CN112755809A - Forward osmosis membrane with mica sheet as intermediate layer and preparation method thereof - Google Patents
Forward osmosis membrane with mica sheet as intermediate layer and preparation method thereof Download PDFInfo
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- CN112755809A CN112755809A CN202011432011.9A CN202011432011A CN112755809A CN 112755809 A CN112755809 A CN 112755809A CN 202011432011 A CN202011432011 A CN 202011432011A CN 112755809 A CN112755809 A CN 112755809A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/26—Electrical properties
Abstract
The invention relates to a forward osmosis membrane with mica sheets as an intermediate layer and a preparation method thereof. The invention applies the mica sheet to the forward osmosis membrane for the first time, selects the mica sheet as the intermediate layer and is positioned between the base membrane and the polyamide layer, and the two-dimensional nano mica sheet has good hydrophilicity, good layered nano structure and strong electronegativity, and can shorten the water flux of a water molecule transmission path and greatly improve the salt interception performance. The novel TFC membrane is prepared by using a mica sheet-containing base membrane as a substrate and enabling a two-dimensional mica sheet to be positioned between the base membrane and a polyamide layer through interfacial polymerization reaction between polyamine and polybasic acyl chloride. Compared with an unmodified TFC membrane, the micro membrane shortens a water molecule transfer path, reduces water quality transfer resistance and promotes the rapid transportation of water molecules.
Description
Technical Field
The invention relates to a forward osmosis membrane with mica sheets as an intermediate layer and a preparation method thereof, belonging to the technical field of membrane preparation.
Background
With the development of society and the continuous increase of population, fresh water resources are increasingly reduced, the problem of water pollution is gradually serious, and in order to solve the problem, a method for producing fresh water by separating seawater and brackish water through a membrane method has gained wide attention. The forward osmosis process, a natural phenomenon in water transport processes, has received increasing attention in recent years, and has several major advantages over traditional pressure driven processes such as reverse osmosis, nanofiltration: (1) the forward osmosis process does not need or only needs low external hydraulic pressure, so that the energy consumption and the equipment cost can be reduced; (2) the potential water recovery rate in the forward osmosis process is high; (3) the forward osmosis process has wide application range and lower membrane pollution tendency.
The thin film composite forward osmosis membrane (TFC-FO) prepared by interfacial polymerization reaction is widely applied due to the characteristics of low energy consumption, high flux, simple operation and the like. However, in practical applications, the salt back-diffusion and the porous structure of the support layer cause a decrease in osmotic pressure and cause severe concentration polarization problems during separation. The development of forward osmosis membranes is restricted by the problem of "upper balance" between water flux and salt cut-off, and by the problem of membrane fouling.
The natural mica is cheap and easy to obtain, the preparation method is simple and has no environmental pollution, in recent years, the two-dimensional nano mica sheet is successfully peeled from the natural mica stone, so that the application field of the two-dimensional nano mica sheet is widened, and the two-dimensional nano mica sheet layer obtained by peeling has the characteristics of higher aspect ratio, good light transmittance, ultraviolet shielding performance, atom level flatness, electrical insulation, chemical durability and the like, and is widely applied to the electronic field. Good hydrophilicity, regular lamellar structure, certain rigidity, excellent stability, low price and easy obtaining, and shows high application potential in the field of water treatment.
In general, the TFC-FO membrane can be modified by adding a porous support material to adjust a support layer, so that the thin film composite membrane has better separation performance and excellent bacteriostatic and anti-fouling performance. The hydrophilicity, porosity and tortuosity of the porous support material have a large impact on the separation performance of the FO membrane. The performance of the support layer is optimized mainly through increasing the porosity of the support layer and through coating hydrophilic materials to increase the hydrophilicity of the support layer so as to improve the water flux. Most of the current composite forward osmosis membrane (TFC-FO) porous supporting materials are added into a polyamide layer, so that the water quality transfer resistance is large, the water molecule transportation is slow, the water flux still cannot meet the requirement, and the separation stability is low.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a forward osmosis membrane with mica sheets as an intermediate layer and a preparation method thereof.
The mica sheet is a forward osmosis membrane in the middle layer, the two-dimensional nano mica sheet is positioned between the base membrane and the polyamide layer, the two-dimensional nano mica sheet reduces water transfer resistance, promotes the rapid transportation of water molecules, greatly improves water flux and enhances the membrane stability.
In order to solve the problems, the invention is realized by the following technical scheme:
a forward osmosis membrane with mica sheets as an intermediate layer comprises a base membrane and a polyamide membrane layer positioned on the base membrane, wherein a two-dimensional nano mica sheet intermediate layer is arranged between the base membrane and the polyamide membrane layer.
The invention also provides a preparation method of the forward osmosis membrane with the mica sheet as the intermediate layer.
A preparation method of a forward osmosis membrane with mica sheets as an intermediate layer comprises the following steps:
(1) preparation of mica sheet dispersion
Dispersing two-dimensional nanoscale mica sheets in deionized water, and performing ultrasonic dispersion uniformly to obtain a mica dispersion liquid;
(2) preparation of aqueous solutions
Dissolving polyamine in water, and uniformly mixing to obtain a water phase solution;
(3) preparation of oil phase solution
Dissolving polyacyl chloride in an organic solvent to prepare an oil phase solution;
(4) preparation of mica sheet-containing base film
Taking the mica dispersion liquid obtained in the step (1), loading two-dimensional nano-scale mica sheets on a base film in a suction filtration mode, and drying to obtain a mica sheet-containing base film;
(5) interfacial polymerization
Pouring the aqueous phase solution on a mica sheet-containing base film, keeping the aqueous phase solution for 30-180 s, removing the redundant aqueous phase solution, vertically drying, pouring the oil phase solution, keeping the aqueous phase solution for 30-80 s, removing the redundant oil phase solution after reaction, and drying to obtain the forward osmosis membrane taking the mica sheet as the middle layer.
Preferably, in the step (1), the ultrasonic dispersion is carried out for 20-40min by using an ultrasonic cell crusher, and the power of the ultrasonic cell crusher is 400-600W.
In the preparation method, preferably, in the step (1), the concentration of the two-dimensional nano-scale mica plates in the mica dispersion liquid is 0.1-0.8 mg/mL.
In the preparation method, it is further preferable that in the step (1), the concentration of the two-dimensional nano-sized mica flakes in the mica dispersion liquid is 0.5 to 0.75 mg/ml.
In the above preparation method, preferably, in the step (2), the concentration of the polyamine in the aqueous phase solution is 0.02% to 10%.
In the above preparation method, preferably, in the step (2), the polyamine is one of o-phenylenediamine, p-phenylenediamine, m-phenylenediamine and piperazine.
In the above production method, preferably, in the step (2), the polyamine is m-phenylenediamine.
In the above preparation method, preferably, in the step (3), the polybasic acyl chloride is one of trimesoyl chloride, m-trimesoyl chloride, n-hexane triacyl chloride, cyclopentane triacyl chloride, propane triacyl chloride or pentane triacyl chloride; the organic solvent is one of n-hexane, n-heptane, dodecane or tetradecane.
In the preparation method, in the step (3), the mass concentration of the polyacyl chloride in the oil phase solution is preferably 0.02-0.2%.
In the preparation method, preferably, in the step (4), the base film is polysulfone, polyethersulfone, polyethylene, polyamideimide, polypropylene or polyacrylonitrile.
In the above production method, preferably, in the step (4), the base film is a circular film having a diameter of 5 cm.
In the above production method, preferably, in the step (4), the mica dispersion is used in an amount of 4 to 6ml in suction filtration.
In the above preparation method, preferably, in the step (5), after the aqueous phase solution is poured, the retention time is 120s, and the oil phase solution is poured, and the reaction time is 60 s.
Preferably, in the step (5), the drying is performed by using an oven, and the drying time is 4-8 min.
The invention has the technical characteristics and advantages that:
1. the invention applies the mica sheet to the forward osmosis membrane for the first time, selects the mica sheet as the intermediate layer and is positioned between the base membrane and the polyamide layer, and the two-dimensional nano mica sheet has good hydrophilicity, good layered nano structure and strong electronegativity, and can shorten the water flux of a water molecule transmission path and greatly improve the salt interception performance.
2. The invention takes a mica sheet-containing basement membrane as a substrate, and the two-dimensional mica sheet is positioned between the basement membrane and a polyamide layer through interfacial polymerization reaction between polyamine and polyacyl chloride, so as to prepare the novel TFC membrane. Compared with an unmodified TFC membrane, the micro membrane shortens a water molecule transfer path, reduces water quality transfer resistance and promotes the rapid transportation of water molecules.
3. The mica sheet is selected as the intermediate layer of the forward osmosis membrane, and the two-dimensional nano mica sheet has abundant negative charges, so that the electronegativity of the surface of the membrane is increased. As the conventional pollutants are rich in negative charges, and the membrane surface with electronegativity is not easy to adsorb the pollutants, the anti-fouling performance of the membrane can be obviously improved.
4. The mica sheet is selected as the intermediate layer of the forward osmosis membrane, so that the forward osmosis membrane is not easy to collapse and deform, and the stability is greatly enhanced.
Drawings
FIG. 1 is a magnified surface scanning electron micrograph of a forward osmosis membrane with mica platelets as an intermediate layer prepared in example 1.
Detailed Description
The invention will be further explained with reference to the drawings and examples.
Example 1
A preparation method of a forward osmosis membrane with mica sheets as an intermediate layer comprises the following steps:
(1) preparation of mica dispersion: adding 75mg of prepared two-dimensional nano-scale mica plate into 100mL of deionized water, carrying out ultrasonic treatment for 30min with 600W power to uniformly disperse the two-dimensional nano-scale mica plate to obtain 0.75mg/mL mica dispersion liquid, and storing the mica dispersion liquid at room temperature;
(2) preparation of aqueous phase solution: dissolving m-phenylenediamine in water, and uniformly mixing the m-phenylenediamine with the water by ultrasonic waves to obtain an aqueous phase solution; the concentration of m-phenylenediamine in the aqueous phase solution is 2 percent;
(3) preparation of oil phase solution: dissolving trimesoyl chloride in n-hexane, and performing ultrasonic mixing to obtain an oil phase solution; the mass concentration of trimesoyl chloride in the oil phase solution is 0.1 percent;
(4) preparing a mica sheet-containing base film: cutting a PES (polyether sulfone) base film into a circular membrane with the diameter of 5cm, taking 7ml of mica dispersion liquid, loading two-dimensional nano-scale mica sheets on the base film by using a suction filtration device, and drying to obtain a mica sheet-containing base film;
(5) interfacial polymerization reaction: clamping the mica sheet-containing base film by using a mold clamp, slightly pouring the water phase solution onto the film, pouring out the redundant water phase solution on the surface after keeping for 100s, vertically drying, then pouring the oil phase solution onto the surface of the film, removing the redundant oil phase solution on the surface after contacting for 60s, naturally drying, and putting into an oven at 80 ℃ for drying for 5min to obtain the forward osmosis membrane with the mica sheet as the intermediate layer.
The magnified surface scanning electron micrograph of the forward osmosis membrane with the mica sheet as the intermediate layer is shown in FIG. 1.
Example 2
The preparation method of the forward osmosis membrane with the mica sheet as the intermediate layer is the same as that of the embodiment 1, except that:
in the step (1), 60mg of prepared two-dimensional nano-scale mica sheets are added into 100mL of deionized water, and are subjected to ultrasonic treatment with 600W power for 30min to be uniformly dispersed to obtain mica dispersion liquid with the concentration of 0.6mg/mL, and the mica dispersion liquid is stored at room temperature;
the other steps were carried out as in example 1.
Example 3
The preparation method of the forward osmosis membrane with the mica sheet as the intermediate layer is the same as that of the embodiment 1, except that:
in the step (1), 50mg of prepared two-dimensional nano-scale mica sheet is added into 100mL of deionized water, ultrasonic treatment is carried out for 30min at 600W power so as to lead the two-dimensional nano-scale mica sheet to be dispersed uniformly, thus obtaining mica dispersion liquid with the concentration of 0.5mg/mL, and the mica dispersion liquid is placed at room temperature for storage;
the other steps were carried out as in example 1.
Example 4
The preparation method of the forward osmosis membrane with the mica sheet as the intermediate layer is the same as that of the embodiment 1, except that:
in the step (1), 65mg of prepared two-dimensional nano-scale mica sheets are added into 100mL of deionized water, and are subjected to ultrasonic treatment with 600W power for 30min to be uniformly dispersed to obtain 0.65mg/mL mica dispersion liquid, and the mica dispersion liquid is stored at room temperature;
the other steps were carried out as in example 1.
Application test effects
Five different groups of forward osmosis membranes were obtained by changing the concentrations of the mica dispersion in step (1) of example 1 to 0mg/mL, 0.25mg/mL, 0.5mg/mL, 0.75mg/mL and 1mg/mL, respectively. The five groups of forward osmosis membranes were placed in a forward osmosis membrane module for testing the separation performance thereof. The details are as follows:
the forward osmosis testing device is an independent membrane component, and the effective testing area of the membrane component is 3cm2The drawing liquid is a 1mol/L NaCl solution, the mass counting is carried out on the side of the drawing liquid by an electronic balance, the stock solution is deionized water, and the reverse salt flux is measured by a conductivity meter for the stock solution measurement. The gear pump and cross flow operation mode are adopted, and the flow rate is controlled to be 1500 cm/s. Fixing the forward osmosis membrane on a membrane component, opening a gear pump, running for 10-30min, starting counting by using an electronic balance, and measuring the conductivity of the stock solution every two minutes. The water flux as well as the reverse salt flux of the forward osmosis membrane was calculated from the added mass of the balance and the measured conductivity. The water flux and reverse salt flux for five groups of forward osmosis membranes are shown in table 1:
TABLE 1
| Concentration of mica Dispersion (mg/mL) | Water flux (LMH) | Reverse salt flux (gMH) |
| 0 | 12 | 0.39 |
| 0.25 | 11.0 | 0.27 |
| 0.5 | 59.33 | 0.99 |
| 0.75 | 76.33 | 2.05 |
| 1 | 49.77 | 0.82 |
As can be seen from Table 1, the water flux and the reverse salt flux are gradually increased along with the increase of the two-dimensional mica addition concentration, the water flux and the reverse salt flux are maximum when the concentration of the mica dispersion liquid is 0.75mg/mL, and the water flux and the reverse salt flux are reduced on the contrary when the two-dimensional mica addition concentration is more than 1mg/mL, so that the two-dimensional nano-scale mica sheet concentration is 0.5-0.75mg/mL, and the obtained forward osmosis membrane has the best effect.
Claims (10)
1. A forward osmosis membrane with mica sheets as an intermediate layer comprises a base membrane and a polyamide membrane layer positioned on the base membrane, wherein a two-dimensional nano mica sheet intermediate layer is arranged between the base membrane and the polyamide membrane layer.
2. A preparation method of a forward osmosis membrane with mica sheets as an intermediate layer comprises the following steps:
(1) preparation of mica sheet dispersion
Dispersing two-dimensional nanoscale mica sheets in deionized water, and performing ultrasonic dispersion uniformly to obtain a mica dispersion liquid;
(2) preparation of aqueous solutions
Dissolving polyamine in water, and uniformly mixing to obtain a water phase solution;
(3) preparation of oil phase solution
Dissolving polyacyl chloride in an organic solvent to prepare an oil phase solution;
(4) preparation of mica sheet-containing base film
Taking the mica dispersion liquid obtained in the step (1), loading two-dimensional nano-scale mica sheets on a base film in a suction filtration mode, and drying to obtain a mica sheet-containing base film;
(5) interfacial polymerization
Pouring the aqueous phase solution on a mica sheet-containing base film, keeping the aqueous phase solution for 30-180 s, removing the redundant aqueous phase solution, vertically drying, pouring the oil phase solution, keeping the aqueous phase solution for 30-80 s, removing the redundant oil phase solution after reaction, and drying to obtain the forward osmosis membrane taking the mica sheet as the middle layer.
3. The method according to claim 2, wherein in the step (1), the ultrasonic dispersion is performed for 20-40min by using an ultrasonic cell crusher, and the power of the ultrasonic cell crusher is 400-600W.
4. The method according to claim 2, wherein in step (1), the concentration of the two-dimensional nano-sized mica platelets in the mica dispersion is 0.1 to 0.8mg/mL, and preferably, the concentration of the two-dimensional nano-sized mica platelets in the mica dispersion is 0.5 to 0.75 mg/mL.
5. The preparation method according to claim 2, wherein in the step (2), the concentration of the polyamine in the aqueous phase solution is 0.02 to 10 percent, and the polyamine is one of o-phenylenediamine, p-phenylenediamine, m-phenylenediamine or piperazine; preferably, the polyamine is m-phenylenediamine.
6. The method according to claim 2, wherein in the step (3), the polybasic acid chloride is one of trimesoyl chloride, m-trimesoyl chloride, n-hexane triacyl chloride, cyclopentane triacyl chloride, propane triacyl chloride or pentane triacyl chloride; the organic solvent is one of n-hexane, n-heptane, dodecane or tetradecane; the mass concentration of the polyacyl chloride in the oil phase solution is 0.02-0.2%.
7. The method according to claim 2, wherein in the step (4), the base film is polysulfone, polyethersulfone, polyethylene, polyamideimide, polypropylene or polyacrylonitrile; the base film is a circular film with a diameter of 5 cm.
8. The method according to claim 2, wherein in the step (4), the mica dispersion is used in an amount of 4 to 6ml in suction filtration.
9. The method according to claim 2, wherein in the step (5), after the aqueous phase solution is poured, the retention time is 120s, and the oil phase solution is poured, and the reaction time is 60 s.
10. The preparation method according to claim 2, wherein in the step (5), the drying is performed by using an oven, and the drying time is 4-8 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114073898A (en) * | 2021-11-18 | 2022-02-22 | 江南大学 | Forward osmosis membrane with two-dimensional MOFs as intermediate layer and preparation method thereof |
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Application publication date: 20210507 |