CN111440615A - Preparation of waste source calcium salt-biomass charcoal composite material and application thereof in soil - Google Patents
Preparation of waste source calcium salt-biomass charcoal composite material and application thereof in soil Download PDFInfo
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- CN111440615A CN111440615A CN202010255121.6A CN202010255121A CN111440615A CN 111440615 A CN111440615 A CN 111440615A CN 202010255121 A CN202010255121 A CN 202010255121A CN 111440615 A CN111440615 A CN 111440615A
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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
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
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- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D3/00—Calcareous fertilisers
- C05D3/02—Calcareous fertilisers from limestone, calcium carbonate, calcium hydrate, slaked lime, calcium oxide, waste calcium products
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- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
- C09K17/06—Calcium compounds, e.g. lime
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
Preparation of a waste source calcium salt-biomass charcoal composite material and application thereof in soil, belonging to the field of material preparation and application. According to the invention, eggshell waste and agriculture, forestry and animal husbandry biomass waste are mixed and subjected to high-temperature and anaerobic carbonization to form a calcium salt-biomass charcoal composite material which is used for repairing heavy metal polluted acid soil. The invention skillfully couples the co-carbonization process of the eggshell waste and the agriculture, forestry and animal husbandry biomass waste, and the high-performance calcium salt-biomass carbon composite material is prepared conveniently in one step at low cost. The composite material can slowly release alkaline calcium salt, continuously improve the pH value of soil and passivate biologically available heavy metals; the biomass charcoal in the compound is stable and has a developed pore structure, so that the negative effect generated by the application of single calcium salt can be relieved, the soil fertility is increased for a long time, the acid soil is improved fundamentally, and the heavy metal in a biological effective state can be passivated efficiently.
Description
Technical Field
The invention relates to the field of material preparation and application thereof, in particular to preparation of a waste source calcium salt-biomass charcoal composite material and application thereof in soil.
Background
The acid soil is widely distributed in the southern agricultural regions in China, has the defects of low pH and organic matter content, and extremely limits the development of agriculture in the regions. With the acceleration of the industrialization process and the emission of a large amount of acid gas, the soil acidification degree and range are further increased. Therefore, improvement of acid soil is imperative, important and urgent. In addition, the phenomenon that heavy metals in acid soil exceed standards is caused by a large amount of mining in various regions in south China. It is worth noting that in acid soil, the content of heavy metals in free state is high, namely the content of biological available state is high, so that the heavy metals are easy to be enriched in the crops, and further generate toxicity to human bodies. In recent years, the heavy metal overproof events in rice grains of rice are reported successively in regions such as Hunan province. Therefore, it is necessary to improve acidic soil and reinforce the restoration of the current heavy metal pollution.
The waste recycling and environmental remediation can be realized simultaneously by a waste treatment strategy, the waste disposal and environmental remediation cost is greatly reduced, and the method is a research hotspot and key point in the field of agricultural environment and has profound significance. Eggshells and biomass for agriculture, forestry and animal husbandry are common solid wastes in life and production. The method has been researched and used for repairing acid soil and heavy metal contaminated soil, but the unique characteristics and advantages of the two wastes are not exerted, and the combination strategy needs to be improved.
Through retrieval, related applications are disclosed in the prior art, for example, a tea garden soil conditioner and an application thereof disclosed in the application with the Chinese patent application number of 2018107292155 and the application publication date of 2018, 11 and 13 are disclosed, and the tea garden soil conditioner comprises the following components in parts by weight: 12-25 parts of biochar, 4-10 parts of egg shells, 1.5-3.7 parts of humic acid and 0.2-2.3 parts of hydroxy carboxylic acid compounds. The soil conditioner in the application comprises the main components of biochar, wherein the biochar is alkaline, has large porosity and specific surface area, and also contains various mineral elements; the egg shell can provide protein and calcium, consume acid in soil and provide high-quality nutrition for soil; the humic acid and hydroxycarboxylic acid compounds contain hydroxyl and carboxyl functional groups, and have strong exchange capacity and adsorption effect on hydrogen ions and aluminum ions in soil when applied to acid soil; the biomass and the egg shells are both of porous structures and can load humic acid and hydroxy carboxylic acid compounds, and the substances are matched according to the proportion to enhance the improvement effect on acid soil. The components in the application are more, and all need to prepare alone, use by mixing again, and is with high costs, is difficult to be applicable to the wide range of big pollution current situation.
The invention discloses a photocatalytic soil heavy metal restoration agent, which is prepared from the following raw materials in parts by weight as disclosed in application No. 201610153166.6 filed on 2016, 9 and 28 in 2016: 4-5 parts of titanium dioxide, 12-13 parts of egg shells, 5-6 parts of calcium ammonium nitrate, 6-8 parts of fly ash, 10-14 parts of water hyacinth powder, 2-4 parts of potassium pyrophosphate, 85-95 parts of seedless sunflower discs, 40-45 parts of pig manure, 23-26 parts of kaolin, 12-14 parts of calcium carbonate, 32-35 parts of slash pine needles and a proper amount of water; the soil repairing agent uses organic biomass charcoal, organic fermentation materials and the like as adsorption carriers, can adsorb organic pollutants such as a large amount of heavy metal ions, pesticide residues and the like on the surfaces of particles, and can oxidize and degrade organic matters by catalyzing and repairing titanium dioxide on the surfaces of the particles through transmitted light in soil, so that the effect of removing harmful substances in the soil more thoroughly is achieved. Although the repairing agent prepared by the application can have a good adsorption effect on heavy metals in soil, the preparation process is complex, the material consumption is high, the cost is high, the time-consuming longer preparation processes such as fermentation are needed, and the large-scale production and utilization are not facilitated.
Based on the defects of the prior art, the invention needs to invent a simple, low-cost and high-efficiency repairing-improving material based on eggshell waste and biomass waste for agriculture, forestry and animal husbandry, realizes repairing and improving simultaneously, and assists crops in the acid soil area polluted by heavy metal in China to safely and stably produce high yield.
Disclosure of Invention
1. Technical problem to be solved by the invention
Aiming at the problem of restoring the heavy metal polluted acid soil, the invention adopts eggshell waste and agriculture, forestry and animal husbandry biomass waste as raw materials, prepares the calcium salt loaded porous biomass carbon composite material through one-step high-temperature carbonization, and directly improves the pH and organic matter content of the soil and reduces the content of heavy metal biological effective state when being applied to the heavy metal polluted acid soil, thereby realizing the comprehensive and long-term effective restoration and improvement of the heavy metal polluted acid soil.
2. Technical scheme
In order to solve the technical problems, the technical scheme of the invention is as follows:
the invention provides a preparation method of a waste source calcium salt-biomass charcoal composite material, which comprises the following steps:
a) respectively crushing eggshell waste and agriculture, forestry and animal husbandry biomass waste into certain granularity to prepare eggshell waste powder and agriculture, forestry and animal husbandry biomass waste powder, and uniformly mixing the eggshell waste powder and the agriculture, forestry and animal husbandry biomass waste powder to obtain a mixture;
b) carbonizing the mixture under the protection of inert gas, and specifically operating as follows: firstly heating to 600-900 ℃, carbonizing for a certain time under the condition of 600-900 ℃, and then cooling to room temperature to obtain the waste source calcium salt-biomass charcoal composite material.
As a further improvement of the present invention, the mixing ratio of the eggshell waste and the biomass waste in agriculture, forestry and animal husbandry in step a) is: the mass ratio (0.1-6): 1.
as a further improvement of the invention, the temperature rise rate during carbonization in the step b) is 1-10 ℃/min.
As a further improvement of the invention, the tail gas in the step b) is passed through a sodium hydroxide solution to remove CO2。
As a further improvement of the invention, in the step b), the carbonization time is 0.5-5 h.
As a further improvement of the invention, the agriculture, forestry and animal husbandry biomass waste comprises rice straw and/or soybean straw.
As a further improvement of the invention, the flow rate of inert gas is kept at 50-600 m L/min in the carbonization process, and the inert gas is nitrogen.
As a further improvement of the invention, the composite material is used for repairing heavy metal polluted acid soil.
As a further improvement of the invention, the waste source calcium salt-biomass charcoal composite material is uniformly applied to the surface layer of soil; and (5) carrying out rotary tillage on the plough layer soil, and adding water to 60% of the maximum water holding capacity in the field.
As a further improvement of the invention, in the remediation process, the calcium salt-biomass charcoal composite is applied in an amount of 1% of the soil mass.
As a further improvement of the invention, the heavy metal in the heavy metal contaminated acidic soil comprises any one or combination of Cu, Zn, Cd or Pb, but is not limited to the above.
3. Advantageous effects
Compared with the prior art, the technical scheme provided by the invention has the following remarkable effects:
(1) according to the waste source calcium salt-biomass carbon composite material, eggshell waste and agriculture, forestry and animal husbandry biomass waste are respectively adopted as raw materials and are directly subjected to high-temperature carbonization treatment, decomposition of the eggshell waste plays a role in activating the agriculture, forestry and animal husbandry biomass waste in the carbonization process, the agriculture, forestry and animal husbandry biomass waste is promoted to be converted into porous biomass carbon, compared with biomass carbon prepared by single carbonization, the porous biomass carbon composite material has a very developed pore structure, and adsorption and fixation of biologically effective heavy metals in soil can be realized. In addition, in the carbonization treatment process, calcium salt formed by decomposing eggshell waste can play a role in quickly increasing the pH value of acid soil and provide calcium element. The whole process is simple, convenient and low in cost, not only solves the problem of environmental pollution caused by solid waste, but also carries out resource utilization, and is finally used for repairing and improving heavy metal polluted acid soil, thereby changing waste into valuable and treating pollution by waste.
(2) According to the waste source calcium salt-biomass charcoal composite material, biomass charcoal and calcium salt are organically combined, and the calcium salt can make up for the defect that the soil pH improving capability of organic material conditioners such as single biomass charcoal is weak; meanwhile, the biomass charcoal can relieve the negative effects of soil hardening, element imbalance and the like caused by the application of the single calcium salt modifier, can solve various problems in soil at the same time, and has wide application range.
(3) According to the invention, eggshell waste and agriculture, forestry and animal husbandry biomass waste are mixed, the mixture is carbonized under the protection of inert gas, the temperature is firstly increased to 600-900 ℃, the mixture is carbonized for a certain time under the condition of 600-900 ℃, and the temperature is reduced to room temperature to obtain the composite material, calcium salt is embedded on a biomass charcoal carrier with a developed pore structure, and on one hand, the calcium salt can be uniformly dispersed into heavy metal polluted acid soil along with the biomass charcoal; on the other hand, the composite material can also play a role in slow release, weaken the adverse effect of the addition of the calcium salt on soil organisms and continuously improve the acid soil.
(4) The waste source calcium salt-biomass charcoal composite material disclosed by the invention and eggshell waste co-activated and carbonized biomass charcoal not only have a developed pore structure, but also are more stable and difficult to decompose compared with the traditional biomass charcoal, and the action time of passivating biological effective heavy metals in soil and improving acid soil is longer.
(5) The waste source calcium salt-biomass charcoal composite material of the inventionThe method adopts the mode of CO-carbonization of the eggshell wastes and the biomass wastes in agriculture, forestry and animal husbandry, and the CO generated by the decomposition of the eggshell wastes can be removed by high-temperature carbonization2Avoiding secondary environmental pollution (CO) caused by independently applying eggshell wastes to the heavy metal polluted acid soil2Released).
Drawings
FIG. 1 is an X-ray diffraction pattern of the waste source calcium salt-biomass char composite of example 1;
FIG. 2 is a comparison graph of nitrogen adsorption-desorption isotherms and a comparison graph of pore size distribution before and after acid washing of the waste source calcium salt-biomass charcoal composite in example 1; wherein, figure (1) is a comparison graph of nitrogen adsorption-desorption isotherms, and figure (2) is a comparison graph of pore size distribution;
FIG. 3 is a graph showing the change in pH after the waste source calcium salt-biomass charcoal composite material of example 1 is added to model heavy metal contaminated acidic soil;
fig. 4 is a graph showing the change of the content of the bio-available state of the heavy metal after the waste source calcium salt-biomass charcoal composite material is added to the model heavy metal contaminated acidic soil in example 1.
Detailed Description
Example 1
The embodiment provides a preparation method of a waste source calcium salt-biomass charcoal composite material, which comprises the following steps:
respectively crushing eggshell waste and rice straw waste into powder with certain granularity, uniformly mixing 40g of eggshell powder and 10g of rice straw powder to obtain a mixture, wherein the mass ratio of the eggshell waste to the agriculture, forestry and animal husbandry biomass waste in the mixture is 4: 1, placing the mixture in a corundum crucible, heating to 800 ℃ at the speed of 5 ℃/min, keeping the temperature for 2 hours, then cooling to room temperature, wherein the nitrogen flow in the whole process is 300m L/min, black residues are waste source calcium salt-biomass carbon composite materials, and removing CO from tail gas through a sodium hydroxide solution2。
FIG. 1 is an X-ray diffraction pattern of a waste source calcium salt-biomass charcoal composite showing successful loading of calcium salt on biomass charcoal.
Setting a comparison group: the comparison group is a material for removing the calcium salt from the waste source calcium salt-biomass carbon composite material by acid washing, the material prepared by the invention and the material for removing the calcium salt after the acid washing are respectively subjected to a nitrogen adsorption-desorption experiment, the nitrogen adsorption-desorption isotherm and the pore size distribution comparison graph of the material and the material are shown in figure 2, and the BET specific surface area of the waste source calcium salt-biomass carbon composite material is 21.35m2A pore volume of 0.02 m/g3The BET specific surface area of the waste source calcium salt-biomass charcoal composite material after acid washing is 509.12m2(g) pore volume of 0.42m3(ii)/g, average pore diameter 3.26 nm. After acid washing, the specific surface area and the pore volume are greatly increased, and the average pore diameter is reduced, which again shows that the calcium salt is successfully loaded in the pores of the biomass charcoal.
The results show that on one hand, calcium salt in the eggshell waste is successfully loaded in the pore structure of the biomass charcoal, so that the slow release effect can be realized, the acid soil can be improved for a long time, and the improvement effect is more durable than that of the calcium salt directly applied; on the other hand, compared with biomass charcoal generated by directly pyrolyzing agriculture, forestry and animal husbandry biomass wastes, the biomass charcoal has a developed pore structure, and the capability of passivating the bioavailable heavy metals is gradually enhanced along with the gradual release of calcium salt. In addition, the biomass charcoal can increase soil organic matters, improve the physical structure of the soil, the structure of a microbial community and the like, improve the acid resistance of the soil and relieve the acidification process. Therefore, the material of the invention can efficiently repair and improve the acid soil polluted by heavy metal for a long time.
Example 2
The embodiment provides a preparation method of a waste source calcium salt-biomass charcoal composite material, which comprises the following steps of respectively crushing eggshell waste and rice straw waste into powder with certain particle size, uniformly mixing 1g of eggshell powder and 10g of rice straw powder to obtain a mixture, wherein the mixing mass ratio of the eggshell waste to the agriculture, forestry and animal husbandry biomass waste is 0.1: 1, then placing the mixture into a corundum crucible, heating to 600 ℃ at the speed of 1 ℃/min, keeping the temperature for 5 hours, cooling to room temperature, wherein the nitrogen flow in the whole process is 600m L/min, and black residues are waste residuesRemoving CO from waste calcium salt-biomass charcoal composite material by passing tail gas through sodium hydroxide solution2。
Example 3
The embodiment provides a preparation method of a waste source calcium salt-biomass charcoal composite material, which comprises the following steps of respectively crushing eggshell waste and rice straw waste into powder with certain particle size, uniformly mixing 60g of eggshell powder with 10g of rice straw powder to obtain a mixture, placing the mixture in a corundum crucible, heating to 900 ℃ at a speed of 10 ℃/min, keeping the temperature for 0.5h, cooling to room temperature, enabling the nitrogen flow in the whole process to be 50m L/min, enabling black residues to be the waste source calcium salt-biomass charcoal composite material, and removing CO from tail gas through a sodium hydroxide solution2。
Example 4
This example is an application experiment of applying the material prepared in example 1 to soil, and the specific steps are as follows:
weighing 0.1g of waste source calcium salt-biomass charcoal composite material prepared in example 1 and 10g of acid soil polluted by heavy metal (collected from heavy metal polluted red soil of Guixi river in Jiangxi), uniformly stirring, adding deionized water to 60% of field water capacity, culturing for 30d, and measuring soil pH (soil-water ratio is 1: 2.5) and biological effective state content (CaCl) of heavy metal2Solution extraction method).
Meanwhile, a blank control group is set, and the specific steps are as follows: weighing 10.1g of heavy metal contaminated acid soil (collected from heavy metal contaminated red soil in Guixi Jiangxi), uniformly stirring, adding deionized water to 60% of field water capacity, culturing for 30d, and measuring the pH value of the soil and the content of heavy metal biological effective state.
FIG. 3 is a graph showing the change of pH after the waste source calcium salt-biomass charcoal composite material is added to the model heavy metal contaminated acidic soil; as can be seen from FIG. 3, the pH of the soil after the remediation with the material of the present invention increased significantly from 4.91 to 9.63.
FIG. 4 shows the content of the biological available state of heavy metal after the waste source calcium salt-biomass charcoal composite material is added into the model heavy metal contaminated acidic soilAnd (5) a variation graph. CaCl2The content results of the bioavailable heavy metals measured by the solution extraction method show that after the waste source calcium salt-biomass charcoal composite material prepared in example 1 is added, the bioavailable content of Cu, Zn, Cd and Pb in soil is obviously reduced, and the reduction rates are respectively as follows: 99.95%, 99.97%, 99.76% and 99.98%.
Fig. 3 and 4 show that the waste source calcium salt-biomass charcoal composite material has the functions of efficiently improving acid soil and repairing heavy metal contaminated soil.
The invention has been described in detail hereinabove with reference to specific exemplary embodiments thereof. It will, however, be understood that various modifications and changes may be made without departing from the scope of the invention as defined in the appended claims. The detailed description and drawings are to be regarded as illustrative rather than restrictive, and any such modifications and variations are intended to be included within the scope of the present invention as described herein. Furthermore, the background is intended to be illustrative of the state of the art as developed and the meaning of the present technology and is not intended to limit the scope of the invention or the application and field of application of the invention.
Claims (10)
1. A preparation method of a waste source calcium salt-biomass charcoal composite material is characterized by comprising the following steps: the method comprises the following steps:
a) respectively crushing eggshell waste and agriculture, forestry and animal husbandry biomass waste into certain granularity to prepare eggshell waste powder and agriculture, forestry and animal husbandry biomass waste powder, and uniformly mixing the eggshell waste powder and the agriculture, forestry and animal husbandry biomass waste powder to obtain a mixture;
b) carbonizing the mixture under the protection of inert gas, and specifically operating as follows: firstly heating to 600-900 ℃, carbonizing for a certain time under the condition of 600-900 ℃, and then cooling to room temperature to obtain the waste source calcium salt-biomass charcoal composite material.
2. The preparation method of the waste source calcium salt-biomass charcoal composite material according to claim 1, characterized in that: the mixing proportion of the eggshell waste and the agriculture, forestry and animal husbandry biomass waste in the step a) is as follows: the mass ratio (0.1-6): 1.
3. the method for preparing the waste source calcium salt-biomass charcoal composite material according to claim 1 or 2, characterized in that: and the temperature rise rate during carbonization in the step b) is 1-10 ℃/min.
4. The preparation method of the waste source calcium salt-biomass charcoal composite material according to claim 3, characterized in that: in the step b), the carbonization time is 0.5-5 h.
5. The method for preparing the waste source calcium salt-biomass charcoal composite material according to claim 4, wherein: the agriculture, forestry and animal husbandry biomass waste comprises rice straws and/or soybean straws.
6. The preparation method of the waste source calcium salt-biomass charcoal composite material according to claim 3, wherein the flow rate of inert gas is kept at 50-600 m L/min in the carbonization process, and the inert gas is nitrogen.
7. A waste source calcium salt-biomass charcoal composite material is characterized in that: the composite material is prepared by the preparation method of the waste source calcium salt-biomass charcoal composite material as claimed in any one of claims 1 to 7.
8. The use of the waste-derived calcium salt-biomass char composite of claim 7, wherein: the composite material is used for repairing heavy metal polluted acid soil.
9. The use of the waste source calcium salt-biomass char composite of claim 8, wherein: uniformly applying the waste source calcium salt-biomass charcoal composite material to the surface layer of soil; and (5) carrying out rotary tillage on the plough layer soil, and adding water to 60% of the maximum water holding capacity in the field.
10. The use of the waste source calcium salt-biomass char composite of claim 9, wherein: the heavy metal in the heavy metal polluted acid soil comprises any one or combination of Cu, Zn, Cd and Pb.
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| CN113789175A (en) * | 2021-08-19 | 2021-12-14 | 桂林理工大学 | Preparation method and application of calcium carbonate biomass charcoal composite material |
| CN116216947A (en) * | 2023-03-14 | 2023-06-06 | 中铁四局集团有限公司 | Wetland ecosystem restoration method based on total nutrient level |
| CN116924856A (en) * | 2023-07-19 | 2023-10-24 | 山西大学 | Preparation method of solid waste base artificial soil |
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