CN113736472B - Sustained-release arsenic fixing agent, preparation method thereof and application thereof in arsenic-polluted soil remediation - Google Patents
Sustained-release arsenic fixing agent, preparation method thereof and application thereof in arsenic-polluted soil remediation Download PDFInfo
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Abstract
The invention discloses a slow-release arsenic fixing agent, a preparation method thereof and application thereof in arsenic-polluted soil remediation. Adding vanillin into acetic acid solution dissolved with chitosan to perform condensation reaction to obtain vanillin modified chitosan; mixing fly ash with kaolin, and roasting to obtain an adsorption material; mixing an adsorption material with calcium sulfide powder and red mud powder, and performing oscillation treatment to obtain an arsenic fixing agent; and mixing the arsenic fixing agent with vanillin modified chitosan, performing hot melting treatment, cooling, and granulating to obtain the slow-release arsenic fixing agent. The slow-release arsenic fixing agent can realize efficient fixation of arsenic in the polluted soil in the modes of adsorption, chemical reaction and the like, the arsenic leaching toxicity of the repaired arsenic polluted soil reaches the GB 14848-2017 III standard, and the slow-release arsenic fixing agent can slowly release active substances for fixing the arsenic, so that the arsenic fixing effect on the soil is durable and long-term effective.
Description
Technical Field
The invention relates to an arsenic fixing agent, in particular to a slow-release arsenic fixing agent, a preparation method thereof and application of the slow-release arsenic fixing agent in arsenic-polluted soil restoration, and belongs to the technical field of arsenic-polluted soil restoration.
Background
In recent years, the industrialization and the urban industry of China are continuously advanced, and the soil pollution problem is increasingly serious. Soil is one of the important natural resources that humans depend on to survive, and is also an important component of the human ecological environment. Along with the aggravation of industrial and urban pollution, pollutants containing heavy metals enter the soil through various ways, so that the enrichment of corresponding heavy metal elements in the soil is caused. The heavy metal pollution has the characteristics of concealment, long-term property and irreversibility. The heavy metal pollution prevention and control work has become the important point of the environmental protection work in China. Arsenic is widely used in many industries, and is largely remained in soil through processes of exploitation, processing, use, discarding and the like, so that arsenic pollution in the soil worldwide is ubiquitous.
The method mainly comprises an engineering physicochemical method and a biological repair method for repairing the heavy metal contaminated soil. The engineering physical and chemical methods comprise a soil-filling method, a washing complexing method, an electric chemical method, a heat treatment method and the like, and are not suitable for soil with larger pollution area. Bioremediation methods include phytoremediation, microbial remediation, animal remediation, and the like, and the effects of plant and lower animal remediation methods on soil remediation are not significant; the microorganism repairing utilizes certain microorganisms in the soil to have the functions of absorbing, precipitating, oxidizing, reducing and the like on heavy metals, so that the toxicity of the heavy metals in the soil is reduced. The technology has small influence on the surrounding environment, does not produce secondary pollution, and has huge soil restoration potential. However, the existing microorganism restoration technology for heavy metal contaminated soil has certain limitations, such as long microorganism restoration duration, slow effect, general formation of complex to reduce the harm of heavy metal, and incapability of removing heavy metal from soil.
The Chinese patent literature discloses a preparation and use method (CN 201610071104.0) of a slow-release type iron-based biochar soil heavy metal passivator, which adopts iron-based biochar, kaolin and biological starch as core materials, takes an acidic silica sol and chitosan solution composite material as an envelope, and prepares the core materials and films into the passivator suitable for farmland treatment of cadmium and arsenic combined pollution. The passivating agent prepared by the method can simultaneously passivate cadmium and arsenic, has a slow release effect, and can be effective on heavy metals for a long time. However, the passivating agent is mainly suitable for paddy fields, and the pollution degree of heavy metals such as arsenic in the soil of paddy fields is mostly low, and the passivating effect on other polluted sites is unknown.
The Chinese patent literature discloses a repairing agent, a preparation method thereof and a method for repairing heavy metal contaminated soil (CN 201711076050.8) by using the repairing agent, wherein the repairing agent is prepared from biochar, sepiolite, monocalcium phosphate, bagasse, lime powder, eyelid, tartaric acid, hydroxyethylidene triphosphonic acid, potassium lignosulfonate, malic acid, chitosan and bean root straw as raw materials, and can synchronously remove mercury, cadmium, lead, arsenic and pyrene in the contaminated soil. However, the raw material components required by the production of the repairing agent are complex, the sources are not easy to obtain, and the industrial production is difficult to realize.
Disclosure of Invention
Aiming at the prior art, the first aim of the invention is to provide a slow-release arsenic fixing agent for repairing arsenic-polluted soil, which can realize the efficient fixation of arsenic in the polluted soil in the modes of adsorption, chemical reaction and the like, the arsenic leaching toxicity in the repaired polluted soil reaches the grade III standard of groundwater quality standard (GB 14848-2017), and the slow-release arsenic fixing agent can slowly release active substances for fixing arsenic, so that the arsenic fixing effect in the soil is durable and long-term effective.
The second aim of the invention is to provide a preparation method of the slow-release arsenic fixing agent for arsenic-polluted soil, which is simple, has low raw material cost and is beneficial to mass production.
The invention aims to provide the application of the slow-release arsenic fixing agent in the aspect of repairing the arsenic-polluted soil, and the slow-release arsenic fixing agent is added into the arsenic-polluted soil to slowly release active ingredients acting on arsenic, so that the long-term effectiveness of the arsenic fixing effect in the soil can be ensured, meanwhile, the utilization rate of the arsenic fixing agent is improved, the problems of agglomeration and low utilization rate caused by one-time release of the arsenic fixing agent are avoided, and the arsenic leaching toxicity in the repaired arsenic-polluted soil reaches the III class standard of the quality standard of groundwater (GB 14848-2017).
In order to achieve the technical aim, the invention provides a preparation method of a slow-release arsenic fixing agent, which comprises the following steps:
1) Adding vanillin into acetic acid solution dissolved with chitosan to perform condensation reaction to obtain vanillin modified chitosan;
2) Mixing fly ash with kaolin, and roasting to obtain an adsorption material;
3) Mixing an adsorption material with calcium sulfide powder and red mud powder, and performing oscillation treatment to obtain an arsenic fixing agent;
4) And mixing the arsenic fixing agent with vanillin modified chitosan, performing hot melting treatment, cooling, and granulating to obtain the slow-release arsenic fixing agent.
As a preferable scheme, the vanillin is 50% -100% of the chitosan. The vanillin mainly utilizes the condensation of aldehyde groups and amino groups in chitosan to modify a large amount of phenolic hydroxyl groups in the chitosan, and the ortho positions of the phenolic hydroxyl groups in the vanillin contain methoxy groups, so that the vanillin has higher capacity of coordinating and adsorbing arsenic ions compared with common hydroxyl groups or phenolic hydroxyl groups, and the capacity of adsorbing arsenic ions of the chitosan can be improved by utilizing the vanillin to modify the chitosan. If the dosage of vanillin is too low, the modified vanillin on the chitosan is too low to achieve the modification effect, and if the dosage of vanillin is too high, the modified vanillin cannot be further improved due to the limited number of active amino groups of the chitosan.
As a preferred embodiment, the condensation reaction conditions are: the temperature is 50-80 ℃ and the time is 0.5-2 h.
As a preferable scheme, the mass ratio of the fly ash to the kaolin is 50-70:30-50. The fly ash is a product obtained after combustion of coal, has a porous structure, has a good adsorption effect on arsenic, and the kaolin is a layered silicate mineral, has good adsorption performance, has good water retention performance, and has higher adsorption activity after being matched according to a proper proportion and subjected to high-temperature activation treatment, so that a solid adsorption material with good adsorption performance on arsenic can be obtained. And the fly ash and the kaolin are easy to obtain raw materials, particularly the fly ash has a certain harm to the environment, and the fly ash is used as a raw material for producing the arsenic fixing agent, thereby being beneficial to recycling resources. If the proportion of kaolin is too high, the arsenic adsorption performance of the adsorption material is reduced, and too low can easily cause larger loss of water in the soil, cause local caking, and reduce the effective contact between the medicament and the polluted soil.
As a preferable embodiment, the conditions of the baking treatment are as follows: the temperature is 600-800 ℃ and the time is 1-4 h. If the temperature is too low, it is difficult to fully activate the fly ash and kaolin, and if the temperature is too high, energy waste is caused.
As a preferable scheme, the mass ratio of the adsorption material to the calcium sulfide powder to the red mud powder is 5-20:1-5:75-94. The calcium sulfide powder can provide active sulfur ions to form stable sulfide with arsenic, the red mud has iron with higher content, the iron can react with the arsenic to generate low-mobility ferric arsenate, the three are combined according to a proper proportion, the organic combination of physical adsorption and chemical reaction fixation of the arsenic can be realized, and particularly, the porous structure of the adsorption material can contain active components acting on the arsenic, such as the calcium sulfide powder, the red mud powder and the like, and the slow release effect can be realized. The red mud is used as industrial solid waste, the emission amount is huge, the pollution to the environment is more and more serious, the red mud is utilized in a recycling way to the greatest extent, the slow-release arsenic fixing agent adopts the red mud as the raw material, and the environment risk is reduced while the treatment of waste by waste is realized.
As a preferable embodiment, the condition of the oscillation treatment is as follows: the oscillating frequency is 300-400 rpm and the time is 1-2 h. The high-frequency oscillation can mix materials more uniformly, and simultaneously realizes that active ingredients such as calcium sulfide powder and red mud powder which can act with arsenic enter gaps of the adsorption material, thereby being beneficial to improving the slow release effect.
As a preferable scheme, the mass ratio of the arsenic fixing agent to the lan modified chitosan is 85-95:5-15. When the dosage of the lan modified chitosan is too low, the adhesion molding is difficult, and the slow release effect cannot be realized, and when the dosage is too high, the arsenic fixing agent is difficult to release effectively.
The acetic acid solution dissolved with chitosan is prepared from chitosan and acetic acid solution with pH value of 5-7 according to a liquid-solid ratio of 10-20 mL:1g of the mixture. The acetic acid solution serves as a cosolvent for dissolving chitosan on the one hand and serves as a catalyst for the condensation reaction on the other hand.
The adsorption material is ground to 50-100 meshes.
The red mud powder is obtained by drying red mud at the temperature of 95-105 ℃ and grinding the dried red mud to 200-400 meshes.
The particle size of the slow-release arsenic fixing agent is 3-5 mm.
The invention also provides a preparation method of the slow-release arsenic fixing agent for arsenic-polluted soil, which is obtained by the preparation method. The slow-release arsenic fixing agent provided by the invention is prepared by compositing vanillin modified chitosan with an adsorption material, calcium sulfide powder and red mud powder, wherein the vanillin modified chitosan is used as a good adhesive, the particles can be wrapped, adhered and formed to form a particle material, meanwhile, the vanillin modified chitosan contains a large number of polar groups, particularly, a large number of phenolic hydroxyl groups are modified after being modified by vanillin, the vanillin modified chitosan can produce chelating adsorption effect with arsenic ions, the calcium sulfide powder and the red mud powder contain active iron ions and active sulfur anions, the arsenic ions can be acted through chemical reaction and the like, the adsorption material is a roasting product of fly ash and kaolin, is a porous structure material, has strong adsorption capacity, and after the components are compounded, the vanillin modified chitosan can chelate, adsorb and enrich the free arsenic ions in the soil, and slowly dissolve the vanillin modified chitosan with the vanillin, the calcium sulfide and the adsorption material release the calcium sulfide ions, the arsenic ions can be converted into insoluble arsenic ions, the insoluble arsenic ions can be adsorbed by the red mud, and the insoluble arsenic ions can be greatly absorbed by the adsorption material, and the insoluble arsenic ions can be greatly absorbed by the arsenic-containing the insoluble arsenic ions.
The invention also provides application of the slow-release arsenic fixing agent in repairing arsenic-polluted soil.
Compared with the prior art, the technical scheme of the invention has the beneficial technical effects that:
(1) The slow-release arsenic fixing agent provided by the invention is used for repairing arsenic-polluted soil, the arsenic leaching toxicity reaches the III class standard of groundwater quality standard (GB 14848-2017), and the arsenic leaching toxicity of the repaired arsenic-polluted soil is less than 1mg/L.
(2) The slow-release arsenic fixing agent provided by the invention adopts solid wastes such as red mud, fly ash and the like as raw materials, has low cost, realizes resource utilization, and achieves the purpose of treating wastes with the wastes.
(3) The slow-release arsenic fixing agent provided by the invention has a slow-release effect, can slowly release the arsenic fixing agent in a soil environment, can ensure that the arsenic fixing agent has long-term effectiveness on arsenic in soil, and simultaneously, the slow release of the arsenic fixing agent effectively prevents caking and agglomeration caused by one-time addition of the arsenic fixing agent, and effectively improves the use efficiency of the arsenic fixing agent.
(4) The slow-release arsenic fixing agent for arsenic-polluted soil has the advantages of simple production process, no secondary pollution and the like, and is easy to realize industrialized application.
Drawings
FIG. 1 is a flow chart of a process for preparing a slow-release arsenic fixing agent for arsenic-contaminated soil according to the present invention.
Detailed Description
The present invention will be described in further detail below with reference to the attached drawings and specific examples, which are given by way of illustration and explanation only, and should not be construed to limit the scope of the present invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
The instruments, reagents, etc. used in the examples below are available by conventional commercial means unless otherwise indicated.
Example 1
(1) Chitosan was placed in a container at a liquid-to-solid ratio of 10mL:1g of glacial acetic acid solution with pH of 6 is added, stirring is started, heating and maintaining the temperature at 60 ℃, and vanillin with 60% of the mass of chitosan is added while stirring. Stirring at constant temperature for reaction for 0.5h, filtering while the reaction is hot, flushing filter residues with distilled water, transferring into a constant-temperature oven, and drying at 80 ℃ to constant weight to obtain vanillin modified chitosan.
(2) 60 parts of fly ash and 40 parts of kaolin are mixed and then baked for 4 hours at 600 ℃, and then ground to 50 meshes, so that the high-activity adsorption material is prepared.
(3) Drying the red mud at 95 ℃ and grinding the red mud to 200 meshes.
(4) 10 parts of high-activity adsorption material, 3 parts of calcium sulfide powder and 87 parts of red mud powder are mixed and then are vibrated on a shaking table for 2 hours, and the vibration frequency is 300rpm.
(5) Adding 6 parts of vanillin modified chitosan into the fixing agent prepared in the step (4), stirring and heating to a molten state, continuously stirring for 1h, and cooling to prepare particles with the particle size of 3 mm.
Example 2
(1) Chitosan was placed in a container at a liquid-to-solid ratio of 20mL:1g of glacial acetic acid solution with pH of 7 is added, stirring is started, heating and maintaining the temperature at 80 ℃, and vanillin with the mass of chitosan of 90% is added while stirring. Stirring at constant temperature for reaction for 2h, filtering while the reaction is hot, flushing filter residues with distilled water, transferring into a constant-temperature oven, and drying at 60 ℃ to constant weight to obtain vanillin modified chitosan.
(2) 70 parts of fly ash and 30 parts of kaolin are mixed and then baked for 1 hour at 800 ℃, and then ground to 80 meshes, so that the high-activity adsorption material is prepared.
(3) The red mud is dried at 100 ℃ and then ground to 300 meshes.
(4) 5 parts of high-activity adsorption material, 5 parts of calcium sulfide powder and 90 parts of red mud powder are mixed and then are vibrated on a shaking table for 1h, wherein the vibration frequency is 400rpm.
(5) Adding 8 parts of vanillin modified chitosan into the fixing agent prepared in the step (4), stirring and heating to a molten state, continuously stirring for 0.5h, and cooling to prepare particles with the particle size of 4 mm.
Comparative example 1
(1) 60 parts of fly ash and 40 parts of kaolin are mixed and then baked for 4 hours at 600 ℃, and then ground to 50 meshes, so that the high-activity adsorption material is prepared.
(2) Drying the red mud at 95 ℃ and grinding the red mud to 200 meshes.
(3) 10 parts of high-activity adsorption material, 3 parts of calcium sulfide powder and 87 parts of red mud powder are mixed and then are vibrated on a shaking table for 2 hours, and the vibration frequency is 300rpm.
(4) Adding 6 parts of unmodified chitosan into the fixing agent prepared in the step (3), stirring and heating to a molten state, continuously stirring for 1h, and cooling to prepare particles with the particle size of 3 mm.
Comparative example 2
(1) Chitosan was placed in a container at a liquid-to-solid ratio of 10mL:1g of glacial acetic acid solution with pH of 6 is added, stirring is started, heating and maintaining the temperature at 60 ℃, and vanillin with 60% of the mass of chitosan is added while stirring. Stirring at constant temperature for reaction for 0.5h, filtering while the reaction is hot, flushing filter residues with distilled water, transferring into a constant-temperature oven, and drying at 80 ℃ to constant weight to obtain vanillin modified chitosan.
(2) Drying the red mud at 95 ℃ and grinding the red mud to 200 meshes.
(3) 3.3 parts of calcium sulfide powder and 96.7 parts of red mud powder are mixed and then are subjected to shaking on a shaking table for 2 hours, wherein the shaking frequency is 300rpm.
(4) Adding 6 parts of vanillin modified chitosan into the fixing agent prepared in the step (3), stirring and heating to a molten state, continuously stirring for 1h, and cooling to prepare particles with the particle size of 3 mm.
Comparative example 3
(1) 60 parts of fly ash and 40 parts of kaolin are mixed and then baked for 4 hours at 600 ℃, and then ground to 50 meshes, so that the high-activity adsorption material is prepared.
(2) The red mud is dried at 95 ℃ and then ground to 200 meshes.
(3) 10 parts of high-activity adsorption material, 3 parts of calcium sulfide powder and 87 parts of red mud powder are mixed and then are vibrated on a shaking table for 2 hours, and the vibration frequency is 300rpm.
Examples 1 to 2 and comparative examples 1 to 3 were examined for arsenic fixation effect of 5 slow-release arsenic fixatives in total:
the method comprises the steps of selecting soil of a certain arsenic pollution site treatment project in Hunan province as a test material, leaching the polluted soil according to a horizontal oscillation method of a solid waste leaching toxicity leaching method (HJ 557-2009), and detecting the arsenic content in leaching liquid. The detection shows that the arsenic leaching toxicity of the polluted soil is 0.52402mg/L.
(1) Test of arsenic fixing effect of the slow-release arsenic fixing agent prepared in example 1:
and (3) spraying a small amount of distilled water to keep a wet state in a reaction container, adding the slow-release arsenic fixing agent prepared in the embodiment 1 according to 3% of the soil mass, uniformly stirring, curing, and sampling and detecting the leaching toxicity of arsenic in the test soil every day during the curing period of 1 week.
(2) Slow release arsenic fixing agent arsenic fixing effect test prepared in example 2, comparative example 1, comparative example 2, comparative example 3:
the sustained-release arsenic fixing agents prepared in example 2, comparative example 1, comparative example 2 and comparative example 3 were tested according to the experimental method of example 1, respectively.
(3) Experimental results and analysis:
TABLE 1 test of arsenic fixing Effect of sustained-release arsenic fixing agent
As can be seen from table 1, according to comparison of example 1, comparative example 1 and comparative example 3, it was found that the arsenic fixing agent coated with vanillin-modified chitosan improved the action time, had a better slow release effect and was better for fixing arsenic, since the vanillin-modified chitosan was able to form a stable chelate with arsenic while playing a slow release role, the effect after modification was better, whereas the chitosan not subjected to vanillin modification did not contain phenolic hydroxyl groups having chelating arsenic ions, and was inferior to the vanillin-modified chitosan in fixing arsenic. Comparative example 1 and comparative example 2 have found that the introduction of the activated high adsorption material has a better effect on reducing arsenic mobility, because the activated adsorption material has a larger specific surface area, and can adsorb and encapsulate the immobilized arsenic-enriched material, reducing the possibility of releasing the arsenic-enriched material due to environmental damage.
Claims (6)
1. A preparation method of a slow-release arsenic fixing agent is characterized in that: the method comprises the following steps:
1) Adding vanillin into acetic acid solution dissolved with chitosan to perform condensation reaction to obtain vanillin modified chitosan;
2) Mixing fly ash with kaolin, and roasting to obtain an adsorption material;
3) Mixing an adsorption material with calcium sulfide powder and red mud powder, and performing oscillation treatment to obtain an arsenic fixing agent;
4) Mixing the arsenic fixing agent with vanillin modified chitosan, performing hot melting treatment, cooling, and granulating to obtain a slow-release arsenic fixing agent;
the mass of the vanillin is 50% -100% of that of the chitosan; the mass ratio of the fly ash to the kaolin is 50-70:30-50; the mass ratio of the adsorption material to the calcium sulfide powder to the red mud powder is as follows: 5-20:1-5:75-94; the mass ratio of the arsenic fixing agent to the vanillin modified chitosan is 85-95:5-15.
2. The method for preparing a sustained-release arsenic fixing agent according to claim 1, wherein: the conditions of the condensation reaction are as follows: the temperature is 50-80 ℃ and the time is 0.5-2 h.
3. The method for preparing a sustained-release arsenic fixing agent according to claim 1, wherein: the conditions of the roasting treatment are as follows: the temperature is 600-800 ℃ and the time is 1-4 h.
4. The method for preparing a sustained-release arsenic fixing agent according to claim 1, wherein: the conditions of the oscillation treatment are as follows: the oscillating frequency is 300-400 rpm, and the time is 1-2 h.
5. A slow release arsenic fixing agent, which is characterized in that: obtained by the production process according to any one of claims 1 to 4.
6. The use of a slow release arsenic fixing agent according to claim 5, characterized in that: the method is applied to the restoration of arsenic-polluted soil.
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