CN111389225A - Vermiculite-based ion screening membrane and preparation method thereof - Google Patents
Vermiculite-based ion screening membrane and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of film preparation and separation and purification, and discloses a vermiculite-based ion screening membrane and a preparation method thereof.
Description
Technical Field
The invention belongs to the technical field of film preparation and separation and purification, and particularly relates to a vermiculite-based ion screening film and a preparation method thereof.
Background
Monovalent metal ions are closely related to human life, and are an important resource, especially in industrial applications. For example, Na+As coolants for some nuclear reactors, K+Can be used for producing chemical fertilizer L i+Can be used for manufacturing lithium batteries. The seawater, salt water and bittern in nature have monovalent metal ions widely distributed, but also contain a large amount of polyvalent metal ions, such as alkaline earth metal ions Mg2+And Ca2+. Therefore, it is a significant challenge to obtain high-purity single ions and salts thereof under the condition of coexistence of multiple metal ions, especially in China, where the consumption of metals is increasing.
Membrane technology has proven to be an effective method of screening monovalent/polyvalent metal ions by enabling screening of the charge and size of the metal ions by using membranes with specific physicochemical properties. In recent years, a layered membrane formed by parallel and regular stacking of two-dimensional nanosheets becomes a research and development hotspot in the technical field of novel efficient membrane separation. The two-dimensional layered film is formed by stacking two-dimensional nano materials, and has a large number of interlayer nano channels and a certain amount of surface charges, so that the transport rates of monovalent/multivalent metal ions in the channels are different. Therefore, compared with the traditional membrane technology, the two-dimensional layered membrane can realize more efficient and rapid selective screening. At present, most of two-dimensional nano materials have high precursor cost, and the preparation process is accompanied by the use of a large amount of toxic, harmful and environment-friendly reagents such as acid, alkali and the like, so that the yield is relatively low, and the large-scale production of the two-dimensional layered film is limited. In addition, the ion sieving selectivity of the existing two-dimensional layered membrane is limited by the size and surface chemical influence of two-dimensional nanomaterials, and the selectivity needs to be further improved so as to be widely applied to practical application.
Vermiculite is an expandable, layered silicate mineral containing water molecules and exchangeable cations between layers, and has the basic structure of two layers of tetrahedra and one layer of octahedra. Since part of the silicon ions in the center of the tetrahedron are replaced by aluminum ions, the surface of the vermiculite sheet will have a certain negative charge. The vermiculite reserves in China account for about one sixth of the world, and the vermiculite is only used in the traditional fields of buildings, agriculture and the like for a long time, so that the increase of the added value is greatly limited. Compared with other two-dimensional nano materials, the vermiculite has excellent chemical stability and thermal stability, is low in price and is an ideal nano material for preparing and screening monovalent/polyvalent metal ions.
Disclosure of Invention
In view of the above-mentioned shortcomings and drawbacks of the prior art, the present invention is directed to: provides a vermiculite-based ion screening membrane and a preparation method thereof, and solves the technical problems of efficiently screening monovalent/polyvalent metal ions and how to produce the vermiculite-based ion screening membrane on a large scale.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a vermiculite-based ion screening membrane comprises the following steps:
mixing expanded vermiculite with saturated NaCl solution according to the mass volume ratio of 1g (200-400) m L, heating at the high temperature of 70-110 ℃ for 2-4 h, and performing suction filtration and washing to obtain powder A;
step two, mixing the powder A and L iCl solution with the concentration of 2-3 mol/L according to the mass-volume ratio of 1g, (200-400) m L, heating at the high temperature of 70-110 ℃ for 2-4 h, and performing suction filtration and washing to obtain powder B;
mixing the powder B with deionized water according to the mass volume ratio of 1g (200-400) m L, stirring and stripping by a high-shear dispersion emulsion homogenizer to obtain a suspension C;
step four: centrifuging the suspension C, removing non-peeled vermiculite particles and impurities through low-speed centrifugation, and performing gradient centrifugation to prepare vermiculite nanosheet dispersion liquid in different rotating speed ranges;
step five: stacking the vermiculite nanosheet dispersion liquid on the surface of a porous substrate layer by layer regularly, and drying to obtain the vermiculite-based ion screening membrane with the loading capacity of 0.3-0.6 mg/cm2。
Specifically, the washing solution in the first step is deionized water and ethanol.
Specifically, the washing solution in the second step is deionized water and ethanol.
Specifically, the rotating speed of the medium-high shear dispersed emulsion homogenizer in the third step is 18000-20000 revolutions per minute, and the stirring and stripping time is 10 min.
Specifically, in the fourth step, the rotation speed of low-speed centrifugation is 300-500 revolutions per minute, the centrifugation time is 60min, the centrifugation temperature is 5-10 ℃, after the low-speed centrifugation is finished, the upper-layer dispersion liquid is taken for gradient centrifugation, and the un-peeled vermiculite and impurities precipitated at the bottom are discarded.
Specifically, the rotation speed of the gradient centrifugation in the fourth step is 1000 revolutions per minute, 2000 revolutions per minute, 3000 revolutions per minute and 6000 revolutions per minute, the centrifugation time is 60 minutes, and the centrifugation temperature is 5-10 ℃. Gradient centrifugation specific operation: and after the centrifugation of the wheel is finished, taking out the upper-layer dispersion liquid for the next centrifugation, wherein the rest lower-layer dispersion liquid is the vermiculite nanosheet dispersion liquid corresponding to the rotation speed range of the wheel.
Specifically, the concentration of the vermiculite nanosheet dispersion liquid prepared in the fourth step is 4-10 mg/m L.
Specifically, in the fifth step, the porous substrate is an anodic alumina filter membrane, a mixed cellulose ester membrane and a polypropylene membrane, and the pore diameter is 20-450 nm.
Specifically, the method for stacking the layers in the fifth step is a suction filtration method, a spin coating method or a spraying method.
Specifically, the drying in the fifth step is vacuum drying, and the drying is carried out for 6 hours at room temperature.
The vermiculite-based ion screening membrane is prepared by the method.
Compared with the prior art, the invention has the following characteristics:
(1) the invention utilizes the methods of ion exchange, hydrothermal reaction and gradient centrifugation to prepare the vermiculite nano sheet solution, the sizes of the corresponding nano sheets are different along with the difference of the rotating speed range, and the vermiculite-based ion sieving membrane prepared by the vermiculite nano sheets with controllable sizes has the controllability on the transportation rate of monovalent/polyvalent metal ions.
(2) The width of the channel between the vermiculite-based ion screening membranes prepared by the invention can reach
And the surface of the channel is charged with negative charges, so that the interlayer channel allows partial water molecules removed by the hydrated metal ions to pass through at different speeds and repels anions, thereby realizing more efficient and rapid selective screening.
(3) The preparation method of the vermiculite-based ion screening membrane provided by the invention is simple, low in energy consumption and cost, free of acid and alkali, wide in applicability and suitable for industrial production.
Drawings
FIG. 1 is an X-ray diffraction pattern of a vermiculite-based ion sieving membrane;
FIG. 2 is a cross-sectional scanning electron micrograph of a vermiculite-based ion sieving membrane;
FIG. 3 shows the respective metal ions relative to L i+Selectivity (ratio of permeation rate) versus hydration radius.
Detailed Description
The steps of the present invention are described in more detail with reference to some examples, but the embodiments of the present invention are not limited to the specific examples listed below, and any combination between the examples is included.
Example 1:
step one, mixing 0.3g of expanded vermiculite with 100m L of saturated NaCl solution, putting the mixture into a high-temperature oven, setting the temperature of the oven at 110 ℃, heating for 2 hours, repeatedly performing suction filtration and washing for 3 times by using 100m L deionized water and performing suction filtration and washing for 1 time by using 100m L of absolute ethyl alcohol respectively after heating is finished, and preparing powder A;
step two, mixing the powder A with 100m L and 2 mol/L L iCl solution, putting the mixture into a high-temperature oven, setting the temperature of the oven at 110 ℃, heating for 2 hours, repeatedly performing suction filtration and washing for 3 times by using 100m L deionized water and performing suction filtration and washing for 1 time by using 100m L anhydrous ethanol after heating is finished, and preparing powder B;
mixing the powder B with 80m L deionized water, stirring and stripping by a high-shear dispersed emulsion homogenizer at the rotation speed of 20000 revolutions per minute for 10min to obtain suspension A;
removing non-peeled vermiculite and impurities in the suspension by low-speed centrifugation under the conditions of the rotating speed of 300 revolutions per minute, the centrifugation time of 60min and the centrifugation temperature of 5 ℃, and then preparing nanosheet vermiculite dispersion liquid with the rotating speed of 300-1000, 1000-2000, 2000-3000 and 3000-6000 revolutions per minute and the concentration of 8.57, 5.83, 5.5 and 8.07mg/m L by gradient centrifugation under the conditions of the rotating speed of 1000, 2000, 3000 and 6000 revolutions per minute, the centrifugation time of 60min and the centrifugation temperature of 5 ℃;
step five: selecting vermiculite nano-sheet dispersion liquid with the rotation speed range of 1000-2000 r/min, wherein the loading amount is 0.3mg/cm2Stacking vermiculite nano sheets on an anodic alumina filter membrane with the aperture of 0.02 mu m through a vacuum filtration device, and putting the anodic alumina filter membrane into a vacuum drier for drying for 6 hours to prepare the vermiculite-based ion screening membrane.
Verification of the width of the interlayer channel of the vermiculite-based ion screening membrane:
the vermiculite-based ion sieving membrane is tested by an X-ray diffractometer (XRD), and the vermiculite-based ion sieving membrane in the example 1 has a diffraction peak at 7.45 degrees within the range of 3-15 degrees of 2 theta, so that the vermiculite-based ion sieve is verifiedThe film is formed by stacking single-layer vermiculite nano sheets, and the interlayer distance d is calculated according to a Bragg formula
And the thickness of the single-layer vermiculite nano sheet is
So that the width of the channel between the vermiculite-based ion screening membrane layers is
The specific data of the XRD diffraction pattern are shown in figure 1.
The verification of the layered structure of the vermiculite-based ion screening membrane comprises the following steps:
the cross section of the vermiculite-based ion sieving membrane is tested by using a Scanning Electron Microscope (SEM), the vermiculite-based ion sieving membrane in example 1 has a good layered structure and nano-channels, and can be used for selectively sieving monovalent/polyvalent metal ions, and a scanning electron microscope picture is shown in figure 2.
Selectivity of the vermiculite-based ion sieving membrane for monovalent/polyvalent metal ions:
the supporting amount in example 1 was 0.3mg/cm2The vermiculite-based ion sieving membrane is placed in a U-shaped permeation device, and the raw material side is filled with 100m L and 1 mol/L chloride salt solution (L i)+、Na+、K+、Cs+、Mg2+One of the above), the permeate side was charged with 100m L of deionized water, left for 12h to allow forward osmosis driven by concentration differences, and L i was measured by measuring and recording the change in conductivity of the solution on the permeate side, combined with the conductivity versus salt concentration+、Na+、K+、Cs+、Mg2+The permeation rates of (a) and (b) are respectively 0.466, 0.078, 0.110, 0.291, 0.0392mol h-1m-2It can be seen that the vermiculite-based ion sieving membrane of example 1 can achieve effective sieving of monovalent/polyvalent metal ions, each relative to L i+The selectivity (ratio of permeation rate) of (c) to hydration radius is shown in fig. 3.
Example 2:
the difference between the embodiment and the embodiment 1 is that the volume of the saturated NaCl solution mixed with the expanded vermiculite in the first step of the embodiment is 70m L, the volume of the solution L iCl mixed with the powder A in the second step of the embodiment is 70m L, the concentration of the dispersion liquid of the vermiculite nano-sheets obtained by gradient centrifugation at the rotating speed range of 1000-2000 r/min is slightly reduced to 5.52mg/m L, and the vermiculite-based ion sieving membrane pair L i prepared in the embodiment is measured through experiments+、Na+、K+、Cs+、Mg2+The permeation rates of (a) and (b) are respectively 0.453, 0.073, 0.109, 0.287 and 0.0384mol h-1m-2Substantially in accordance with example 1.
Example 3:
the difference between the embodiment and the embodiment 1 is that the heating time of the oven in the first step and the second step of the embodiment is 4 hours, the concentration of the dispersion liquid of the vermiculite nano sheets obtained by gradient centrifugation at the rotating speed range of 1000-2000 r/min is slightly increased to 6.03mg/m L, and through experimental measurement, the concentration of the dispersion liquid of the vermiculite-based ion screening membrane pair L i prepared in the embodiment is measured+、Na+、K+、Cs+、Mg2+The permeation rates of (a) and (b) are respectively 0.470, 0.080, 0.112, 0.293 and 0.0404mol h-1m-2Substantially in accordance with example 1.
Example 4:
the difference between the embodiment and the embodiment 1 is that the heating temperature of the oven in the first step and the second step of the embodiment is 70 ℃, the concentration of the dispersion liquid of the vermiculite nano sheets obtained by gradient centrifugation at the rotation speed range of 1000-2000 r/min is slightly reduced to 5.60mg/m L, and experimental measurement shows that the vermiculite-based ion screening membrane pair L i prepared in the embodiment is L i+、Na+、K+、Cs+、Mg2+Respectively has a permeation rate of 0.462, 0.075, 0.105, 0.288, 0.0374mol h-1m-2Substantially in accordance with example 1.
Example 5:
the difference between the embodiment and the embodiment 1 is that the concentration of the L iCl solution in the second step of the embodiment is 3 mol/L, and the yield of the vermiculite nanosheets in each rotating speed range in the embodiment is all the sameThe concentration of the vermiculite nanosheet dispersion liquid at 1000-2000 rpm is 6.25mg/m L, and through experimental measurement, the vermiculite-based ion screening membrane pair L i prepared in the embodiment+、Na+、K+、Cs+、Mg2+The permeation rates of (a) and (b) are respectively 0.474, 0.082, 0.115, 0.299 and 0.042mol h-1m-2Substantially in accordance with example 1.
Example 6:
the difference between the present example and example 1 is that the volume of deionized water mixed with powder B in step three of the present example is 100m L. the yield of vermiculite nano-sheets in each rotating speed range in the present example is almost unchanged, and the concentrations are 8.60, 5.82, 5.53 and 8.04mg/m L, which are basically consistent with example 1.
Example 7:
the difference between the embodiment and the embodiment 1 is that the rotation speed of the high-shear dispersed emulsion homogenizer in the third step of the embodiment is 18000 r/min, the concentration of the vermiculite nano-sheet dispersion liquid obtained by gradient centrifugation at the rotation speed range of 1000-2000 r/min is obviously reduced to 5.5mg/m L, but the size of the vermiculite nano-sheet at 1000-2000 r/min is not influenced by the stripping rotation speed in the embodiment and is only related to the centrifugal rotation speed, and through experimental measurement, the vermiculite-based ion sieving membrane pair L i prepared in the embodiment is related to L i+、Na+、K+、Cs+、Mg2+The permeation rates of (a) are 0457, 0.069, 0.101, 0.286 and 0.0369mol h respectively-1m-2Substantially in accordance with example 1.
Example 8:
the difference between the embodiment and the embodiment 1 is that the rotation speed of the low-speed centrifugation in the fourth step of the embodiment is 500 r/min, the centrifugation temperature is 10 ℃, the yield of the vermiculite nanosheets in the rotation speed range of 1000-2000 r/min in the embodiment is basically unchanged and is 5.88mg/m L, through measuring the ion permeation rate and through experimental measurement, the vermiculite-based ion sieving membrane pair L i prepared in the embodiment is+、Na+、K+、Cs+、Mg2+The permeation rates of (a) are respectively 0.459, 0.071, 0.104, 0.283 and 0.0388mol h-1m-2Substantially in accordance with example 1.
Example 9:
the difference between the embodiment and the embodiment 1 is that in the fifth step of the embodiment, the vermiculite nano-sheet dispersion liquid with the rotating speed range of 3000-6000 rpm is selected. The vermiculite-based ion screening membrane prepared in the embodiment is tested by XRD, and the result shows that the width of an interlayer channel is
Substantially in accordance with example 1.
Example 10:
this example differs from example 1 in that vermiculite nanosheets were deposited onto a 0.22 μm mixed cellulose ester film using spin coating in step five of this example. The vermiculite-based ion screening membrane prepared in the embodiment is tested by XRD, and the result shows that the width of an interlayer channel is
In keeping with example 1.
Example 11:
the difference between the present embodiment and embodiment 1 is that in step five of the present embodiment, vermiculite nanosheets are stacked onto a 0.22 μm polypropylene film using a spray coating method. The vermiculite-based ion screening membrane prepared in the embodiment is tested by XRD, and the result shows that the width of an interlayer channel is
In keeping with example 1.
Example 12:
the difference between the embodiment and the embodiment 1 is that the loading amount of the vermiculite-based ion sieving membrane in the fifth step of the embodiment is 0.6mg/cm2The vermiculite-based ion sieving membrane pair L i prepared in this example was experimentally measured+、Na+、K+、Cs+、Mg2+The permeation rate of (A) is obviously reduced and is respectively 0.156 mol h, 0.025 mol h, 0.036 mol h, 0.095 mol h and 0.0130mol h-1m-2But selectivelySubstantially in accordance with example 1.
The measurement results show that the vermiculite-based ion screening membrane prepared by the technical scheme provided by the invention has the selectivity of efficiently screening monovalent/polyvalent metal ions, is simple in preparation process and low in price, and has high popularization and application values in the technical field of separation and purification.
Claims (9)
1. The preparation method of the vermiculite-based ion screening membrane is characterized by comprising the following steps:
mixing expanded vermiculite with saturated NaCl solution according to the mass volume ratio of 1g (200-400) m L, heating at the high temperature of 70-110 ℃ for 2-4 h, and performing suction filtration and washing to obtain powder A;
step two, mixing the powder A and L iCl solution with the concentration of 2-3 mol/L according to the mass-volume ratio of 1g, (200-400) m L, heating at the high temperature of 70-110 ℃ for 2-4 h, and performing suction filtration and washing to obtain powder B;
mixing the powder B with deionized water according to the mass volume ratio of 1g (200-400) m L, stirring and stripping by a high-shear dispersion emulsion homogenizer to obtain a suspension C;
step four: centrifuging the suspension C, removing non-peeled vermiculite particles and impurities through low-speed centrifugation, and performing gradient centrifugation to prepare vermiculite nanosheet dispersion liquid in different rotating speed ranges;
step five: stacking the vermiculite nanosheet dispersion liquid on the surface of a porous substrate layer by layer regularly, and drying to obtain the vermiculite-based ion screening membrane with the loading capacity of 0.3-0.6 mg/cm2。
2. The method for preparing the vermiculite-based ion screening membrane of claim 1, wherein the rotation speed of the high-shear dispersion emulsion homogenizer in the third step is 18000-20000 rpm, and the stirring and stripping time is 10 min.
3. The preparation method of the vermiculite-based ion screening membrane according to claim 1, wherein the rotation speed of low-speed centrifugation in the fourth step is 300-500 revolutions per minute, the centrifugation time is 60min, the centrifugation temperature is 5-10 ℃, after the low-speed centrifugation is finished, the upper layer dispersion liquid is taken for gradient centrifugation, and un-peeled vermiculite and impurities deposited at the bottom are discarded, the rotation speed of the gradient centrifugation is 1000, 2000, 3000 and 6000 revolutions per minute, the centrifugation time is 60min, the centrifugation temperature is 5-10 ℃, the specific operation of the gradient centrifugation is that after the centrifugation of the first step is finished, the upper layer dispersion liquid is taken out for the next centrifugation, the rest lower layer dispersion liquid is vermiculite nanosheet dispersion liquid corresponding to the rotation speed range of the first step, and the concentration of the vermiculite dispersion liquid prepared in the fourth step is 4-10 mg/m L.
4. The preparation method of the vermiculite-based ion screening membrane according to claim 1, wherein in the fifth step, the porous substrate is one of an anodic alumina filter membrane, a mixed cellulose ester membrane and a polypropylene membrane, and the pore diameter is 20-450 nm; the layer-by-layer stacking method is one of a suction filtration method, a spin-coating method or a spraying method; the drying is vacuum drying and drying for 6 hours at room temperature.
5. The method for preparing a vermiculite-based ion sieving membrane according to claim 1, wherein in step one the washing solution is deionized water and ethanol.
6. The method for preparing a vermiculite-based ion sieving membrane of claim 1, wherein in step two the washing solution is deionized water and ethanol.
7. The vermiculite-based ion screening membrane prepared by the method of any one of claims 1 to 6.
8. The application of the vermiculite-based ion sieving membrane in the separation and purification field is characterized by comprising the following steps:
the vermiculite-based ion sieving membrane supported on the substrate is placed in a U-shaped permeation device, and the sieving solution contains monovalent/polyvalent metal ions.
9. The method of claim 8, wherein the monovalent/polyvalent metal ion is L i+、Na+、K+、Cs+、Mg2+One of (1) and (b).
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| CN114288875A (en) * | 2021-12-31 | 2022-04-08 | 复旦大学 | Application of PGA composite membrane obtained based on interface super-assembly strategy in ion screening |
| CN114558465A (en) * | 2020-11-27 | 2022-05-31 | 中国科学院大连化学物理研究所 | Preparation and application of porous nickel hydroxide ion screening membrane |
| CN115869941A (en) * | 2022-12-29 | 2023-03-31 | 淮安中顺环保科技有限公司 | Preparation method of two-dimensional layered vermiculite interlayer confinement noble metal nanoparticle catalyst |
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