid sodium salt solution, and then the solution is purified for 72 hours by a dialysis bag with the molecular weight cutoff of 100Da to obtain a clean pure substance.
(2) Distilling the sodium ethylene diamine tetracetate solution obtained in the step (1) under reduced pressure, and then drying for 12 hours in vacuum at 75 ℃ to obtain the EDTA-Na solid.
And (4) analyzing results:
dissolving the solid in the example 1 in deionized water, preparing drawing liquid with the mass fractions of 10 wt%, 15 wt%, 20 wt%, 25 wt% and 30 wt%, taking the deionized water as feed liquid, and using commercial Aquaporin InsideTMForward osmosis membranes were tested for forward osmosis. The test conditions are that the solution temperature is 25 +/-1 ℃, and the effective membrane area is 3.87cm2The water flow rate was 0.3L/min, each concentration was tested for 1.5 hours, and the test was repeated 3 times with three brand new membranes under the same conditions, and the average was taken.
The forward osmosis water flux results are shown in fig. 1, and the forward osmosis reverse solute quality results are shown in fig. 2: the results show that the sodium ethylene diamine tetra methylene phosphonate (EDTMPA-Na) described in example 1 has higher water flux and lower reverse solute flux; at a concentration of 30 wt%, the water flux of example 1 can reach 45.0L m in the draw solution mode of the active layer of the membrane-2h-1Reverse solute flux of about 3.4g m-2h-1。
With 30 wt.% EDTMPA-Na or 1M NaCl asDrawing liquid, taking a calcium sulfate saturated solution with a saturation index of 1.6 as a feed liquid, wherein the concentrations of sodium chloride, sodium sulfate and calcium sulfate in the calcium sulfate saturated solution are respectively 24mM, 25mM and 44mM, and commercial Aquaporin oxide is selectedTMThe forward osmosis membrane is subjected to long-time test for 24 hours, and the difference of fouling conditions of the membrane is examined.
After 24 hours of the test, as shown in FIG. 3, the flux decreased by about 15% when 30 wt% EDTMPA-Na was used as the draw solution; when 1M NaCl is used as the draw solution, the water flux reduction rate is about 40%, which is obviously higher than that of the former, so that the fouling phenomenon is serious when NaCl is used as the draw solution, and the fouling phenomenon on the surface of the forward osmosis membrane is light when EDTMPA-Na is used as the draw solution. The tested membrane is characterized by a scanning electron microscope, as shown in fig. 4, more particles appear on the surface of the membrane using 1M NaCl as the draw solution, and less particles appear on the membrane using 30 wt% EDTMPA-Na as the draw solution, which proves that the fouling phenomenon on the surface of the forward osmosis membrane is less when EDTMPA-Na is used as the draw solution. This is because EDTMPA-Na is an excellent scale inhibitor for CaSO4、BaSO4The scale inhibition effect of the mineral matters is obvious. In the forward osmosis process, the EDTMPA-Na drawing solute diffused reversely can be mixed with Ca in the feed liquid2+Chelating to reduce Ca in the feed liquid2+The concentration of (c); EDTMPA-Na can also be adsorbed on mineral crystals to prevent further growth, thereby relieving the scaling pollution on the surface of the forward osmosis membrane.
The method comprises the steps of directly adding a certain mass of EDTMPA-Na into calcium sulfate saturated solution feed liquid with the saturation index of 1.6, carrying out 24-hour test by taking 1M NaCl as an extraction liquid, inspecting the pollution condition of a membrane, and comparing test results by taking 30 wt% EDTMPA-Na solution as the extraction liquid.
As shown in FIG. 5, the water flux reduction rate increases with the addition of EDTMPA-Na in the feed liquid, which indicates that EDTMPA-Na is an excellent scale inhibitor and can effectively relieve the scaling pollution on the surface of the forward osmosis membrane. After 24 hours of the test, the rate of decrease in water flux with 30 wt% EDTMPA-Na as draw solution was lower than that with 3mg of EDTMPA-Na added directly to the feed solution. In the forward osmosis process, EDTMPA-Na in the drawing liquid penetrates through the forward osmosis membrane and diffuses towards the feed liquid, and the concentration of the EDTMPA-Na in the drawing liquid is higher near an interface formed by the feed liquid and the membrane, so that a good scale inhibition effect can be achieved. The conventional method for controlling the fouling pollution of the fouling on the surface of the forward osmosis membrane by using the organic phosphonate compound as an extraction solution is simple and efficient.
In addition, compared with the effect of the common scale inhibitor EDTA-Na in the experiment, EDTMPA-Na or EDTA-Na with the same mass concentration is used as an extraction solution, the concentration is set to be 0.5M, a calcium sulfate saturated solution with the saturation index of 1.6 is used as a feed solution, and a commercial Aquaporin oxide is selectedTMThe forward osmosis membrane is subjected to long-time test for 24 hours, and the difference of fouling conditions of the membrane is examined.
The water flux retention results are shown in fig. 6, when 0.5M EDTMPA-Na is used as the draw solution, the water flux retention rate is higher than that when 0.5M EDTA-Na is used as the draw solution, which indicates that EDTMPA-Na has more excellent scale inhibition performance than EDTA-Na draw solute in the forward osmosis process. The diluted organic phosphonate compound drawing solution can be directly applied to a boiler cooling water circulation system or oilfield reinjection water, and can inhibit scaling of a boiler or an oilfield formation pipeline. The direct utilization of the drawing liquid saves the energy consumed in the regeneration process of the diluted drawing liquid.
In summary, the organic phosphonate compound forward osmosis draw solution provided by the invention can generate higher water flux and lower reverse solute flux. In a membrane mineral scale fouling test, a back-diffusing organophosphate compound draw solute can inhibit mineral scale fouling of the membrane surface. Compared with the common scale inhibitor, namely the ethylene diamine tetraacetic acid salt draw solution, the ethylene diamine tetramethylene phosphonate draw solution has more excellent scale inhibition performance in the forward osmosis process. After the forward osmosis process is finished, the diluted organic phosphonate compound absorption liquid does not need to be regenerated, and can be directly applied to a boiler cooling water circulation system or oilfield reinjection water to inhibit scaling of a boiler or an oilfield stratum pipeline and save energy consumed in the absorption liquid regeneration process.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (11)
1. The application of the organic phosphonate compound as a forward osmosis drawing solute is characterized in that the organic phosphonate compound has a chemical structural formula shown in a formula I;
in the formula I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and the others are H; or R1、R2、R3、R4、R5、R6、R7And R8At least one is K, and the others are H;
in the formula I, n is 1, 2 or 3.
2. The use of claim 1, wherein the diluted draw solution obtained after the forward osmosis draw solute is used in forward osmosis is used in a scale inhibitor.
3. The application of claim 2, wherein the diluted draw solution obtained after the forward osmosis draw solute is used for forward osmosis is applied to a scale inhibitor of boiler cooling circulating water or oilfield reinjection water.
4. The use of claim 1, wherein the forward osmotic draw solute is formulated as a solution containing from 5% to 35% by weight of the organophosphonate compound as a forward osmotic draw solution.
5. The use of claim 4, wherein the organic phosphonate compound is present in an amount of 15% to 30% by weight.
6. The use of claim 1, wherein the forward draw solute is formulated as a solution having a pH of 5 to 10 as the forward draw solution.
7. A forward osmosis device is characterized in that an absorption liquid of the forward osmosis device is an organic phosphonate solution, and the organic phosphonate has a chemical structural formula shown in a formula I;
in the formula I, R1、R2、R3、R4、R5、R6、R7And R8At least one is Na, and the others are H; or R1、R2、R3、R4、R5、R6、R7And R8At least one is K, and the others are H;
in the formula I, n is 1, 2 or 3.
8. The forward osmosis apparatus of claim 7, wherein the organic phosphonate solution comprises 5% to 35% by weight of organic phosphonate; the pH value of the organic phosphonate solution is 5-10.
9. The forward osmosis apparatus of claim 8, wherein the organic phosphonate solution comprises 15% to 30% by weight of organic phosphonate.
10. A forward osmosis apparatus according to claim 7 or 8, wherein the permeable membrane of the forward osmosis apparatus is a flat sheet membrane or a hollow fibre membrane.
11. A forward osmosis apparatus according to claim 7 or 8, wherein the permeable membrane of the forward osmosis apparatus is a polysulfone-based forward osmosis membrane, a polyvinylidene fluoride-based forward osmosis membrane or a polyethersulfone-based forward osmosis membrane.
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| 杨菲菲.改性聚偏氟乙烯螯合膜吸附铅离子的研究.《中国优秀硕士学位论文全文数据库》.2018,(第5期),第3-9页. * |
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