CN112090393A - Preparation method of green functional clay repairing material for composite pollution - Google Patents
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Abstract
A preparation method of a green functional clay repairing material for composite pollution belongs to the field of environmental protection material preparation, and can solve the problems of environmental risk, high cost and incapability of ensuring adsorption performance caused by the fact that the existing surfactant is used for clay modification.
Description
Technical Field
The invention belongs to the technical field of preparation of environment-friendly materials, and particularly relates to a preparation method of a green functional clay repairing material for composite pollution.
Background
The clay minerals such as bentonite, attapulgite, vermiculite are widely applied to the water body, the environment restoration fields such as pollutant adsorption in soil and degrading microbial inoculum load because of the characteristics of wide sources, low cost, strong adsorbability, high mechanical strength, small environmental influence and the like, but the hydrophilicity of the clay surface limits the restoration effect of the clay to organic pollutants, so that certain hydrophobic modification is required to be carried out to improve the adsorption of the materials to hydrophobic organic pollutants, the heavy metal adsorption capacity of the clay is further enhanced, the metal toxicity is reduced, the inhibition effect of heavy metals on the biodegradation of organic pollutants is relieved, and the restoration efficiency of the materials to composite pollution is further improved.
At present, the clay surface modification mainly uses a surfactant as a modifier, for example, CN111185474A discloses a chromium-contaminated soil in-situ remediation composite agent and a using method thereof, alkyl quaternary ammonium salt surfactants such as tetradecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium bromide, octadecyl trimethyl ammonium bromide and the like are used for carrying out intercalation modification on clay minerals, the specific surface area and the pore volume of the material are increased, the surface electrical property is also changed, and the adsorption performance of the material on Cr (VI) is obviously enhanced; CN104437384A discloses a composite modified bentonite, which is modified by sequentially using hexadecyl trimethyl ammonium bromide and sulfonated thiacalixarene, and the heavy metal ions are selectively complexed by using a modifier so as to realize the adsorption and removal of heavy metals in water; CN109569536A discloses a modified bentonite and a preparation process thereof, wherein reagents such as octadecyl dimethyl benzyl ammonium chloride, polyacrylamide and the like are used for modifying the bentonite, the interlamellar spacing, the specific surface area and the content of organic components of the obtained modified bentonite are increased, the adsorption capacity is enhanced, and the removal rate of COD in wastewater is effectively improved. The modification treatment in the patent documents can improve the adsorption capacity of the material to pollutants to a certain extent, but most of the related surfactants are chemically synthesized surfactants such as cetyl trimethyl ammonium bromide and stearyl trimethyl ammonium bromide, and when the surfactants enter soil and water environment along with the remediation material, the surfactants can generate toxic effects on soil microorganisms, aquatic organisms and the like, indirectly inhibit the degradation of the pollutants, further influence the remediation efficiency, and part of the surfactants are relatively poor in degradability and have certain environmental risks, so that the selection of an environment-friendly green modifier to replace the traditional surfactants has important environmental significance. CN108641681A discloses a preparation method of modified attapulgite clay particles as an oil spill dispersant, which selects environment-friendly biosurfactants such as rhamnolipid and sophorolipid as modifiers, and prepares an environment-friendly modified attapulgite material as an oil spill pollution dispersant based on intermolecular interaction; CN107445423A discloses a covering blanket for in-situ remediation of bottom mud polluted by refractory organic matters and a paving method thereof, wherein a solubilization layer is filler of rhamnolipid modified montmorillonite mixed with activated carbon, and the affinity of the rhamnolipid modified montmorillonite to the refractory organic matters such as PCB, PAHs and the like is enhanced, so that the covering blanket is beneficial to solubilization and adsorption fixation of the filler to target pollutants. Although the problem of environmental risk of the traditional surfactant is solved, the production cost of the rhamnolipid and the sophorolipid is high, and the yield is relatively low, so that the industrial production of the modified material is limited. Therefore, the environmental risk and modification effect of the modifier should be considered, and the modifier should be suitable for large-scale mass production.
Disclosure of Invention
The invention provides a preparation method of a green functional clay repairing material for composite pollution, aiming at the problems of environmental risk, high cost and incapability of ensuring adsorption performance caused by the fact that the existing surfactant is used for clay modification. The invention selects the soybean lecithin as amphoteric surfactant and the biochemical fulvic acid as nonionic surfactant as modifiers to modify clay, so as to realize the replacement of the traditional chemical synthesis surfactant, and the compound modification of the surfactant and the clay also improves the content of organic components of the clay, on the premise of retaining the adsorption performance of the amphoteric modifier to heavy metals, the modification of the biochemical fulvic acid further increases the adsorption performance of the material to organic pollutants and heavy metals, meanwhile, the modifier also has the functions of promoting the growth and the reproduction of microorganisms and the metabolic activity and the biocompatibility of the microorganism, it can be used for loading microbial agents to further cooperate with microorganisms to realize the degradation of organic pollutants, in addition, the fixation of the modified clay to the heavy metal can reduce the toxicity of the heavy metal to degradation bacteria in the environment, thereby relieving the inhibition effect of the heavy metal to the biodegradation process of organic pollutants.
The invention adopts the following technical scheme:
a preparation method of a green functional clay repairing material for composite pollution comprises the following steps:
firstly, mixing clay mineral which is purified by washing and is subjected to impurity removal with water in proportion, uniformly stirring to obtain a suspension, adding an absolute ethyl alcohol solution containing soybean lecithin in proportion to obtain a mixed solution, adjusting the pH of the mixed solution to be acidic, carrying out ultrasonic treatment for 15min, vibrating at a constant temperature of 40 ℃ for 24h, carrying out centrifugal separation, washing and drying to obtain lecithin modified clay;
and secondly, mixing the lecithin modified clay and water in proportion, uniformly stirring to obtain a suspension, adding an aqueous solution containing the biochemical fulvic acid in proportion to obtain a mixed solution, oscillating at a constant temperature of 25 ℃ for 24 hours, then carrying out centrifugal separation, washing and drying, and grinding and sieving with a 200-mesh sieve to obtain the lecithin-biochemical fulvic acid modified functional clay.
The modified clay obtained by the method can be used for adsorption and fixation of hydrophobic organic pollutants and heavy metals.
The clay mineral water washing purification method in the first step comprises the following steps: clay mineral and water according to a ratio of 1 g: mixing at a ratio of 20-100mL, stirring at a rotation speed of 600rpm for 24h at 25 ℃, taking the suspension, centrifuging at a rotation speed of 6000rpm for 15min, removing bottom impurities, collecting the supernatant, drying at 110 ℃ for 12-24h, grinding and sieving with a 200-mesh sieve to obtain the clay purified by water washing.
In the first step, the clay mineral comprises any one of bentonite, attapulgite and vermiculite.
In the first step, the clay mineral is sodium bentonite.
In the first step, the mixing ratio of the clay mineral and water after washing, purifying and removing impurities is 1 g: 20-100 mL.
The addition amounts of the soybean lecithin in the first step and the biochemical fulvic acid in the second step are respectively calculated according to the following formulas: m = m1X CEC x a x M x 0.01, wherein M is the mass/g of soybean lecithin or biochemical fulvic acid, M1The mass/kg of the clay mineral after water washing purification and impurity removal, and CEC is the cation exchange capacity/cmol.kg of the clay mineral after water washing purification and impurity removal-1And a is a modification ratio, the value is 0.25-2, and M is the relative molecular mass of the soybean lecithin.
In the first step the pH is adjusted to 2-3.
In the second step, the mixing ratio of the lecithin modified clay to water is 1 g: 20-100 mL.
The drying conditions in the first step and the second step are vacuum drying at 60 ℃ for 12-24 h.
The invention has the following beneficial effects:
compared with the prior art, the invention has the beneficial effects that:
1. the preparation method of the green functional clay remediation material for composite pollution is degradable, environment-friendly, free of ecological toxicity to microorganisms, aquatic plants and the like, simple, available in raw materials and low in cost.
2. A process for preparing the clay repairing material with green function to prevent the pollution of clay includes such steps as modifying soybean lecithin and biochemical fulvic acid to increase the content of organic carbon in clay, improving its surface hydrophobicity and adsorbing organic pollutants, and complexing the heavy metal ions by the active groups including hydroxy, carboxy, phosphate, carbonyl and amino groups.
3. The modified clay material can be used for adsorbing and fixing pollutants in water and soil, lecithin and biochemical fulvic acid can be used as a phosphorus source, a carbon source and a nitrogen source to promote the growth and the propagation of microorganisms and improve the metabolic activity of the microorganisms, the lecithin has good biocompatibility and can keep the activity of the microorganisms and secretase thereof, so that the modified clay can be used for loading the microorganisms, the degradation of the adsorbed organic pollutants is further realized by combining the loaded microorganisms, and the migration and the biotoxicity of heavy metals can be reduced by complexing and fixing active functional groups such as carboxyl, hydroxyl and the like contained in the material to the heavy metals, and the inhibition effect of the heavy metals on the biodegradation of organic matters when the heavy metals and the organic pollutants coexist can be favorably relieved.
4. Biochemical fulvic acid can promote and improve the soil acidity and alkalinity, the granular structure, the crop yield, the enzyme activity and the like to a certain extent, and biochemical fulvic acid and soybean lecithin can also indirectly supplement soil nutrients, so that the soil quality after pollution remediation can be further recovered and improved. Therefore, the application range and the efficacy of the clay material obtained by modifying the two modifiers are increased, so that the clay material becomes a functional clay material with adsorption performance, biostimulation and biocompatibility, and is further suitable for repairing and improving water and soil environments.
Detailed Description
A preparation method of a green functional clay repairing material for composite pollution comprises the following steps:
firstly, mixing clay mineral which is purified by washing and is subjected to impurity removal with water in proportion, uniformly stirring to obtain a suspension, adding an absolute ethyl alcohol solution containing soybean lecithin in proportion to obtain a mixed solution, adjusting the pH of the mixed solution to be acidic, carrying out ultrasonic treatment for 15min, vibrating at a constant temperature of 40 ℃ for 24h, carrying out centrifugal separation, washing and drying to obtain lecithin modified clay;
and secondly, mixing the lecithin modified clay and water in proportion, uniformly stirring to obtain a suspension, adding an aqueous solution containing the biochemical fulvic acid in proportion to obtain a mixed solution, oscillating at a constant temperature of 25 ℃ for 24 hours, then carrying out centrifugal separation, washing and drying, and grinding and sieving with a 200-mesh sieve to obtain the lecithin-biochemical fulvic acid modified functional clay.
Example 1
1g of water is taken to wash and purify sodiumAdding bentonite into 80mL water solution to obtain suspension, adding 20mL soybean lecithin anhydrous ethanol solution with modification ratio of 0.5 (containing soybean lecithin 0.3654 g), and adding 0.1 mol/L-1HNO of (2)3Adjusting the pH of the mixed solution to 2.29 by using the solution, carrying out ultrasonic treatment on the mixed solution for 15min, carrying out vibration on the mixed solution for 24h at 40 ℃ and 180rpm on a constant temperature oscillator, carrying out centrifugal separation, sequentially washing the clay for 5 times by using absolute ethyl alcohol and deionized water, and finally carrying out vacuum drying for 12h at 60 ℃ to obtain lecithin modified clay; adding the prepared lecithin modified clay into 20mL of aqueous solution to prepare suspension, adding 20mL of biochemical fulvic acid aqueous solution with the modification ratio of 1.0 (containing 0.2973g of biochemical fulvic acid), shaking the mixed solution on a constant temperature oscillator at 25 ℃ and 180rpm for 24h, then carrying out centrifugal separation, washing the clay for 5 times by using deionized water, carrying out vacuum drying at 60 ℃ for 12h, and grinding and sieving by using a 200-mesh sieve to obtain the lecithin-biochemical fulvic acid modified bentonite.
Example 2
Adding 1g of water-washed pure sodium bentonite into 80mL of water solution to obtain suspension, adding 20mL of soybean lecithin anhydrous ethanol solution with modification ratio of 1.0 (containing 0.7308g of soybean lecithin), and adding 0.1 mol/L-1HNO of (2)3Adjusting the pH of the mixed solution to 2.30 by using the solution, carrying out ultrasonic treatment on the mixed solution for 15min, carrying out vibration on the mixed solution for 24h at 40 ℃ and 180rpm on a constant temperature oscillator, carrying out centrifugal separation, sequentially washing the clay for 5 times by using absolute ethyl alcohol and deionized water, and finally carrying out vacuum drying for 12h at 60 ℃ to obtain lecithin modified clay; adding the prepared lecithin modified clay into 20mL of aqueous solution to prepare suspension, adding 20mL of biochemical fulvic acid aqueous solution with the modification ratio of 0.5 (containing 0.1487g of biochemical fulvic acid), shaking the mixed solution on a constant temperature oscillator at 25 ℃ and 180rpm for 24h, then carrying out centrifugal separation, washing the clay for 5 times with deionized water, carrying out vacuum drying at 60 ℃ for 12h, and then grinding and sieving with a 200-mesh sieve to obtain the lecithin-biochemical fulvic acid modified bentonite.
Example 3
Adding 1g of water-washed pure sodium bentonite into 80mL of water solution to obtain suspension, adding 20mL of soybean lecithin anhydrous ethanol solution with modification ratio of 1.0 (containing 0.7308g of soybean lecithin), and adding 0.1 mol/L-1HNO of (2)3The solution adjusts the pH of the mixture to 2.32, and thenPerforming ultrasonic treatment on the mixed solution for 15min, then performing centrifugal separation after shaking for 24h at 40 ℃ and 180rpm on a constant temperature oscillator, sequentially washing the clay for 5 times by using absolute ethyl alcohol and deionized water, and finally performing vacuum drying for 12h at 60 ℃ to obtain lecithin modified clay; adding the prepared lecithin modified clay into 20mL of aqueous solution to prepare suspension, adding 20mL of biochemical fulvic acid aqueous solution with the modification ratio of 1.0 (containing 0.2973g of biochemical fulvic acid), shaking the mixed solution on a constant temperature oscillator at 25 ℃ and 180rpm for 24h, then carrying out centrifugal separation, washing the clay for 5 times by using deionized water, carrying out vacuum drying at 60 ℃ for 12h, and then grinding and sieving by using a 200-mesh sieve to obtain the lecithin-biochemical fulvic acid modified bentonite.
The modified clay prepared in the above examples 1, 2 and 3 adsorbs cadmium and naphthalene in water:
the concentration of the extract in 25mL is 7.5 mg.L-1Naphthalene, 50 mg. L-1Cd (2)2+0.1g of the modified clay prepared in examples 1, 2 and 3 was added to the mixed solution, and the amount of the modified clay was adjusted to 0.01 mol. L-1HNO of (2)3And adjusting the initial pH of the solution to be about 7.0 with NaOH, oscillating the solution at 25 ℃ and 180rpm for 24 hours, performing centrifugal separation to determine the concentration of the pollutants in the supernatant, and simultaneously setting unmodified bentonite for comparison, wherein the result shows that the adsorption performance of the modified clay is improved, and the removal rate of the modified clay to the pollutants is greatly higher than that of the unmodified clay.
TABLE 1 removal efficiency of naphthalene and cadmium by modified sodium bentonite with different modification ratios
Claims (9)
1. A preparation method of a green functional clay repairing material for composite pollution is characterized by comprising the following steps: the method comprises the following steps:
firstly, mixing clay mineral which is purified by washing and is subjected to impurity removal with water in proportion, uniformly stirring to obtain a suspension, adding an absolute ethyl alcohol solution containing soybean lecithin in proportion to obtain a mixed solution, adjusting the pH of the mixed solution to be acidic, carrying out ultrasonic treatment for 15min, vibrating at a constant temperature of 40 ℃ for 24h, carrying out centrifugal separation, washing and drying to obtain lecithin modified clay;
and secondly, mixing the lecithin modified clay and water in proportion, uniformly stirring to obtain a suspension, adding an aqueous solution containing the biochemical fulvic acid in proportion to obtain a mixed solution, oscillating at a constant temperature of 25 ℃ for 24 hours, then carrying out centrifugal separation, washing and drying, and grinding and sieving with a 200-mesh sieve to obtain the lecithin-biochemical fulvic acid modified functional clay.
2. The preparation method of the green functional clay remediation material for combined pollution according to claim 1, wherein the preparation method comprises the following steps: the clay mineral water washing purification method in the first step comprises the following steps: clay mineral and water according to a ratio of 1 g: mixing at a ratio of 20-100mL, stirring at a rotation speed of 600rpm for 24h at 25 ℃, taking the suspension, centrifuging at a rotation speed of 6000rpm for 15min, removing bottom impurities, collecting the supernatant, drying at 110 ℃ for 12-24h, grinding and sieving with a 200-mesh sieve to obtain the clay purified by water washing.
3. The preparation method of the green functional clay remediation material for combined pollution according to claim 1, wherein the preparation method comprises the following steps: in the first step, the clay mineral comprises any one of bentonite, attapulgite and vermiculite.
4. The preparation method of the green functional clay remediation material for combined pollution according to claim 1, wherein the preparation method comprises the following steps: in the first step, the clay mineral is sodium bentonite.
5. The preparation method of the green functional clay remediation material for combined pollution according to claim 1, wherein the preparation method comprises the following steps: in the first step, the mixing ratio of the clay mineral and water after washing, purifying and removing impurities is 1 g: 20-100 mL.
6. The preparation method of the green functional clay remediation material for combined pollution according to claim 1, wherein the preparation method comprises the following steps: the addition amounts of the soybean lecithin in the first step and the biochemical fulvic acid in the second step are respectively according to the following formulasAnd (3) calculating: m = m1X CEC x a x M x 0.01, wherein M is the mass/g of soybean lecithin or biochemical fulvic acid, M1The mass/kg of the clay mineral after water washing purification and impurity removal, and CEC is the cation exchange capacity/cmol.kg of the clay mineral after water washing purification and impurity removal-1And a is a modification ratio, the value is 0.25-2, and M is the relative molecular mass of the soybean lecithin.
7. The preparation method of the green functional clay remediation material for combined pollution according to claim 1, wherein the preparation method comprises the following steps: in the first step the pH is adjusted to 2-3.
8. The preparation method of the green functional clay remediation material for combined pollution according to claim 1, wherein the preparation method comprises the following steps: in the second step, the mixing ratio of the lecithin modified clay to water is 1 g: 20-100 mL.
9. The preparation method of the green functional clay remediation material for combined pollution according to claim 1, wherein the preparation method comprises the following steps: the drying conditions in the first step and the second step are vacuum drying at 60 ℃ for 12-24 h.
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| CN114590978A (en) * | 2022-01-30 | 2022-06-07 | 中国环境科学研究院 | Material for inhibiting release of endogenous phosphorus and arsenic in sediment and using method |
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