CN114535277B - Application of iron-containing steel slag combined with thermal desorption technology in repairing phthalate polluted soil and repairing method thereof - Google Patents
Application of iron-containing steel slag combined with thermal desorption technology in repairing phthalate polluted soil and repairing method thereof Download PDFInfo
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- CN114535277B CN114535277B CN202210218722.9A CN202210218722A CN114535277B CN 114535277 B CN114535277 B CN 114535277B CN 202210218722 A CN202210218722 A CN 202210218722A CN 114535277 B CN114535277 B CN 114535277B
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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
- B09C1/06—Reclamation of contaminated soil thermally
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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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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention belongs to the technical field of thermal desorption restoration of Phthalate (PAEs) polluted soil, and discloses application of an iron-containing steel slag combined thermal desorption technology in restoration of phthalate polluted soil and a restoration method thereof. The method mainly comprises three steps of soil pretreatment, soil modification and thermal desorption treatment for polluted soil. According to the invention, the iron-containing steel slag is added into the phthalate polluted soil for modification treatment, and the thermal desorption restoration is carried out in combination with an anaerobic environment, so that the phthalate removal efficiency is improved, the thermal desorption restoration cost is reduced, and the method has a good application prospect.
Description
Technical Field
The invention relates to the technical field of thermal desorption restoration of Phthalate (PAEs) polluted soil, in particular to application of iron-containing steel slag combined thermal desorption technology in restoration of phthalate polluted soil and a restoration method thereof.
Background
Phthalate esters (PAEs) are widely used as a class of plasticizers in the production and processing of polymers to enhance the flexibility of plastics and the like. PAEs mainly include di (2-ethylhexyl) phthalate (DEHP), dibutyl phthalate (DBP) and diisobutyl phthalate (DIBP). Among them DEHP is one of the most widely used plasticizers in PAEs. Because no chemical bond is formed between the PAEs and the polymer matrix, but the PAEs are combined by physical action, the PAEs can be directly or indirectly transferred to the surrounding environment and collected into soil during the manufacturing, using and discarding processes of plastic products. PAEs, an endocrine disruptor, have oxidative stress, metabolic disorders, immunosuppression, and carcinogenesis. PAEs continue to accumulate in the soil and pose potential risks to human health and ecosystems through food chain transfer. Therefore, the method has important practical significance for repairing PAEs polluted soil.
At present, the repair method for PAEs polluted soil mainly comprises the following steps: physical repair (leaching, extraction, solvent extraction, etc.), chemical repair (Fenton, fenton-like oxidation, etc.), biological repair (phytoremediation, microbial remediation, etc.). The off-site thermal desorption method is a common physical repair method, and the pollutants are separated from the soil in a direct or indirect heating mode under vacuum or by introducing carrier gas such as nitrogen. The ectopic thermal desorption has the advantages of wide application range, short treatment period and high removal efficiency, but the technology has low energy utilization rate and high temperature damage to soil, which affects the application range of thermal desorption. At present, by adding synergistic materials in the thermal desorption repair process to strengthen the thermal desorption effect, the reduction of the repair cost has become the development trend of the technology.
Iron-containing steel slag is a by-product of the steel production process, mainly arising from different dust removal and wastewater treatment processes, and Fe 2 O 3 The content is higher. The iron-containing steel slag has large production quantity but low utilization rate, and belongs to wastes in the iron and steel industry. Therefore, the development of iron-containing steel slag to synergistically treat pae contaminated soil is highly desirable in the art.
Disclosure of Invention
In view of the above, the invention provides an application of a combined thermal desorption technology of iron-containing steel slag in repairing phthalate polluted soil and a repairing method thereof, so as to solve the problems that the existing ectopic thermal desorption method is low in energy utilization rate and high in temperature damages soil when used for treating phthalate polluted soil, and solve the problems that the existing iron-containing steel slag is large in production amount but low in utilization rate.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides an application of a combined thermal desorption technology of iron-containing steel slag in repairing phthalate polluted soil.
The invention also provides a method for repairing phthalate polluted soil by combining the iron-containing steel slag with a thermal desorption technology, which comprises the following steps:
step S1: mixing the iron-containing steel slag with the pretreated phthalate polluted soil to obtain modified soil;
step S2: and carrying out thermal desorption treatment on the modified soil to obtain the restored soil.
Preferably, in the step S1, the preprocessing includes the following steps: and (3) crushing, grinding and screening the phthalate polluted soil in sequence, and adjusting the water content of the soil to obtain the pretreated phthalate polluted soil.
Preferably, the particle size of the pretreated phthalate polluted soil is more than or equal to 10 meshes, and the soil moisture content of the pretreated phthalate polluted soil is 2-10%.
Preferably, in the step S1, fe of the iron-containing steel slag 2 O 3 The content of the iron-containing steel slag is 20-80%, and the addition amount of the iron-containing steel slag is 1-2% of the mass of the pretreated phthalate polluted soil.
Preferably, in the step S1, the mixing is performed by stirring at a rotation speed of 30 to 50r/min.
Preferably, in the step S2, the thermal desorption treatment is performed under a protective gas atmosphere, and the flow rate of the protective gas is 200 to 400mL/min.
Preferably, in the step S2, the temperature of the thermal desorption treatment is 150 to 300 ℃, and the time of the thermal desorption treatment is 20 to 30 minutes.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the method, a certain amount of iron-containing steel slag is added into phthalate polluted soil to modify the polluted soil, so that the phthalate thermal desorption removal rate is improved, and compared with the method which only adopts an ectopic thermal desorption technology, the method can effectively reduce the thermal desorption temperature and reduce the energy input; meanwhile, the invention has the characteristics of high repair efficiency, small soil damage and the like;
(2) In the thermal desorption restoration process of the polluted soil, the iron-containing steel slag is used as a thermal desorption additive, and Fe contained in the iron-containing steel slag is used as a thermal desorption additive 2 O 3 The heat conductivity of the soil can be improved, and mass transfer and heat transfer of the soil are promoted, so that the thermal desorption and removal of phthalate are accelerated, and the repair period is shortened. In addition, compared with the method adopting the ectopic thermal desorption technology, the method can achieve the same repairing effect at a lower thermal desorption temperature after adding the iron-containing steel slag, and reduces the repairing cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only embodiments of the present invention, and that other drawings can be obtained according to the provided drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for restoring phthalate polluted soil by combining iron-containing steel slag with a thermal desorption technology;
FIG. 2 is a graph showing the effect of iron-containing steel slag addition change on the removal efficiency of di (2-ethylhexyl) phthalate when the thermal desorption treatment time is 20min in the method for restoring phthalate contaminated soil by using the iron-containing steel slag combined thermal desorption technology;
FIG. 3 is a graph showing the effect of the change of thermal desorption treatment time on the removal efficiency of di (2-ethylhexyl) phthalate when 1% of iron-containing steel slag is added in the method for restoring phthalate contaminated soil by combining the iron-containing steel slag with the thermal desorption technology.
Detailed Description
The invention provides an application of a combined thermal desorption technology of iron-containing steel slag in repairing phthalate polluted soil.
The invention also provides a method for repairing phthalate polluted soil by combining the iron-containing steel slag with a thermal desorption technology, which comprises the following steps:
step S1: mixing the iron-containing steel slag with the pretreated phthalate polluted soil to obtain modified soil;
step S2: and carrying out thermal desorption treatment on the modified soil to obtain the restored soil.
In the present invention, in the step S1, the preprocessing includes the steps of: and (3) crushing, grinding and screening the phthalate polluted soil in sequence, and adjusting the water content of the soil to obtain the pretreated phthalate polluted soil.
In the present invention, the particle size of the pretreated phthalate contaminated soil is preferably not less than 10 mesh, more preferably not less than 16 mesh.
In the present invention, the soil moisture content of the pretreated phthalate contaminated soil is preferably 2 to 10%, more preferably 5 to 8%.
In the present invention, in the step S1, fe of the iron-containing steel slag 2 O 3 The content is preferably 20 to 80%, more preferably 30 to 50%; the addition amount of the iron-containing steel slag is preferably 1 to 2% by mass of the pretreated phthalate contaminated soil, and more preferably 1 to 1.5% by mass of the pretreated phthalate contaminated soil.
In the present invention, in the step S1, the mixing is performed by stirring, and the rotation speed of stirring is preferably 30 to 50r/min, more preferably 35 to 40r/min.
In the present invention, in the step S2, the thermal desorption treatment is performed under a protective gas atmosphere, and the flow rate of the protective gas is preferably 200 to 400mL/min, and more preferably 250 to 300mL/min;
in the present invention, the shielding gas is preferably nitrogen or hydrogen, and more preferably nitrogen.
In the present invention, in the step S2, the temperature of the thermal desorption treatment is preferably 150 to 300 ℃, and more preferably 200 to 250 ℃; the time for the thermal desorption treatment is preferably 20 to 30 minutes, more preferably 25 minutes.
In the invention, the thermal desorption treatment is carried out in a tube furnace, and the specific treatment process is as follows: before heating, a protective gas carrier gas is firstly opened to maintain an anaerobic environment in the tube furnace; and adding the modified soil into a tube furnace for thermal desorption treatment, and continuously introducing nitrogen in the thermal desorption treatment process.
In the invention, the selection and the addition amount of the iron-containing steel slag are critical to improving the thermal desorption effect of the phthalate. On one hand, the selection and the addition amount of the steel slag can influence the heat transfer and mass transfer effects of the soil and indirectly influence the repair cost; on the other hand, the type of steel slag affects the soil heat transfer efficiency. The higher the thermal conductivity of the soil, the lower the required thermal desorption effective temperature, the less input energy, and the less destructive the soil structure and ecosystem.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
In the following examples, the preparation of phthalate contaminated soil used comprises the following steps:
0.3g of di (2-ethylhexyl) phthalate (DEHP) was weighed into a glass beaker containing 100mL of acetone, after thorough stirring, the solution was poured into 1kg of soil, after stirring well, placed into a fume hood for soil aging test for 1 month.
The iron-containing steel slag used in the examples is LT ash provided by a certain iron and steel enterprise, fe thereof 2 O 3 The content range is 20-80%.
Example 1
(1) Air-drying soil polluted by di (2-ethylhexyl) phthalate, adjusting to obtain soil with water content of 3%, crushing, grinding, and sieving with a 40-mesh sieve to obtain a standby soil sample;
(2) Adding LT ash into the standby soil sample for soil sample modification treatment, wherein the addition amount of the LT ash is 2wt% of the mass of the standby soil sample, and stirring the standby soil sample in a turnover oscillator at the stirring speed of 30r/min to obtain modified soil;
(3) And (3) carrying out thermal desorption treatment on the modified soil at 200 ℃, wherein the nitrogen flow rate is 200mL/min, cooling to room temperature after the thermal desorption treatment is carried out for 20min, and obtaining the repaired soil.
Example 2
(1) Air-drying soil polluted by di (2-ethylhexyl) phthalate, adjusting to obtain soil with water content of 3%, crushing, grinding, and sieving with a 40-mesh sieve to obtain a standby soil sample;
(2) Adding LT ash into the standby soil sample for soil sample modification treatment, wherein the addition amount of the LT ash is 1wt% of the mass of the standby soil sample, and stirring the standby soil sample in a turnover oscillator at the stirring speed of 30r/min to obtain modified soil;
(3) And (3) carrying out thermal desorption treatment on the modified soil at 200 ℃, wherein the nitrogen flow rate is 200mL/min, cooling to room temperature after the thermal desorption treatment for 30min, and obtaining the repaired soil.
Example 3
(1) Air-drying soil polluted by di (2-ethylhexyl) phthalate, adjusting to obtain soil with water content of 3%, crushing, grinding, and sieving with a 40-mesh sieve to obtain a standby soil sample;
(2) Adding LT ash into the standby soil sample for soil sample modification treatment, wherein the addition amount of the LT ash is 1.5wt% of the mass of the standby soil sample, and stirring the standby soil sample in a turning oscillator at the stirring speed of 30r/min to obtain modified soil;
(3) And (3) carrying out thermal desorption treatment on the modified soil at the temperature of 250 ℃, wherein the nitrogen flow rate is 200mL/min, and cooling to room temperature after the thermal desorption treatment for 20min to obtain the repaired soil.
Comparative example 1
(1) Air-drying soil polluted by di (2-ethylhexyl) phthalate, adjusting to obtain soil with water content of 3%, crushing, grinding, and sieving with a 40-mesh sieve to obtain a standby soil sample;
(2) And (3) carrying out thermal desorption treatment on the standby soil sample at 150 ℃, wherein the nitrogen flow rate is 200mL/min, and cooling to room temperature after the thermal desorption treatment for 20min to obtain the repaired soil.
Comparative example 2
(1) Air-drying soil polluted by di (2-ethylhexyl) phthalate, adjusting to obtain soil with water content of 3%, crushing, grinding, and sieving with a 40-mesh sieve to obtain a standby soil sample;
(2) Adding LT ash into the standby soil sample for soil sample modification treatment, wherein the addition amount of the LT ash is 0.5wt% of the mass of the standby soil sample, and stirring the standby soil sample in a turning oscillator at the stirring speed of 30r/min to obtain modified soil;
(3) And (3) carrying out thermal desorption treatment on the modified soil at 200 ℃, wherein the nitrogen flow rate is 200mL/min, cooling to room temperature after the thermal desorption treatment is carried out for 20min, and obtaining the repaired soil.
Comparative example 3
(1) Air-drying soil polluted by di (2-ethylhexyl) phthalate, adjusting to obtain soil with water content of 3%, crushing, grinding, and sieving with a 40-mesh sieve to obtain a standby soil sample;
(2) Adding LT ash into the standby soil sample for soil sample modification treatment, wherein the addition amount of the LT ash is 1wt% of the mass of the standby soil sample, and stirring the standby soil sample in a turnover oscillator at the stirring speed of 30r/min to obtain modified soil;
(3) And (3) carrying out thermal desorption treatment on the modified soil at 200 ℃, wherein the nitrogen flow rate is 200mL/min, and cooling to room temperature after thermal desorption treatment for 10min to obtain the repaired soil.
Comparative example 4
(1) Air-drying soil polluted by di (2-ethylhexyl) phthalate, adjusting to obtain soil with water content of 3%, crushing, grinding, and sieving with a 40-mesh sieve to obtain a standby soil sample;
(2) And (3) carrying out thermal desorption treatment on the soil at the temperature of 250 ℃, wherein the nitrogen flow rate is 200mL/min, cooling to room temperature after the thermal desorption treatment is carried out for 20min, and obtaining the repaired soil.
Comparative example 5
(1) Air-drying soil polluted by di (2-ethylhexyl) phthalate, adjusting to obtain soil with water content of 3%, crushing, grinding, and sieving with a 40-mesh sieve to obtain a standby soil sample;
(2) Adding LT ash into the standby soil sample for soil sample modification treatment, wherein the addition amount of the LT ash is 0.5wt% of the mass of the standby soil sample, and stirring the standby soil sample in a turning oscillator at the stirring speed of 30r/min to obtain modified soil;
(3) And (3) carrying out thermal desorption treatment on the modified soil at 150 ℃, wherein the nitrogen flow rate is 200mL/min, and cooling to room temperature after the thermal desorption treatment for 20min to obtain the repaired soil.
The di (2-ethylhexyl) phthalate in the soil after restoration obtained in examples 1 to 3 and comparative examples 1 to 5 was measured, and the measurement results are shown in tables 1 and 2.
The measuring method comprises the following steps: the PAEs were measured by gas chromatography mass spectrometry (GC-MS) under the following conditions: the sample injection amount is 1.0 mu L each time, and the flow is not split; chromatographic conditions: sample inlet temperature: 250 ℃; air flow rate: 1.5mL/min; column temperature: maintaining at 80deg.C for 1min; raising the temperature to 180 ℃ at a speed of 20 ℃/min, then raising the temperature to 280 ℃ at a speed of 10 ℃/min, and keeping the temperature for 2min. Mass spectrometry conditions: an electron bombardment source (EI); ion source temperature: 230 ℃; ionization energy: 70eV; interface temperature: 280 ℃; quadrupole temperature: 150 ℃; mass scan range: 35u-450u; the data acquisition mode is as follows: full scan mode.
TABLE 1 removal of di (2-ethylhexyl) phthalate from post-remediation soil obtained in examples 1-3
| Example 1 | Example 2 | Example 3 | |
| Removal of di (2-ethylhexyl) phthalate (%) | 89.90 | 91.37 | 91.89 |
TABLE 2 removal of di (2-ethylhexyl) phthalate from post-remediation soil obtained in comparative examples 1 to 5
In example 1, 2% iron-containing steel slag (LT ash) was used as a modifying material to modify di (2-ethylhexyl) phthalate contaminated soil, and thermal desorption restoration treatment was performed. Compared with the experimental conditions in comparative example 2, the addition amount of LT ash was increased from 0.5% to 2% and the removal rate of di (2-ethylhexyl) phthalate was increased from 76.25% to 89.90% at the same temperature and time, and the removal rate was increased by 17.90%. Comparison of the experimental results of comparative example 2 and comparative example 5 shows that the thermal desorption temperature is increased from 150 ℃ to 200 ℃ and the di (2-ethylhexyl) phthalate removal rate is increased from 9.74% to 76.25% and the removal rate is increased by 472.58% under the same thermal desorption time and LT ash addition amount conditions. The experimental results and the results shown in fig. 1 show that the influence of the temperature change on the thermal desorption result is more obvious than the variation of the addition amount of LT ash, and the conclusion can be obtained by comparing the experimental results of comparative example 1 and comparative example 4.
The di (2-ethylhexyl) phthalate contaminated soil was subjected to thermal desorption restoration treatment using different thermal desorption times at the same temperature and iron-containing steel slag (LT ash) addition amount in example 2 and comparative example 3. Compared with comparative example 3, the removal rate of di (2-ethylhexyl) phthalate was increased from 35.11% to 91.37% and 160.24% as the thermal desorption time was prolonged. The results of the related experiments are shown in FIG. 2. Comparing the experimental result with the corresponding thermal desorption result of the temperature change and the LT ash addition amount, the result shows that: among three factors of temperature, time and LT ash addition, the influence degree of the temperature and the LT ash on thermal desorption is sorted from big to small: temperature > time > LT ash addition. The method is characterized in that LT ash mainly plays a role in improving the heat and mass transfer effect of the soil surface in the thermal desorption treatment process, pollutant molecules on the surface of soil particles are firstly heated and removed in the initial stage of heat transfer of polluted soil, and pollutant molecules in the particles are limited by heat and mass transfer, so that the good phthalate removal effect can be achieved only by strictly controlling the temperature and time.
In example 3, 1.5% iron-containing steel slag (LT ash) was used as a modifying material to modify di (2-ethylhexyl) phthalate contaminated soil, and thermal desorption restoration treatment was performed. Compared with the thermal desorption experimental effect of comparative example 4 without LT ash, the removal rate of di (2-ethylhexyl) phthalate was increased from 79.85% to 91.89% at the same temperature and time, and the removal rate was increased by 15.08%.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. The application of the iron-containing steel slag combined thermal desorption technology in repairing phthalate polluted soil is characterized in that the specific repairing method of the application of the iron-containing steel slag combined thermal desorption technology in repairing phthalate polluted soil comprises the following steps:
step S1: mixing the iron-containing steel slag with the pretreated phthalate polluted soil to obtain modified soil;
step S2: carrying out thermal desorption treatment on the modified soil to obtain restored soil;
in the step S1, fe of the iron-containing steel slag 2 O 3 The content of the iron-containing steel slag is 20-80%, and the addition amount of the iron-containing steel slag is 1-1.5% of the mass of the pretreated phthalate polluted soil;
in the step S2, the temperature of thermal desorption treatment is 150-300 ℃, and the time of thermal desorption treatment is 20-30 min;
the phthalate is di (2-ethylhexyl) phthalate.
2. The method for repairing phthalate polluted soil by combining iron-containing steel slag with thermal desorption technology is characterized by comprising the following steps of:
step S1: mixing the iron-containing steel slag with the pretreated phthalate polluted soil to obtain modified soil;
step S2: carrying out thermal desorption treatment on the modified soil to obtain restored soil;
in the step S1, fe of the iron-containing steel slag 2 O 3 The content of the iron-containing steel slag is 20-80%, and the addition amount of the iron-containing steel slag is 1-2% of the mass of the pretreated phthalate polluted soil;
in the step S2, the temperature of thermal desorption treatment is 150-300 ℃, and the time of thermal desorption treatment is 20-30 min;
the phthalate is di (2-ethylhexyl) phthalate.
3. The method for restoring phthalate polluted soil by combining the iron-containing steel slag with the thermal desorption technology according to claim 2, wherein in the step S1, the pretreatment comprises the following steps: and (3) crushing, grinding and screening the phthalate polluted soil in sequence, and adjusting the water content of the soil to obtain the pretreated phthalate polluted soil.
4. The method for repairing phthalate polluted soil by combining iron-containing steel slag with thermal desorption technology according to claim 3, wherein the particle size of the pretreated phthalate polluted soil is more than or equal to 10 meshes, and the soil moisture content of the pretreated phthalate polluted soil is 2-10%.
5. The method for restoring phthalate polluted soil by combining iron-containing steel slag with thermal desorption technology according to any one of claims 2 to 4, wherein in the step S1, mixing is performed in a stirring manner, and the stirring speed is 30 to 50r/min.
6. The method for restoring phthalate polluted soil by combining iron-containing steel slag with thermal desorption technology according to claim 2, wherein in the step S2, thermal desorption treatment is carried out under the atmosphere of protective gas, and the flow rate of the protective gas is 200-400 mL/min.
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