CN111214958A - Method for extracting soil rare earth nanoparticles - Google Patents
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- CN111214958A CN111214958A CN202010054077.2A CN202010054077A CN111214958A CN 111214958 A CN111214958 A CN 111214958A CN 202010054077 A CN202010054077 A CN 202010054077A CN 111214958 A CN111214958 A CN 111214958A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/83—Mixing plants specially adapted for mixing in combination with disintegrating operations
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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
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/025—Reverse osmosis; Hyperfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
- B01F31/80—Mixing by means of high-frequency vibrations above one kHz, e.g. ultrasonic vibrations
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a method for extracting soil rare earth nanoparticles, which utilizes a field flow meter to separate the soil rare earth nanoparticles. And (3) selecting a 3KD filtering membrane by using a field flow meter, filtering ionic substances in the soil rare earth nanoparticle solution, and further purifying the soil rare earth nanoparticle solution. The invention can reduce the loss of the soil rare earth nanoparticles in the dispersion process and the extraction process to the maximum extent, and can quickly and effectively extract a large amount of soil rare earth nanoparticles.
Description
Technical Field
The invention relates to the field of soil chemistry, in particular to a method for extracting soil rare earth nanoparticles.
Background
Soil Nanoparticles (Mineral Nanoparticles) refer to crystalline and amorphous solid materials having a particle size of about 1-100 nm formed during natural soil formation. Nanoparticles are very common in soil and are the most important constituent of environmental nanoparticles. Research shows that the nano particles in the soil are important carriers of elements in the environment and have important influence on the biogeochemical process of the elements; it controls the migration, transformation, circulation and biological effectiveness of heavy rare earth and organic pollutants in soil to achieve efficacy and effect. It strongly influences important environmental processes such as soil occurrence, soil physicochemical properties and environmental quality evolution. In addition, the synthesized nano particles such as nano ferric oxide and the like are new materials for controlling soil pollution, and have wide application prospects in the aspects of removing heavy rare earth and persistent organic pollutants in soil and controlling polluted environment. Therefore, understanding the surface structure, micro-morphology, interface behavior and function of nanoparticles in soil environment and their environmental effect mechanism are an important development trend in the soil and environmental field. The method has important theoretical significance for understanding the migration, transformation and self-purification of the heavy rare earth and organic pollutants in the soil effect, and is also an important theoretical basis for developing nano materials to restore the polluted environment. For example, Hochella published a related paper in Science, 21Mar 2008: 1631-.
It is worth pointing out that nanotechnology is a new technology that is widely used. Environmental applications of synthetic nanoparticles will cause these substances to enter the environment. It is important to assess the environmental risks of these artificial nanoparticles, such as their mobility, reactivity, ecotoxicology, persistence and health impact. Therefore, extracting nanoparticles from soil is an important technology for understanding and studying the physicochemical characteristics of soil nanoparticles and their environmental behaviors. Because soil nanoparticles have specific characteristics that are different from other macro-particles and micro-molecules, they have many unique physical and chemical characteristics. In order to understand these characteristics, environmental behavior and effects of nanoparticles in soil, it is necessary to separate and extract these nanoparticles from the soil. At present, a method system for soil nano-science research is still explored, and a systematic method for separating and extracting soil nano-particles is lacked.
At present, the main methods for separating and extracting soil nanoparticles mainly comprise a vibration-sedimentation method, a chemical dispersion-sedimentation method, a centrifugal method and an ultrafiltration method. The methods mainly solve the extraction problem of the nanoparticles, but the nanoparticles in the soil have various shapes and have obvious interaction with different components in the soil, such as organic matters, the separation effect of different nanoparticles is not ideal, and the chemical dispersion has the defects of environmental risk, insufficient dispersion degree of physical dispersion, long extraction time, small extraction amount, uneconomic performance and the like; in addition, the operation conditions of the currently adopted extraction method are not strict enough, and human errors are easily introduced into the extracted products, particularly the granularity; the extracted nanoparticles have large variation in particle size range, lack uniform standards, and cannot ensure the parallelism and accuracy of analysis. Particularly, an effective method for extracting rare earth nanoparticles in rare earth polluted soil is lacked at present.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for extracting soil rare earth nanoparticles, which comprises the following steps: s1, grinding and sieving: removing surface soil from a soil sample to be extracted, taking a proper amount of soil, air-drying, grinding and sieving, and uniformly mixing the sieved soil; s2, preparing soil liquid: adding high-purity water into the uniformly mixed soil, horizontally vibrating and dispersing the water-soil mixture, adding the high-purity water after the vibration is finished, and uniformly mixing to obtain a soil solution; s3, preparing soil clay components: carrying out ultrasonic dispersion treatment on the soil liquid, standing and settling, calculating the settling time of the soil nanoparticles with the particle size of less than 100nm settling to a certain specific position according to the temperature of the soil liquid and a Stokes equation, and then removing supernatant after settling and layering to obtain a soil clay component; s4, preparing a soil nanoparticle solution precursor: carrying out ultrasonic dispersion treatment on the soil clay component, carrying out centrifugal treatment on the soil clay component after ultrasonic treatment, and transferring supernatant to a plastic small bottle to obtain a soil nanoparticle solution precursor; s5, separating by a field flow instrument: selecting a 3KD filtering membrane by using a field flow meter, filtering ionic substances in the soil rare earth nanoparticle solution, and further purifying the soil rare earth nanoparticle solution; and S6, carrying out ultralow-temperature freezing preservation on the soil nanoparticle solution, and carrying out freeze drying treatment after the soil nanoparticle solution is completely frozen to obtain the soil nanoparticles.
The method for extracting the rare earth nanoparticles in the soil can fully disperse the rare earth nanoparticles in the soil without adding any chemical reagent, ensures the natural original structure of the nanoparticles in the soil, can reduce the loss of the rare earth nanoparticles in the soil in the dispersion process and the extraction process to the maximum extent, and can quickly and effectively extract a large amount of rare earth nanoparticles in the soil.
In a preferred embodiment, a reverse osmosis purification step is added between the step S3 and the step S4: removing impurities from the soil clay component by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
In a preferred embodiment, a reverse osmosis purification step is added between the step S4 and the step S5: removing impurities in the soil nanoparticle precursor by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
In a preferred embodiment, a reverse osmosis purification step is added between the step S5 and the step S6: removing impurities in the soil nanoparticle solution by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
In a preferred embodiment, the weight ratio of the soil to the used high purity water in step S2 is 1: 1-1: 200.
in a preferred embodiment, the ultrasonic dispersion treatment method in step S3 is to use an ultrasonic cell disruptor.
In a preferred embodiment, an ultrasonic dispersion step is added between step S3 and step S4, and the soil clay component is dispersed using an ultrasonic cell disruptor.
Drawings
The invention and its advantages will be better understood by studying the following detailed description of specific embodiments, given by way of non-limiting example, and illustrated in the accompanying drawings, in which:
fig. 1 is a graph for observing the particle size distribution of the prepared rare earth nanoparticles.
Detailed Description
The word "embodiment" is used herein to mean serving as an example, instance, or illustration. In addition, the articles "a" and "an" as used in this specification and the appended claims may generally be construed to mean "one or more" unless specified otherwise or clear from context to be directed to a singular form.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art may recognize applications of other processes and/or uses of other materials.
Example 1
First, a method for extracting soil rare earth nanoparticles according to example 1 of the present invention will be described, which includes the steps of:
s1) grinding and sieving: removing surface soil with the thickness of about 10cm from a soil sample to be used, naturally air-drying the residual soil to constant weight, removing broken stone residues, plant roots and branches and other residues in the air-dried soil, coarsely grinding the soil, sieving the soil by a 20-mesh sieve, and uniformly mixing the sieved soil.
S2) preparing soil liquid: adding 100.0g of the uniformly mixed soil and 200.0mL of high-purity water into a 1L glass bottle, horizontally oscillating for 6 hours at the temperature of 20 ℃ at 150rpm, adding 600.0mL of high-purity water after oscillating and resolving the stagnation, and oscillating and shaking uniformly to obtain a soil solution.
S3) soil clay component preparation: carrying out ultrasonic dispersion treatment on the soil liquid by using an ultrasonic cell disruptor, and carrying out ultrasonic treatment for 33min and 20s at the rated power of 120W;
and standing the soil liquid subjected to ultrasonic treatment, naturally settling the soil liquid for 35h 44min, calculating the settling time according to the temperature of the soil liquid and a Stokes equation, and transferring the upper-layer suspension into a 1L centrifugal bottle by using a peristaltic pump after the settling is finished to obtain the soil clay component.
S4) subjecting the soil clay component to ultrasonic dispersion treatment by using an ultrasonic cell disruptor, and performing ultrasonic treatment for 4min 10S at a rated power of 30% (1200W × 10% ═ 120W);
centrifuging the ultrasonically treated soil clay component by using a centrifuge (Beckman Coulter, model Avanti JXN-26, rotor JLA-8.1000, based on Stokes' law formula), wherein the centrifuging parameters are as follows: ROTORF 0685; RPM 5200; TIME 11; TEMP ═ 20; ACCE is 0; DEACCE is 0, and the supernatant, i.e., the soil nanoparticle solution, is obtained.
S5) reverse osmosis purification: the soil nanoparticle solution is purified to remove impurities therein using a reverse osmosis membrane, which uses polyvinyl alcohol (PVA) with a negatively charged surface in order to inhibit the contaminants from being adsorbed on the membrane by charge repulsion since the contaminants (fouling substances) in the treated soil are generally negatively charged, and has a spiral membrane structure. The reverse osmosis purification method comprises the following steps: the control system opens the sample injection valve and the sample outlet valve to carry out reverse osmosis for the first time, the soil nanoparticle solution enters from the sample injection valve, and the impurity solution enters the central liquid collecting pipe under the action of the filter element reverse osmosis membrane, so that impurities such as dissolved salts, colloids and microorganisms flow out through the outlet of the central liquid collecting pipe. The soil clay component with impurities removed is gathered near the pressure balloon, and flows out through the sample outlet valve after the pressure balloon is compressed. When pressure sensor detects that the soil nanoparticle solution pressure of getting rid of impurity rises to given pressure, control system control closes the injection valve and goes out the appearance valve and carry out reverse osmosis purification for the second time, and the pressure sacculus receives the pressure counteraction that the compression of soil clay component produced soil nanoparticle solution, soil nanoparticle solution is reverse to be carried out the reutilization through the filter core for the impurity solution who generates gets into central collecting tube, and the export of back edge central collecting tube flows, and the pressure that the pressure sacculus produced reduces along with the output of impurity solution, and pressure sensor detects soil nanoparticle solution lateral pressure drops to given pressure, and control system control opens the injection valve and goes out the appearance valve, repeats reverse osmosis purification again.
S6) field-flow instrument separation: and after reverse osmosis purification, selecting a 3KD filter membrane by using a field flow meter, filtering ionic substances, non-metallic nanoparticles and metal nanoparticles with low density in the soil rare earth nanoparticle solution, and further purifying the soil rare earth nanoparticle solution.
S7) transferring the purified soil rare earth nanoparticle solution into a plastic small bottle, sealing the bottle mouth with tinfoil, pricking a plurality of small holes on the tinfoil, and freezing and storing in a refrigerator at-80 ℃; and after the frozen soil rare earth nanoparticle solution is completely frozen, freeze-drying by using a freeze dryer to obtain the soil rare earth nanoparticles.
Example 2
The method for extracting rare earth nanoparticles from soil of example 2 of the present invention is illustrated, and comprises the steps of:
s1) grinding and sieving: removing surface soil with the thickness of about 10cm from a soil sample to be used, naturally air-drying the residual soil to constant weight, removing broken stone residues, plant roots and branches and other residues in the air-dried soil, coarsely grinding the soil, sieving the soil by a 50-mesh sieve, and uniformly mixing the sieved soil.
S2) preparing soil liquid: adding 100.0g of the uniformly mixed soil and 200.0mL of high-purity water into a 1L glass bottle, horizontally oscillating for 6 hours at the temperature of 20 ℃ at 150rpm, adding 600.0mL of high-purity water after oscillating and resolving the stagnation, and oscillating and shaking uniformly to obtain a soil solution.
S3) soil clay component preparation: carrying out ultrasonic dispersion treatment on the soil liquid by using an ultrasonic cell disruptor, and carrying out ultrasonic treatment for 33min and 20s at the rated power of 120W;
and standing the soil liquid subjected to ultrasonic treatment, naturally settling the soil liquid for 35h 44min, calculating the settling time according to the temperature of the soil liquid and a Stokes equation, and transferring the upper-layer suspension into a 1L centrifugal bottle by using a peristaltic pump after the settling is finished to obtain the soil clay component.
S4) subjecting the soil clay component to ultrasonic dispersion treatment by using an ultrasonic cell disruptor, and performing ultrasonic treatment for 4min 10S at a rated power of 30% (1200W × 10% ═ 120W);
centrifuging the ultrasonically treated soil clay component by using a centrifuge (Beckman Coulter, model Avanti JXN-26, rotor JLA-8.1000, based on Stokes' law formula), wherein the centrifuging parameters are as follows: ROTORF 0685; RPM 5200; TIME 11; TEMP ═ 20; ACCE is 0; DEACCE is 0, and the supernatant, i.e., the soil nanoparticle solution, is obtained.
S5) field-flow instrument separation: and after reverse osmosis purification, selecting a 3KD filter membrane by using a field flow meter, filtering ionic substances, non-metallic nanoparticles and metal nanoparticles with low density in the soil rare earth nanoparticle solution, and further purifying the soil rare earth nanoparticle solution.
S6) reverse osmosis purification: the soil nanoparticle solution is purified to remove impurities therein using a reverse osmosis membrane, which uses polyvinyl alcohol (PVA) with a negatively charged surface in order to inhibit the contaminants from being adsorbed on the membrane by charge repulsion since the contaminants (fouling substances) in the treated soil are generally negatively charged, and has a spiral membrane structure. The reverse osmosis purification method comprises the following steps: the control system opens the sample injection valve and the sample outlet valve to carry out reverse osmosis for the first time, the soil nanoparticle solution enters from the sample injection valve, and the impurity solution enters the central liquid collecting pipe under the action of the filter element reverse osmosis membrane, so that impurities such as dissolved salts, colloids and microorganisms flow out through the outlet of the central liquid collecting pipe. The soil clay component with impurities removed is gathered near the pressure balloon, and flows out through the sample outlet valve after the pressure balloon is compressed. When pressure sensor detects that the soil nanoparticle solution pressure of getting rid of impurity rises to given pressure, control system control closes the injection valve and goes out the appearance valve and carry out reverse osmosis purification for the second time, and the pressure sacculus receives the pressure counteraction that the compression of soil clay component produced soil nanoparticle solution, soil nanoparticle solution is reverse to be carried out the reutilization through the filter core for the impurity solution who generates gets into central collecting tube, and the export of back edge central collecting tube flows, and the pressure that the pressure sacculus produced reduces along with the output of impurity solution, and pressure sensor detects soil nanoparticle solution lateral pressure drops to given pressure, and control system control opens the injection valve and goes out the appearance valve, repeats reverse osmosis purification again.
S7) transferring the purified soil rare earth nanoparticle solution into a plastic small bottle, sealing the bottle mouth with tinfoil, pricking a plurality of small holes on the tinfoil, and freezing and storing in a refrigerator at-80 ℃; and after the frozen soil rare earth nanoparticle solution is completely frozen, freeze-drying by using a freeze dryer to obtain the soil rare earth nanoparticles.
Claims (7)
1. The method for extracting the soil rare earth nanoparticles is characterized by comprising the following steps of:
s1, grinding and sieving: removing surface soil from a soil sample to be extracted, taking a proper amount of soil, air-drying, grinding and sieving, and uniformly mixing the sieved soil;
s2, preparing soil liquid: adding high-purity water into the uniformly mixed soil, horizontally vibrating and dispersing the water-soil mixture, adding the high-purity water after the vibration is finished, and uniformly mixing to obtain a soil solution;
s3, preparing soil clay components: carrying out ultrasonic dispersion treatment on the soil liquid, standing and settling, calculating the settling time of the soil nanoparticles with the particle size of less than 100nm settling to a certain position according to the temperature of the soil liquid and a Stokes equation, and then removing supernatant after settling and layering to obtain a soil clay component;
s4, preparing a soil nanoparticle solution precursor: carrying out ultrasonic dispersion treatment on the soil clay component, carrying out centrifugal treatment on the soil clay component after ultrasonic treatment, and transferring supernatant to a plastic small bottle to obtain a soil nanoparticle solution precursor;
s5, separating by a field flow instrument: selecting a 3KD filtering membrane by using a field flow meter, filtering ionic substances in the soil rare earth nanoparticle solution, and further purifying the soil rare earth nanoparticle solution;
and S6, carrying out ultralow-temperature freezing preservation on the soil nanoparticle solution, and carrying out freeze drying treatment after the soil nanoparticle solution is completely frozen to obtain the soil nanoparticles.
2. The method for extracting soil rare earth nanoparticles as claimed in claim 1, wherein: a reverse osmosis purification step is added between the step S3 and the step S4: removing impurities from the soil clay component by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
3. The method for extracting soil rare earth nanoparticles as claimed in claim 1, wherein: a reverse osmosis purification step is added between the step S4 and the step S5: removing impurities in the soil nanoparticle precursor by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
4. The method for extracting soil rare earth nanoparticles as claimed in claim 1, wherein: a reverse osmosis purification step is added between the step S5 and the step S6: removing impurities in the soil nanoparticle solution by using a reverse osmosis membrane; the impurities include at least one of dissolved salts, colloids, microorganisms, and organic substances.
5. The method for extracting soil rare earth nanoparticles as claimed in claim 1, wherein: the weight ratio of the soil to the used high-purity water in step S2 is 1: 1-1: 200.
6. the method for extracting soil rare earth nanoparticles as claimed in claim 1, wherein: the ultrasonic dispersion treatment method in step S3 is to use an ultrasonic cell disruptor.
7. The method for extracting soil rare earth nanoparticles as claimed in claim 1, wherein: an ultrasonic dispersion step is added between the step S3 and the step S4, and the soil clay component is dispersed by using an ultrasonic cell disruptor.
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|---|---|---|---|---|
| CN114088750A (en) * | 2021-11-25 | 2022-02-25 | 中山大学 | Soil nanoparticle quantification method based on X-ray diffraction and ICP-MS |
| CN114088750B (en) * | 2021-11-25 | 2023-06-20 | 中山大学 | Soil nano particle quantification method based on X-ray diffraction and ICP-MS |
| CN114804212A (en) * | 2022-03-29 | 2022-07-29 | 中山大学 | Preparation method of nano goethite |
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