CN111676023B - Semi-wrapping stabilizing material and preparation method and use method thereof - Google Patents
Semi-wrapping stabilizing material and preparation method and use method thereof Download PDFInfo
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Abstract
The invention discloses a method for preparing a semi-wrapped stabilizing material, the semi-wrapped stabilizing material prepared by the method and a using method. The semi-wrapping stabilizing material takes at least one of sodium salt, calcium salt and magnesium salt and/or hydroxide as a core, silicate minerals as capsules, the wrapping material is prepared by a semi-wrapping granulation method in one step, and the other active ingredient is an iron compound and/or a manganese compound which are doped in a proportional compatibility manner to form the semi-wrapping stabilizing material with heavy metals such as stabilized soil arsenic and cadmium. The material has the advantages of simple preparation process and low material cost, effectively prevents the components from reacting with each other, can exert the stabilization effect of each effective component on various heavy metals, and has the advantage of efficiently stabilizing arsenic and cadmium at the same time. The material can keep long-term effectiveness, is easy to store and use, and can be widely applied to the remediation of arsenic-cadmium composite polluted sites.
Description
Technical Field
The invention belongs to the field of soil heavy metal remediation, and particularly relates to a semi-wrapped stabilizing material, and a preparation method and a use method thereof.
Background
In recent years, the problem of heavy metal pollution has attracted extensive attention from academia, government and the public due to the increasing content of pollutants in soil environments. Heavy metals can enter soil through various ways, are not easy to be leached with water, are difficult to degrade by microorganisms, and have obvious biological enrichment effect. The soil pollution has a long latent period, has the characteristics of concealment, irreversibility, universality, surface aggregation and the like, and poses threats to the ecological environment and human health.
The site soil heavy metal pollution mainly takes lead, cadmium, arsenic, copper, zinc, nickel and the like as main materials, and mostly appears in a combined pollution form, different from single heavy metal pollution, different heavy metal elements in the combined pollution have different restoration requirements, different heavy metal elements can influence the restoration effect mutually, and the restoration risk is increased. The arsenic and cadmium associated combined pollution is the most representative, and the arsenic and cadmium combined pollution is accompanied with the soil near a plurality of mining plants and metal smelting plants. Reduction of arsenic in oxidationH is mainly used under the conditions of higher original potential, weak acidity and neutrality2AsO4-The shape of the compound is existed, so that the compound is more stable in soil; cadmium is more stable under the conditions of lower oxidation-reduction potential and alkaline condition, because the adsorption of organic and inorganic colloids and the like in the soil to cadmium is improved when the pH value of the soil is increased, thereby improving the content of the combined cadmium in the soil and the content of OH in the soil-And the cadmium ions are combined into insoluble cadmium hydroxide. The antagonism between different heavy metals brings great difficulty to the remediation of the heavy metal contaminated soil in the field.
Aiming at the problem, at present, a stabilization technology is mostly adopted in China, one of the cores of the technology is a stabilization material, one of the main ideas of the domestic engineering application-based research and development of the composite contaminated soil stabilization agent is to mix chemical materials with different characteristics, the cost is low, the repair requirement can be met in a short time, but the stabilization materials are easily influenced by factors such as soil pH value, organic matter content and the like, the repair effect of the stabilization materials on heavy metals is different, and the interaction between different heavy metal types, concentrations and materials and soil heavy metal pollutants can also influence the repair effect of the materials; the materials are mostly formed by compounding acidic and alkaline materials, are not easy to store, and are easy to react with each other and generate heat to generate danger in the transportation process; the repairing effect of the stabilizing material is also influenced by external environment change and moisture content, and the original adsorbed heavy metal can be released secondarily to cause environmental damage along with rainfall scouring, flooding treatment or soil pH reduction; the powder materials in the market are more, and dust is easy to generate in the application process, so that the operation difficulty is improved, and waste and secondary pollution are caused; therefore, the research of arsenic and cadmium pollution remediation materials is a current research key point aiming at the composite pollution characteristics of the field.
For the soil singly polluted by arsenic and cadmium, the sodium-calcium-magnesium salt or hydroxide has good stabilizing effect on cadmium, which is reported in documents. Based on the aim of improving the synergistic effect of the components of the medicament, the research on the compounding of stabilizing materials and the optimization of component structures is developed, for example, Dongfuxiu and the like (2019) adopt FeSO4The composite stabilizer is used for stabilizing the arsenic, cadmium, lead and zinc composite polluted soil with CaO, and FeSO is found4And the addition sequence of CaO directly influences the stabilizing effect of arsenic, cadmium, lead and zinc, and the antagonistic action among As, Cd and Zn can be weakened under the conditions of certain addition sequence and optimized component structure. A great deal of literature reports that the iron and manganese containing material has strong binding capacity to arsenic and can reduce the bioavailability of arsenic in soil. Sun et al (2015) discovered that these materials can significantly reduce the bioavailability of arsenic in contaminated soil by studying the effect of sepiolite, red mud, iron sand, gypsum, ferrihydrite, iron phosphate, and layered oxides on arsenic effectiveness in soil, but ferrihydrite works best. Moscomb et al (2017) add ferrous sulfide, carbide slag and mushroom slag compound materials to stabilize arsenic contaminated soil, and the results show that the arsenic-containing composite material can greatly reduce the leaching concentration and bioavailability of arsenic in soil, and is more beneficial to the stabilization of arsenic when the pH is neutral and acidic. Therefore, how to combine the stabilization of the sodium-calcium-magnesium salt or hydroxide and the iron-manganese containing material to prepare the composite stabilization material solves the problems that the component materials are easy to react with each other, the effect is easy to change by external environmental conditions, the application is difficult and the like, thereby simultaneously stabilizing the arsenic and the cadmium in the soil and having important significance.
There have been some studies on wrapping materials, and although the wrapping materials in the past have a core-capsule structure and can achieve the stabilizing effect on arsenic and cadmium, the wrapping materials have the following disadvantages: (1) the materials used in the preparation process are various, such as: biochar, metal silicate, emulsifier, catalyst, reducing agent and the like, and the purity is required to be high, the price is high and the environment is not green; (2) the preparation steps are complex, generally relate to the high-temperature carbonization and activation of biomass, the redox reaction of materials containing iron and the like, and the core-spun and the encapsulation are prepared in two steps, so the reaction is violent and the energy consumption is high; (3) the active ingredients are all granulated and wrapped by adopting a full wrapping method, so that the release rate of the material is limited, the release speed of various active ingredients is not easy to control, and the stabilization efficiency is further influenced.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and the invention aims to provide a semi-wrapping stabilizing material, which adopts a semi-wrapping method for effective ingredients, is not limited in material release rate, is easy to control the release rate of various effective ingredients and has high stabilizing rate.
Another object of the present invention is to provide a method for preparing a semi-encapsulated stabilized material, in which the purity and composition of the raw materials are not particularly limited, the preparation method is simple, and the core-wrapped and encapsulated materials can be prepared in one step.
The invention also aims to provide a using method of the semi-wrapped stabilizing material, the stabilizing material has the characteristics of high stabilizing rate, stable performance, long-term effectiveness maintenance, easiness in storage and easiness in use, and is beneficial to remediation of heavy metal pollution of soil arsenic and cadmium.
A preparation method of a semi-wrapped stabilizing material comprises the following steps:
s1, preparing a salt and/or a hydroxide into a slurry, wherein the salt is at least one of a sodium salt, a calcium salt and a magnesium salt;
s2, stirring the silicate mineral, adding the slurry into the silicate mineral, and uniformly stirring to obtain a mixture of the slurry and the silicate mineral;
s3, granulating and drying the mixture of the slurry and the silicate mineral to obtain a wrapping material;
and S4, adding an iron compound and/or a manganese compound, and mixing with the wrapping material to obtain a semi-wrapping stabilizing material.
The composite stabilizer is prepared by adopting a semi-wrapping method, namely, sodium salt, calcium salt, magnesium salt and/or hydroxide are taken as core wraps, silicate minerals are taken as capsules, a wrapping material is prepared by a one-step method, the other active ingredient is an iron compound and/or a manganese compound, wrapping is not carried out, the preparation process is simple, the material cost is low, the mutual reaction of the ingredients is effectively prevented, the stabilizing effect of each active ingredient on various heavy metals is effectively exerted, the aim of simultaneously stabilizing arsenic and cadmium is fulfilled, compared with the traditional stabilizing material, the stabilizing performance is stable, the long-term effectiveness can be maintained, the storage is easy, the use is easy, and the composite stabilizer can be applied to repairing of heavy metal composite polluted sites.
Preferably, in S3, a binder solution is added to the mixture of the slurry and the silicate mineral, and then the mixture is uniformly stirred, granulated and dried;
the added mass of the adhesive is 0.25-2% of the mass of the mixture of the slurry and the silicate mineral; further preferably, from 0.25 to 1%; further preferably, 0.3%;
the mass fraction of the binder in the binder solution in S3 is 1 to 3%, more preferably 2 to 3%, still more preferably 2%;
the stirring time in S3 is 8-15min, and the drying temperature is 100-110 ℃. Further preferably, the stirring time in S3 is 12-15min, and the drying temperature is 105-110 ℃.
Adding a binder solution into the mixture of the slurry and the silicate mineral to granulate to form a core-spun product which takes sodium salt, calcium salt, magnesium salt and/or hydroxide as wrapping materials, the silicate mineral as an encapsulation material, the proportion of the core-spun product and the encapsulation is proper, and the addition of a proper amount of the binder avoids the excessive wrapping of the core-spun product to influence the release and diffusion of active ingredients in soil; the method that the wrapping material is matched with the iron compound and/or the manganese compound according to a certain proportion is adopted, so that the iron compound and/or the manganese compound and arsenic are fully stabilized, the core-spun material is slowly released and is combined with cadmium in soil, and the antagonism between arsenic and cadmium is effectively weakened. Therefore, the semi-wrapping stabilizing material has strong stabilizing capability on heavy metals with antagonism to arsenic, cadmium and the like, has stable performance, can be effective for a long time, and is easy to store and use.
Preferably, the mass fraction of the slurry in S2 is equal to or more than 30%, and the mass ratio of the volume of the slurry to the silicate mineral is 1:4-4:1mL/g, further preferably, the mass ratio of the volume of the slurry to the silicate mineral is 1:2-2:1mL/g, further preferably, 1: 1 mL/g;
the slurry in S2 is dripped into the silicate mineral;
and in S2, adding the slurry into the silicate mineral, and stirring for 8-15 min.
Preferably, the salt is at least one of sodium carbonate, calcium carbonate and magnesium carbonate, the hydroxide is at least one of sodium hydroxide, calcium hydroxide and magnesium hydroxide, preferably, the salt and/or hydroxide is calcium hydroxide;
the silicate mineral is at least one of sepiolite, bentonite, montmorillonite, kaolin and zeolite, preferably zeolite.
Preferably, the adhesive is at least one of polyaluminium chloride, polyvinyl alcohol, carboxymethyl cellulose and starch, and preferably, the adhesive is polyaluminium chloride.
Preferably, the iron compound is at least one of polymeric ferric sulfate, ferrous sulfate heptahydrate and anhydrous ferric chloride, the manganese compound is at least one of anhydrous manganese chloride and manganese sulfate, and preferably, the iron compound and/or the manganese compound is ferrous sulfate heptahydrate;
the ratio of the mass of the iron compound and/or manganese compound to the mass of the wrapping material in S4 is 1:4-4:1, further preferably, the ratio of the mass of the iron compound and/or manganese compound to the mass of the wrapping material in S4 is 4: 1-1: 1, further preferably, 3.25: 1.
the invention also discloses a semi-wrapped stabilizing material, which is prepared by the method. The stabilizing material has strong stabilizing capability and stable performance on heavy metals with antagonism to arsenic, cadmium and the like, can be effective for a long time, and is easy to store and use.
Preferably, the average particle size of the wrapping material is 2-6mm, preferably 2-4 mm.
The invention also discloses a using method of the semi-wrapped stabilizing material, which comprises the following steps:
after the soil is screened and naturally dried, applying a semi-wrapped stabilizing material to the soil, and uniformly mixing, wherein the mass ratio of the semi-wrapped stabilizing material to the soil is 1: 100-3: 100, when the soil is applied, the water content of the soil is 10-30%, and the soil is maintained for 1-3 days.
And (5) sampling after maintenance to perform a leaching toxicity experiment, and determining the stabilization rate. Therefore, the stabilizing material is granulated by half-wrapping salt and/or hydroxide, and simultaneously has the method of proportionally combining the iron-containing compound and/or the manganese compound, so that the stabilizing capability of the stabilizing material on heavy metal composite pollution such as arsenic, cadmium and the like is obviously improved, the stabilizing rate can be stable for a long time, the storage and the use are easy, and the cost is low.
Preferably, the mass ratio of the semi-coating stabilizing material to the soil is 2: 100-3: 100, preferably, 2: 100, respectively;
the water content of the soil is 20-30%, preferably 20%;
the curing time is 1-2 days, preferably 1 day.
The invention has the following advantages:
1. compared with the traditional full-wrapping method and the simple compounding method, the semi-wrapping stabilizing material only needs to wrap salt and/or hydroxide directly with silicate minerals by using the semi-wrapping method, and does not need to prepare capsules independently; by utilizing a compatibility method, the wrapping material and the iron compound and/or the manganese compound are subjected to proportional compatibility, so that the problem that chemical reaction is generated after the salt and/or the hydroxide are mixed with the iron compound and/or the manganese compound to reduce or lose respective stabilization functions on the heavy metals in the soil is solved, and the wrapping material has a good stabilization effect on the compound pollution of acid radical state and cation state heavy metals such as arsenic, cadmium and the like.
2. The semi-wrapping stabilizing material provided by the invention has the advantages of uniform particles, convenience in use and difficulty in forming flying dust, and can efficiently stabilize various heavy metals after being applied, so that the dosage is small, and the material and manpower are saved.
3. According to the semi-wrapping stabilizing material, the core-wrapping slurry and the capsule are granulated by a simple and cheap one-step semi-wrapping method, the capsule can effectively prevent the reaction between the core and the iron compound and/or the manganese compound, and can slowly release the effective ingredients of the core, so that the semi-wrapping stabilizing material is easy to store and can continuously stabilize heavy metals in soil.
4. The raw materials adopted by the material preparation of the invention have wide sources and low price; and the preparation method is simple, the production period is short, and large-scale industrial production is easy to realize.
Drawings
FIG. 1 shows the effect of the application of a semi-wrapped stabilizing material prepared by different adhesive addition ratios on the stabilization effect of arsenic and cadmium in soil;
FIG. 2 shows the effect of application of semi-encapsulated stabilizing materials prepared from raw materials of different purities on the stabilization effect of arsenic and cadmium in soil;
FIG. 3 illustrates the stabilizing effect of a single cored material application on arsenic and cadmium in soil;
FIG. 4 is a graph of the cadmium stabilization effect on soil with a single application of encapsulating material;
FIG. 5 is a graph of the arsenic stabilization effect on soil with a single iron compound and/or manganese compound application;
FIG. 6 shows the effect of different semi-encapsulated stabilizing material applications on soil arsenic and cadmium stabilization;
FIG. 7 shows the effect of stabilizing arsenic and cadmium in semi-encapsulated stabilizing materials in soils with different water contents;
FIG. 8 shows the effect of stabilizing As and Cd in the semi-encapsulated stabilizing material at different curing times;
FIG. 9 shows the effect of semi-encapsulated stabilizing material application on soil arsenic and cadmium stabilization at different standing times.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
It should be noted that the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. Further, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
Semi-encapsulated stabilizing material and preparation method thereof
According to a first aspect of the invention, there is provided a method of preparing a semi-encapsulated stabilising material. According to the preparation method of the semi-wrapped stabilizing material, under the stirring condition, a semi-wrapped granulation method is adopted, salt and/or hydroxide core-wrapped slurry is dropwise added into silicate minerals, then a binder solution is added, and a core-wrapped-and-encapsulated structure is formed through granulation, wherein the core-wrapped proportion and the encapsulation proportion are proper, and the binder is added in a proper amount, so that the core-wrapped is prevented from being excessively wrapped, and the release and diffusion of effective components in soil are prevented from being influenced; the method that the wrapping material is matched with the iron compound and/or the manganese compound according to a certain proportion is adopted, so that the iron compound and/or the manganese compound and arsenic are fully stabilized, the core-spun material is slowly released and is combined with cadmium in soil, and the antagonism between arsenic and cadmium is effectively weakened. Therefore, the low-cost semi-wrapped stabilizing material has strong stabilizing capability on heavy metals with antagonism to arsenic, cadmium and the like, has stable performance, can be effective for a long time, and is easy to prepare, store and use.
According to an embodiment of the present invention, a method for preparing a stabilized material is explained, the method comprising:
s100 semi-wrapping granulation treatment
According to the embodiment of the invention, the salt and/or the hydroxide are prepared into slurry with the mass fraction of 30% to saturation; under the condition of stirring, dropwise adding the slurry into silicate minerals by using a liquid-transferring gun, and continuously stirring for 8-15 min; adding 0-2% of adhesive solution into the reactor, continuing stirring for 8-15min for granulation, and drying at 100-110 ℃ to obtain the wrapping material taking salt and/or hydroxide as the core and silicate mineral as the capsule. Therefore, the core-spun slurry and the capsule can be granulated by a simple and cheap one-step synthesis method, the capsule can effectively prevent the reaction between the core-spun and the iron compound and/or the manganese compound, and can slowly release the effective ingredients of the core-spun, thereby achieving the multiple purposes of simultaneously stabilizing arsenic and cadmium for a long time and being easy to store and use. Therefore, the prepared semi-wrapping stabilizing material is high in stabilizing rate, low in cost, easy to prepare and easy to regulate and control.
According to the examples of the present invention, the purity and composition of the raw materials used are not particularly limited, and may be adjusted by the production method as long as they have a good stabilizing effect on heavy metals. The inventor adopts the core-spun (salt and/or hydroxide), the capsule (silicate mineral) and the iron compound and/or the manganese compound which have simple components and low price as raw materials, and the adding proportion of the adhesive is 0-2%. Through single-factor experiments of the adhesive, as can be seen from fig. 1, the stabilization rates of arsenic and cadmium of the semi-wrapping stabilization material prepared by adding and not adding the adhesive are not greatly different. As shown in fig. 2, the semi-wrapped stabilized materials prepared by analyzing pure and industrial grade materials have little influence on the stabilization rate through a raw material purity comparison experiment. The preparation process utilizes the characteristic that silicate minerals are easy to be agglomerated when meeting water, and the silicate minerals can be prepared at normal temperature and normal pressure; the semi-wrapping method is adopted for granulation, and the release of the core-spun can be controlled by adjusting the proportion of silicate minerals. The salt is at least one of sodium salt, calcium salt and magnesium salt, specifically at least one of sodium carbonate, calcium carbonate and magnesium carbonate, and the hydroxide is at least one of sodium hydroxide, calcium hydroxide and magnesium hydroxide. According to a preferred embodiment of the invention, the salt and/or hydroxide is preferably calcium hydroxide. According to an embodiment of the present invention, the silicate mineral is at least one of sepiolite, bentonite, montmorillonite, kaolin, and zeolite, and according to a preferred embodiment of the present invention, the silicate mineral is zeolite. According to an embodiment of the invention, the mass ratio of the volume of the slurry to the silicate mineral is 1:4 to 4:1mL/g, according to a preferred embodiment of the invention, the volume to mass ratio is 1: 1 mL/g. According to an embodiment of the present invention, the binder is at least one of polyaluminium chloride, polyvinyl alcohol, carboxymethyl cellulose, starch, and according to a preferred embodiment of the present invention, the binder is polyaluminium chloride. According to an embodiment of the invention the binder is added in an amount of 0-2% by mass of the wrapping material, according to a preferred embodiment of the invention the binder is added in an amount of 0.3%. Therefore, semi-wrapping granulation can be completed at normal temperature in one step, the type and proportion of the core-wrapping capsule can be regulated and controlled, and the stabilization rate of heavy metal is high.
S200 proportion compatibility treatment
According to an embodiment of the invention, the wrapping material is compatible with an iron compound and/or a manganese compound in order to obtain said stabilizing material. Therefore, after compatibility treatment, the proportion of the wrapping material and the iron compound and/or the manganese compound is appropriate, heavy metals with antagonistic action such as arsenic, cadmium and the like can be stabilized, and the coating material is stable in performance, effective for a long time, easy to store and easy to use.
According to an embodiment of the present invention, the iron compound is at least one of polymeric ferric sulfate, ferrous sulfate heptahydrate, and anhydrous ferric chloride, and the manganese compound is at least one of anhydrous manganese chloride and manganese sulfate; according to a preferred embodiment of the invention, the iron compound and/or manganese compound is ferrous sulfate heptahydrate. According to an embodiment of the present invention, the ratio of the mass of the iron compound and/or manganese compound to the mass of the wrapping material in S4 is 1:4-4: according to a preferred embodiment of the invention, the mass ratio is 3.25: 1. therefore, for the soil with different heavy metal pollution degrees and pollution types, the compatibility method is convenient for regulating and controlling the types and the proportions of the core-spun materials, the capsule materials and the iron compounds and/or the manganese compounds, so that the stabilization effect of the semi-wrapped stabilization materials on the heavy metals is better.
According to an embodiment of the invention, the wrapping material is mixed with ferrous sulfate heptahydrate in a ratio of 1: 3.25 in order to obtain the stabilized material. Therefore, the wrapping material and the ferrous sulfate heptahydrate are suitable in compatibility proportion, and the semi-wrapping stabilizing material is favorable for fully stabilizing heavy metals such as arsenic, cadmium and the like in the soil.
On this basis, according to a second aspect of the invention, the invention provides a semi-wrapped stabilizing material. According to an embodiment of the invention, the semi-wrapping stabilizing material is prepared using the method described previously. Therefore, the stabilizing material has strong stabilizing capability on heavy metals with antagonism on arsenic, cadmium and the like, has stable performance, can be effective for a long time, and is easy to prepare, store and use.
According to an embodiment of the invention, the average particle size of the wrapping material is 2-6 mm. According to a preferred embodiment of the invention, the average particle size of the wrapping material is 2-4 mm. Therefore, the wrapping material has proper particle size, proper core-spun release rate, easy use and strong stabilization capability.
Method of using semi-wrapped stabilizing material
Further, according to a third aspect of the present invention, there is provided a method of using the aforementioned semi-encapsulated stabilizing material in the remediation of heavy metal pollution in soil. According to an embodiment of the invention, the method comprises: after soil is screened and naturally dried, applying a certain amount of semi-wrapped stabilizing material to the polluted soil; uniformly mixing, and ensuring certain soil moisture content when in application; after maintaining for several days, sampling again to perform leaching toxicity test, and measuring the stabilization rate.
According to the embodiment of the invention, the heavy metal pollution is composite pollution of acid heavy metal such as arsenic and cationic heavy metal such as cadmium. The semi-wrapping stabilizing material disclosed by the embodiment of the invention has a good stabilizing effect on the acid radical heavy metal and the cation heavy metal in the soil environment, and can be effectively applied to stabilizing treatment of heavy metal pollutants in the soil.
According to the using method of the embodiment of the invention, the stabilizing material is granulated by half-wrapping sodium-calcium-magnesium salt or hydroxide, and meanwhile, the stabilizing capability of the stabilizing material on heavy metal composite pollution such as arsenic and cadmium is remarkably improved by a method of proportionally combining iron compounds and/or manganese compounds, the stabilizing rate can be stable for a long time, and the stabilizing material is easy to store, use and low in cost.
According to the embodiment of the invention, the mass ratio of the semi-coating stabilizing material to the soil is 1: 100-3: 100, according to a preferred embodiment of the invention, the ratio by mass of the semi-wrapping stabilizing material to the soil is 2: 100. therefore, the addition amount of the semi-wrapping stabilizing material is appropriate, and the effects of not wasting the stabilizing material and achieving higher stabilizing rate can be achieved.
According to an embodiment of the present invention, the soil has a water content of 10 to 30%, and according to a preferred embodiment of the present invention, the soil has a water content of 20%. Therefore, the diffusion and release rates of the iron compound and/or the manganese compound of the semi-coated stabilizing material and the core-spun core are appropriate, the iron compound and/or the manganese compound can be fully combined with acid radical state and cation state heavy metals such as arsenic, cadmium and the like in the polluted soil, and the stabilizing and repairing efficiency is high.
According to an embodiment of the invention, the curing time is 1-3 days, according to a preferred embodiment of the invention, the curing time is 1 day. Therefore, the utility of the semi-wrapped stabilizing material can be fully utilized, the engineering period (maintenance time) is short, and the engineering cost can be effectively saved.
The present invention is described below with reference to specific examples, which are intended to be illustrative only and are not to be construed as limiting the invention.
The scheme of the invention will be explained with reference to the examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or apparatus used are conventional products which are commercially available, e.g. from Sigma, without reference to the manufacturer.
Example 1 preparation of a semi-wrapped stabilizing Material (S1)
(1) Preparing calcium carbonate into slurry with the mass fraction of 30%; under the condition of stirring, dropwise adding the calcium carbonate into the sepiolite by using a liquid-transferring gun, and ensuring that the mass ratio of the calcium carbonate to the sepiolite is 4:1, continuously stirring for 10 min;
(2) adding 2% polyvinyl alcohol solution accounting for 0.5% of the total mass of the powder in the step (1), continuing stirring for 10min for granulation, and drying at 105 ℃ for 5 hours to obtain a wrapping material taking calcium carbonate as a core and sepiolite as a capsule;
(3) mixing the wrapping material in the step (2) with an iron compound and/or a manganese compound (polymeric ferric sulfate and manganese sulfate) according to the ratio of 1: 3, so as to obtain the semi-wrapped stabilizing material.
Example 2 preparation of a semi-wrapped stabilizing Material (S2)
(1) Preparing slurry with the mass fraction of 40% by using calcium hydroxide and magnesium hydroxide; under the condition of stirring, dropwise adding the montmorillonite powder into a liquid-transfering gun, and ensuring that the mass ratio of calcium hydroxide, magnesium hydroxide and montmorillonite is 1: 3, continuing stirring for 10 min;
(2) adding a 2% polyaluminium chloride solution accounting for 1.5% of the total mass of the powder in the step (1), continuously stirring for 10min for granulation, and drying at 105 ℃ to obtain a wrapping material taking calcium hydroxide and magnesium hydroxide as a core and montmorillonite as an encapsulation;
(3) mixing the wrapping material in the step (2) with ferrous sulfate heptahydrate according to the weight ratio of 2:1, so as to obtain the semi-wrapped stabilizing material.
Example 3 preparation of a semi-wrapped stabilizing Material (S3)
(1) Preparing 30% slurry of calcium carbonate and sodium carbonate; under the condition of stirring, dropwise adding the calcium carbonate and sodium carbonate into zeolite and bentonite by using a liquid-transfering gun, and ensuring that the ratio of the mass sum of the calcium carbonate and the sodium carbonate to the mass sum of the zeolite and the bentonite is 3: 1, continuously stirring for 10 min;
(2) adding a 2% carboxymethyl cellulose solution accounting for 1% of the total mass of the powder into the powder obtained in the step (1), continuously stirring for 10min for granulation, and drying at 105 ℃ to obtain a wrapping material which takes calcium carbonate and sodium carbonate as core-wrapping materials and takes zeolite and bentonite as encapsulation materials;
(3) mixing the wrapping material in the step (2) with an iron compound and/or a manganese compound (anhydrous ferric chloride and manganese chloride) according to the ratio of 1: 1, so as to obtain the semi-wrapped stabilizing material.
Example 4 preparation of a semi-wrapped stabilizing Material (S4)
(1) Preparing calcium hydroxide into slurry with the mass fraction of 40%; dropwise adding the calcium hydroxide into the zeolite by using a liquid-transferring gun under the condition of stirring, and ensuring that the mass ratio of the calcium hydroxide to the zeolite is 1: 1, continuously stirring for 10 min;
(2) adding a 2% polyaluminium chloride solution accounting for 0.3% of the total mass of the powder in the step (1), continuously stirring for 10min for granulation, and drying at 105 ℃ to obtain a wrapping material taking calcium hydroxide as a core and zeolite as an encapsulation;
(3) mixing the wrapping material in the step (2) with ferrous sulfate heptahydrate according to the weight ratio of 1: 3.25 in order to obtain a semi-wrapped stabilized material.
Example 5 preparation of a semi-wrapped stabilizing Material (S5)
(1) Preparing 30% slurry of calcium carbonate and sodium hydroxide; under the condition of stirring, dropwise adding the calcium carbonate and sodium hydroxide into sepiolite and montmorillonite by using a liquid-transferring gun, and ensuring that the mass ratio of the calcium carbonate and the sodium hydroxide to the sepiolite and the montmorillonite is 1:2, continuing stirring for 10 min;
(2) adding 2% polyvinyl alcohol solution accounting for 0.8% of the total mass of the powder in the step (1), continuing stirring for 10min for granulation, and drying at 105 ℃ to obtain a wrapping material taking calcium carbonate and sodium hydroxide as core-wrapping materials and taking sepiolite and montmorillonite as encapsulation materials;
(3) mixing the wrapping material in the step (2) with manganese-containing compounds (manganese chloride and manganese sulfate) according to the ratio of 1: 1.5, so as to obtain the semi-wrapping stabilizing material.
Example 6 preparation of a semi-wrapped stabilizing Material (S6)
(1) Preparing 30% slurry of calcium hydroxide and calcium carbonate; under the condition of stirring, dropwise adding the calcium hydroxide and the calcium carbonate into the montmorillonite and the zeolite by using a liquid-transfering gun, and ensuring that the mass ratio of the calcium hydroxide to the calcium carbonate to the montmorillonite to the zeolite is 2:1, continuously stirring for 10 min;
(2) adding a 2% polyaluminium chloride solution accounting for 0.5% of the total mass of the powder in the step (1), continuously stirring for 10min for granulation, and drying at 105 ℃ to obtain a wrapping material taking calcium hydroxide and calcium carbonate as core-wrapping materials and montmorillonite and zeolite as encapsulation materials;
(3) mixing the wrapping material in the step (2) with ferrous sulfate heptahydrate according to the weight ratio of 2: 3, so as to obtain the semi-wrapped stabilizing material.
Example 7 soil stabilization Effect of Single core, Capsule and iron and/or manganese Compounds
The soil of the test field is collected from an arsenic-cadmium composite pollution field in the east China ditch basin of Baiyin City of Gansu province, the sampling depth is 0-20cm, the soil is naturally dried, and then is sieved by a 10-mesh sieve, and the soil is repeatedly mixed for later use. The basic properties of the soil are shown in table 1. According to the mass ratio of the polluted soil to the salt and/or hydroxide core-spun material/silicate mineral encapsulation material/iron compound and/or manganese compound of 100: 1. 100, and (2) a step of: 3. 100, and (2) a step of: 1, the water content of the soil is 20% when the stabilizing agent is applied, the soil is uniformly mixed and then is put into a self-sealing bag, after 1 day of maintenance, a proper amount of soil is weighed, deionized water lixiviant is added according to the water content of the soil according to the liquid-solid ratio of 10:1 (L: kg), the mixture is placed in a horizontal oscillator oscillation device, the mixture is taken out after 8 hours of oscillation at room temperature, the mixture is kept still for 16 hours, the mixture passes through a 0.45 mu m filter membrane, the lixivium is collected, the concentrations of arsenic and cadmium in the lixivium are measured by inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and then. The control group was field soil (CK) without added core, capsule and iron and/or manganese compounds, with three replicates per treatment set up.
TABLE 1 basic physicochemical Properties of the soil tested
As shown in fig. 3, 4 and 5, after applying the core-spun materials such As sodium hydroxide, sodium carbonate, calcium hydroxide, calcium carbonate, magnesium hydroxide and the like, the stabilization rates of cadmium in the soil are respectively 99.2%, 94.7%, 99.0%, 6.2% and 89.9%, and the stabilization rates of As in the soil are respectively 37.4%, -18.5%, 78.7%, 1.1% and 34.2%; after applying encapsulating materials such as sepiolite, bentonite, montmorillonite, kaolin, zeolite and the like, the stabilization rates of the soil cadmium are respectively 38.6%, 40.8%, 64.4%, 20.8% and 68.3%; after iron compounds and/or manganese compounds such as polymeric ferric sulfate, ferrous sulfate heptahydrate, anhydrous ferric chloride, anhydrous manganese chloride, manganese sulfate and the like are/is applied, the stabilization rates of the arsenic in the soil are respectively 98.7%, 97.2%, 96.7%, 64.2% and 72.1%. Therefore, in the core-spun material, calcium hydroxide has a good stabilizing effect on cadmium and a good stabilizing effect on arsenic, and is low in price; among the encapsulation materials, zeolite has the best effect of stabilizing cadmium; in the iron compound and/or the manganese compound, the polymeric ferric sulfate has the best stabilizing effect on arsenic, but the price is higher, so the invention finally selects the cheaper ferrous sulfate heptahydrate.
Example 8 soil stabilization Effect experiment and results of semi-wrapping stabilization Material
According to the mass ratio of the contaminated soil (contaminated soil used in example 7) to the common compound material (FP, the same as the corresponding semi-encapsulated stabilizing material S4 in terms of component ratio, but only mixed without any treatment)/the semi-encapsulated stabilizing material (S1, S2, S3, S4, S5, S6) is 100: 2. 100, and (2) a step of: 1.5, 100: 1. 100, and (2) a step of: 2. 100, and (2) a step of: 2. 100, and (2) a step of: 2. 100, and (2) a step of: 1, the water content of soil is respectively 20%, 10%, 30%, 15%, 20%, 15% and 10% when the stabilizing agent is applied, the soil is uniformly mixed and then is put into a self-sealing bag, the self-sealing bag is respectively maintained for 1 day, 3 days, 2 days, 1 day, 2 days and 1 day, then a proper amount of soil is weighed, deionized water lixiviant is added according to the water content of the soil according to the liquid-solid ratio of 10:1 (L: kg), the mixture is placed in a horizontal oscillator oscillation device, the mixture is taken out after oscillation for 8 hours at room temperature, the mixture is kept still for 16 hours and is filtered through a 0.45 mu m filter membrane, the lixivium is collected, and the concentrations of arsenic and cadmium in the lixivium are measured by inductively coupled plasma-atomic emission spectroscopy (ICP. The control group was field soil (CK) without the addition of the normal compound material and the semi-encapsulated stabilization material, with three replicates per treatment set.
As shown in fig. 6, the common compound material only has a certain stabilizing effect on arsenic in soil, has a side effect on cadmium stabilization, and can increase the leaching concentration of cadmium in soil; compared with the control, the soil cadmium stabilization rate is-139.8% and the soil arsenic stabilization rate is 91.1% after the common compound material is applied. After the semi-wrapping stabilizing material prepared by the invention is applied, the leaching concentrations of arsenic and cadmium in soil can be obviously reduced. The stabilization rates of arsenic in the soil after application of the semi-wrapped stabilization materials prepared in examples 1-6 were 88.9%, 76.1%, 79.5%, 95.5%, 80.2%, and 80.3%, respectively, compared to control; the soil cadmium stabilization rates are 99.0%, 99.3%, 99.2%, 94.6%, 98.8% and 98.2%, respectively. Therefore, compared with the common compound material, the semi-wrapped stabilizing material prepared by the invention can effectively stabilize arsenic and cadmium in soil at the same time; among them, the semi-coated stabilizing material prepared in example 4 is most effective in stabilizing heavy metals arsenic and cadmium in soil.
Example 9 Effect of soil moisture content on stabilization Effect of semi-wrapped stabilization Material
According to the mass ratio of the contaminated soil (the contaminated soil used in example 7) to the semi-wrapped stabilizing material (S4) of 100: 2, uniformly mixing the soil with the water content of 10%, 15%, 20%, 25% and 30%, putting the mixture into a self-sealing bag, curing for 1 day, weighing a proper amount of soil, adding a deionized water leaching agent according to the water content of the soil and the liquid-solid ratio of 10:1 (L: kg), putting the mixture into a horizontal oscillator oscillation device, oscillating at room temperature for 8 hours, taking out, standing for 16 hours, filtering through a 0.45 mu m filter membrane, collecting the leachate, and measuring the concentrations of arsenic and cadmium in the leachate by using inductively coupled plasma-atomic emission spectroscopy (ICP-AES) so as to calculate the stabilization rate. The control group was field soil (CK) without added semi-encapsulated stabilizing material, with three replicates per treatment set up.
As shown in fig. 7, when the soil moisture content was 10%, 15%, 20%, 25%, and 30% after applying the semi-wrapped stabilizing material, the stabilizing rates of arsenic in the soil were 95.8%, 95.0%, 95.5%, 96.7%, and 96.1%, respectively, as compared with the control; the stabilization rates of the soil cadmium are 66.8%, 92.5%, 94.6%, 91.2% and 85.8% respectively. Therefore, when the water content of the soil is 20%, the effect of stabilizing arsenic and cadmium in the soil is the best.
Example 10 curing time Effect on stabilizing Effect of semi-wrapped stabilizing Material
According to the mass ratio of the contaminated soil (the contaminated soil used in example 7) to the semi-wrapped stabilizing material (S4) of 100: 2, the soil moisture content is respectively 20% when the stabilizing agent is applied, the soil is uniformly mixed and then is put into a self-sealing bag, the self-sealing bag is maintained for 2 hours, 4 hours, 6 hours, 16 hours, 20 hours, 24 hours, 48 hours and 72 hours, then a proper amount of soil is weighed, deionized water lixiviant is added according to the water content of the soil and the liquid-solid ratio of 10:1 (L: kg), the mixture is placed in a horizontal oscillator oscillation device, is oscillated for 8 hours at room temperature and then is taken out, the mixture is kept stand for 16 hours, is filtered through a 0.45 mu m filter membrane, leachate is collected, and the concentrations of arsenic and cadmium in the leachate are measured by inductively coupled plasma-atomic emission spectroscopy (ICP-AES), so that the stabilizing rate. The control group was field soil (CK) without added semi-encapsulated stabilizing material, with three replicates per treatment set up.
As shown in fig. 8, when compared with the control, the stabilization rates of the soil arsenic were 94.2%, 94.8%, 95.1%, 95.3%, 95.5%, 95.8%, 96.1%, and 96.2% after applying the semi-wrapped stabilization material and curing for 2h, 4h, 6h, 16h, 20h, 24h, 48h, and 72h, respectively; the soil cadmium stabilization rates are 89.1%, 92.1%, 93.0%, 93.8%, 94.3%, 94.7%, 94.9% and 95.0%, respectively. Therefore, when the curing time is 1 day (24 hours), the effect of stabilizing arsenic and cadmium in the soil is the best.
Example 11 Long-term effectiveness test and results of semi-wrapping stabilizing Material
The mass ratio of the contaminated soil (the contaminated soil used in example 7) to the S4 semi-wrapped stabilizing material placed for 0 day, 3 days, 7 days, 15 days, 30 days and 60 days is respectively 100: 2, the water content of the soil is respectively 20% when the stabilizing agent is applied, the soil is uniformly mixed and then is filled into a self-sealing bag, a proper amount of soil is weighed after 1 day of maintenance, deionized water lixiviant is added according to the water content of the soil according to the liquid-solid ratio of 10:1 (L: kg), the mixture is placed in a horizontal oscillator oscillation device, the mixture is taken out after 8 hours of oscillation at room temperature, the mixture is kept still for 16 hours and passes through a 0.45 mu m filter membrane, leachate is collected, the concentrations of arsenic and cadmium in the leachate are measured by inductively coupled plasma-atomic emission spectroscopy (ICP-AES), and then the stabilization rate is calculated. The control group was field soil (CK) supplemented with common compounded materials, with three replicates per treatment set.
As shown in fig. 9, after applying the common compound materials with the standing time of 0 day, 3 days, 10 days, 30 days, 60 days, 180 days and 365 days, the stabilization rates of the arsenic in the soil are respectively 91.1%, 90.9%, 90.2%, 89.5%, 88.7%, 88.3% and 87.1%; the stabilizing rate of the soil cadmium is-139.9, -239.4, -278.3, -304.4, -312.2, -336.5 and-340.6 respectively; after the ordinary compound material is placed for 365 days, the stabilizing rate of the common compound material to arsenic and cadmium is reduced by 4.4 percent and 143.4 percent; compared with the control, after the semi-wrapped stabilizing material with the standing time of 0 day, 3 days, 10 days, 30 days, 60 days, 180 days and 365 days is applied, the stabilizing rate of the arsenic in the soil is respectively 95.6%, 95.1%, 94.9%, 95.3%, 95.0%, 94.3% and 92.1%; the stabilization rates of the cadmium in the soil are respectively 94.5%, 94.3%, 94.1%, 94.2%, 93.9%, 92.6% and 90.2%; after the semi-wrapping stabilizing material is placed for 365 days, the stabilizing rate of the semi-wrapping stabilizing material to arsenic and cadmium is reduced by only 3.7 percent and 4.6 percent. Therefore, the semi-wrapped stabilizing material prepared by the preparation method disclosed by the invention effectively solves the problem of mutual reaction among the components of the common compound material, can keep effectiveness for a long time, and can keep higher stabilizing rate after being placed for 1 year (365 days).
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (17)
1. A preparation method of a semi-wrapped stabilizing material aiming at arsenic-cadmium acid radical state and cation state heavy metal composite pollution is characterized by comprising the following steps:
s1, preparing a salt and/or a hydroxide into a slurry, wherein the salt is at least one of a calcium salt and a magnesium salt;
s2, stirring the silicate mineral, adding the slurry into the silicate mineral, and uniformly stirring to obtain a mixture of the slurry and the silicate mineral;
s3, granulating and drying the mixture of the slurry and the silicate mineral to obtain a wrapping material;
s4, adding an iron compound or an iron and manganese compound, and mixing with the wrapping material to obtain a semi-wrapping stabilizing material;
in S2, under the condition of stirring, a semi-wrapping granulation method is adopted to dropwise add the salt and/or hydroxide core-spun slurry into the silicate mineral;
the mass fraction of the slurry in S2 is more than or equal to 30%, and the mass ratio of the volume of the slurry to the silicate mineral is 1: 1 mL/g;
the salt is at least one of calcium carbonate and magnesium carbonate, and the hydroxide is at least one of calcium hydroxide and magnesium hydroxide;
s3, adding a binder solution into the mixture of the slurry and the silicate mineral, uniformly stirring, granulating and drying;
the added mass of the adhesive is 0.25-2% of the mass of the mixture of the slurry and the silicate mineral;
the mass fraction of the adhesive in the adhesive solution in the S3 is 1-3%;
the manganese compound in S4 is at least one of anhydrous manganese chloride and manganese sulfate;
the iron compound is at least one of polymeric ferric sulfate, ferrous sulfate heptahydrate and anhydrous ferric chloride;
the ratio of the mass of the iron compound or the iron and manganese compounds to the mass of the wrapping material in S4 is 1:4-4: 1.
2. the method according to claim 1, characterized in that the mass of the binder addition is 0.3% of the mass of the mixture of slurry and silicate mineral;
the mass fraction of the binder in the binder solution in S3 is 2%;
the stirring time in S3 is 8-15min, and the drying temperature is 100-110 ℃.
3. The method according to claim 1, wherein the slurry in S2 is added dropwise to the silicate mineral;
and in S2, adding the slurry into the silicate mineral, and stirring for 8-15 min.
4. The method of claim 1, wherein the silicate mineral is at least one of sepiolite, bentonite, montmorillonite, kaolin, and zeolite.
5. The method according to claim 1, characterized in that the silicate mineral is a zeolite.
6. The method of claim 1, wherein the hydroxide is calcium hydroxide.
7. The method of claim 1, wherein the binder is at least one of polyaluminum chloride, polyvinyl alcohol, carboxymethyl cellulose, starch.
8. The method of claim 1, wherein the binder is a polyaluminum chloride.
9. The method of claim 1, wherein the iron compound or iron and manganese compound is ferrous sulfate heptahydrate;
the ratio of the mass of the iron compound or iron and manganese compounds to the mass of the wrapping material in S4 is 3.25: 1.
10. a semi-encapsulated stabilizing material, wherein said semi-encapsulated stabilizing material is prepared by the method of any one of claims 1 to 9.
11. The semi-wrapped stabilizing material of claim 10, wherein said wrapping material has an average particle size of 2-6 mm.
12. The semi-wrapped stabilizing material of claim 10, wherein said wrapping material has an average particle size of 2-4 mm.
13. A method of using a semi-wrapped stabilising material according to any one of claims 10 to 12, comprising the steps of:
after the soil is screened and naturally dried, applying a semi-wrapped stabilizing material to the soil, and uniformly mixing, wherein the mass ratio of the semi-wrapped stabilizing material to the soil is 1: 100-3: 100, when the soil is applied, the water content of the soil is 10-30%, and the soil is maintained for 1-3 days.
14. The method of claim 13, wherein the semi-encapsulated stabilizing material to soil mass ratio is 2: 100-3: 100, respectively;
the water content of the soil is 20-30%;
the curing time is 1-2 days.
15. The method of claim 13, wherein the semi-encapsulated stabilizing material to soil mass ratio is 2: 100.
16. the method of claim 13, wherein the soil moisture content is 20%.
17. The method of claim 13, wherein the curing time is 1 day.
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