CN110699084B - Soil heavy metal pollution curing and repairing composite reagent and curing and repairing method - Google Patents
Soil heavy metal pollution curing and repairing composite reagent and curing and repairing method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K17/06—Calcium compounds, e.g. lime
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明公开一种土壤重金属污染固化修复复合药剂及固化修复方法。按质量含量计，该复合药剂包括以下组分：生石灰20％‑40％，铁基生物炭改性磷酸盐矿物60％‑80％；其中，铁基生物炭改性磷酸盐矿物为铁盐与生物质混合均匀并干燥后，与磷酸盐矿物混合均匀、共热解得到。利用该复合药剂对重金属污染土壤进行固化修复的方法为：先将铁基生物炭改性磷酸基矿物与生石灰混合均匀，得到土壤重金属污染固化修复复合药剂；然后将复合药剂加入重金属污染土壤中，加入水，搅拌均匀；最好标准养护，完成对重金属污染土壤的固化修复。本发明的土壤重金属污染固化修复复合药剂能够有效地避免重金属的二次溶出，极大增强了重金属污染土壤固化的长期稳定性。The invention discloses a composite agent for solidifying and repairing soil heavy metal pollution and a solidifying and repairing method. In terms of mass content, the compound agent includes the following components: 20%-40% of quicklime, 60%-80% of iron-based biochar-modified phosphate minerals; wherein, the iron-based biochar-modified phosphate minerals are iron salt and After the biomass is uniformly mixed and dried, it is uniformly mixed with phosphate minerals and co-pyrolyzed. The method for solidifying and remediating heavy metal contaminated soil by using the composite agent is as follows: firstly, the iron-based biochar-modified phosphate-based minerals and quicklime are mixed uniformly to obtain a composite agent for soil heavy metal pollution solidification and repair; then the composite agent is added to the heavy metal-contaminated soil, Add water and stir evenly; it is best to maintain it in a standard way to complete the solidification and restoration of heavy metal contaminated soil. The soil heavy metal pollution solidification and repair composite agent of the invention can effectively avoid the secondary dissolution of heavy metals, and greatly enhances the long-term stability of heavy metal pollution soil solidification.
Description
Technical Field
The invention relates to a soil heavy metal pollution curing and repairing composite reagent and a method for curing and repairing heavy metal polluted soil by using the same, and belongs to the technical field of soil repairing and treatment.
Background
Soil is an important component of the ecological environment and is also a major natural resource on which humans live. In the rapid industrialization process of China, because the environment management mode is not perfect and the pollution control system is not strict, a large amount of heavy metal pollutants are discharged into soil in long-term industrial production activities, such as electroplating, smelting and other industries, so that the large-area soil of China is suffering from a serious pollution problem; soil pollution has concealment and hysteresis, and reasonable and effective measures must be taken to reduce environmental risks brought by pollutants. The research on repairing typical industrial heavy metal polluted sites is urgently developed by combining the characteristics of high heavy metal content and coexistence of various pollutants in industrial polluted sites in China.
For heavy metal pollution of soil, common remediation techniques include: physical repair techniques, chemical repair techniques, biological repair techniques, combined repair techniques, and the like. In a plurality of restoration technologies, physical restoration such as thermal desorption, soil replacement, electric restoration and the like damages the soil structure, so that the engineering quantity is large, and the cost is high; the bioremediation repair cycle is long and has high requirements on the soil environment. The fixation/stabilization repair technology in chemical repair is receiving wide attention due to its short time and good stability. The solidification stabilization technology (S/S technology for short) is a technology for forming a solidified body with low permeability coefficient or converting pollutants into stable forms by forcibly mixing a curing agent and polluted soil and utilizing the physical and chemical actions of the curing agent so as to reduce the migration and solubility of the pollutants. Compared with other restoration technologies (such as chemical leaching and biological restoration), the method has the unique advantages of low restoration cost, convenient construction, high intensity of the processed soil and strong stability, and is particularly suitable for restoring heavy metal polluted sites.
Aiming at the in-situ chemical immobilization repair technology, the key point is to select a proper fixative. In industrial sites, traditional curing agents are based on inorganic materials (about 94%), with high-alkali cement (39%) and lime (8%) being the most common. However, the solidified body after cement treatment has more pores, so that heavy metals in the solidified body are easy to desorb, and the soil after cement and lime solidification has high alkalinity, which is not beneficial to long-term stability of heavy metal sealing.
Moreover, in the remediation of a composite polluted site polluted by heavy metals and organic matters, when chemical oxidation is adopted for treatment, the addition of hydrogen peroxide usually destroys the original balance environment of soil, improves the oxidation-reduction potential, releases the heavy metals existing in an organic combination state, and destroys the metal form distribution structure; simultaneously, the structure of the solidified material is damaged, so that the heavy metal is secondarily dissolved out; not beneficial to the long-term solidification of heavy metals.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problem that the heavy metal contaminated soil repaired by the existing curing agent cannot be stably cured for a long time, the invention provides a composite agent for curing and repairing heavy metal contaminated soil, which can effectively enhance the long-term stability of curing of the heavy metal contaminated soil; the invention also provides a method for curing and repairing the heavy metal contaminated soil by using the composite reagent.
The technical scheme is as follows: the invention relates to a soil heavy metal pollution curing and repairing composite reagent, which comprises the following components in percentage by mass: 20-40% of quicklime and 60-80% of iron-based biochar modified phosphate mineral; the iron-based biochar modified phosphate mineral is obtained by uniformly mixing iron salt and biomass, drying, uniformly mixing the dried iron salt and the biomass with phosphate mineral, and performing co-pyrolysis.
Specifically, the iron-based biochar modified phosphate mineral can be prepared according to the following steps:
A. cleaning, drying, grinding and sieving biomass, placing the biomass in a beaker, adding iron salt and water, uniformly mixing, and drying for later use;
B. grinding and sieving the dried iron-based biomass, and mechanically mixing the iron-based biomass with phosphate minerals for 2-4 hours; and placing the obtained mixture in a tubular furnace, and roasting for 30-180 min at 600-900 ℃ in a carrier gas environment.
In the step A, the mass ratio of the iron salt to the biomass is preferably 0.1-0.8: 1. In step B, the carrier gas atmosphere can be nitrogen, carbon dioxide or a mixed carrier gas of the nitrogen and the carbon dioxide.
In the iron-based biochar modified phosphate mineral, biomass can be selected from one of straw, rice hull and bamboo dust. The phosphate mineral material is selected from one of calcium dihydrogen phosphate, hydroxyapatite, and calcium superphosphate.
According to a preferable technical scheme, in the composite reagent, the mass ratio of the quicklime to the iron-based biochar modified phosphate mineral is preferably 0.25-0.5: 1.
The method for curing and repairing the heavy metal contaminated soil by using the composite medicament comprises the following steps:
(1) uniformly mixing the iron-based biochar modified phosphate mineral and quicklime to obtain a soil heavy metal pollution curing and repairing composite reagent;
(2) adding the composite medicament into heavy metal contaminated soil, adding water, and uniformly stirring;
(3) and (5) standard maintenance, namely finishing the solidification restoration of the heavy metal polluted soil.
In the step (1), the mass ratio of the quicklime to the iron-based biochar modified phosphate mineral is preferably 0.25-0.5: 1.
In the step (2), the adding amount of the composite reagent is 1-10% of the mass of the soil polluted by the heavy metal. Preferably 6 to 8%. Furthermore, after water is added, the water content of the heavy metal contaminated soil is 30-80%.
The invention principle is as follows: in the composite medicament, the biochar has a relatively large specific surface area, a high pH value and Cation Exchange Capacity (CEC), and rich functional groups (such as carboxyl, phenolic groups, hydroxyl, carbonyl, quinone substances and the like), has a strong adsorption effect on heavy metal ions in an environmental medium, and can change the oxidation-reduction potential of soil by improving the pH and organic matter content of the soil, so that the migration and homing of the heavy metal ions are influenced. After the phosphate material is added into the soil polluted by the heavy metal, the heavy metal is promoted to be converted from an exchangeable state and a carbonate combined state to a stable state, and the migration and the bioavailability of the heavy metal in the soil are reduced; the main reaction mechanism comprises: after the phosphate is dissolved, the phosphate and heavy metal ions generate precipitate; complexing and adsorbing the surface of phosphate; dissolving hydroxyapatite and then coprecipitating or exchanging ions on the surface of the phosphate ore. Furthermore, phosphate-based minerals have a smaller K than carbonates, sulfides, and the like by forming phosphate precipitates with heavy metal ionsspThe product has certain stability; the phosphate mineral is modified by adding the iron salt, which is beneficial to generating KspSmaller metal precipitates can effectively avoid secondary dissolution of heavy metals and enhance long-term stability.
In addition, in the remediation of the heavy metal and organic compound contaminated soil, because the iron-based biochar modified phosphate mineral is obtained by co-pyrolysis of phosphate and biochar, phosphate can promote the generation of metaphosphate and C-O-PO with stable heat in the biomass pyrolysis process3And C-PO3Functional groups and the likeThe functional groups can serve as physical barriers or block active sites of carbon so as to inhibit oxidative decomposition of the biochar, thereby effectively reducing the risk of secondary dissolution of heavy metal ions caused by change of soil environment and damage to the structure of a solidified body due to chemical oxidation and greatly increasing the long-term stability of the solidified body.
Has the advantages that: compared with the prior art, the invention has the advantages that: (1) the soil heavy metal pollution curing and repairing composite medicament can effectively avoid secondary dissolution of heavy metals, and greatly enhances the long-term stability of the heavy metal pollution soil curing; (2) the soil heavy metal pollution curing and repairing composite reagent disclosed by the invention is simple in component, easy in raw material obtaining, low in cost, free of heavy metal or low in content, and free of secondary pollution risk; (3) the soil remediation composite agent for soil heavy metal pollution curing and remediation is simple in process operation and suitable for popularization and application.
Detailed Description
The technical solution of the present invention is further explained below.
The invention relates to a soil heavy metal pollution curing and repairing composite medicament, which comprises the following components in percentage by mass: 20-40% of quicklime and 60-80% of iron-based biochar modified phosphate mineral; the iron-based biochar modified phosphate mineral is obtained by uniformly mixing iron salt and biomass, drying, uniformly mixing the dried iron salt and the biomass with phosphate mineral, and performing co-pyrolysis.
Example 1
The formula of the soil heavy metal pollution curing and repairing composite medicament comprises the following components:
20% of quicklime and 80% of iron-based biochar modified calcium superphosphate.
The preparation process of the iron-based biochar modified calcium superphosphate comprises the following steps:
cleaning, drying, grinding and screening biomass by a 2mm sieve, then placing the biomass in a beaker, adding iron salt and water according to the mass ratio of the iron salt to the biomass being 0.2:1, stirring for 2 hours, and drying for later use; grinding the dried iron-based biomass, sieving the ground iron-based biomass by a 2mm sieve, and mechanically mixing the ground iron-based biomass with calcium superphosphate for 2 hours; the obtained mixture is placed inIn a tube furnace, in N2+CO2Roasting at 600 deg.C for 60min under atmosphere.
And (3) uniformly dry-mixing the prepared iron-based biochar modified calcium superphosphate and quicklime according to the mass ratio of 4:1 to obtain the composite medicament.
Example 2
The formula of the soil heavy metal pollution curing and repairing composite medicament comprises the following components:
30% of quicklime and 70% of iron-based biochar modified calcium superphosphate.
The preparation process of the iron-based biochar modified calcium superphosphate comprises the following steps:
cleaning, drying, grinding and screening biomass by a 2mm sieve, then placing the biomass in a beaker, adding iron salt and water according to the mass ratio of the iron salt to the biomass being 0.5:1, stirring for 2 hours, and drying for later use; grinding the dried iron-based biomass, sieving the ground iron-based biomass by a 2mm sieve, and mechanically mixing the ground iron-based biomass with calcium superphosphate for 2 hours; the mixture obtained is placed in a tube furnace under N2+CO2Roasting at 800 deg.C for 60min under atmosphere.
And (3) uniformly dry-mixing the prepared iron-based biochar modified calcium superphosphate and quicklime according to the mass ratio of 7:3 to obtain the composite medicament.
Example 3
The formula of the soil heavy metal pollution curing and repairing composite medicament comprises the following components:
40% of quicklime and 60% of iron-based biochar modified calcium superphosphate.
The preparation process of the iron-based biochar modified calcium superphosphate comprises the following steps:
cleaning, drying, grinding and screening biomass by a 2mm sieve, then placing the biomass in a beaker, adding iron salt and water according to the mass ratio of the iron salt to the biomass being 0.8:1, stirring for 2 hours, and drying for later use; grinding the dried iron-based biomass, sieving the ground iron-based biomass by a 2mm sieve, and mechanically mixing the ground iron-based biomass with calcium superphosphate for 2 hours; the mixture obtained is placed in a tube furnace under N2+CO2Roasting at 900 deg.C for 120min under atmosphere.
And (3) uniformly dry-mixing the prepared iron-based biochar modified calcium superphosphate and quicklime according to the mass ratio of 3:2 to obtain the composite medicament.
Comparative example
The biochar modified calcium superphosphate composite medicament comprises the following components:
30% of quicklime and 70% of biochar modified calcium superphosphate.
The preparation method of the biochar modified calcium superphosphate comprises the following steps:
cleaning biomass, drying, grinding, sieving with 2mm sieve, placing into a beaker, mechanically mixing uniformly with the mass ratio of calcium superphosphate to biomass being 0.5:1, placing the obtained mixture into a tube furnace, and adding N2+CO2Roasting at 800 deg.C for 60min in carrier gas environment.
And (3) uniformly dry-mixing the prepared biochar modified calcium superphosphate and quicklime according to the mass ratio of 7:3 to obtain the biochar modified calcium superphosphate composite medicament.
EXAMPLE 4 testing of the adsorption and Oxidation resistance of pharmaceutical Agents in liquid phase System
Preparing a zinc ion solution with the concentration of 1000mg/L, accurately weighing 0.4g of calcium superphosphate + calcium oxide (mass ratio of 7:3), the biochar modified superphosphate composite medicament prepared in the comparative example 1 and the iron-based biochar modified superphosphate composite medicament prepared in the example 2 in 50ml of solution respectively under the conditions that the pH of the solution is controlled to be 5 and the temperature is 298K, and measuring the saturated adsorption capacity of the curing agent after shaking reaction for 24 hours.
Tests show that under the condition, the saturated adsorption capacity of the three curing agents after reaction is 125mg/g, and the three curing agents have strong adsorption capacity.
And (3) carrying out suction filtration and drying on solid residues in the solution, respectively weighing 0.1g, adding 10ml of 5% hydrogen peroxide solution, and after reacting for 24 hours, determining the solubility of zinc ions in the solution.
The secondary elution of heavy metals after addition of hydrogen peroxide was tested as in table 1 below.
TABLE 1 cured body antioxidant Capacity test results
Therefore, the oxidation resistance of the three curing agents for adsorbing heavy metals in a liquid phase is respectively that the iron-based biochar modified superphosphate composite medicament is larger than the superphosphate composite medicament.
Example 5 testing of the curing Properties and Oxidation resistance of Agents in actual soil systems
A shallow polluted soil sample of a place left after the removal of an electroplating workshop of a gas distribution factory in Jiangsu province is taken to carry out a solidification experiment, and the conductivity, the pH and the leaching toxicity of heavy metals of the soil sample to be treated are respectively evaluated by referring to an electrode method for measuring the soil conductivity (HJ802-2016), a standard method for testing the soil engineering (GB/T50123-1999) and a method for identifying the standard toxicity leaching of the hazardous wastes in the United states of America (USEPA 1311 TCLP).
The results of the conductivity, pH and heavy metal leaching toxicity evaluation tests of the soil sample to be tested are shown in the following table 2. As can be seen from Table 2, the leaching concentration value of Zn is 500.67mg/L, which is 5 times higher than the hazardous waste identification standard (GB 5085.3-2007) in the hazardous waste identification standard leaching toxicity identification.
TABLE 2 evaluation test results of conductivity, pH and heavy metal leaching toxicity of soil sample to be tested
| Cured body | Electrical conductivity of | pH | Leaching toxicity (mg/L) |
| Soil sample with zinc pollution | 4.58 | 3.22 | 500.67 |
Accurately weighing 1.6g of calcium superphosphate and calcium oxide (mass ratio is 7:3), the biochar modified superphosphate composite medicament prepared in the comparative example 1 and the iron-based biochar modified superphosphate composite medicament prepared in the example 2 in a mixing ratio of 8%, uniformly mixing the three curing agents in a plastic beaker filled with 20g of a polluted soil sample, adding 12ml of water, keeping the water content at 60%, placing the mixture in a standard curing chamber, and after curing for 28 days, measuring the conductivity, pH and leaching toxicity (mg/L) of a cured body.
After curing, the conductivity, pH and cure rate in the contaminated soil samples are shown in table 3 below.
TABLE 3 evaluation test results of conductivity, pH and heavy metal leaching toxicity of treated soil sample to be tested
1g of the treated soil sample and a plastic test tube after curing of the three curing agents are respectively taken, 10ml of hydrogen peroxide solution with the concentration of 5% is respectively added, after oscillation for 24 hours, centrifugal filtration is carried out, and the concentration of zinc ions in the filtrate is tested.
After the reaction is finished, the test result of the oxidation resistance of the soil sample to be tested is shown in the following table 4.
TABLE 4 test results of the antioxidant capacity of the soil sample to be tested
Therefore, the oxidation resistance of the three curing agents for curing heavy metals in soil is respectively that the iron-based biochar modified superphosphate composite agent is larger than the superphosphate composite agent.
Example 6 testing of the curing Capacity of pharmaceutical Agents in actual composite heavy Metal contaminated soil
A shallow layer polluted soil sample of a lead-copper tailing left field in Jiangxi province is taken to carry out a solidification experiment, and the conductivity, the pH and the heavy metal leaching toxicity of the soil sample to be treated are evaluated by referring to an electrode method for measuring soil conductivity (HJ802-2016), a soil engineering test method standard (GB/T50123-1999) and an American hazardous waste identification standard toxicity leaching method USEPA 1311TCLP method respectively.
The results of the conductivity, pH and heavy metal leaching toxicity evaluation tests of the soil sample to be tested are shown in the following table 5.
TABLE 5 evaluation test results of conductivity, pH and heavy metal leaching toxicity of soil sample to be tested
| Contaminated soil sample | Electrical conductivity of | pH | Lead leaching toxicity (mg/L) | Copper leaching toxicity (mg/L) |
| Lead-zinc-copper polluted soil | 6.09 | 2.80 | 6.36 | 8.75 |
Accurately weighing 1.2g of calcium superphosphate and calcium oxide (mass ratio is 7:3), the biochar modified superphosphate composite medicament prepared in comparative example 1 and the iron-based biochar modified superphosphate composite medicament prepared in example 2 in a 6% mixing ratio in a plastic beaker filled with 20g of a polluted soil sample, uniformly mixing, adding 12ml of water, keeping the water content at 60%, placing in a standard curing chamber, and after curing for 7 days, measuring the conductivity, pH and leaching toxicity (mg/L) of a cured body.
After curing, the conductivity, pH and cure rate in the contaminated soil samples are shown in Table 6 below.
TABLE 6 evaluation test results of conductivity, pH and heavy metal leaching toxicity of treated soil sample to be tested
In conclusion, the iron-based biochar modified phosphate mineral composite medicament can be used for curing heavy metal contaminated soil with different degrees and different types, effectively improves the pH value of the soil body, reduces the conductivity, reduces the leaching toxicity of the heavy metal in the soil and the risk of dissolving out of metal ions in the cured body due to chemical oxidation, greatly enhances the stability of long-term curing, and has good practical application prospect.
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