CN114288985A - Black talc adsorption material and preparation method and application thereof - Google Patents
Black talc adsorption material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a black talc soil adsorbing material and a preparation method thereof, and belongs to the field of non-metallic mineral materials. The black talc soil adsorption material prepared by the method has rich chemical active sites and Mg coordination unsaturated sites, and can be interacted with heavy metal in soil through hydrogen bonds, electrostatic attraction and van der Waals force, so that the binding capacity of the black talc soil adsorption material with heavy metal ions is improved. The preparation method is simple, reaction conditions are easy to control, the soil remediation method has the advantages of stable skeleton structure, lasting remediation effect, capability of properly adjusting the pH and air permeability of the soil, environmental friendliness, no secondary pollution and the like, has a good remediation effect on the soil polluted by different pollutants, and has a very wide application prospect.
Description
Technical Field
The invention belongs to the field of non-metallic mineral materials, and particularly relates to a black talc adsorption material and a preparation method and application thereof.
Background
Soil is a natural resource on which human beings rely to live, and consists of three substances, namely a solid phase, a liquid phase and a gas phase, and mainly comprises mineral substances, organic matters, moisture, air and microorganisms. Healthy soil should contain about 45% minerals, about 25% air, about 25% water, about 5% organic matter and about 1% microbes. However, the cultivation of crops on soil is in a state of high intensification, high multiple cropping index and high fertilizer input for a long time, and a series of soil obstacles such as crop yield reduction, soil secondary salinization, soil acidification, nutrient imbalance and the like are caused.
In contaminated soils, over 80% are toxic inorganic contaminants, the most common of which is Pb2+、Cd2+、Cr3 +、Cu2+、Co2+、Ni2+、Zn2+Heavy metal ions, and toxic anions such as arsenate, chromate, selenate, sulfate, etc. Besides, the pollution of typical organic matters such as Polycyclic Aromatic Hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), petroleum and the like to the soil is not negligible. Pollutants dispersed in the soil, which affect the growth of plants or enter human bodies through food chains, cause great harm to human health. Therefore, the remediation and treatment of the soil pollution are urgent. Among the treatment options available, adsorption is generally considered to be the most economically attractive technology, capable of treating a wide variety of pollutants, efficient, simple in design, easy to operate, and produces fewer toxic by-products. Natural clay minerals (such as diatomite, black talc, bentonite, attapulgite, sepiolite, kaolin and the like) have the advantages of rich sources, low price, large specific surface area and the like, are paid more attention in recent years, and gradually become materials capable of effectively replacing conventional adsorbents. However, most of them have disadvantages of low adsorption amount, few effective adsorption sites, and easy agglomeration, and therefore, development of an adsorbent which is highly efficient, stable, and easily separated from a solvent after treatment is important.
The black talc is a natural clay mineral, has a T-O-T type layered structure, is composed of two silica tetrahedral sheets and a magnesia octahedron, has excellent chemical stability as a layered silicate mineral without interlayer charges, simultaneously contains active functional groups on the surface of the black talc, such as Mg-O, Si-O, OH, Si-OH and the like, is exposed after being crushed, generates surface active sites, and has certain adsorbability. However, the black talc with a layered structure has high surface energy, so that the black talc is easy to accumulate groups, the specific surface area is reduced, surface active sites are hidden, the number of exposed functional groups is small, and the adsorption performance is limited; the organic acid and coupling agent grafted modified black talc mineral material has the advantages of stable skeleton structure, lasting repairing effect, capability of properly adjusting the pH and air permeability of soil, environmental friendliness, no secondary pollution and the like when being used for the soil repairing process, has a good repairing effect on the soil polluted by different pollutants, and has a very wide application prospect.
Disclosure of Invention
The invention aims to provide a black talc adsorption material, a preparation method thereof and application thereof in adsorbing heavy metals in soil.
In order to solve the problems, the invention adopts the following technical scheme:
the invention provides a black talc adsorbing material which is prepared by the following method:
(1) purification of black talc: adding water A and disodium hydrogen phosphate into the black talcum powder with the average particle size of 400-500nm, stirring at 25-40 ℃ for 12-20h (preferably stirring at 30 ℃ for 15h), and carrying out aftertreatment A on the obtained mixture to obtain purified black talcum powder; the mass ratio of the steatite powder to the disodium hydrogen phosphate is 100: 2-7 (preferably 100: 2.5);
(2) adding ethanol and water B into the purified black talcum powder obtained in the step (1), uniformly mixing, and performing ultrasonic dispersion; adding a modifier, stirring and reacting at 75-95 ℃ for 6-12h (preferably at 85 ℃ for 6h), and carrying out aftertreatment B on the obtained reaction liquid to obtain the black talc adsorption material; the volume ratio of the ethanol to the water B is 7-10:1 (preferably 7.5: 1); the volume of the ethanol is 4-8mL/g (preferably 7.5mL/g) based on the mass of the black talc; the modifier is citric acid or tartaric acid (preferably citric acid); the mass ratio of the purified black talcum powder to the modifier is 1-10:1 (preferably 1-5:1, and most preferably 5: 1).
The water A and the water B are both water, and different letters are used only for distinguishing the water added at different stages, and no other special meanings are given.
Further, the black talc powder in the step (1) is ultra-fine black talc powder, and the average particle size is 400-500 nm. The black talcum powder is prepared by the following steps: crushing and grinding black talc (the black talc is from Shanghai Guangfeng region in Jiangxi), sieving by a 50-mesh sieve to obtain 50-mesh black talc powder, placing the black talc powder into a ball milling tank, adding ethanol, carrying out wet ball milling for 6-9h at 800 r/min, centrifuging, washing with water, precipitating, centrifuging again, and drying for 24h at 60 ℃ to obtain the black talc powder with the average particle size of 400-500 nm.
Preferably, the mass ratio of the hydrotalcite powder to the water A in the step (1) is 1:8-12 (preferably 1: 9-10.5, most preferably 1: 9).
Further, the post-treatment A in the step (1) is as follows: and (3) standing the mixture (preferably standing for 12h), centrifuging an upper layer black talc suspension (discarding a bottom precipitate), washing the obtained precipitate with water (three times), and drying at the temperature of 80-110 ℃ for 6-12h (preferably drying at the temperature of 105 ℃ for 6h) to obtain the purified black talc.
Further, the post-treatment B in the step (2) is as follows: and centrifuging the reaction solution, washing the obtained precipitate with water, removing water, and drying at 80-110 ℃ for 6-12h (preferably at 105 ℃ for 12h) to obtain the black talc adsorbing material.
The invention also provides an application of the black talc adsorption material in adsorption of heavy metals in soil.
Preferably, the heavy metal is Pb2+。
Further preferably, the application is: adding the black talc adsorption material into the air-dried soil, fully mixing, adding deionized water to keep the water content of the soil at 60%, and performing mixed culture for 7 days to finish adsorption; wherein the mass ratio of the black talc adsorbing material to the air-dried soil is 1: 20.
Compared with the prior art, the invention has the beneficial effects that: the black talc soil adsorbing material produced by the process has larger specific surface area, is in a regular lamellar shape and is not stacked with each other, and has stronger adsorption performance and high stability. The black talc soil adsorption material prepared by the method has rich-COOH, Si-O, -OH, long alkane chains and Mg coordination unsaturated sites, can be firmly combined with a modifier through the interaction of hydrogen bonds, electrostatic attraction and van der Waals force, has higher stability and hydrophobic effect, greatly increases the surface active sites, improves the binding capacity with heavy metal ions, and has high adsorption rate and high adsorption capacity, thereby achieving the purposes of adsorption and passivation. The preparation method is simple, the reaction conditions are easy to control, and the black talc soil adsorbing material has excellent mechanical stability, dispersibility and adsorbability and wide application prospect.
Drawings
FIG. 1 is a scanning electron microscope image of modified black talc powder.
FIG. 2 is an infrared spectrum of black talc (lower) and modified black talc (upper) prepared in example 1.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples, and various modifications and implementations are intended to be included within the technical scope of the present invention without departing from the content and scope of the present invention.
In the following examples, the black talc is from Shanghai Guangfeng region in Jiangxi;
the measurement method and conditions of the adsorption amount in the following examples were:
the soil is taken from garden near experimental building of rockery school district of Zhejiang industrial university, air-dried at room temperature, accurately weighed 500g of soil after being sieved by 2mm, and added with 200mg/L Pb (NO) according to 100mg Pb/kg of soil3)2And (3) mixing the solution with 250mL of the solution, keeping water, maintaining for 60 days, naturally drying, grinding, and sieving by using a 2mm sieve to prepare the simulated lead-polluted soil serving as the soil to be tested. To an air-dried soil sample (10g) was added 0.5g of dry sorbent powder, which was then thoroughly mixed in a polyethylene cup. The mass of black talc adsorbent in soil was 5% of the air dried soil sample. Deionized water was then added to maintain the soil at 60% moisture and mixed for 7 days. Finally, 20mL of acetic acid was added to a 50mL centrifuge tubeSolution (pH 2.88) 1.0g of soil sample was extracted. The tubes were shaken in a rotary shaker at 30r/min for 18 hours. Then, the supernatant was collected and tested for the concentration of heavy metals remaining in the soil leachate by ICP-OES. Finally, the adsorption capacity of the adsorbent is calculated by the formula q ═ Co-Ce ═ V/m, wherein Co is the concentration of heavy metals in the soil leachate to which the adsorbent is not added (2.5mg/L), Ce is the concentration of heavy metals in the soil leachate to which the adsorbent is added (mg/L), V is the volume of the leachate (0.02L), and m is the mass of the adsorbent (0.05g)
The preparation method of the black talcum powder in the following examples comprises the following steps:
manually crushing 80g of black talc, grinding, sieving by using a 50-mesh sieve to obtain 70g of 50-mesh black talc powder, weighing 50g of black talc powder, putting the black talc powder into a ball milling tank, adding 80ml of ethanol, carrying out wet grinding for 6h by using a ball mill at 800 rpm, centrifuging, washing the obtained precipitate for 3 times by using water, centrifuging, and drying for 24h at 60 ℃ to prepare 40g of black talc powder. The prepared hydrotalcite powder had an average particle size of 400nm as observed with a scanning electron microscope.
Example 1
(1) Adding 20g of black talcum powder into a 300ml conical flask, then adding 180g of water and 0.5g of disodium hydrogen phosphate, and stirring at the constant temperature of 30 ℃ for 15 hours; standing for 12h, extracting the upper layer black talc suspension, centrifuging, washing with water three times, and drying at 105 deg.C for 6h to obtain 11.3g of purified black talc powder.
(2) Adding 1.0g of the obtained purified black talc into a 50ml three-necked bottle, adding 7.5ml of ethanol and 1ml of water, uniformly mixing, and performing ultrasonic dispersion for 30 min; adding 0.2g of modifier citric acid, stirring and reacting at 85 ℃ for 6h, centrifuging, washing with water, and drying at 105 ℃ for 12h to obtain 0.95g of black talc soil adsorbing material. Mixing 0.5g of the black talc adsorption material with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (pH is 2.88), wherein the volume of a leaching solution is 0.02L, and measuring the concentration of heavy metal in the soil leaching solution to be 2.481mg/L by ICP-OES; the black talc adsorbing material has good Pb-removing effect2+The amount of adsorbed was 7.6 mg/kg.
Example 2
(1) Adding 20g of black talcum powder into a 300ml conical flask, then adding 210g of water and 0.7g of disodium hydrogen phosphate, and stirring at the constant temperature of 30 ℃ for 15 hours; standing for 12h, extracting the upper layer black talc suspension, centrifuging, washing with water three times, and drying at 105 deg.C for 6h to obtain 10.4g of purified black talc powder.
(2) Adding 1.0g of the obtained purified black talc into a 50ml three-necked bottle, adding 7.5ml of ethanol and 1ml of water, uniformly mixing, and performing ultrasonic dispersion for 30 min; adding 0.5g of citric acid, stirring and reacting at 85 ℃ for 6h, centrifuging, washing with water, and drying at 105 ℃ for 12h to obtain 0.92g of black talc soil adsorbing material. Mixing 0.5g of the black talc adsorption material with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (pH is 2.88), wherein the volume of a leaching solution is 0.02L, and measuring the concentration of heavy metal in the soil leaching solution to be 2.491mg/L by ICP-OES; the black talc soil adsorbing material has good effect on Pb2+The amount of adsorbed was 3.6 mg/kg.
Example 3
(1) Adding 20g of black talcum powder into a 300ml conical flask, then adding 240g of water and 0.7g of disodium hydrogen phosphate, and stirring at the constant temperature of 30 ℃ for 15 hours; standing for 12h, extracting the upper layer black talc suspension, centrifuging, washing with water three times, and drying at 105 ℃ for 6h to obtain 9.9g of purified black talc.
(2) Adding 1.0g of the obtained purified black talc into a 50ml three-necked bottle, adding 7.5ml of ethanol and 1ml of water, uniformly mixing, and performing ultrasonic dispersion for 30 min; adding 0.1g of citric acid, stirring and reacting at 85 ℃ for 6h, centrifuging, washing with water, and drying at 105 ℃ for 12h to obtain 0.92g of black talc soil adsorbing material. Mixing 0.5g of the black talc adsorption material with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (pH is 2.88), wherein the volume of a leaching solution is 0.02L, and measuring the concentration of heavy metal in the soil leaching solution to be 2.489mg/L by ICP-OES; the black talc soil adsorbing material has good effect on Pb2+The amount of adsorbed was 4.4 mg/kg.
Example 4
(1) Adding 20g of black talcum powder into a 300ml conical flask, then adding 210g of water and 0.5g of disodium hydrogen phosphate, and stirring at the constant temperature of 30 ℃ for 15 hours; standing for 12h, extracting the upper layer black talc suspension, centrifuging, washing with water three times, and drying at 105 deg.C for 6h to obtain 11.0g of purified black talc powder.
(2) Adding 1.0g of the obtained purified black talc into a 50ml three-necked bottle, adding 7.5ml of ethanol and 1ml of water, uniformly mixing, and performing ultrasonic dispersion for 30 min; adding 0.2g of citric acid, stirring and reacting at 85 ℃ for 12h, centrifuging, washing with water, and drying at 105 ℃ for 12h to obtain 0.90g of black talc soil adsorbing material. Mixing 0.5g of the black talc adsorption material with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (pH is 2.88), wherein the volume of a leaching solution is 0.02L, and measuring the concentration of heavy metal in the soil leaching solution to be 2.482mg/L by ICP-OES; the black talc soil adsorbing material has good effect on Pb2+The amount of adsorbed was 7.2 mg/kg.
Example 5
(1) Adding 20g of black talcum powder into a 300ml conical flask, then adding 180g of water and 0.4g of disodium hydrogen phosphate, and stirring at the constant temperature of 30 ℃ for 15 hours; standing for 12h, extracting the upper layer black talc suspension, centrifuging, washing with water three times, and drying at 105 ℃ for 6h to obtain 10.8g of purified black talc.
(2) Adding 1.0g of the obtained purified black talc into a 50ml three-necked bottle, adding 7.5ml of ethanol and 1ml of water, uniformly mixing, and performing ultrasonic dispersion for 30 min; adding 0.2g of citric acid, stirring and reacting at 60 ℃ for 12h, centrifuging, washing with water, and drying at 105 ℃ for 12h to obtain 0.85g of black talc soil adsorbing material. Mixing 0.5g of the black talc adsorption material with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (pH is 2.88), wherein the volume of a leaching solution is 0.02L, and measuring the concentration of heavy metal in the soil leaching solution to be 2.491mg/L by ICP-OES; the black talc soil adsorbing material has good effect on Pb2+The amount of adsorbed was 3.6 mg/kg.
Example 6
(1) Adding 20g of black talcum powder into a 300ml conical flask, then adding 240g of water and 0.4g of disodium hydrogen phosphate, and stirring at the constant temperature of 30 ℃ for 15 hours; standing for 12h, extracting the upper layer black talc suspension, centrifuging, washing with water three times, and drying at 105 deg.C for 6h to obtain 9.0g of purified black talc powder.
(2) Adding 1.0g of the obtained purified black talc into a 50ml three-necked bottle, adding 7.5ml of ethanol and 1ml of water, uniformly mixing, and performing ultrasonic dispersion for 30 min; adding 0.2And g of citric acid, stirring and reacting for 6 hours at 95 ℃, centrifuging, washing with water, and drying for 12 hours at 105 ℃ to obtain 0.93g of black talc soil adsorbing material. Mixing 0.5g of the black talc adsorption material with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (the pH value is 2.88), wherein the volume of a leaching solution is 0.02L, and measuring the concentration of heavy metal in the soil leaching solution to be 2.485mg/L by ICP-OES; the black talc soil adsorbing material has good effect on Pb2+The amount of adsorbed was 6.0 mg/kg.
Example 7
(1) Adding 20g of black talcum powder into a 300ml conical flask, then adding 180g of water and 0.7g of disodium hydrogen phosphate, and stirring at the constant temperature of 30 ℃ for 15 hours; standing for 12h, extracting the upper layer black talc suspension, centrifuging, washing with water three times, and drying at 105 deg.C for 6h to obtain 9.4g of purified black talc powder.
(2) Adding 1.0g of the obtained purified black talc into a 50ml three-necked bottle, adding 7.5ml of ethanol and 1ml of water, uniformly mixing, and performing ultrasonic dispersion for 30 min; adding 0.2g of tartaric acid as a modifier, stirring and reacting at 85 ℃ for 6h, centrifuging, washing with water, and drying at 105 ℃ for 12h to obtain 0.92g of modified black talc adsorbent. Mixing 0.5g of the black talc adsorption material with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (pH is 2.88), wherein the volume of a leaching solution is 0.02L, and measuring the concentration of heavy metal in the soil leaching solution to be 2.486mg/L by ICP-OES; the black talc soil adsorbing material has good effect on Pb2+The amount of adsorbed was 5.6 mg/kg.
Comparative example 1
(1) Directly adding 1.0g of the non-purified steatite powder into a 50ml three-necked bottle, adding 7.5ml of ethanol and 1ml of water, uniformly mixing, and performing ultrasonic dispersion for 30 min; adding 0.2g of modifying agent citric acid, stirring and reacting at 85 ℃ for 6h, centrifuging, washing with water, and drying at 105 ℃ for 12h to obtain 0.92g of black talc adsorbing material. Mixing 0.5g of the black talc soil adsorbing material with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (the pH value is 2.88), wherein the volume of a leaching solution is 0.02L, and measuring the concentration of heavy metal in the soil leaching solution to be 2.494mg/L by ICP-OES; the black talc adsorbing material has good Pb-removing effect2+Adsorption of (2)The amount was 2.4 mg/kg.
Comparative example 2
(1) Mixing 0.5g of unmodified black talc (purified) with 10g of soil to be tested, adding 6ml of water, culturing at room temperature for 7 days, air-drying the soil, taking 1.0g of the soil, extracting a soil sample by using an acetic acid solution (pH is 2.88), wherein the volume of the leaching solution is 0.02L, and the concentration of heavy metal in the soil leaching solution is 2.499mg/L by ICP-OES; the black talc adsorbing material has good Pb-removing effect2+The amount of adsorption of (B) was 0.4 mg/kg.
Claims (10)
1. The black talc adsorbing material is characterized by being prepared by the following method:
(1) purification of black talc: adding water A and disodium hydrogen phosphate into the black talcum powder with the average particle size of 400-500nm, stirring for 12-20h at 25-40 ℃, and carrying out aftertreatment on the obtained mixture A to obtain purified black talcum powder; the mass ratio of the steatite powder to the disodium hydrogen phosphate is 100: 2-7;
(2) adding ethanol and water B into the purified black talcum powder obtained in the step (1), uniformly mixing, and performing ultrasonic dispersion; adding a modifier, stirring and reacting at 75-95 ℃ for 6-12h, and carrying out aftertreatment B on the obtained reaction liquid to obtain the black talc adsorption material; the volume ratio of the ethanol to the water B is 7-10: 1; the volume of the ethanol is 4-8mL/g based on the mass of the black talc; the modifier is citric acid or tartaric acid; the mass ratio of the purified black talcum powder to the modifier is 1-10: 1.
2. The black talc adsorbent material of claim 1, wherein: the method for preparing the black talc powder in the step (1) comprises the following steps: crushing and grinding the black talc powder, sieving the crushed black talc powder by using a 50-mesh sieve to obtain 50-mesh black talc powder, placing the black talc powder into a ball milling tank, adding ethanol, carrying out wet ball milling for 6-9h at 800 r/min, centrifuging, washing the precipitate with water, centrifuging again, and drying the precipitate for 24h at 60 ℃ to obtain the black talc powder with the average particle size of 400-500 nm.
3. The black talc adsorbent material of claim 1, wherein: the mass ratio of the black talc powder to the water A in the step (1) is 1: 8-12.
4. The black talc adsorbent material of claim 1, wherein said post-treatment a in step (1) is: and standing the mixture, centrifuging the suspension of the black talc at the upper layer, washing the obtained precipitate with water, and drying at the temperature of 80-110 ℃ for 6-12h to obtain the purified black talc.
5. The black talc adsorbent material of claim 1, wherein: the modifier is citric acid.
6. The black talc adsorbent material of claim 1, wherein: the mass ratio of the purified black talcum powder to the modifier is 1-5: 1.
7. The black talc adsorbent material of claim 1, wherein said post-treatment B in step (2) is: and centrifuging the reaction solution, washing the obtained precipitate with water, removing water, and drying at the temperature of 80-110 ℃ for 6-12h to obtain the black talc adsorption material.
8. The use of the black talc adsorbent of claim 1 for adsorbing heavy metals from soil.
9. The use of claim 8, wherein: the heavy metal is Pb2+。
10. The use according to claim 8, characterized in that the use is: adding the black talc adsorption material into the air-dried soil, fully mixing, adding deionized water to keep the water content of the soil at 60%, and performing mixed culture for 7 days to finish adsorption; wherein the mass ratio of the black talc adsorbing material to the air-dried soil is 1: 20.
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| CN115367832A (en) * | 2022-07-11 | 2022-11-22 | 中南大学 | Application of calcium iron garnet As As (III) adsorption material |
| CN115715970A (en) * | 2022-11-18 | 2023-02-28 | 浙江工业大学 | Black talc-based nano mineral crystal and preparation method thereof |
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