CN114540037A - Preparation method of modified fly ash-based soil conditioner - Google Patents
Preparation method of modified fly ash-based soil conditioner Download PDFInfo
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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
- C09K17/08—Aluminium compounds, e.g. aluminium hydroxide
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- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
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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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Abstract
The invention provides a preparation method of a modified fly ash-based soil conditioner, which comprises the following steps: mixing the fly ash and the rice hull ash, performing ball milling for 0.5-8 hours to obtain a mixture, mixing the mixture with a calcium-containing raw material, an alkali activator and an auxiliary agent, putting the mixture into a closed reactor to perform hydrothermal reaction, filtering and washing the obtained reacted slurry to obtain modified fly ash-based porous calcium silicate, mixing and stirring the modified fly ash-based porous calcium silicate with a nitrogen-phosphorus aqueous solution or nitrogen-phosphorus wastewater for 1-8 hours, and performing solid-liquid separation to obtain the modified fly ash-based soil conditioner. The soil conditioner prepared by the invention has the effects of reducing the volume weight of soil, increasing the porosity of the soil, effectively increasing the effective silicon, nitrogen, phosphorus and potassium of the soil, preserving water and fertilizer, adsorbing and slowly releasing nitrogen and phosphorus, adsorbing and fixing heavy metals in the soil, improving the yield of crops and the like.
Description
Technical Field
The invention relates to the technical field of solid waste recycling, in particular to a preparation method of a modified fly ash-based soil conditioner.
Background
Fly ash is a solid waste produced by coal-fired power plants and is fine ash collected from coal combustion flue gas. Because the energy of China is mainly coal and the power generation amount of fire coal is huge, the fly ash production amount of China reaches 7.48 hundred million t in 2019, and is predicted to reach 9.25 hundred million t in 2024. China makes great efforts on the research and industrialization of fly ash resource utilization, the utilization rate of fly ash is increased year by year, but a large amount of fly ash is not utilized, the total amount of fly ash accumulated in an ash yard reaches more than 30 hundred million t, a large amount of land resources are occupied, the environment is greatly polluted, and large-scale resource utilization is urgently needed.
The soil in partial areas of China faces serious heavy metal pollution, soil hardening, poor water and fertilizer retention capability and the like. The chemical component of the fly ash is mainly SiO2And Al2O3And also some Fe2O3、CaO、MgO、K2O、TiO2And Na2O and the like, which have a large amount of medium and trace elements, can be used for preparing a soil conditioner, but the fly ash has small particles, is easy to agglomerate, has small specific surface area and low porosity and needs to be activated or modified. The method for preparing the soil conditioner by using the high-alkali fly ash disclosed by the Chinese invention patent 201810611290.1 is characterized in that the soil conditioner is prepared by mixing the high-alkali fly ash and solid alkali and heating at high temperature, and can treat acid soil polluted by heavy metal, but the soil conditioner is strong in alkalinity and only can treat the acid soil, and the preparation process needs high temperature (up to 800 ℃) and high energy consumption. The key point of the preparation of the soil conditioner by the fly ash is to carry out modification activation under mild conditions and improve the pores of the soil conditionerThe effective silicon content is increased, the water and fertilizer retention performance is enhanced, and the crop yield is further improved.
Disclosure of Invention
The invention aims to provide a preparation method of a modified fly ash-based soil conditioner, and the modified fly ash-based porous calcium silicate hydrate soil conditioner prepared by the method can reduce the volume weight of soil, increase the porosity of the soil, increase the effective silicon, nitrogen, phosphorus and potassium in the soil, retain water and fertilizer, adsorb nitrogen and phosphorus and release slowly, adsorb and fix heavy metals in the soil, improve the yield of crops and the like. The invention takes the solid waste as the raw material, the raw material belongs to the bulk industrial solid waste, and the method has the advantages of low price, easy obtainment, environmental protection, simple preparation method, low process and equipment cost, economy and easy implementation. The invention can relieve the pollution problem of the fly ash to the environment, and simultaneously improve the problems of heavy metal pollution of soil, soil hardening, poor water and fertilizer retention capability and the like.
In order to realize the purpose, the invention provides a preparation method of a modified fly ash-based soil conditioner, which comprises the following steps:
step 3, filtering and washing the slurry B obtained in the step 2 to obtain modified fly ash-based porous calcium silicate hydrate;
and 4, mixing and stirring the modified fly ash-based porous calcium silicate hydrate obtained in the step 3 and a nitrogen-phosphorus-containing aqueous solution or nitrogen-phosphorus wastewater for 1-8 hours, and performing solid-liquid separation to obtain the modified fly ash-based soil conditioner.
The ratio of the fly ash to the rice hull ash used in the step 1 is 1: 0-1.
In the step 2, the calcium-containing raw material comprises one or more of calcium oxide, calcium hydroxide, calcium chloride, calcium nitrate or waste residue with CaO as a main component, and is added according to the calcium-silicon molar ratio of 0.6-1.4.
In the step 2, the alkali activator is one or more than two mixed solutions of sodium hydroxide solution, sodium silicate solution, potassium hydroxide solution and potassium silicate solution, and the concentration of Na + or K + in the mixed solution is 0.5-2M.
And in the step 2, the liquid-solid ratio of the alkali exciting agent to the solid material is 5-30 mL/g.
In the step 2, the structural auxiliary agent is sodium polyacrylate PAAS or polyethylene glycol PEG or P123EO20PO70EO20, and the addition amount is 0.1-5 wt%.
In the step 2, the closed reactor is a high-pressure reaction kettle or a homogeneous reactor, and the reaction pressure is 0.5-1.5 MPa.
The reaction temperature of the hydrothermal reaction in the step 2 is 150-220 ℃, and the reaction time is 3-12 h.
And 3, filtering and washing the slurry B obtained in the step 2, wherein the washing method comprises the following steps: the washing was performed 3 times in countercurrent with water and ethanol, respectively.
In the step 4, the nitrogen-phosphorus-containing aqueous solution or the nitrogen-phosphorus wastewater is obtained by mixing a nitrogen-containing aqueous solution and a phosphorus-containing aqueous solution, wherein the nitrogen-containing aqueous solution comprises an ammonium chloride aqueous solution, an ammonium nitrate aqueous solution, an ammonium sulfate aqueous solution, an ammonium carbonate aqueous solution, an ammonium bicarbonate aqueous solution, an ammonium dihydrogen phosphate aqueous solution, a diammonium hydrogen phosphate aqueous solution and an ammonium phosphate aqueous solution; the phosphorus-containing aqueous solution comprises potassium dihydrogen phosphate aqueous solution, dipotassium hydrogen phosphate aqueous solution, potassium phosphate aqueous solution, sodium dihydrogen phosphate aqueous solution, disodium hydrogen phosphate aqueous solution and sodium phosphate aqueous solution.
The invention has the beneficial effects that:
1. the method takes the fly ash and the rice hull ash as raw materials, the raw materials are cheap and easy to obtain, the cost is low, the method is simple, the problem of environmental pollution caused by the mass accumulation of the fly ash and the rice hull ash is solved, and high-value resource utilization is realized;
2. the modified fly ash-based soil conditioner synthesized by the invention has the effects of reducing the volume weight of soil, increasing the porosity of the soil, increasing the effective silicon, nitrogen, phosphorus and potassium of the soil, preserving water and fertilizer, adsorbing nitrogen and phosphorus and slowly releasing, adsorbing and fixing heavy metals in the soil, improving the yield of crops and the like;
3. the preparation method disclosed by the invention is simple in preparation process, economical and easy to implement, suitable for industrial production, environment-friendly and economic, and opens up a new way for high-value resource utilization of the fly ash.
Drawings
FIG. 1 is a flow chart of a preparation method of a modified fly ash-based soil conditioner of the invention;
FIG. 2 is an X-ray diffraction pattern of a modified fly ash-based porous calcium silicate prepared in example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of modified fly ash-based porous calcium silicate hydrate prepared in example 1 of the present invention;
FIG. 4 is a nitrogen adsorption desorption curve of the modified fly ash-based porous calcium silicate hydrate prepared in example 1 of the present invention;
FIG. 5 is a plot of the pore size distribution of a modified fly ash-based porous calcium silicate hydrate prepared in example 1 of the present invention;
FIG. 6 is an adsorption isotherm of modified fly ash-based porous calcium silicate hydrate prepared in example 1 of the present invention for phosphate;
fig. 7 is an adsorption isotherm of modified fly ash-based porous calcium silicate hydrate prepared in example 1 of the present invention for ammonia nitrogen.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present specification, the technical solutions in the embodiments of the present specification will be clearly and completely described below with reference to the drawings in the embodiments of the present specification, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments.
In the following examples, fly ash from somewhere in Guizhou is taken as an example, and the main chemical component of the fly ash is 38.03 wt% SiO221.55 wt% of Al2O312.69 wt% Fe2O3And 11.23 wt% CaO; the main chemical component of the rice hull ash is SiO with more than 85 wt percent2。
Example (b): see fig. 1-7.
As shown in figure 1, the preparation method of the modified fly ash-based soil conditioner comprises the following steps:
step 3, filtering and washing the slurry B obtained in the step 2 to obtain modified fly ash-based porous calcium silicate hydrate;
and 4, mixing and stirring the modified fly ash-based porous calcium silicate hydrate obtained in the step 3 and a nitrogen-phosphorus aqueous solution or nitrogen-phosphorus wastewater for 1-8 hours, and performing solid-liquid separation to obtain the modified fly ash-based soil conditioner.
Example 1
Performing ball milling on 95 wt% of fly ash and 5 wt% of rice hull ash for 0.5 h, adding calcium oxide with a Ca/Si molar ratio of 0.8, adding 1M sodium hydroxide dilute solution to mix into slurry, controlling the liquid-solid ratio of the slurry, namely the ratio of the liquid volume to the solid mass to be 10 mL/g, and adding 0.5 wt% of PAAS. Adding the obtained slurry into a reaction kettle, stirring and heating to 170 ℃, and reacting for 8 hours at the temperature with the stirring speed of 200 r/min. And filtering and separating the slurry after the reaction, washing a filter cake with water and ethanol respectively in a counter-current manner for 3 times to obtain modified fly ash-based porous calcium silicate hydrate, and adsorbing nitrogen and phosphorus to obtain the modified fly ash-based soil conditioner.
Example 2
Performing ball milling on fly ash (80 wt%) and rice hull ash (20 wt%) for 2 h, adding calcium hydroxide according to a Ca/Si molar ratio of 1.2, adding 0.5M potassium hydroxide dilute solution to mix into slurry, controlling a liquid-solid ratio of the slurry, namely a ratio of liquid volume to solid mass to be 20 mL/g, and adding 1 wt% of P123. Adding the obtained slurry into a reaction kettle, stirring and heating to 150 ℃, and reacting for 12 hours at the temperature with the stirring speed of 300 r/min. And filtering and separating the slurry after the reaction, washing a filter cake with water and ethanol respectively in a counter-current manner for 3 times to obtain modified fly ash-based porous calcium silicate hydrate, and adsorbing nitrogen and phosphorus to obtain the modified fly ash-based soil conditioner.
Example 3
Performing ball milling on 60 wt% of fly ash and 40 wt% of rice hull ash for 6 h, adding calcium chloride according to the Ca/Si molar ratio of 1.4, adding 2M sodium silicate dilute solution to mix into slurry, controlling the liquid-solid ratio of the slurry, namely the ratio of liquid volume to solid mass to be 5 mL/g, and adding 5 wt% of PEG. Adding the obtained slurry into a reaction kettle, stirring and heating to 200 ℃, and reacting for 4 hours at the temperature with the stirring speed of 100 r/min. And filtering and separating the slurry after the reaction, washing a filter cake with water and ethanol respectively in a counter-current manner for 3 times to obtain modified fly ash-based porous calcium silicate hydrate, and adsorbing nitrogen and phosphorus to obtain the modified fly ash-based soil conditioner.
Example 4
Performing ball milling on the fly ash (50 wt%) and the rice hull ash (50 wt%) for 8h, adding calcium nitrate with the Ca/Si molar ratio of 1.0, adding 1.5M potassium silicate dilute solution to mix into slurry, controlling the liquid-solid ratio of the slurry, namely the ratio of the liquid volume to the solid mass to be 30 mL/g, and adding 3 wt% of PAAS. Adding the obtained slurry into a reaction kettle, stirring and heating to 220 ℃, and reacting for 3 hours at the temperature with the stirring speed of 400 r/min. And filtering and separating the slurry after the reaction, washing a filter cake with water and ethanol respectively in a counter-current manner for 3 times to obtain modified fly ash-based porous calcium silicate hydrate, and adsorbing nitrogen and phosphorus to obtain the modified fly ash-based soil conditioner.
Referring to fig. 2-7, the modified fly ash-based porous calcium silicate hydrate soil conditioner prepared by the method of example 1 is tested as follows:
as shown in fig. 2, the X-ray diffraction pattern of the modified fly ash-based porous calcium silicate hydrate shows: the phases of the modified fly ash-based porous calcium silicate obtained in the embodiment 1 are calcium silicate hydrate and ferric oxide;
as shown in fig. 3, the scanning electron micrograph of the modified fly ash-based porous calcium silicate hydrate shows that: the obtained modified fly ash-based porous calcium silicate hydrate is a porous aggregate particle with the diameter of dozens of microns, has rich pore structure and strong adsorption capacity;
as shown in fig. 4, the nitrogen adsorption desorption curve of the modified fly ash-based porous calcium silicate hydrate is type IV and has a hysteresis loop of type H3, which indicates that it has a mesoporous structure and the pore structure is a crack-shaped pore of a flaky aggregate particle, and the result is consistent with the scanning electron microscope photograph;
as shown in FIG. 5, the pore size distribution diagram of the modified fly ash-based porous calcium silicate hydrate is shown, and it can be seen from the diagram that the pore size distribution of the modified fly ash-based porous calcium silicate hydrate is more concentrated at 2-10 nm, which indicates that the modified fly ash-based porous calcium silicate hydrate is a mesoporous structure and has a larger specific surface area (BET specific surface area of 84.17 m)2/g）；
As shown in fig. 6, the adsorption isotherm of the modified fly ash-based porous calcium silicate hydrate for phosphate indicates that the equilibrium adsorption capacity of the modified fly ash-based porous calcium silicate hydrate for phosphate is 184.5 mg/g;
as shown in fig. 7, the adsorption isotherm of the modified fly ash-based porous calcium silicate hydrate on ammonia nitrogen indicates that the equilibrium adsorption capacity of the modified fly ash-based porous calcium silicate on ammonia nitrogen is 301.5 mg/g.
Specifically, a tomato planting field is divided into two parts, one part of the planting field is applied with the modified fly ash-based soil conditioner prepared by the method of the invention by 0.5 wt% as an experimental group, the other part of the planting field is used as a control group, and after harvesting in one season, the soil quality of the planting field is detected, and the results are shown in the following table 1:
TABLE 1 soil texture test results
As can be seen from the data in Table 1, the soil volume weight of the planted field applied with the soil conditioner is 1.466 g/cm compared with the planted field not applied with the soil conditioner3Reduced to 1.393 g/cm3The porosity of soil is increased from 14.15% to 25.59%, the water content of soil is increased from 16.48% to 34.4%, the effective silicon content of soil is increased from 52.6 mg/kg to 139.49 mg/kg, the plant height and stem thickness of the tomato in the planting field applied with the soil conditioner are obviously improved, the transverse diameter, longitudinal diameter and single fruit weight average of tomato fruits are obviously increased, the fruit setting number of the tomato is nearly doubled, and the contents of heavy metals such As Pb, Cd, Cr, Hg, As and the like in the soil and the tomato fruits are far lower than the corresponding national standard limit values.
In conclusion, the modified fly ash-based soil conditioner prepared by the method disclosed by the invention takes the modified fly ash-based porous calcium silicate hydrate as a main component, has a rich pore structure, has the pore diameter concentrated in 2-10 nm, is large in specific surface area, is strong in adsorption capacity on phosphate and ammonia nitrogen, can reduce the volume weight of soil, increase the porosity of the soil, increase the effective silicon, nitrogen, phosphorus and potassium content of the soil, retain water and fertilizer, adsorb heavy metals in the soil, and can effectively improve the yield of crops.
While the preferred embodiments of the present invention have been illustrated and described, it will be understood by those skilled in the art that the present invention is not limited to the details of the embodiments shown and described, but is capable of numerous equivalents and substitutions without departing from the spirit of the invention as set forth in the claims appended hereto.
Claims (10)
1. A preparation method of a modified fly ash-based soil conditioner is characterized by comprising the following steps:
step 1, mixing and ball-milling fly ash and rice hull ash according to a certain proportion for 0.5-8 h to obtain a mixture A;
step 2, mixing the mixture A obtained in the step 1 with a calcium-containing raw material, an alkali activator and a structural auxiliary agent according to a certain proportion, and putting the mixture into a closed reactor for hydrothermal reaction to obtain slurry B;
step 3, filtering and washing the slurry B obtained in the step 2 to obtain modified fly ash-based porous calcium silicate hydrate;
and 4, mixing and stirring the modified fly ash-based porous calcium silicate hydrate obtained in the step 3 and a nitrogen-phosphorus-containing aqueous solution or nitrogen-phosphorus wastewater for 1-8 hours, and performing solid-liquid separation to obtain the modified fly ash-based soil conditioner.
2. The preparation method of the modified fly ash-based soil conditioner according to claim 1, wherein the ratio of the fly ash to the rice husk ash used in the step 1 is 1: 0-1.
3. The preparation method of the modified fly ash-based soil conditioner according to claim 1, wherein the calcium-containing raw material in the step 2 comprises one or more of calcium oxide, calcium hydroxide, calcium chloride, calcium nitrate or waste residue mainly containing CaO, and is added according to the calcium-silicon molar ratio of 0.6-1.4.
4. The method for preparing the modified fly ash-based soil conditioner according to claim 1, wherein the alkali activator in the step 2 is one or a mixture of two or more of a sodium hydroxide solution, a sodium silicate solution, a potassium hydroxide solution and a potassium silicate solution, and Na in the mixture is contained in the mixture+Or K+The concentration is 0.5-2M.
5. The preparation method of the modified fly ash-based soil conditioner according to claim 1, wherein the liquid-solid ratio of the alkali activator to the solid material in the step 2 is 5-30 mL/g.
6. The method for preparing the modified fly ash-based soil conditioner as claimed in claim 1, wherein the structural assistant in step 2 is sodium polyacrylate PAAS or polyethylene glycol PEG or P123EO20PO70EO20The amount of the additive is 0.1 to 5 wt%.
7. The preparation method of the modified fly ash-based soil conditioner according to claim 1, wherein the closed reactor in the step 2 is a high-pressure reactor or a homogeneous reactor, and the reaction pressure is 0.5-1.5 MPa.
8. The preparation method of the modified fly ash-based soil conditioner according to claim 1, wherein the reaction temperature of the hydrothermal reaction in the step 2 is 150-220 ℃, and the reaction time is 3-12 h.
9. The preparation method of the modified fly ash-based soil conditioner according to claim 1, wherein the slurry B obtained in the step 2 is filtered and washed in the step 3, and the washing method comprises the following steps: the washing was performed 3 times in countercurrent with water and ethanol, respectively.
10. The method for preparing the modified fly ash-based soil conditioner according to claim 1, wherein in the step 4, the nitrogen-phosphorus-containing aqueous solution or the nitrogen-phosphorus wastewater is obtained by mixing a nitrogen-containing aqueous solution and a phosphorus-containing aqueous solution, wherein the nitrogen-containing aqueous solution comprises an ammonium chloride aqueous solution, an ammonium nitrate aqueous solution, an ammonium sulfate aqueous solution, an ammonium carbonate aqueous solution, an ammonium bicarbonate aqueous solution, an ammonium dihydrogen phosphate aqueous solution, a diammonium hydrogen phosphate aqueous solution and an ammonium phosphate aqueous solution; the phosphorus-containing aqueous solution comprises potassium dihydrogen phosphate aqueous solution, dipotassium hydrogen phosphate aqueous solution, potassium phosphate aqueous solution, sodium dihydrogen phosphate aqueous solution, disodium hydrogen phosphate aqueous solution and sodium phosphate aqueous solution.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114790393A (en) * | 2021-01-26 | 2022-07-26 | 中国科学院过程工程研究所 | Soil conditioner and preparation method and application thereof |
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| CN108239536A (en) * | 2016-12-26 | 2018-07-03 | 中国科学院过程工程研究所 | A kind of soil conditioner and preparation method thereof |
| CN108641723A (en) * | 2018-06-14 | 2018-10-12 | 国电新能源技术研究院有限公司 | A kind of high-alkali coal ash for manufacturing for soil conditioner method |
| CN110484267A (en) * | 2019-07-27 | 2019-11-22 | 华南理工大学 | A kind of mineral soil conditioner and preparation method thereof using flyash production |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108239536A (en) * | 2016-12-26 | 2018-07-03 | 中国科学院过程工程研究所 | A kind of soil conditioner and preparation method thereof |
| CN108641723A (en) * | 2018-06-14 | 2018-10-12 | 国电新能源技术研究院有限公司 | A kind of high-alkali coal ash for manufacturing for soil conditioner method |
| CN110484267A (en) * | 2019-07-27 | 2019-11-22 | 华南理工大学 | A kind of mineral soil conditioner and preparation method thereof using flyash production |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114790393A (en) * | 2021-01-26 | 2022-07-26 | 中国科学院过程工程研究所 | Soil conditioner and preparation method and application thereof |
| CN114790393B (en) * | 2021-01-26 | 2024-04-19 | 中国科学院过程工程研究所 | Soil conditioner and preparation method and application thereof |
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