CN111154491A - Preparation and application of heavy metal polluted acid soil remediation-improvement material - Google Patents
Preparation and application of heavy metal polluted acid soil remediation-improvement material Download PDFInfo
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- CN111154491A CN111154491A CN202010062038.7A CN202010062038A CN111154491A CN 111154491 A CN111154491 A CN 111154491A CN 202010062038 A CN202010062038 A CN 202010062038A CN 111154491 A CN111154491 A CN 111154491A
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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
- C09K17/06—Calcium compounds, e.g. lime
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Abstract
The invention discloses a preparation method and application of a heavy metal polluted acid soil remediation-improvement material, and belongs to the technical field of environmental science and engineering. According to the invention, calcium carbonate and the agricultural and forestry waste after hydrothermal treatment are mixed and subjected to high-temperature and anaerobic carbonization to form a calcium salt-porous biomass carbon compound, and the calcium salt-porous biomass carbon compound is applied to soil and has the functions of efficiently increasing the pH value of the soil and passivating the biologically effective heavy metals. After the compound is added into soil, the compound can slowly release calcium salt, continuously improve the pH value of the soil and provide calcium element; the porous biomass charcoal has a developed pore structure, and biologically effective heavy metals in soil are passivated under the action of pore filling and the like; the porous biomass charcoal improves the organic matter content and improves acid soil, and avoids potential negative effects such as soil hardening and element balance imbalance caused by calcium salt; the porous biomass charcoal is more stable than the traditional biomass charcoal, and can passivate heavy metals in soil and improve acid soil for a long time.
Description
Technical Field
The invention relates to the technical field of environmental science and engineering, in particular to a preparation method and application of a heavy metal polluted acid soil remediation-improvement material.
Background
Acid soil means pH of soil in the plough layer<6.6 the soil is mostly distributed in tropical and subtropical areas with high temperature, rainy and hot-humid seasons, and the formation reasons are mainly the rapid mineralization of soil organic matters and the high-strength leaching of salt-based ions such as potassium, calcium and the like. In addition, with the acceleration of global industrialization progress, a large amount of acid gases (sulfur dioxide, nitrogen oxides and the like) are continuously discharged into the atmosphere and settle into the soil to accelerate the soil acidification process. According to statistics, the acid soil accounts for about 50 percent of the culturable soil in the world, in China, the red soil is typical acid soil and is mainly distributed in Jiangxi province and Hunan province, and the covered farmland area is about 5690 kilohm2. Acid soil has the defects of low pH and low organic matter content, and seriously influences agricultural production, so that improvement is urgently needed to ensure high and stable yield of crops. The lime used for improving the acid soil is a conventional means for rapidly increasing the pH value of the acid soil, but the long-term or large-amount use of lime has been reported to cause the acid soil to be hardened, reduce the microbial activity and cause the element balance imbalance of the acid soil. In recent years, the biomass charcoal has attracted much attention for improving acid soil, and can improve the fertility of acid soil, improve the physical structure of acid soil, reduce the leaching of acid soil nutrients, enhance the microbial activity of acid soil and promote the nutrient circulation of acid soil, but the effect of the biomass charcoal in improving the pH value of acid soil is weaker.
In acid soil areas in the southeast of China, a large amount of mineral resources are distributed, and development of mines causes a large amount of heavy metals to flow out, so that acid farmland soil is seriously polluted. In addition, the acid soil has high effective state concentration of heavy metal and strong migration capacity due to low pH and low organic matter content, and seriously threatens the safe production of crops. Therefore, the remediation of the heavy metal pollution in the acid soil is imperative and urgent.
Through retrieval, related applications have been disclosed in the prior art, for example, the application with the chinese patent application number of 201510602213.6 and the publication date of 2018, 12 and 25 discloses a calcium-iron-silicon-based composite material for repairing heavy metal contaminated acidic soil and an application thereof, wherein the composite material comprises the following components in percentage by mass: calcium: iron: silicon: manganese: magnesium: phosphorus: 30-40% of aluminum: 19-25: 8-12: 1-3: 5-6: 1-3: 2-5; the paint specifically comprises the following components in percentage by volume: 55-70% of calcium silicate, 20-30% of calcium ferrite and 5-15% of a composite mixture, wherein the composite mixture is a mixture of calcium-iron-aluminum oxide, calcium-iron silicate, calcium aluminate, calcium-aluminum oxide, calcium-manganese-iron oxide, aluminum hydroxyphosphate and manganese hydroxyphosphate. The composite material is used for improving and repairing heavy metal polluted acid soil, the pH value of the soil can be increased by 0.5-2.5 units, and the content of effective heavy metal in the soil is reduced by 64-98%. However, the method of the application only adopts a plurality of substances for preparation, can only improve the polluted soil once, and cannot achieve the effect of slow release after long-term use, and the materials do not contain organic matters, so that the method is not beneficial to long-term application.
The application with the Chinese patent application number of 201410466726.4 and the granted announcement date of 2016.08.24 discloses a method for repairing modified biomass charcoal and heavy metal contaminated soil. The application of the modified biomass charcoal is prepared by the following steps: (1) after sieving the biomass charcoal, washing the biomass charcoal with water to remove floating dust and impurities on the surface of the biomass charcoal until the pH value of a washing liquid is 6.5-7.5; (2) mixing the obtained biomass charcoal with a phosphoric acid solution according to a mass ratio of 1: 1.5-2.5, uniformly mixing, and then soaking for more than 24 hours at normal temperature, wherein the mass percentage concentration of the phosphoric acid solution is 10-40%; (3) and carrying out solid-liquid separation on the soaking solution, and then drying the obtained solid material to obtain the modified biomass charcoal. The method of the application adopts phosphoric acid modified activated carbon at normal temperature to activate the activated carbon so as to more easily adsorb and fix heavy metal elements (such as Pb and Cd) in soil, but the preparation process is environment-friendly, complex and high in cost, and the specific surface area needs to be further optimized. In addition, the material reduces the pH of the soil, and cannot improve the acid soil polluted by heavy metals.
Therefore, based on the current situation of heavy metal pollution of acidic soil in China and the defects of the prior art, a simple, low-cost and efficient repairing-improving material is needed to be developed, the heavy metal repairing and the acidic soil improving are realized, the slow release effect can be achieved for a long time, and the safe, high and stable yield of crops in the acidic soil area in China is boosted.
Disclosure of Invention
1. Technical problem to be solved by the invention
Aiming at the problems of crop yield reduction and potential food safety caused by heavy metal polluted acid soil, the invention adopts agricultural and forestry wastes as basic raw materials, carries out hydrothermal treatment, designs the agricultural and forestry wastes after calcium carbonate high-temperature activation and carbonization hydrothermal treatment, skillfully combines the decomposition of calcium carbonate and the preparation of porous biomass charcoal together, successfully prepares a calcium salt-porous biomass charcoal composite material with high calcium salt content and developed pore structure, is applied to the heavy metal polluted acid soil, comprehensively improves the acid soil and passivates the heavy metal, and simultaneously efficiently realizes the restoration and improvement of the heavy metal polluted acid soil.
2. Technical scheme
In order to solve the technical problems, the technical scheme of the invention is as follows:
the invention provides a heavy metal contaminated acidic soil remediation-improvement material, which is prepared by uniformly mixing agricultural and forestry wastes subjected to hydrothermal carbonization with calcium carbonate to obtain a mixture, and then carbonizing the mixture at high temperature under the protection of inert gas. The agricultural and forestry waste can be soybean straw powder, but is not limited to the soybean straw powder.
As a further improvement of the invention, the preparation method of the heavy metal polluted acid soil restoration-improvement material comprises the following steps:
a) performing hydrothermal carbonization treatment on the agricultural and forestry waste, and uniformly mixing the treated agricultural and forestry waste with calcium carbonate to obtain a mixture;
b) and heating the mixture to 600-900 ℃ under the protection of inert gas, carbonizing the mixture for a certain time at the temperature of 600-900 ℃, and then cooling the carbonized mixture to room temperature to obtain the soil remediation-improvement material.
As a further improvement of the invention, in the step a), the solid-liquid ratio is controlled to be 100-500 g/L during hydrothermal carbonization, the hydrothermal carbonization temperature is 150-300 ℃, and the hydrothermal time is 1-12 h.
As a further improvement of the invention, the mixing ratio of the calcium carbonate and the agricultural and forestry waste in the step a) is as follows: the mass ratio (0.1-6): 1.
as a further improvement of the invention, the temperature rise rate during carbonization in the step b) is 1-10 ℃/min.
As a further improvement of the invention, in the step b), the carbonization time is 0.5-5 h.
As a further improvement of the invention, the flow rate of inert gas is kept to be 50-500 mL/min in the carbonization process, and the inert gas is nitrogen.
As a further improvement of the invention, the heavy metal polluted acid soil remediation-improvement material is simultaneously used for reducing the content of bioavailable heavy metals in soil and increasing the pH of the soil.
As a further improvement of the invention, the heavy metal polluted acid soil restoration-improvement material is uniformly applied to the surface layer of the soil; and (5) carrying out rotary tillage on the plough layer soil, and adding water to 60% of the maximum water holding capacity in the field.
3. Advantageous effects
Compared with the prior art, the technical scheme provided by the invention has the following remarkable effects:
(1) the heavy metal polluted acid soil restoration-improvement material adopts a mode of co-carbonizing calcium carbonate and agricultural and forestry waste hydrothermal carbon, and is a high-performance material which is low in cost, simple and convenient to prepare and has the functions of efficiently improving acid soil and restoring heavy metal polluted soil.
(2) According to the heavy metal polluted acid soil restoration-improvement material, a mode of co-carbonizing calcium carbonate and agricultural and forestry waste hydrothermal carbon is adopted, and in the carbonization process, the calcium carbonate plays a role in activating the hydrothermal carbon, so that on one hand, the hydrothermal carbon can be promoted to be converted into biomass carbon with a high pore structure, and the heavy metal in the soil can be efficiently fixed; on the other hand, calcium carbonate is decomposed to form calcium salt, which can rapidly increase the pH value of acid soil and provide calcium element. In addition, the biomass charcoal can also improve acid soil and relieve negative effects such as soil hardening and element balance imbalance caused by lime application, and make up for the deficiency of improving acid soil by lime.
(3) According to the heavy metal polluted acid soil restoration-improvement material, a calcium salt and porous biomass carbon complex can be formed by adopting a mode of co-carbonization of calcium carbonate and agricultural and forestry waste hydrothermal carbon, wherein the calcium salt is distributed on a porous biomass carbon carrier, so that the calcium salt can be uniformly dispersed in heavy metal polluted acid soil on one hand, and the calcium salt and the porous biomass carbon can play a role in restoring and improving heavy metal polluted acid soil on the other hand.
(4) According to the heavy metal polluted acid soil restoration-improvement material, a mode of co-carbonizing calcium carbonate and agricultural and forestry waste hydrothermal carbon is adopted, after carbonization, calcium salt is inlaid on a biomass carbon carrier with a developed pore structure, a slow release effect can be achieved, on one hand, an effect of continuously improving acid soil can be achieved, on the other hand, a buffering effect can be achieved, and adverse effects of one-time addition of the calcium salt on soil organisms are reduced.
(5) According to the heavy metal polluted acid soil restoration-improvement material, a mode of co-carbonizing calcium carbonate and agricultural and forestry waste hydrothermal carbon is adopted, and after the calcium carbonate is activated and carbonized, the biomass carbon not only has a developed pore structure, but also is more stable and difficult to decompose compared with the traditional biomass carbon, so that the action time of passivating the biological effective heavy metals in the soil and improving the acid soil is longer.
(6) According to the heavy metal contaminated acid soil remediation-improvement material, a mode of co-carbonizing calcium carbonate and agricultural and forestry waste hydrothermal carbon is adopted, carbon elements and oxygen elements in the calcium carbonate can be removed through high-temperature carbonization, and release of carbon dioxide after the material is applied to heavy metal contaminated acid soil is reduced.
Drawings
FIG. 1 is an X-ray diffraction pattern of the calcium salt-porous biomass charcoal composite in example 1;
FIG. 2 is a graph comparing nitrogen adsorption-desorption isotherms of the calcium salt-porous biomass charcoal composite and the pickled composite in example 1;
FIG. 3 is a graph showing the change in pH after the calcium salt-porous biomass charcoal complex of example 1 is added to acidic soil contaminated with model heavy metals;
fig. 4 is a graph showing the content of bioavailable state of heavy metal in the calcium salt-porous biomass charcoal composite added to acidic soil contaminated by model heavy metal in example 1.
Detailed Description
Example 1
The embodiment provides a preparation method of a calcium salt-porous biomass charcoal composite material, which comprises the following steps:
1) weighing a certain mass of soybean straw powder in a beaker, adding water until the solid-to-liquid ratio is 320g/L, putting the soybean straw powder in a hydrothermal reaction kettle, heating the soybean straw powder for 4 hours at 220 ℃, cooling the soybean straw powder, taking the soybean straw powder out, and drying the soybean straw powder in an oven at 70 ℃ to obtain the soybean straw hydrothermal carbon.
2) And (2) uniformly mixing 6g of soybean straw hydrothermal carbon with 12g of calcium carbonate powder (the mass ratio of the calcium carbonate to the agricultural and forestry waste is 2: 1) placing the mixture in a corundum crucible, heating to 800 ℃ at the speed of 5 ℃/min, keeping the temperature for 1h, and then cooling to room temperature, wherein the nitrogen flow in the whole process is 200mL/min, and black residues are the calcium salt-porous biomass carbon composite material.
Fig. 1 is an X-ray diffraction pattern of the calcium salt-porous biomass charcoal composite, which shows successful loading of calcium salt on porous biomass charcoal.
Setting a comparison group: the comparison group is a material for removing the calcium salt by acid cleaning, the material prepared by the invention and the material for removing the calcium salt after acid cleaning are respectively subjected to nitrogen adsorption-desorption experiments, the comparison graph of the nitrogen adsorption-desorption isotherms of the material and the material is shown in figure 2, and the comparison result shows that the porous biomass carbon surface is loaded by the invention even if the porous biomass carbon surface is loadedCalcium salt, but specific surface area (BET specific surface area 58.74 m)2The/g) is still larger than that of the common biomass carbon, and the heavy metal in the soil can be passivated efficiently. After removing calcium salt by hydrochloric acid pickling, the porous biomass charcoal has a highly developed pore structure (BET specific surface area of 798.58 m)2Per g, pore volume of 0.41cm3In terms of/g, the mean pore diameter is 2.03 nm). After acid washing, the specific surface area is increased sharply, and the calcium salt is supported in the pores of the porous biomass charcoal successfully.
The results show that the calcium salt is successfully loaded in the pore structure of the porous biomass carbon, can realize the slow release effect, improves the acid soil for a long time, and has longer improvement effect than the improvement effect of directly applying the calcium salt. On the other hand, compared with biomass charcoal produced by directly pyrolyzing biomass, the porous biomass charcoal has a developed pore structure, and shows that the capacity of passivating the bioavailable heavy metals of the porous biomass charcoal is gradually enhanced along with the gradual release of calcium salt. In addition, the porous biomass charcoal can increase soil organic matters and the like, and relieve the soil acidification process. Therefore, the material of the invention can efficiently repair and improve the acid soil polluted by heavy metal for a long time.
Example 2
The embodiment provides a preparation method of a calcium salt-porous biomass charcoal composite material, which comprises the following steps:
1) weighing a certain mass of soybean straw powder in a beaker, adding water until the solid-to-liquid ratio is 100g/L, putting the soybean straw powder in a hydrothermal reaction kettle, heating the soybean straw powder for 12 hours at 150 ℃, cooling the soybean straw powder, taking the soybean straw powder out, and drying the soybean straw powder in an oven at 70 ℃ to obtain the soybean straw hydrothermal carbon.
2) And (2) uniformly mixing 6g of soybean straw hydrothermal carbon with 0.6g of calcium carbonate powder (the mass ratio of the calcium carbonate to the agricultural and forestry waste is 0.1: 1) and placing the mixture in a corundum crucible, heating to 600 ℃ at the speed of 1 ℃/min, keeping for 5 hours, and then cooling to room temperature, wherein the nitrogen flow in the whole process is 500mL/min, and black residues are the calcium salt-porous biomass carbon composite material.
Example 3
The embodiment provides a preparation method of a calcium salt-porous biomass charcoal composite material, which comprises the following steps:
1) weighing a certain mass of soybean straw powder in a beaker, adding water until the solid-to-liquid ratio is 500g/L, putting the soybean straw powder in a hydrothermal reaction kettle, heating the soybean straw powder for 1h at 300 ℃, cooling the soybean straw powder, taking the soybean straw powder out, and drying the soybean straw powder in an oven at 7 ℃ to obtain the soybean straw hydrothermal carbon.
2) And (2) uniformly mixing 6g of soybean straw hydrothermal carbon with 36g of calcium carbonate powder (the mass ratio of the calcium carbonate to the agricultural and forestry waste is 6: 1) placing the mixture in a corundum crucible, heating to 900 ℃ at the speed of 10 ℃/min, keeping the temperature for 0.5h, and then cooling to room temperature, wherein the nitrogen flow in the whole process is 50mL/min, and black residues are the calcium salt-porous biomass charcoal composite material.
Example 4
This example is an application experiment of applying the material prepared in example 1 to soil, and the specific steps are as follows:
weighing 1g of the calcium salt-porous biomass charcoal composite material prepared in example 1 and 10g of acid soil polluted by heavy metal (collected from Guixi heavy metal polluted red soil in Jiangxi), uniformly stirring, adding deionized water to 60% of field water capacity, culturing for 30d, measuring pH of soil and biological effective state content of heavy metal, and measuring biological effective state content of heavy metal by adopting CaCl2Solution extraction method.
Meanwhile, a blank control group is set, and the specific steps are as follows: weighing 11g of heavy metal contaminated acidic soil (collected from heavy metal contaminated red soil of Guixi river in Jiangxi), stirring uniformly, adding deionized water to 60% of field water capacity, culturing for 30d, and measuring soil pH and heavy metal biological available state content (CaCl)2Solution extraction method).
FIG. 3 is a graph showing the change in pH after calcium salt-porous biomass charcoal complex is added to acidic soil contaminated with model heavy metals; as can be seen from fig. 3, the soil pH increased significantly from 5.00 to 8.23.
FIG. 4 is a graph showing the change of the content of the bioavailable state of the heavy metal after the calcium salt-porous biomass charcoal composite is added into the acidic soil polluted by the model heavy metal.
CaCl2The content results of the bioavailable heavy metals measured by a solution extraction method show that the bioavailable heavy metals in the soil are obviously reduced in effective content of Cu, Zn, Cd and Pb and reduced in rate after the calcium salt-porous biomass charcoal composite material prepared in example 1 is addedRespectively, the following steps: 99.71%, 99.92%, 99.30% and 99.98%.
Fig. 3 and 4 show that the calcium salt-porous biomass charcoal composite material has the functions of efficiently improving acid soil and repairing heavy metal contaminated soil.
The invention has been described in detail hereinabove with reference to specific exemplary embodiments thereof. It will, however, be understood that various modifications and changes may be made without departing from the scope of the invention as defined in the appended claims. The detailed description and drawings are to be regarded as illustrative rather than restrictive, and any such modifications and variations are intended to be included within the scope of the present invention as described herein. Furthermore, the background is intended to be illustrative of the state of the art as developed and the meaning of the present technology and is not intended to limit the scope of the invention or the application and field of application of the invention.
Claims (9)
1. The heavy metal contaminated acid soil restoration-improvement material is characterized by comprising the following components in parts by weight: the material is obtained by uniformly mixing the agricultural and forestry wastes subjected to hydrothermal carbonization treatment with calcium carbonate to obtain a mixture, and then carbonizing the mixture at a high temperature under the protection of inert gas.
2. The method for preparing a heavy metal contaminated acidic soil remediation-improving material as claimed in claim 1, wherein: the method comprises the following steps:
a) performing hydrothermal carbonization treatment on the agricultural and forestry waste, and uniformly mixing the treated agricultural and forestry waste with calcium carbonate to obtain a mixture;
b) and heating the mixture to 600-900 ℃ under the protection of inert gas, carbonizing the mixture for a certain time at the temperature of 600-900 ℃, and then cooling the carbonized mixture to room temperature to obtain the soil remediation-improvement material.
3. The method for preparing a heavy metal contaminated acidic soil remediation-improving material according to claim 2, wherein: and b) controlling the solid-liquid ratio to be 100-500 g/L during hydrothermal carbonization in the step a), controlling the hydrothermal carbonization temperature to be 150-300 ℃ and controlling the hydrothermal time to be 1-12 h.
4. The method for preparing a heavy metal contaminated acidic soil remediation-improving material according to claim 2, wherein: the mixing proportion of the calcium carbonate and the agricultural and forestry waste in the step a) is as follows: the mass ratio (0.1-6): 1.
5. the method for preparing a heavy metal contaminated acidic soil remediation-improving material according to claim 2, wherein: and the temperature rise rate during carbonization in the step b) is 1-10 ℃/min.
6. The method for preparing a heavy metal contaminated acidic soil remediation-improving material according to claim 2, wherein: in the step b), the carbonization time is 0.5-5 h.
7. The method for preparing a heavy metal contaminated acidic soil remediation-improving material according to claim 6, wherein: and in the carbonization process, the flow of inert gas is kept at 50-500 mL/min, and the inert gas is nitrogen.
8. The application of the heavy metal polluted acid soil restoration-improvement material is characterized in that: the heavy metal contaminated acidic soil remediation-modifying material of claim 1 for use in both reducing the content of biologically available heavy metals in soil and increasing the pH of soil.
9. The use of the heavy metal contaminated acidic soil remediation-improving material of claim 8, wherein: uniformly applying the heavy metal polluted acid soil restoration-improvement material to the surface layer of the soil; and (5) carrying out rotary tillage on the plough layer soil, and adding water to 60% of the maximum water holding capacity in the field.
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