CN107057705B - Heavy metal contaminated soil remediation material, preparation method and application - Google Patents
Heavy metal contaminated soil remediation material, preparation method and application Download PDFInfo
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- CN107057705B CN107057705B CN201710389112.4A CN201710389112A CN107057705B CN 107057705 B CN107057705 B CN 107057705B CN 201710389112 A CN201710389112 A CN 201710389112A CN 107057705 B CN107057705 B CN 107057705B
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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
- C09K17/08—Aluminium compounds, e.g. aluminium hydroxide
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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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- 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
- C09K2109/00—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE pH regulation
Abstract
The invention discloses a heavy metal contaminated soil remediation material, a preparation method and application. The repair material contains light-burned dolomite powder and blast furnace slag powder. The dolomite is calcined and then mixed with blast furnace slag powder to obtain the slag. The repair material is low in cost, simple in process, green and environment-friendly, and can well repair heavy metal contaminated soil.
Description
Technical Field
The invention relates to the technical field of soil remediation, and particularly discloses a heavy metal contaminated soil remediation material, a preparation method and application.
Background
With the continuous promotion of industrialization and urbanization, the problem of heavy metal pollution of soil in China is more and more highly valued by people. The pollution of heavy metals in soil directly causes the content of heavy metals in agricultural products to exceed the standard, and seriously affects the quality of cultivated land, the food safety and the human health. The research on physical/chemical remediation materials and methods for heavy metal pollution of soil is very important for all countries in the world.
Currently, the most common physical/chemical methods for soil remediation are thermal desorption technology, steam extraction technology, solidification/stabilization technology, leaching technology, oxidation/reduction technology, photocatalytic interpretation technology, electrodynamics remediation, and the like. The solidification/stabilization technology is used for fixing pollutants in a polluted medium to enable the pollutants to be in a long-term stable state, is a rapid control and restoration method which is commonly applied to soil heavy metal pollution, and has obvious advantages for simultaneously treating multiple heavy metal compound polluted soil. The treatment technology has low cost, and can greatly reduce the site pollution treatment cost for the polluted soil in some non-sensitive areas. The common curing stabilizers include fly ash, lime, asphalt, portland cement, and the like. The silicate cement in the common curing stabilizers is most widely applied, has low cost and wide application range, can effectively reduce the migration capacity of heavy metal pollutants, and improves the mechanical properties of soil bodies or tailings, but researches show that certain heavy metals (such as Cu and Zn) can influence the hydration process of the silicate cement and seriously reduce the early strength of the silicate cement. On the other hand, the silicate cement has a high hydration pH value (stable at 13 or more), which is not beneficial to the reduction of the mobility of various amphoteric heavy metals. In addition, the production process of the portland cement consumes great energy (the calcination temperature is 1450 ℃), and discharges a large amount of greenhouse gases (accounting for 5-8% of the total discharge of human beings), which does not meet the requirements of energy conservation and emission reduction. Therefore, it is necessary to develop green environmental protection, which can effectively replace portland cement and be applied to the fields of polluted soil remediation and the like.
In recent years, attempts have been made from various aspects. On one hand, industrial waste (such as slag, fly ash and the like) materials are used to replace portland cement; on the other hand, new additives are explored to ensure that the curing stabilizer has effectiveness in different sites. The patent CN102174325A discloses a composite passivator for polluted soil heavy metals, which comprises 33-54% of power plant slag, 25-39% of sepiolite ore powder and 21-28% of quicklime by mass. However, the use of too much quicklime greatly increases the activity of the hydration product and thus affects the durability of the setting stabilizer.
Patent CN103756682A discloses a curing agent for repairing high-concentration multiple metal contaminated sites, which comprises the following components in percentage by weight: 60-80% of modified phosphate rock powder and 20-40% of light-burned magnesia. However, in the method, the preparation process of the modified powdered rock phosphate is complex, the pH value of the curing agent is low, and the application range is limited.
Patent CN105271630A discloses an energy-saving and environment-friendly sludge modified material, which comprises, by weight, 60-85% of industrial waste residues, 5-15% of cement clinker, 5-15% of dihydrate gypsum, 2-10% of limestone, 1-3% of an exciting agent and 0.05-0.5% of a grinding aid. Wherein the industrial waste residue is a mixture of blast furnace slag and at least one of steel slag, fly ash, phosphorous slag, silicomanganese slag, ferrochromium slag, burnt shale, burnt clay and coal slag, and the excitant is at least one of sodium carbonate, sodium hydroxide and sodium silicate. However, the method also has the defects of limited application range, complicated preparation process and the like.
In conclusion, a heavy metal contaminated soil remediation material which is environment-friendly, simple in process and wide in applicability is urgently needed to make up for the defects of the existing curing stabilizer.
Disclosure of Invention
The invention aims to provide a heavy metal contaminated soil remediation material based on blast furnace slag, which contains light-burned dolomite powder. The repair material is low in cost and can efficiently repair heavy metal contaminated soil.
The invention also aims to provide a preparation method of the heavy metal contaminated soil remediation material, which is simple to operate and can be industrially produced.
Still another object of the present invention is to provide a use of the heavy metal contaminated soil remediation material.
The invention provides a heavy metal contaminated soil remediation material which contains light-burned dolomite powder and blast furnace slag powder.
Dolomite is a widely occurring mineral product. In China, the method is mainly distributed in Liaoning province, inner Mongolia province, Shanxi province, Jiangsu province, Fujian province, Hubei province, Guangxi province and the like, and the reserve volume exceeds 40 hundred million tons. I.e. the dolomite has wide sources and easily obtained raw materials. After high-temperature calcination, dolomite is decomposed into an admixture of magnesia and lime, so that the blast furnace slag powder and the light-burned dolomite powder are the admixture of the blast furnace slag powder, the magnesia and the lime. Blast furnace slag is a novel soil remediation material at present, and can effectively reduce the filtration of harmful heavy metal ions; hydration of activated magnesium oxide to produce brucite (Mg (OH)2) The lamellar crystal structure of the hydrate can limit heavy metal ions between layers, thereby achieving the effect of fixing the heavy metal ions. The main function of the lime is to increase the pH value of the admixture and ensure the proper hydration rate of the admixture.
The magnesia and the lime generated by lightly burning the dolomite are both effective components of the repair material, and the purification step required for separately producing the magnesia and the lime is omitted. On the other hand, a small amount of calcium carbonate remained when the dolomite powder is not sufficiently decomposed is also beneficial to improving the strength of the repair soil, so that the repair effect is improved, and the cost of the repair material can be reduced to a certain extent. And the blast furnace slag powder is industrial waste, so that the recycling of the industrial waste greatly reduces the disposal cost of the waste, and simultaneously reduces the additional energy consumption and the greenhouse gas emission.
The dolomite in the present invention may include various kinds of dolomite in various purities.
Preferably, the weight ratio of the dolomite powder to the blast furnace slag powder is 1:3 to 1: 20.
Preferably, the dolomite powder has a median particle size of 3-8 μm, a maximum content of particles greater than 25 μm of no more than 0.1%, and a dolomite purity of greater than 98%.
Preferably, the dolomite powder has an oil absorption of 17g/100g and an aerated powder density of 900kg/m3The density of the extracted powder is 1500kg/m3。
Preferably, the dolomite powder is DRB20 dolomite powder.
The method for preparing the heavy metal contaminated soil remediation material is characterized by comprising the following steps: the method comprises the following steps: calcining dolomite powder, and mixing the light-burned dolomite with blast furnace slag powder.
The dolomite produces magnesium oxide and calcium oxide after calcination, but the two substances are not produced simultaneously, but MgO is produced first and then CaO is produced. The thermal decomposition of dolomite can be generally divided into two stages, magnesium oxide is firstly generated at a lower temperature, and calcium oxide is further generated along with the temperature increase, wherein the specific decomposition equation is as follows:
CaMg(CO3)2→CaCO3+Mg+CO2first stage
CaCO3→CaO+CO2Second stage
Different calcination temperatures can result in different proportions of MgO and CaO in the calcined product. In addition, the calcination temperature has an effect on the activity of MgO, lower calcination temperatures produce higher MgO activity, and higher activity is more beneficial to exciting blast furnace slag. However, the low calcination temperature also causes low CaO content, and the pH of the pore water after hydration is too low, which is not beneficial to the excitation of blast furnace slag.
The invention also provides a preparation method of the heavy metal contaminated soil remediation material, which comprises the following steps: calcining dolomite powder, and mixing the light-burned dolomite with blast furnace slag powder.
In order to ensure the activity of the magnesium oxide in the calcined product, the preferred calcining temperature of the dolomite is 600-1000 ℃, and the calcining time is 1-4 h.
According to the invention, the decomposition rate of the light calcined dolomite after calcination at different temperatures and different time periods is researched (Table 1), and the decomposition of the dolomite can be promoted by increasing the calcination temperature or the calcination time, but the decomposition efficiency is gradually reduced. Meanwhile, the repairing effect of the repairing material calcined at different temperatures on heavy metal polluted sites is researched, and the calcining temperature is preferably 700-1000 ℃, and the calcining time is 1-4 h. At the moment, the solidification stabilizing effect on heavy metals in the polluted soil is the best, the decomposition effect can be better considered, and the energy waste is reduced.
TABLE 1 decomposition rates of dolomite powder under different conditions
The blast furnace slag may include various types of blast furnace slag. Such as blast furnace slag powder from Hanson corporation of the uk and S95 slag, which is common in the chinese market. But preferably, the specific surface area of blast furnace slag is 490m2Kg, bulk density 1050kg/m3(ii) a Blast furnace slag powder of Hanson, UK is preferred.
Blast furnace slag powder generally comprises the following chemical composition: SiO 22、Al2O3、CaO、MgO、K2O、Na2O、SO3. The preferred chemical composition of the blast furnace slag powder of the present invention is: in weight percent, SiO237％、Al2O313％、CaO 40％、MgO8％、K2O 0.6％、Na2O 0.3％、SO31.0％。
The pH value of the pore water of the silicate cement hydration product is stabilized above 13, which is not beneficial to the precipitation of some heavy metal ions. The pH value of the pore water solution after the light-burned dolomite powder-blast furnace slag hydration is generally not higher than 13, which is beneficial to the precipitation of various amphoteric heavy metals (such as Cu, Zn and the like), thereby reducing the mobility of the amphoteric heavy metals. On the other hand, the hydration product contains a large amount of hydrotalcite-like compounds (hydrotalcite-like phases), which have a good effect on heavy metal adsorption.
The invention further provides an application of the heavy metal contaminated soil remediation material, and the remediation material is mixed with the heavy metal contaminated soil.
In order to fully restore the heavy metal pollution of the soil, the mass ratio of the restoring material to the polluted soil is preferably 1:25-1: 5; the two are directly mixed and then the restoration soil is obtained after the hydration action is finished.
The invention has the following beneficial effects:
1: the repair material has low cost, one of the raw materials, namely dolomite, has abundant reserves in the nature, the calcination process of the dolomite powder is simple, the purification process of calcium oxide and magnesium oxide is omitted, and the cost is greatly reduced.
2: the repair material is green and environment-friendly, the simplified process reduces the energy consumption and the emission of greenhouse gases, and one of the raw materials, namely the blast furnace slag powder, is industrial waste, so that the additional energy consumption and the emission of greenhouse gases are reduced by recycling the blast furnace slag powder.
3: the repairing material can effectively solidify/stabilize heavy metal ions in the polluted soil, so that the aim of repairing the polluted soil is fulfilled.
Detailed Description
The present invention will be further clearly understood from the specific examples and comparative examples of the present invention given below, which are not intended to limit the present invention. The parts of the specific examples and comparative examples which are not described in detail are obtained by means of the prior art, the known technical means and the industry standard.
Parts used in the present invention are parts by weight unless otherwise specified.
Example 1
The source of dolomite powder is DRB20 dolomite powder from IMERYS mineral Ltd, UK (Imerys Minerals Ltd's). The calcining equipment is a common laboratory high-temperature quenching furnace, and the maximum temperature is at least 1300 ℃; the blast furnace slag powder originates from Hanson, UK, and its main chemical composition and physical properties are shown in Table 2. Heavy metal contaminated soil was obtained from a heavy metal contaminated site in the kasford region, yorkshire, uk, where the original concentration ranges of the major heavy metal contaminants are shown in table 3.
TABLE 2Hanson blast furnace slag powder Main chemical composition (mass%) and physical Properties
TABLE 3 concentration of heavy metal pollutants in contaminated site (unit: mg/kg)
Preparing a repairing material:
weighing appropriate amount of DRB20 dolomite powder, and uniformly placing in a crucible; placing into a high temperature oven, and starting heating at a heating rate of 10 deg.C/min. Heating the muffle furnace to 800 ℃, keeping the temperature for 1h, and cooling to obtain the light-burned dolomite No. 1. The light-burned dolomite powder was determined to contain magnesium oxide, calcium oxide and a small amount of undecomposed dolomite. Mixing the light-burned dolomite with commercially available blast furnace slag in a mass ratio of 1:3, and stirring for more than 5 minutes by using a stirrer to ensure uniform mixing to prepare the repair material.
Repairing heavy metal contaminated soil:
the repairing material is evenly mixed with the polluted soil according to the mass percentage of 12 percent and maintained. Unconfined compression tests were performed on samples cured for 7 days, 14 days, and 28 days according to ASTM D1633-00 test Standard. The specific method comprises the following steps: the specimen size was Φ 50X 100mm, pressed on a CONTROLS Uniframe unconfined compression tester at a very constant rate of 1.14mm/min until the specimen failed, and the peak strength of the specimen was recorded.
The samples after 7 days and 28 days of curing were subjected to leaching tests according to the test standard BS EN 12457-2. The specific method comprises the following steps: taking 50g of a sample mixed with a curing stabilizer, and crushing the sample to ensure that the particle diameter is between 1 and 4 mm; adding 500ml of distilled water (pH 5.4) without carbonate and shaking uniformly for 24 h; the leaching liquid passes through a filter paper with the aperture of 0.45 mu m, and the concentration of the heavy metal ions such as Ni, Cu, Zn and Pb in the solution is measured by using ICP-OES.
Example 2
Basically the same as example 1, except that the muffle furnace was heated to 1000 ℃ to obtain light-burned dolomite # 2. The 2# sample was determined to contain magnesium oxide, calcium oxide and a small amount of calcium carbonate. The activity of magnesium oxide in #1 was higher than that in # 2 due to the lower calcination temperature in the preparation of # 1.
Example 3
Basically the same as example 1, except that the mass ratio of the light burned dolomite to the blast furnace slag was 1:9, and this ratio value is used by way of example only in the examples. .
Example 4
Basically the same as example 1 except that the muffle furnace was heated to 1000 ℃ and the mass ratio of the soft-burned dolomite to the blast furnace slag was 1: 9.
Comparative example 1
Basically the same as example 1 except that commercially available activated magnesia and calcia were uniformly mixed in a mass ratio of 1:1 in place of the light burned dolomite #1 in example 1 to prepare a repair reference material (R).
Comparative example 2
Basically the same as example 1, except that the muffle furnace was heated to 600 ℃ to obtain light-burned dolomite No. 3.
Comparative example 3
Essentially the same as example 1, except that the muffle furnace was warmed to 1050 deg.C, product # 4 was produced.
Comparative example 4
The contaminated soil was remediated using 32.5 portland cement as the remediation material (PC) and the leaching test and testing was performed using the same method.
TABLE 4 unconfined compressive strength (unit: MPa) of contaminated soil sample at 12% curing stabilizer dose
Note: NM means no data detected, and the number in parentheses is the standard deviation
Description of sample number: 1# or 2# indicates the kind of light burned dolomite, G indicates blast furnace slag, and the numbers following 1#, 2# and G indicate parts by mass. Taking 1#1G3 as an example, the sample is a solidification stabilizer prepared by mixing 1# light-burned dolomite and blast furnace slag in a mass ratio of 1: 3.
As shown in Table 4, the unconfined compressive strength of the contaminated soil cured and stabilized by 1#1G3 after 7 days can reach 1MPa, but is slightly less than 1.11MPa of 2#1G3, which is mainly due to the faster hydration rate of 2#1G3, so that the contaminated soil can obtain higher strength in a short period. After 14 days and 28 days of curing, the strength of the polluted soil after the 1#1G3 is stably cured respectively reaches 2.17MPa and 3.10MPa, and is respectively higher than that of the soil sample treated by 2#1G3 in the same curing period, which is mainly along with the hydration of magnesium oxide with higher activity in 1# light-burned dolomite, more compact hydration products with high strength are generated, and thus the soil sample obtains higher strength. The strength of the solidified stabilized soil sample is obviously reduced by reducing the use ratio (1: 9) of the light-burned dolomite and the blast furnace slag, but the strength change trend of different curing stages is consistent with the trend.
The unconfined crush results show that the solidification stable materials made of lightly calcined dolomite-blast furnace slag (1#1G3 and 2#1G3) can provide higher strength to contaminated soil than the solidification stable material made of magnesia-calcia-blast furnace slag (R1G 3). In addition, the calcination temperature of dolomite has a great influence on the curing stabilization effect. When the calcining temperature is 600 ℃, the decomposition products of dolomite are less, and blast furnace slag cannot be effectively excited, so that the strength of the polluted soil which is stably solidified in each stage of 3#1G3 is seriously insufficient; when the calcination temperature is 1050 ℃, the activity of the generated magnesium oxide is low, the strength of the hydration product is low, and the strength of the solidified stabilized soil is insufficient. Compared with the currently commonly used Portland Cement (PC) as a curing and stabilizing material, the 1#1G3 and 2#1G3 have slightly lower strength for 7 days, mainly because the hydration rate is relatively slow and the hydration is incomplete; after curing for 14 days and 28 days, the stable curing unconfined compressive strength is higher than that of a sample after the stable curing of PC, so that the Portland cement has certain advantages compared with the traditional Portland cement.
Table 5 shows the results of the leaching tests of the samples of examples 1-4 and comparative examples 1-4. The results show that 1#1G3 and 2#1G3 have good curing and stabilizing effects on different heavy metal ions, and the curing and stabilizing effects of the two curing and stabilizing agents on different heavy metals are slightly different. From the results of 1#1G9 and 2#1G9, it can be seen that changing the amount of the curing stabilizer affects the curing stabilizing effect on the contaminants, and therefore the dosage of the material can be adjusted according to the requirements of the site remediation effect. In addition, the effect of using light burned dolomite is better than that of the activated magnesia-quicklime mixture (see R1G3), and the process of using light burned dolomite is simpler. When the calcination temperature is not in the range of 700-1000 ℃, the effect of the repair material is poor (see 3#1G3 and 4#1G3), mainly because the too low calcination temperature is not enough to decompose dolomite, thereby failing to excite the slag effectively; too high a calcination temperature may lead to a decrease in the activity of magnesium oxide, which is not favorable for the solidification stability of the hydrated product to heavy metals. Compared with the most common Portland Cement (PC) at present, the curing and stabilizing effect of the invention also has obvious advantages, thus the invention has wide application prospect.
TABLE 5 Leaching test results (unit: mg/L) for contaminated soil samples at a setting stabilizer dosage of 12%
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, therefore, the present invention is not limited by the appended claims.
Claims (9)
1. The heavy metal contaminated soil remediation material is characterized in that: the heavy metal contaminated soil remediation material contains light-burned dolomite powder and blast furnace slag powder, the weight ratio of the light-burned dolomite powder to the blast furnace slag powder is 1:3-1:20, and the light-burned dolomite powder is prepared by calcining the dolomite powder at the temperature of 700 ℃ and 1000 ℃ for 1-4 h.
2. The heavy metal contaminated soil remediation material of claim 1, wherein: the dolomite powder has a median particle size of 3-8 μm, and the content of particles with particle size greater than 25 μm is not more than 0.1%.
3. The heavy metal contaminated soil remediation material of claim 1, wherein: the dolomite powder has an oil absorption of 17g/100g and an aerated powder density of 900kg/m3The density of the extracted powder is 1500kg/m3。
4. The heavy metal contaminated soil remediation material of claim 1, wherein: the dolomite powder is DRB20 dolomite powder.
5. The heavy metal contaminated soil remediation material of claim 1, wherein: the specific surface area of the blast furnace slag is 490m2Kg, bulk density 1050kg/m3。
6. The heavy metal contaminated soil remediation material of claim 1, wherein: the dolomite powder is DRB20 dolomite powder, the median particle diameter of the dolomite powder is 3-8 μm, the content of particles with particle diameter larger than 25 μm is not more than 0.1%, the oil absorption of the dolomite powder is 17g/100g, and the density of aerated powder is 900kg/m3The density of the extracted powder is 1500kg/m3The specific surface area of the blast furnace slag is 490m2Kg, bulk density 1050kg/m3。
7. A method for preparing the heavy metal contaminated soil remediation material of claim 1, wherein: the method comprises the following steps: calcining the dolomite powder for 1-4 hours at the temperature of 700-1000 ℃ to prepare light-burned dolomite powder, and mixing the light-burned dolomite powder with blast furnace slag powder.
8. Use of the heavy metal contaminated soil remediation material of any one of claims 1 to 6 for remediation of heavy metal contaminated soil.
9. Use according to claim 8, characterized in that: the mass ratio of the heavy metal contaminated soil remediation material to the heavy metal contaminated soil is 1:25-1: 5.
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| CN108905956B (en) * | 2018-09-26 | 2021-04-06 | 江苏省地质调查研究院 | Modified attapulgite repairing material and preparation method and application thereof |
| CN111249663B (en) * | 2020-03-02 | 2021-01-12 | 清华大学 | Reactive curing stable composition and preparation method and application thereof |
| CN111961474A (en) * | 2020-08-10 | 2020-11-20 | 山东达源环保工程有限公司 | Heavy metal dirt soil repairing agent and preparation method thereof |
| CN112920807A (en) * | 2021-02-03 | 2021-06-08 | 清华大学 | Heavy metal contaminated soil remediation material, preparation method thereof and remediation method of heavy metal contaminated soil |
| CN115521787A (en) * | 2022-10-17 | 2022-12-27 | 中国科学院南京土壤研究所 | Lead-zinc smelting site heavy metal compound contaminated soil remediation agent and application thereof |
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| CN102329620A (en) * | 2011-10-13 | 2012-01-25 | 武汉凯迪工程技术研究总院有限公司 | Heavy-metal-polluted acidic soil repairing material as well as preparation method and application thereof |
| CN105330475A (en) * | 2015-10-30 | 2016-02-17 | 马鞍山市心洲葡萄专业合作社 | Acidified soil restoration fertilizer |
| CN107365589A (en) * | 2016-05-13 | 2017-11-21 | 南京凯杰环境技术有限公司 | A kind of heavy-metal contaminated soil solidification based on magnesia, insoluble material |
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