CN112051198A - Quantitative evaluation method for pore diameter of porous membrane - Google Patents
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- 239000012528 membrane Substances 0.000 title claims abstract description 102
- 239000011148 porous material Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000011158 quantitative evaluation Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 44
- 230000035699 permeability Effects 0.000 claims abstract description 27
- 238000009792 diffusion process Methods 0.000 claims abstract description 11
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 9
- 238000009292 forward osmosis Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 45
- 229920000867 polyelectrolyte Polymers 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 230000004907 flux Effects 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 4
- 229920001448 anionic polyelectrolyte Polymers 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000011156 evaluation Methods 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 238000010998 test method Methods 0.000 abstract 1
- 230000000149 penetrating effect Effects 0.000 description 9
- 239000012466 permeate Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 230000007547 defect Effects 0.000 description 6
- 230000008859 change Effects 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- MAGFQRLKWCCTQJ-UHFFFAOYSA-N 4-ethenylbenzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=C(C=C)C=C1 MAGFQRLKWCCTQJ-UHFFFAOYSA-N 0.000 description 1
- 229920002307 Dextran Polymers 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 102100023116 Sodium/nucleoside cotransporter 1 Human genes 0.000 description 1
- 101710123675 Sodium/nucleoside cotransporter 1 Proteins 0.000 description 1
- 102100021541 Sodium/nucleoside cotransporter 2 Human genes 0.000 description 1
- 101710123669 Sodium/nucleoside cotransporter 2 Proteins 0.000 description 1
- 102100021470 Solute carrier family 28 member 3 Human genes 0.000 description 1
- 101710186856 Solute carrier family 28 member 3 Proteins 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011033 desalting Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002048 multi walled nanotube Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
- G01N15/0826—Investigating permeability by forcing a fluid through a sample and measuring fluid flow rate, i.e. permeation rate or pressure change
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/086—Investigating permeability, pore-volume, or surface area of porous materials of films, membranes or pellicules
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- Health & Medical Sciences (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a quantitative evaluation method for the pore diameter of a porous membrane, which comprises the steps of firstly measuring the convection permeability coefficients of membrane materials with different molecular weight cut-off and a membrane material to be measured, and then establishing the molecular weight cut-off M of the membrane materialwAnd convective permeability coefficient LdLinear relation between them, finally substituting the convection permeability coefficient of the membrane material to be tested into MwAnd LdThe convection diffusion coefficient M of the film is further obtainedw. The method can greatly reduce the dosage of test reagents, test time and test procedures, does not need expensive evaluation devices, and has good application value in quantitative evaluation of the pore diameters of porous membranes such as ultrafiltration membranes, ultrafiltration type forward osmosis membranes and the like.
Description
Technical Field
The invention belongs to the technical field of membrane parameter evaluation, and particularly relates to a quantitative evaluation method for pore diameter of a porous membrane.
Background
The method can accurately determine the pore size of the porous membrane, and has important guiding significance for the regulation and control and the application development of the porous membrane structure. Currently, a commonly used method for evaluating the pore size of a porous membrane is a molecular weight cut-off Method (MWCO). The method calculates the pore size of the porous membrane by measuring the retention rate of the porous membrane to a series of substances with different molecular weights. In order to obtain retention rate data, the MWCO method needs to determine a standard working curve of a standard substance in advance; in addition, in the case of unknown pore, the pore size must be estimated. Therefore, the MWCO method has the disadvantages of complicated operation steps, high time cost, large reagent consumption and large-scale instrument assistance. Therefore, it is important to find a more convenient and efficient method for evaluating the pore diameter of the porous membrane.
In the field of dense membranes, researchers have provided a dissolution-diffusion defect model to describe its permeation-selection mechanism, and demonstrated that the convective permeability coefficient of desalinized dense membranes can enable quantification of membrane surface defects. Based on this, the invention proposes to apply the convective permeability coefficient to the quantitative evaluation of the pore size of the porous membrane. The difference from the desalting membrane is that the defect condition of the surface of the porous membrane is evaluated by using macromolecular polyelectrolyte as solute of feed liquid, and the pore size of the porous membrane is quantified from the side. The method uses only a specific macromolecular polyelectrolyte and can achieve regeneration by simple filtration. Therefore, the method has important significance for green, simple and economical evaluation of membrane parameters.
Disclosure of Invention
The invention provides a quantitative evaluation method for the pore diameter of a porous membrane, which can quickly, simply and economically quantify the pore diameter of the porous membrane and solve the problems of complicated operation, reagent consumption and the like of the conventional molecular weight cut-off method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a quantitative evaluation method for pore diameter of a porous membrane specifically comprises the following steps:
(1) selecting a plurality of known membrane materials with different molecular weight cut-off and membrane materials to be detected, placing the membrane materials and the membrane materials into a membrane pool, introducing a macromolecular polyelectrolyte solution with a certain concentration into the feed liquid side of the membrane pool, communicating pure water with the permeation side, driving the solutions at the two sides to flow through a gear pump, and controlling the temperature of the macromolecular polyelectrolyte solution and the temperature of the pure water to be constant;
(2) emptying system bubbles, and after the temperature of the system is reached, regularly recording the lateral pressure, flow, volume, mass, concentration and other parameters of a feed liquid side and a permeation side at a certain temperature;
(3) after the operation pressure is changed, repeating the operation of the step (2);
(4) calculating the water flux J of different membrane materials according to the first formula and the second formulawAnd salt flux Js，
In the formula, piLowAnd piHiRespectively the osmotic pressure of the raw material liquid side and the draw liquid side; dsThe diffusion coefficient of the solute is 1.61X 10 when the solute is sodium chloride-9m2S; s is a membrane structure parameter
t, and τ are the thickness, porosity and pore tortuosity of the membrane, respectively;
in the formula, beta is a van t hough coefficient; r is a molar gas constant; t is the absolute temperature; a is the permeability coefficient of pure water; b is the permeability coefficient of the solute;
(5) calculating the convection permeability coefficient L of the membrane materials with different known molecular weight cut-off and the membrane material to be measured according to the formula IIId，
In the formula, Cfeed,sThe initial concentration of the feed liquid;
(6) molecular weight cut-off M based on known membrane materialswAnd convective permeability coefficient LdCalculating the molecular weight M of the trapped materialwAnd convective permeability coefficient LdA linear relationship therebetween;
(7) substituting the convection permeability coefficient of the membrane material to be tested obtained in the step (5) into the convection permeability coefficient of the membrane material to be tested in the step (6)wAnd LdThe convection diffusion coefficient M of the film is further obtainedw。
Preferably, the porous membrane includes, but is not limited to, an ultrafiltration membrane, a forward osmosis porous composite membrane; the macromolecular polyelectrolyte includes, but is not limited to, an anionic polyelectrolyte represented by sodium poly (p-styrenesulfonate), a neutral polyelectrolyte represented by dextran, and a cationic polyelectrolyte represented by polyethyleneimine.
A quantitative evaluation device for the pore diameter of a porous membrane comprises a membrane pool, a material liquid tank, a permeating liquid tank, a first gear pump, a second gear pump, a first pressure gauge, a second pressure gauge, a first conductivity meter, a second conductivity meter, a first temperature control system, a second temperature control system and an electronic balance, wherein the membrane pool is divided into a material liquid side and a permeating side by a membrane material, the material liquid side forms a material liquid circulation loop with the material liquid tank through the first gear pump, the permeating side forms a permeating liquid circulation loop with the permeating liquid tank through the second gear pump, the first conductivity meter and the second conductivity meter are respectively arranged in the material liquid tank and the permeating liquid tank, the first pressure meter and the first flow meter are arranged on a pipeline at the front end of the material liquid side, the second pressure meter and the second flow meter are arranged on a pipeline at the front end of the permeating side, the first temperature control system is arranged on the material liquid circulation loop to ensure the temperature of the circulating material liquid to be constant, the temperature of the circulating penetrating fluid is ensured to be constant, the electronic balance is fixed at the bottom of the penetrating fluid tank, and the change of the mass of the solution in the penetrating fluid tank is monitored in real time.
The pore diameter of the porous membrane is evaluated by using the convective permeability coefficient, and the method is obviously different from the conventional pore diameter evaluation method in that the pore diameter of the membrane is not directly measured, but the defect condition of the membrane is evaluated by using the convective permeability coefficient. The method is characterized in that a convection permeability coefficient concept in a dissolution-diffusion defect model theory for describing permeation-selectivity performance of a compact membrane is applied to assessment of the pore diameter or defect degree of the porous membrane for the first time, a certain macromolecular polyelectrolyte solution under a certain concentration is used as a raw material solution, and the convection diffusion coefficient of the porous membrane can be obtained by measuring the diffusion flux of electrolytes under different pressures and simple linear fitting.
Compared with the prior art, the invention has the following advantages: (1) the evaluation equipment is simple, and only a conventional measuring instrument is needed to realize data recording and measurement; (2) the operation steps are few, and only the mass change and the conductivity change under different pressures need to be measured; (3) the reagent dosage is less, only macromolecular polyelectrolyte is needed, and the porous membrane can be recycled, so that the porous membrane has excellent application value in the aspect of porous membrane pore size evaluation.
Description of the drawings:
FIG. 1 is a schematic diagram of the method for quantitative evaluation of pore size of a porous membrane according to the present invention.
FIG. 2 is a schematic diagram of a quantitative evaluation apparatus for pore diameter of a porous membrane according to the present invention.
FIG. 3 is a graph of the convective permeability coefficient data fit for the porous membrane of example 1
FIG. 4 is a graph of data fit for the porous composite membrane of example 2
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
As shown in figure 2, a porous membrane aperture quantitative assessment device, including a membrane pool, a feed liquid tank 9, a permeate liquid tank 2, a first gear pump 10, a second gear pump 3, a first pressure gauge 8, a second pressure gauge 5, a first conductivity meter, a second conductivity meter, a first temperature control system 11, a second temperature control system 4 and an electronic balance 1, the membrane pool is divided into a feed liquid side 7 and a permeate side 6 by a membrane material, the feed liquid side 7 and the feed liquid tank 9 form a feed liquid circulation loop through the first gear pump 10, the permeate side 6 and the permeate liquid tank 2 form a permeate liquid circulation loop through the second gear pump 3, the feed liquid tank 9 and the permeate liquid tank 2 are respectively provided with the first conductivity meter and the second conductivity meter, the first pressure gauge 8 and a first flowmeter are arranged on a pipeline at the front end of the feed liquid side 7, the second pressure gauge 5 and a second flowmeter are arranged on a pipeline at the front end of the permeate side 6, the first temperature control system 11 is installed on the feed liquid circulation loop, the temperature of the circulating feed liquid is guaranteed to be constant, the second temperature control system 4 is installed on a penetrating liquid circulating loop to guarantee the temperature of the circulating penetrating liquid to be constant, the electronic balance 1 is arranged at the bottom of the feed liquid tank 9 or the bottom of the penetrating liquid tank 2 and used for measuring the change of the quality of the solution in the feed liquid tank 9 and the penetrating liquid tank 2, the macromolecular polyelectrolyte is introduced into the feed liquid side, and the pure water is introduced into the penetrating side.
The device for quantitatively evaluating the pore diameter of the porous membrane further comprises a control processing unit, wherein the control processing unit is respectively connected with a first gear pump 10, a second gear pump 3, a first pressure gauge 8, a second pressure gauge 5, a first conductivity meter, a second conductivity meter, a first temperature control system 11, a second temperature control system 4 and an electronic balance 1, controls all parts to work, collects detection data in real time, and calculates the convective permeability coefficient L of membrane materials with known different molecular weight cut-off and membrane materials to be detected according to a formula I, a formula II and a formula IIIdThen based on the molecular weight cut-off M of the known membrane materialwAnd convective permeability coefficient LdCalculating the molecular weight M of the same material liquid and the membrane materialwAnd convective permeability coefficient LdLinear relation between the two, finally substituting the convection permeability coefficient of the membrane material to be measured into MwAnd LdThe convection diffusion coefficient M of the film material to be measured is obtainedw。
Furthermore, the quantitative evaluation device for the pore diameter of the porous membrane can also adopt an ultrafiltration cup for evaluation, and pressure control is realized through a pressure tank.
Ultrafiltration membranes (designated UF-1, UF-2, UF-3, UF-4) with nominal molecular weight cut-off of 9000, 20000, 29000, 67000 Da. Selecting sodium polyterephtylenesulfonate (concentration is 1g/L) with weight-average molecular weight of 70000Da as raw material liquid, and deionized water as penetrating fluid, and obtaining the ratio of salt flux to raw material liquid concentration (J) under different operation pressuress/Cfeed,s) As shown in table 1. Operating pressure is used as abscissa, and J is useds/Cfeed,sThe values are plotted on the ordinate (as shown in FIG. 3), and the convective permeability coefficients of different ultrafiltration membranes, UF-1, UF-2, UF-3 and UF-4, are determined by least squares method, corresponding to 1.683LMH/bar, 3.775LMH/bar, 4.497LMH/bar and 9.925LMH/bar, respectively. For molecular weight cut-off LdAnd convective diffusion coefficient MwBy performing a linear fit, it can be found that both conform to Ld＝0.1530MwWherein R is20.9893. Description of LdThe pore size of the porous membrane can be quantitatively evaluated.
TABLE 1 Ultrafiltration membranes in different operationsJ under pressures/Cfeed,sValue of
Example 2
Selecting a CA water-washed cellulose acetate membrane with the pore diameter of 2 microns as a base membrane, carrying out suction filtration on dopamine-modified multi-walled carbon nanotube dispersion liquid on the surface of the base membrane, respectively carrying out suction filtration on 1 ml, 3 ml, 4 ml and 5ml (respectively marked as CNT-1, CNT-2, CNT-3 and CNT-4), standing and drying, and measuring the molecular weight cut-off by using a molecular weight cut-off method to obtain the molecular weight cut-off of 57000, 25000, 20000 and 10000Da respectively. In the same way, the ratio of the flux of the obtained salt to the concentration of the feed solution (Js/C) was tested at different operating pressuresfeed,s) As shown in table 2. Operating pressure is used as abscissa, and J is useds/Cfeed,sThe values are plotted on the ordinate (as shown in FIG. 4), and the convective permeability coefficients of different ultrafiltration membranes can be obtained by using the least square method, wherein PC-1, PC-2, PC-3 and PC-4 correspond to 5.413LMH/bar, 4.20LMH/bar, 3.83LMH/bar and 3.67LMH/bar, respectively. The molecular weight cut-off and the convection diffusion coefficient are subjected to linear fitting, and the two can be found to accord with Ld＝0.3851Mw+3.20, wherein R20.9774. Description of LdThe pore size of the porous composite membrane can be quantitatively evaluated.
Table 2 porous composite membranes J at different operating pressuress/Cfeed,sValue of
Claims (2)
1. A quantitative evaluation method for pore diameter of a porous membrane is characterized by comprising the following steps:
(1) selecting a plurality of known membrane materials with different molecular weight cut-off and membrane materials to be detected, placing the membrane materials and the membrane materials into a membrane pool, introducing a macromolecular polyelectrolyte solution with a certain concentration into the feed liquid side of the membrane pool, communicating pure water with the permeation side, driving the solutions at the two sides to flow through a gear pump, and controlling the temperature of the macromolecular polyelectrolyte solution and the temperature of the pure water to be constant;
(2) emptying system bubbles, and after the temperature of the system is reached, recording the lateral pressure, flow, volume, mass and concentration of a feed liquid side and a permeation side at a certain temperature at fixed time;
(3) after the operation pressure is changed, repeating the operation of the step (2);
(4) calculating the water flux J of different membrane materialswAnd salt flux Js；
(5) Calculating the convection permeability coefficient L of the membrane materials with different known molecular weight cut-off and the membrane materials to be measuredd；
(6) Molecular weight cut-off M based on known membrane materialswAnd convective permeability coefficient LdCalculating the molecular weight M of the trapped materialwAnd convective permeability coefficient LdA linear relationship therebetween;
(7) substituting the convection permeability coefficient of the membrane material to be tested obtained in the step (5) into the convection permeability coefficient of the membrane material to be tested in the step (6)wAnd LdThe convection diffusion coefficient M of the film is further obtainedw。
2. The method for quantitatively evaluating the pore size of a porous membrane according to claim 1, wherein the porous membrane comprises one of an ultrafiltration membrane, a forward osmosis porous membrane, and a forward osmosis porous composite membrane; the macromolecular polyelectrolyte comprises one of anionic polyelectrolyte, neutral polyelectrolyte and cationic polyelectrolyte.
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| CN115372197A (en) * | 2022-08-22 | 2022-11-22 | 西安石油大学 | Evaluation method for quantifying clay imbibition oil displacement effect based on imbibition-ion diffusion lag time |
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