CN114106838A - Large-particle cadmium passivation material with calcium bentonite as substrate and preparation method thereof - Google Patents
Large-particle cadmium passivation material with calcium bentonite as substrate and preparation method thereof Download PDFInfo
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- CN114106838A CN114106838A CN202111420769.5A CN202111420769A CN114106838A CN 114106838 A CN114106838 A CN 114106838A CN 202111420769 A CN202111420769 A CN 202111420769A CN 114106838 A CN114106838 A CN 114106838A
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
- C09K17/08—Aluminium compounds, e.g. aluminium hydroxide
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- C—CHEMISTRY; METALLURGY
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- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
- C09K17/04—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only applied in a physical form other than a solution or a grout, e.g. as granules or gases
Abstract
The invention discloses a large-particle cadmium passivation material taking calcium bentonite as a substrate and a preparation method thereof, wherein the preparation method comprises the following steps: putting calcium bentonite and calcium hydroxide powder into a reaction container according to a proportion, adding water with the same mass, keeping the humidity of the mixture at 100%, and stirring the mixture at room temperature in an oscillating way to fully and uniformly mix the materials; baking the product in an oven, and then putting the baked product in a pressurizer to obtain a cylindrical passivation material; drying and shrinking the cylindrical passivation material at high temperature, and cutting the cylindrical passivation material into granular passivation material. The powder passivation material is uniformly dispersed and crosslinked by utilizing the strong adsorption force and the viscosity after the water absorption and expansion of the calcium bentonite, and the powder material is further tightly fixed by utilizing the volume shrinkage characteristic after the high-temperature dehydration of the calcium bentonite, so that the powder material is changed into a large-particle material, no dust is generated during the spreading, and the operability and the safety are improved. The slow release performance of the passivation material for releasing hydroxide ions is improved, the ecological toxicity is reduced, and the passivation effect of the passivation material on cadmium is not influenced after modification.
Description
Technical Field
The invention relates to the technical field of cadmium pollution repair materials, in particular to a large-particle cadmium passivation material taking calcium bentonite as a substrate and a preparation method thereof.
Background
In recent years, with the continuous progress of industrialization and urbanization, frequent human activities cause serious damage to the ecological environment of the drainage basin. Wastewater generated by industrial activities such as mining, smelting and the like is discharged to rivers without treatment, a large amount of heavy metal (Cd, Pb and the like) elements directly flow to a water body and enter farmlands through farming irrigation, so that the heavy metal in the farmland soil exceeds the standard, and the Cd pollution situation of the farmland soil is not optimistic. In 2014, national soil pollution survey bulletin shows that the exceeding standard rate of the soil point position in China is 16.1%, the exceeding standard problem of cadmium is the most serious, and the exceeding standard rate of the point position reaches 7%, which indicates that the soil environment quality in China is great. With the exposure of the cadmium rice, heavy metal vegetables and other events in China, the problems of agricultural product safety and farmland soil cadmium pollution have attracted wide social attention. Therefore, research and development of efficient, convenient, low-cost, reproducible and easily-popularized repair technology or material for ensuring safe utilization of cadmium-overproof farmland is urgently needed.
At present, many researches on the treatment and safe utilization of cadmium polluted soil are carried out, including passivant development and application, planting system adjustment, agricultural technology and the like. The passivator is developed more, comprises lime, organic fertilizer, biochar, sepiolite, hydroxyapatite and the like, and can reduce the absorption of cadmium by crops to a certain degree mainly by improving the pH value of soil, changing the form of cadmium and reducing the content of effective cadmium in the soil; the agricultural technology mainly influences the morphological transformation process of the cadmium in the soil by changing the physical and chemical properties of the soil environment such as Eh and the like, and further influences the absorption amount of the cadmium in plants. The in-situ passivation technology is a commonly used repair method at present, and mainly adds alkaline or adsorption materials into soil to enable heavy metals to be subjected to adsorption, complexation, precipitation, ion exchange and other processes in the soil, so that the bioavailability of cadmium in the soil is reduced, and the cadmium absorption of crops is reduced (Liu Yi Yun, etc., 2021; Du Cai, etc., 2019). The technology is low in cost and high in timeliness, is suitable for safe production of large-area farmland with light and medium cadmium exceeding the standard, and is a hot point of current research (Wangzongya and the like, 2021; Wangkou and the like, 2020; Li and the like, 2019).
The commonly used passivation materials at present comprise lime, clay minerals, zeolite, phosphate and the like, and the cadmium in the soil, carbonate and hydroxide form precipitates and the adsorption capacity of the soil to the cadmium is increased by increasing the pH value of the soil, so that the bioavailability and the mobility of the cadmium in the soil are reduced, and the absorption and accumulation of crops are reduced. The materials are relatively low in price, large in earth crust reserve, good in heavy metal fixing effect and small in influence on the texture structure and physical and chemical properties of soil, and are widely applied to remediation of heavy metal polluted farmland soil in recent years. Currently, most passivation materials are still limited in application in two aspects: on the one hand, the basic passivation material has poor operability and safety. The existing passivator has the best application effect of an alkaline material, wherein hydrated lime is widely applied, but most of materials have small particle size and are in a fine powder shape, so that dust is easily raised in the application process, eyes and skin of a person are strongly stimulated, the personal safety of constructors is harmed, and the operability and construction cost of the material are seriously influenced. On the other hand, the acute ecotoxicity caused by the quick release of the alkaline passivation material. After the hydrated lime is applied to the soil, hydroxide ions are quickly released, the pH value of the soil is improved, soil organisms such as fishes, loaches and the like are quickly killed, and the hydrated lime has a strong destructive effect on a soil ecosystem.
Therefore, there is a need for a passivation material and a preparation method thereof, which can improve the operability and safety and reduce the ecological toxicity of the passivation material after being applied into soil without affecting the passivation effect of cadmium.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a large-particle cadmium passivation material taking calcium bentonite as a substrate and a preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme: the large-particle cadmium passivation material is prepared from raw materials of calcium bentonite powder and calcium hydroxide powder, the mass ratio of the calcium bentonite to the calcium hydroxide is 1:1, and the cadmium passivation material is a cylindrical particle material.
Preferably, the height of the cadmium passivation material is 4-6mm, and the diameter of the cross section of the cadmium passivation material is 4-6 mm. Further preferably, the height is 5mm and the cross-sectional diameter is 5 mm.
In addition, in order to achieve the above purpose, the invention also provides a preparation method of the large-particle cadmium passivation material with calcium bentonite as the substrate, which comprises the following steps:
s1, putting the calcium bentonite and the calcium hydroxide powder into a reaction container according to a proportion, adding water with the same mass, keeping the humidity of the mixture at 100%, and stirring under oscillation at room temperature to fully and uniformly mix the materials;
s2, baking the product obtained in the step S1 in an oven, and then putting the baked product in a pressurizer to obtain a cylindrical passivation material;
and S3, drying the cylindrical passivation material and cutting the cylindrical passivation material into the granular passivation material.
Preferably, the particle size of the calcium bentonite powder is 1-10 μm; the particle size of the calcium hydroxide powder is 5-15 mu m.
Preferably, the particle size of the calcium bentonite powder is 5 μm; the particle size of the calcium hydroxide powder is 10 mu m.
Preferably, in the step S1, the agitation is performed with oscillation time of 2-3h and the agitation speed of 170-210 rpm.
Preferably, the baking temperature in the step S2 is 65-75 ℃, and the baking is stopped when the humidity in the oven is 18% -23%.
Preferably, the pressurizer is a piston pressurizing device, and the diameter of an outlet of the pressurizer is 4-6mm of a circular outlet. Further preferably, the outlet diameter is 5 mm.
Preferably, the drying temperature in the step S3 is 300-350 ℃.
The release rate of the large-particle cadmium passivation material is far lower than that of a powder passivation material, so that the problems of poor operability and safety and high ecological toxicity of the powder passivation material are solved, and the large-particle cadmium passivation material has a cadmium pollution repair effect similar to that of the powder material.
The invention has the beneficial effects that: the method of the invention utilizes the strong adsorption force and viscosity of the calcium bentonite after water absorption and expansion to uniformly disperse and crosslink the powder passivation material, and further utilizes the volume shrinkage characteristic of the calcium bentonite after heating and dehydration to tightly fix the powder material, thereby improving the physical properties of the passivation material, changing the powder material into a large-particle material, being easier to spread and not generating raise dust, and improving the operability and safety. The passivation material is agglomerated, fine particles are dispersed and arranged, and can be slowly released after being applied to soil to absorb water and expand, the pH value reaches the highest value after 4 hours, the slow release performance of the passivation material for releasing hydroxyl ions is improved, the ecological toxicity of the passivation material after being applied to the soil is reduced, the pH value is prevented from being rapidly increased to kill organisms in the environment, so that acute ecological toxicity is avoided, and the passivation effect of the passivation material on cadmium is not influenced after the passivation material is modified.
Drawings
FIG. 1 is a schematic flow chart of the steps of the preparation method of the present invention;
FIG. 2 is a graph of the dynamic effect on pH of calcium bentonite and calcium hydroxide 3:1 powder and large particulate material of example 1;
FIG. 3 is a graph showing the effect of passivating cadmium with calcium bentonite and calcium hydroxide 3:1 powder and large particulate material of example 1;
FIG. 4 is a graph of the dynamic effect on pH of calcium bentonite and calcium hydroxide 2:1 powder and large particulate material of example 2;
FIG. 5 is a graph of the effect of calcium bentonite and calcium hydroxide 2:1 powder and large particulate material on cadmium passivation in example 2;
FIG. 6 is a graph of the dynamic effect on pH of calcium bentonite and calcium hydroxide 1:1 powder and large particulate material of example 3;
FIG. 7 is a graph showing the effect of passivating cadmium with calcium bentonite and calcium hydroxide 1:1 powder and large particulate material of example 3;
FIG. 8 is a comparison graph of the passivation performance of particles and powder materials on cadmium under different proportions of calcium bentonite and calcium hydroxide.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Cadmium passivation powder and particle comparison at mass ratio of 3:1
The preparation process comprises the following steps:
1. calcium bentonite: calcium hydroxide 3:1 powder: 37.5g of calcium bentonite powder and calcium hydroxide powder (Ca (OH)2Not less than 95 percent) of 12.5g are mixed evenly.
2. Calcium bentonite: calcium hydroxide 3:1 particles: as shown in FIG. 1, 37.5g of calcium bentonite powder and calcium hydroxide powder (Ca (OH)2And 95 percent or more) 12.5g of the mixture is put into a centrifuge tube, 25mL of water is added into the centrifuge tube, the centrifuge tube is placed into a shaker to be shaken until the mixture is fully mixed, and the mixture is dried in an oven with the heating temperature of 70 ℃ until the humidity is about 20 percent. Placing the viscous material in an injector with a cylinder diameter of 2cm and a small hole diameter of 5mm, extruding to obtain a strip-shaped material, drying in an oven with a heating temperature of 300 ℃ to constant weight, cutting the dried material into a cylindrical large-particle material with a height of 5mm and a cross section diameter of 5 mm.
The application process comprises the following steps:
1. preparing materials: respectively weighing 0.2g of each of the two materials, and adding Cd with the volume of 500mL and the concentration of 50mg/L2+Adsorption experiments were performed in solution.
2. An adsorption process: first preparing Cd2+Adjusting the pH value of the solution to 4.5 by using 1mol/L hydrochloric acid or sodium hydroxide, adding large particles and powdery cadmium passivation materials into different beakers before stirring to serve as experimental groups, and setting a blank control group. Magnetic stirring is used in the adsorption process to ensure that the solid-liquid system is uniformly mixed, and the temperature of the system is kept at 20 +/-1 ℃.
3. Sampling: in order to capture the ion concentration change condition in the adsorption process in detail, the sampling frequency of the experiment is designed as follows: the samples were taken every 2min for the first 10min (5 samples), every 5min for the middle 50min (10 samples), every 10min for the last 60min (6 samples), and every 30min for the last 120min (4 samples). The sampling volume is about 5mL, and after sampling, the sample is immediately filtered by a water-based pinhole filter and diluted to a certain volume, and the acidity is kept at 1%.
4. The testing process comprises the following steps: the pH of the solution is tested before each sampling, and the Cd concentration of the sample is tested by ICP-OES
The results of the pH measurements are shown in FIG. 2, and the Cd concentration of the sample is shown in FIG. 3. Test results show that after calcium bentonite, namely large calcium hydroxide particles with the ratio of 3:1, and calcium bentonite, namely 3:1 powder are added, the pH values of the two-system aqueous solution are close to the maximum values in about 30 minutes and 60 minutes respectively; after 4 hours, the passivation efficiency of calcium bentonite and calcium hydroxide powder to cadmium is 22.4% and 99.8%, respectively.
Example 2
Cadmium passivation powder and particle comparison at mass ratio of 2:1
The preparation process comprises the following steps:
1. calcium bentonite: calcium hydroxide 2:1 powder: 33.3g of calcium bentonite powder and calcium hydroxide powder (Ca (OH)2Not less than 95 percent) of 16.7g are mixed evenly.
2. Calcium bentonite: calcium hydroxide 2:1 particles: 33.3g of calcium bentonite powder and calcium hydroxide powder (Ca (OH)295% or more) of the total weight of the mixture, 16.7g of the mixture was put into a centrifuge tube, 25mL of water was added into the centrifuge tube, the centrifuge tube was placed into a shaker, the mixture was shaken until the mixture was mixed well, and the subsequent preparation process was the same as that of example 1.
The application process comprises the following steps: the same as in example 1. The results of the pH measurements are shown in FIG. 4, and the Cd concentration of the sample is shown in FIG. 5. Test results show that after calcium bentonite, namely calcium hydroxide with large particles of 2:1, and calcium bentonite, namely calcium hydroxide with powder of 2:1, are added, the pH values of the two system aqueous solutions are close to the highest value in about 30 minutes; after 4 hours, the passivation efficiency of calcium bentonite and calcium hydroxide powder to cadmium is 41.7 percent and 80.6 percent respectively.
Example 3
Cadmium passivation powder and particle comparison at mass ratio of 1:1
The preparation process comprises the following steps:
1. calcium bentonite: calcium hydroxide 1:1 powder: weighing 25g of calcium bentonite and calcium hydroxide powder (Ca (OH)2, more than or equal to 95 percent) and uniformly mixing.
2. Calcium bentonite: calcium hydroxide 1:1 particles: 25g of each of the calcium bentonite and the calcium hydroxide powder (Ca (OH)2, more than or equal to 95 percent) is weighed into a centrifuge tube, 25mL of water is added into the centrifuge tube, the centrifuge tube is placed into a vibrator to be vibrated until the calcium bentonite and the calcium hydroxide powder are fully and uniformly mixed, and the subsequent preparation process is the same as that of example 1.
The application process comprises the following steps: the same as in example 1. The results of the pH measurements are shown in FIG. 6, and the Cd concentration of the sample is shown in FIG. 7. Test results show that the pH value of the aqueous solution can be close to the maximum value within 30 minutes after calcium bentonite and calcium hydroxide powder are added, and the pH value of the aqueous solution can reach the maximum value after 4 hours after calcium bentonite and calcium hydroxide powder with the ratio of 1:1 are added; after 4 hours, the passivation efficiency of calcium bentonite and calcium hydroxide powder to cadmium is 92.3 percent and 99.9 percent respectively.
The verification of the examples shows that:
the addition of the normal powdered material reaches the maximum pH faster than the addition of a solution of large particle cadmium passivation material. After adding the powdery calcium bentonite and the calcium hydroxide 1:1 material, the pH value of the solution reaches the highest value within 60 minutes, and the addition of the granular calcium bentonite: after the calcium hydroxide material is prepared into a 1:1 ratio, the pH value of an aqueous solution reaches the highest value after 4 hours, which shows that the release rate of hydroxide ions of the large-particle cadmium passivation material is slower, and acute ecological toxicity cannot be caused.
The granular cadmium passivating material slowly reduces the concentration of cadmium in the solution, while the powdered material rapidly reduces the concentration of cadmium in the solution. By comparing the passivating performances of the granular and powder materials on cadmium under different proportions of the calcium bentonite and the calcium hydroxide, as shown in fig. 8, after 4 hours, the passivating efficiency of the mixture (1:1, 2:1, 3:1) of the powdery calcium bentonite and the calcium hydroxide on cadmium can reach 81% -100%, and the granular calcium bentonite has the following characteristics: the passivation efficiency of calcium hydroxide 3:1 is only 22%, and the granular calcium bentonite: the passivation efficiency of calcium hydroxide 2:1 is only 42%, and the granular calcium bentonite: the passivation efficiency of calcium hydroxide 1:1 can reach 92 percent, which shows that the granular calcium bentonite has the following characteristics: the calcium hydroxide 1:1 passivation material has cadmium passivation capability similar to that of the powder material.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (9)
1. The large-particle cadmium passivation material with calcium bentonite as a substrate is characterized by comprising raw materials of calcium bentonite powder and calcium hydroxide powder, wherein the mass ratio of the calcium bentonite to the calcium hydroxide is 1:1, and the cadmium passivation material is a cylindrical particle material.
2. The calcium bentonite-based large-particle cadmium passivation material as claimed in claim 1, wherein: the height of the cadmium passivation material is 4-6mm, and the diameter of the cross section of the cadmium passivation material is 4-6 mm.
3. A method for preparing a large-particle cadmium passivation material based on calcium bentonite according to claim 1 or 2, which is characterized in that: the method comprises the following steps:
s1, putting the calcium bentonite and the calcium hydroxide powder into a reaction container according to a proportion, adding water with the same mass, keeping the humidity of the mixture at 100%, and stirring under oscillation at room temperature to fully and uniformly mix the materials;
s2, baking the product obtained in the step S1 in an oven, and then putting the baked product in a pressurizer to obtain a cylindrical passivation material;
and S3, drying the cylindrical passivation material and cutting the cylindrical passivation material into the granular passivation material.
4. The preparation method of the large-particle cadmium passivation material taking calcium bentonite as the substrate according to claim 3, characterized in that: the particle size of the calcium bentonite powder is 1-10 mu m; the particle size of the calcium hydroxide powder is 5-15 mu m.
5. The preparation method of the large-particle cadmium passivation material taking calcium bentonite as the substrate according to claim 4, characterized in that: the particle size of the calcium bentonite powder is 5 mu m; the particle size of the calcium hydroxide powder is 10 mu m.
6. The preparation method of the large-particle cadmium passivation material taking calcium bentonite as the substrate according to claim 3, characterized in that: in the step S1, the oscillation time is 2-3h, and the stirring speed is 170-210 rpm.
7. The preparation method of the large-particle cadmium passivation material taking calcium bentonite as the substrate according to claim 3, characterized in that: and in the step S2, the baking temperature is 65-75 ℃, and the baking is stopped when the humidity in the oven is 18% -23%.
8. The preparation method of the large-particle cadmium passivation material taking calcium bentonite as the substrate according to claim 3, characterized in that: the pressurizer is a piston pressurizing device, and the diameter of an outlet of the pressurizer is a circular outlet of 4-6 mm.
9. The preparation method of the large-particle cadmium passivation material taking calcium bentonite as the substrate according to claim 3, characterized in that: the drying temperature in the step S3 is 300-350 ℃.
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