CN114307982A - Preparation method of composite-based modified fly ash particles for static water body restoration - Google Patents
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Abstract
The invention discloses a preparation method of composite-based modified fly ash particles for static water body restoration, belonging to the technical field of environmental protection; the preparation method comprises the steps of preparing modified fly ash and preparing composite-based modified fly ash particles; the method for preparing the composite-base modified fly ash particles comprises three stages of mixing, preparing particles and curing: mixing the modified fly ash and portland cement, adding a chitosan quaternary ammonium salt solution, fully stirring to obtain a raw material mixture, preparing particles through a mold, and maintaining to form composite-based modified fly ash particles for repairing static water; the composite-based modified fly ash particles prepared by the invention can realize the adsorption and removal of nitrogen and phosphorus in overlying water of a static water body, retard the release of pollutants of bottom mud of the static water body, inhibit the growth of algae, effectively improve the water quality condition of the static water body, reduce the eutrophication risk of the static water body, improve the pollution property of the bottom mud for a long time and prevent the occurrence of black and odorous phenomena.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a preparation method of composite-based modified fly ash particles for static water body restoration.
Background
In recent years, industrial wastewater, domestic sewage, urban rainfall runoff and other carried pollutants brought by the rapid development, industrialization and urbanization of China are discharged into a water environment in large quantity, pollution control and comprehensive treatment measures related to the pollution are relatively lagged, and part of sewage is discharged into urban water bodies such as river channels, lakes and reservoirs without treatment or treatment failing to reach the standard, so that the environmental water quality is gradually deteriorated, and even extreme water body black and odorous and eutrophication phenomena occur, so that the urban ecology and the human living environment quality are seriously influenced.
Fly ash is a coal-fired byproduct discharged from coal-fired power plants. Along with the increase of annual emission amount of fly ash and low utilization rate of fly ash in China, the storage of fly ash not only causes waste of capital and land, but also causes environmental pollution and harms human health more seriously. According to statistics, the utilization rate of the fly ash in developed countries such as Europe and America can reach 90 percent basically, and the current reutilization rate of the fly ash in China can only reach 50 percent. At present, the comprehensive utilization conditions of the fly ash at home and abroad are seen that the application technology of the fly ash in building materials, construction, roads, filling and agriculture is mature, and the application of the fly ash in water treatment opens up a new way for the comprehensive utilization of the fly ash and becomes one of the hot subjects in the field of environmental protection research.
The fly ash is composed of powder with various structures and forms, mainly is small glass sphere, and its main component is A12O3、SiO2、Fe2O3CaO, and the like, and also contains a small amount of other substances, the particles of the fly ash are in a porous honeycomb shape, the particle size range is smaller, the specific surface area is larger, the bead walls of the particles are in a porous structure and have higher porosity, and a plurality of active sites such as silicon, aluminum and the like exist. Meanwhile, some important other physical characteristics enable the fly ash to have an irregular active structure, so that the surface has higher absorptionThe fly ash has the advantages of high activity and high water absorption performance, is used for treating sewage, is particularly used for removing nitrogen and phosphorus in water, is convenient and quick, has high effect, can fully utilize the value of the fly ash, realizes the purpose of treating wastes with wastes, and can obtain very good environmental and economic effects.
Although the fly ash has been widely used abroad as a solid waste with a utilization value, the untreated fly ash has a risk of releasing heavy metals and ammonia nitrogen into a water body, and the powdery form also increases the turbidity of the water body and affects the water quality condition. Many researches on modifying fly ash attempt to excite the activity of the fly ash and eliminate potential risks, but a complete technical system is not available, the use standard of the fly ash in China is not perfect, various fly ash materials are produced by various processes, and the preparation of a granular material which takes the fly ash as a raw material, effectively adsorbs pollutants in water and has integrity, wear resistance, adsorption activity and recycling performance is a main research problem.
Disclosure of Invention
The composite base modified fly ash particles prepared by the invention can realize the adsorption and removal of nitrogen and phosphorus in overlying water of a static water body, retard the release of pollutants of bottom mud of the static water body, inhibit the growth of algae, effectively improve the water quality condition of the static water body, reduce the eutrophication risk of the static water body, improve the pollution property of the bottom mud for a long time and prevent the occurrence of black and odorous phenomena.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of composite-based modified fly ash particles for static water body restoration comprises the steps of preparing modified fly ash and preparing composite-based modified fly ash particles.
The preparation of the modified fly ash comprises the steps of heat treatment, activation by an alkaline activator, preparation of biochar, drying of quicklime and calcination.
And in the heat treatment, the fly ash is sieved by a sieve with 200-550 meshes, and then is calcined for 4-5h at the temperature of 500-550 ℃ to obtain the heat-treated fly ash.
And (2) activating the alkaline activator, namely uniformly mixing the alkaline activator with the thermally treated fly ash, continuously stirring for 4-5h at normal temperature, standing after stirring, filtering the fly ash, washing the fly ash with deionized water until the pH value is 7-7.5, baking for 24-25h at the temperature of 100-110 ℃, and grinding the fly ash through a 200-mesh 250-mesh screen to obtain the fly ash activated by the alkaline activator.
The preparation method of the alkaline activator comprises the following steps: and (3) advancing for 24-25h, mixing NaOH particles and a sodium silicate solution according to a mass ratio of 6-7: 4, uniformly mixing to obtain the alkaline activator.
The sodium silicate solution is composed of Na2O 8.29-8.5wt%， SiO21.22-1.5wt% and H2O 90-90.49wt%。
Wherein the mass ratio of the alkaline activator to the fly ash after heat treatment is 0.4-0.5: 1.
the preparation method comprises the steps of cleaning reed straws with deionized water, drying at a low temperature, cutting the dried reed straws into 1-1.5cm small sections, crushing, putting into a muffle furnace at 550 ℃, carrying out constant-temperature anoxic pyrolysis for 1-1.5h, soaking a pyrolyzed sample in 1-1.5mol/L HCl solution for 1-1.5h, washing with deionized water until the pH value is 6.5-7, drying at 80-85 ℃, grinding, and sieving with a 200-fold 250-mesh sieve to obtain the biochar;
the volume fraction of oxygen in the constant-temperature anoxic pyrolysis process is 10-12%.
Drying the quicklime, namely grinding the quicklime to pass through a 200-mesh and 250-mesh screen, and then placing the ground quicklime in a drying oven to be dried to constant weight to obtain dried quicklime;
and in the calcining step, the fly ash activated by the alkaline activator, the biochar and the dried quick lime are uniformly mixed according to the mass ratio of 10-15:1-2:1-3, calcined at the temperature of 500-550 ℃ for 2-2.5h, and then cooled to the normal temperature in the furnace to obtain the modified fly ash.
The preparation of the composite base modified fly ash particles comprises the steps of mixing, granulating and maintaining.
Mixing, namely mixing the modified fly ash and portland cement according to the mass ratio of 9-10:1, adding a chitosan quaternary ammonium salt solution, and fully stirring and mixing to obtain a raw material mixture;
the strength grade of the portland cement is P.O42.5;
the chitosan quaternary ammonium salt solution is an HTCC solution with the mass fraction of 3-5%, and the solvent is an acetic acid aqueous solution with the mass fraction of 2-6%.
The mass ratio of the chitosan quaternary ammonium salt solution to the portland cement is 6-8.8: 1.
the preparation of the particles comprises the step of adding the raw material mixture into a metal die to prepare the particles with the particle size of 3-3.5 mm.
And maintaining, namely after the particles are demoulded, drying at room temperature for 2-2.5 hours, then putting into a maintenance box with the temperature of 20 +/-2 ℃ and the relative humidity of more than or equal to 95 percent, maintaining for 14-15 days, and obtaining the composite-based modified fly ash particles after the maintenance is finished.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the composite-based modified fly ash particles for static water body restoration has the advantages of simple process and lower cost, and realizes the recycling of fly ash;
(2) according to the preparation method of the composite-based modified fly ash particles for repairing static water, redundant impurities in fly ash are thoroughly removed through multiple modification steps, and the risk of heavy metal pollution released into water is avoided;
(3) according to the preparation method of the composite-based modified fly ash particles for static water restoration, the strength can be increased and the volcanic ash reaction can be ensured to be smoothly carried out by adding the portland cement and reasonably controlling the hydration reaction ratio;
(4) according to the preparation method of the composite-based modified fly ash particles for static water body restoration, a chitosan quaternary ammonium salt solution is used, and the chitosan quaternary ammonium salt has good antibacterial property, film forming property, cation adsorption property, moisture absorption and retention property, flocculation property, antistatic property and other properties, so that a slow release effect can be well realized, and the adsorption durability of the material is improved;
(5) the composite-based modified fly ash particles for repairing static water bodies, which are prepared by the invention, have the coverage thickness of 20mm in use, belong to thin-layer coverage and have little influence on the original ecological environment of the water bodies;
(6) the composite-based modified fly ash particles for static water body restoration, which are prepared by the invention, have the volume density of 1.12-1.23g/cm, the porosity of 46.7-49.3%, the sum of the breakage rate and the wear rate of 5.1-5.3%, the hydrochloric acid dissolvability of 0.21-0.3%, and good performance of each index, and all meet the standard requirements of the artificial ceramsite filter material for CJ-T299-2008 water treatment; the water-based paint has the characteristics of light weight, high utilization rate, high tensile strength, good permeability, aging resistance and corrosion resistance, and can effectively separate bottom mud from overlying water, thereby achieving the purpose of adsorbing pollutants and avoiding secondary pollution;
(7) the composite-base modified fly ash particles for static water restoration, which are prepared by the invention, have the particle strength of 1.600-1.630MPa and the bulk density of 803-805kg/m and belong to medium-high strength particles, are not easy to disintegrate after being soaked in water, so that the defect of scum existing after the fly ash powder is added is effectively overcome, and the formed particles are convenient to salvage and replace and can be recycled;
(8) according to the preparation method of the composite-based modified fly ash particles for static water body restoration, the curing and forming are carried out under the room-temperature humid condition, although the curing time is prolonged, the curing process is simple, the cost is low, the hydration reaction is more sufficient, the repeated attempts of air pressure and temperature in steam curing and water bath curing are avoided, the performance optimization is realized, and the particle strength can be increased;
(9) the composite base modified fly ash particles for static water body restoration prepared by the invention have the inhibition rate of 75.06-78.12% on TN and can inhibit NH4 +The inhibition rate of-N can reach 90.91-93.45%, and the inhibition rate of TP can reach 90.63-93.97%;
(10) the composite-based modified fly ash particles for repairing the static water body, which are prepared by the invention, can realize the adsorption and removal of nitrogen and phosphorus in overlying water of the static water body, retard the release of pollutants of bottom mud of the static water body, inhibit the growth of algae, effectively improve the water quality condition of the static water body, reduce the eutrophication risk of the static water body, improve the pollution property of the bottom mud for a long time and prevent the occurrence of black and odorous phenomena.
Drawings
FIG. 1 is a diagram illustrating the effect of the composite-based modified fly ash particles prepared according to the present invention;
FIG. 2 is a schematic diagram of an indoor test of composite-based modified fly ash particles prepared according to the present invention.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
The method of making the composite-based modified fly ash particles of the present invention is further illustrated and described by the following detailed description.
Example 1
A preparation method of modified fly ash comprises the following steps:
1. and (3) heat treatment: sieving the fly ash with a 200-mesh sieve, and calcining at 500 ℃ for 4h to obtain the fly ash after heat treatment;
2. preparing an alkaline activator: and (3) advancing for 24-25h, mixing NaOH particles and a sodium silicate solution according to a mass ratio of 6: 4, uniformly mixing to obtain an alkaline activator, and then sealing and storing the alkaline activator for later use;
the sodium silicate solution is composed of Na2O 8.29wt%， SiO21.22wt% and H2O 90.49wt%；
3. Activation of alkaline activator: uniformly mixing an alkaline activator and the fly ash subjected to heat treatment, continuously stirring for 4 hours at normal temperature, standing after stirring, filtering the fly ash, washing the fly ash with deionized water until the pH is =7, then placing the fly ash in a 100 ℃ oven, baking for 24 hours until the fly ash is completely dried, and grinding the fly ash through a 200-mesh screen to obtain the fly ash activated by the alkaline activator;
wherein the mass ratio of the alkaline activator to the fly ash after heat treatment is 0.4: 1.
4. preparing the biochar: cleaning reed straws with deionized water, drying at a low temperature, cutting the dried reed straws into small sections of 1cm, putting the small sections into a high-speed multifunctional crusher, crushing, putting the crushed samples into a muffle furnace at 500 ℃, carrying out constant-temperature anoxic pyrolysis for 1h to obtain pyrolyzed samples, soaking the pyrolyzed samples in 1mol/L HCl solution for 1h, washing the pyrolyzed samples with deionized water until the pH value is =7, putting the pyrolyzed samples into an electrothermal blowing drying box, drying at 80 ℃, grinding and sieving with a 200-mesh sieve to obtain biochar;
the volume fraction of oxygen in the constant-temperature anoxic pyrolysis process is 10%.
5. Drying quicklime: grinding quicklime, sieving with a 200-mesh sieve, and drying in a drying oven to constant weight to obtain dried quicklime;
6. and (3) calcining: uniformly mixing the fly ash activated by the alkaline activator, the biochar and the dried quicklime according to the mass ratio of 10:1:1, calcining at 500 ℃ for 2h, and cooling to normal temperature in a furnace to obtain the modified fly ash.
Example 2
A preparation method of composite-based modified fly ash particles for static water body restoration comprises the following steps:
1. mixing: mixing the modified fly ash prepared in the example 1 and portland cement according to the mass ratio of 9:1, adding a chitosan quaternary ammonium salt (HTCC) solution, and fully stirring and mixing to obtain a raw material mixture;
the strength grade of the portland cement is P.O42.5;
the HTCC solution is an HTCC solution with the mass fraction of 2%, and the solvent is an acetic acid aqueous solution with the mass fraction of 5%.
The mass ratio of the HTCC solution to the Portland cement is 6: 1.
2. preparing into particles: adding the raw material mixture into a metal mold to prepare particles with the particle size of 3 mm;
3. and (5) maintenance: and (3) after the particles are demoulded, drying for 2 hours at room temperature, then putting the particles into a curing box with the temperature of 20 +/-2 ℃ and the relative humidity of more than or equal to 95 percent, curing for 14 days, and obtaining the composite-based modified fly ash particles after the curing is finished.
The volume density of the prepared composite-based modified fly ash particles is 1.12g/cm, the porosity is 46.7%, the sum of the breakage rate and the wear rate is 5.3%, the hydrochloric acid solubility is 0.3%, and the standard requirement of the artificial ceramsite filter material for CJ-T299-2008 water treatment is met.
The grain strength of the prepared composite-based modified fly ash grains is 1.630MPa, the bulk density is 805kg/m, and the grains belong to medium-high strength grains.
Example 3
A preparation method of modified fly ash comprises the following steps:
1. and (3) heat treatment: sieving the fly ash with a 250-mesh sieve, and calcining at 550 ℃ for 5 hours to obtain the fly ash after heat treatment;
2. preparing an alkaline activator: and (2) advancing by 25h, mixing NaOH particles and a sodium silicate solution according to a mass ratio of 7: 4, uniformly mixing to obtain an alkaline activator, and then sealing and storing the alkaline activator for later use;
the sodium silicate solution is composed of Na2O 8.5wt%， SiO21.5wt% and H2O 90wt%；
3. Activation of alkaline activator: uniformly mixing an alkaline activator and the fly ash subjected to heat treatment, continuously stirring for 5 hours at normal temperature, standing after stirring, filtering the fly ash, washing the fly ash with deionized water until the pH is =7.5, then placing the fly ash in a 110 ℃ oven, baking for 25 hours until the fly ash is completely dried, and grinding the fly ash through a 250-mesh screen to obtain the fly ash activated by the alkaline activator;
wherein the mass ratio of the alkaline activator to the fly ash after heat treatment is 0.5: 1.
4. preparing the biochar: cleaning reed straws with deionized water, drying at a low temperature, cutting the dried reed straws into small sections of 1.5cm, putting the small sections into a high-speed multifunctional crusher, crushing, putting the crushed samples into a muffle furnace at 550 ℃, carrying out constant-temperature anoxic pyrolysis for 1.5h to obtain pyrolyzed samples, soaking the pyrolyzed samples in 1.5mol/L HCl solution for 1.5h, washing the pyrolyzed samples with deionized water until the pH value is =6.5, putting the pyrolyzed samples into an electrothermal blowing drying box, drying at 85 ℃, grinding and sieving with a 250-mesh sieve to obtain biochar;
the volume fraction of oxygen in the constant-temperature anoxic pyrolysis process is 12%.
5. Drying quicklime: grinding quicklime, screening the ground quicklime by a screen of 250 meshes, and then placing the ground quicklime in a drying oven to be dried to constant weight to obtain dried quicklime;
6. and (3) calcining: the fly ash activated by the alkaline activator, the biochar and the dried quicklime are mixed and stirred uniformly according to the mass ratio of 15:2:3, calcined at 550 ℃ for 2.5 hours, and then cooled to normal temperature in a furnace to obtain the modified fly ash.
Example 4
A preparation method of composite-based modified fly ash particles for static water body restoration comprises the following steps:
1. mixing: mixing the modified fly ash prepared in the embodiment 1 with portland cement according to the mass ratio of 10:1, adding a chitosan quaternary ammonium salt (HTCC) solution, and fully stirring and mixing to obtain a raw material mixture;
the strength grade of the portland cement is P.O42.5;
the HTCC solution is 3% by mass, and the solvent is 6% by mass of acetic acid aqueous solution.
The mass ratio of the HTCC solution to the Portland cement is 8.8: 1.
2. preparing into particles: adding the raw material mixture into a metal mold to prepare particles with the particle size of 3.5 mm;
3. and (5) maintenance: and (3) after the particles are demoulded, drying for 2 hours at room temperature, then putting the particles into a curing box with the temperature of 20 +/-2 ℃ and the relative humidity of more than or equal to 95 percent, curing for 15 days, and obtaining the composite-based modified fly ash particles after the curing is finished.
The volume density of the prepared composite-based modified fly ash particles is 1.23g/cm, the porosity is 49.3%, the sum of the breakage rate and the wear rate is 5.1%, the hydrochloric acid solubility is 0.21%, and the standard requirement of the artificial ceramsite filter material for CJ-T299-2008 water treatment is met.
The grain strength of the prepared composite-based modified fly ash grains is 1.600MPa, the bulk density is 803kg/m, and the method belongs to medium-high strength grains.
Comparative example 1
The method for preparing the composite-based modified fly ash particles for static water restoration described in example 2 is different in that: no chitosan quaternary ammonium salt (HTCC) solution was added in the mixing step.
Example 5
Taking a certain black and odorous river channel in Jinan city as an example, after sampling, detecting and analyzing river channel river water and river bottom, averagely dividing the river channel river water and river bottom into 3 parts, respectively filling the 3 parts into conical flasks, respectively marking a water sample 1, a water sample 2 and a water sample 3 on the conical flasks, and then respectively treating the water samples 1-3 by using the composite base modified fly ash particles prepared in the example 2, the example 4 and the comparative example 1, wherein the treatment method is as follows:
as shown in fig. 1, the conical flask is covered with the composite modified fly ash particles according to the volume ratio of water to mud to composite modified fly ash particles =5:2:1, the composite modified fly ash particles cover the upper layer of the mud, the vertical thickness of the covering layer of the composite modified fly ash particles is 20mm, and tinfoil is used for enclosing the bottom mud part of the conical flask to simulate the dark environment of the bottom of a lake. And (3) carrying out an effect experiment for 22 days at room temperature in a laboratory, detecting and recording concentration changes of ammonia nitrogen, total nitrogen and total phosphorus, and setting a control group without adding a compound-based modified fly ash particle covering layer. The inhibition ratio was calculated according to formula (1).
（1）
C1: the concentration of water pollutants on the substrate sludge without the composite base modified fly ash particle covering layer is increased;
c2: adding the composite base modified fly ash particles to cover the water pollutant concentration on the substrate sludge.
The results of the water samples tested on day 22 were as follows:
the laboratory test examples of the present invention have been described above by way of illustration only, and the effects of external factors on the materials of the present invention still exist in practical applications, and it will be apparent to those skilled in the art that the described examples can be modified in various different ways without departing from the spirit and scope of the present invention. Accordingly, the foregoing description is illustrative in nature and is not to be construed as limiting the scope of the invention as claimed.
Claims (10)
1. A preparation method of composite-based modified fly ash particles for static water body restoration is characterized by comprising the steps of preparing modified fly ash and preparing composite-based modified fly ash particles;
the preparation of the composite base modified fly ash particles comprises the steps of mixing, granulating and maintaining;
mixing, namely mixing the modified fly ash and portland cement according to the mass ratio of 9-10:1, adding a chitosan quaternary ammonium salt solution, and fully stirring to obtain a raw material mixture;
the chitosan quaternary ammonium salt solution is an HTCC solution with the mass fraction of 3-5%, and the solvent is an acetic acid aqueous solution with the mass fraction of 2-6%.
2. The preparation method of the composite-based modified fly ash particles for repairing static water bodies as claimed in claim 1, wherein the mass ratio of the chitosan quaternary ammonium salt solution to the portland cement is 6-8.8: 1.
3. the method for preparing the composite-based modified fly ash particles for repairing the static water body as claimed in claim 1, wherein the preparing of the modified fly ash comprises heat treatment, activation by an alkaline activator, preparation of biochar, drying of quicklime and calcination.
4. The preparation method of the composite-based modified fly ash particle for static water restoration as claimed in claim 3, wherein the alkaline activator is activated, the alkaline activator and the fly ash after heat treatment are uniformly mixed, then the mixture is continuously stirred for 4-5h at normal temperature, the mixture is kept stand after stirring is finished, then the fly ash is filtered and washed by deionized water until the pH value is 7-7.5, then the mixture is baked for 24-25h at the temperature of 100-110 ℃ and then ground by a 200-mesh and 250-mesh screen to obtain the fly ash after activation by the alkaline activator.
5. The preparation method of the composite-based modified fly ash particles for repairing static water bodies according to claim 3, wherein the preparation method of the alkaline activator comprises the following steps: and (3) advancing for 24-25h, mixing NaOH particles and a sodium silicate solution according to a mass ratio of 6-7: 4, uniformly mixing to obtain an alkaline activator;
composition of the sodium silicate solutionIs Na2O 8.29-8.5wt%，SiO21.22-1.5wt% and H2O 90-90.49wt%。
6. The method for preparing the composite-based modified fly ash particles for repairing the static water body as claimed in claim 4, wherein the mass ratio of the alkaline activator to the fly ash subjected to the heat treatment is 0.4-0.5: 1.
7. the preparation method of the composite-based modified fly ash particle for static water restoration as claimed in claim 3, wherein the preparation of the biochar comprises the steps of cleaning reed straws with deionized water, drying at a low temperature, cutting the dried reed straws into 1-1.5cm sections, crushing, putting into a muffle furnace at 550 ℃ with 500-fold materials, carrying out anoxic pyrolysis at a constant temperature for 1-1.5h, soaking the pyrolyzed samples in 1-1.5mol/L HCl solution for 1-1.5h, washing with deionized water until the pH value is 6.5-7, drying at 80-85 ℃, and grinding through a 200-fold 250-mesh sieve to obtain the biochar.
8. The method for preparing the composite-based modified fly ash particles for repairing the static water body as claimed in claim 7, wherein the volume fraction of oxygen in the constant-temperature anoxic pyrolysis process is 10-12%.
9. The preparation method of the composite-based modified fly ash particle for static water restoration as claimed in claim 3, wherein the calcination comprises uniformly mixing the fly ash activated by the alkaline activator, the biochar and the dried quick lime according to the mass ratio of 10-15:1-2:1-3, calcining at 500-550 ℃ for 2-2.5h, and cooling to normal temperature in a furnace to obtain the modified fly ash.
10. The preparation method of the composite modified fly ash particles for static water restoration according to claim 1, wherein the curing is carried out for 14-15 days by drying at room temperature for 2-2.5h after the particles are demoulded, then putting the particles into a curing box with the temperature of 20 +/-2 ℃ and the relative humidity of more than or equal to 95%, and obtaining the composite modified fly ash particles after the curing is finished.
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