CN110759696A - Preparation method of porous light ceramsite by taking phosphorus solid waste as raw material - Google Patents
Preparation method of porous light ceramsite by taking phosphorus solid waste as raw material Download PDFInfo
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- CN110759696A CN110759696A CN201911108886.0A CN201911108886A CN110759696A CN 110759696 A CN110759696 A CN 110759696A CN 201911108886 A CN201911108886 A CN 201911108886A CN 110759696 A CN110759696 A CN 110759696A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/142—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
- C04B28/143—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being phosphogypsum
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
The invention relates to a preparation method of porous light ceramsite by taking phosphorus solid waste as a raw material, which adopts the technical scheme that the preparation method comprises the steps of placing polydopamine modified foaming polystyrene microspheres in a tubular furnace, controlling the temperature at 350-550 ℃ in an inert gas protective atmosphere, and keeping the temperature for 30 minutes-2 hours to obtain nitrogen-doped carbonized porous hollow spheres; mixing and stirring 10 parts by weight of phosphorus solid waste powder, 1-2 parts by weight of gypsum excitant, 1-2 parts by weight of foaming agent, 5-10 parts by weight of cement clinker and 3-5 parts by weight of nitrogen-doped carbonized porous hollow spheres, granulating, and normally maintaining to obtain the porous light ceramsite. The method has the advantages of simple process, low energy consumption, high utilization rate of phosphorus solid waste, low cost and environmental friendliness, and the prepared porous light ceramsite has high porosity, strong heavy metal adsorption effect and strong dirt-removing capacity.
Description
Technical Field
The invention relates to the field of environment-friendly materials, in particular to a preparation method of porous light ceramsite by taking phosphorus solid waste as a raw material.
Background
In recent years, with the continuous development of world economy, the modern industry is highly concentrated. Industrial wastewater contains a large amount of heavy metals, which, although low in content, have become one of the major environmental problems threatening the development of human beings. As a method for effectively removing heavy metals, the adsorption technology plays an irreplaceable important role in the fields of water pollution control and water purification. At present, the traditional methods for treating heavy metal wastewater at home and abroad mainly comprise a chemical precipitation method, an oxidation-reduction method, an ion exchange method, a membrane technology method and the like, and have certain limitations, such as harsh operating conditions, high cost, poor low-concentration wastewater treatment effect, difficult precious metal recovery and the like.
The phosphate tailings are solid wastes which cannot be utilized when the phosphate ore is flotation concentrate. China is a large country of phosphorite, has proved that the total amount of phosphorite resources is the second place in the world, but is mainly characterized by more middle-low grade ores and less rich ores. Most phosphorite can meet the production requirements of phosphoric acid and high-concentration phosphate fertilizer only by mineral separation and enrichment, a large amount of phosphate tailings are discarded while part of high-grade phosphorite is utilized by mineral separation, and harmful ingredients such as phosphorus, fluorine and the like can be dissolved out from a large amount of accumulated phosphate tailings, so that severe environmental pollution is caused to regional soil and water systems.
At present, the traditional ceramsite production process is prepared by taking raw materials with high content of silicon-aluminum oxides such as kaolin, bentonite and the like as main materials and mixing a small amount of quicklime and the like, and the traditional process formula has high cost and serious waste of mineral resources. The porcelain granules are mostly closed-pore porcelain granules, have uniform size, compact texture, enamel formation on the surface and higher strength, and are mainly used for building materials or light aggregates. The porous ceramsite has a macroscopic and abundant macroporous structure, is mainly used as a biofilm carrier and is widely applied to sewage treatment, but the conventional porous ceramsite has a single pore channel type, a small specific surface area and low removal efficiency of pollutants in water, and the application range of the porous ceramsite is severely limited.
In recent years, patent CN201910152856.3 proposes a method for preparing a heavy metal sewage adsorbing material, which is to mix, heat and grind sodium aluminosilicate, polyacrylamide, sodium acetate, resorcinol, etc. to finally prepare the adsorbing material. The patent CN201810521713.0 provides an adsorption membrane for sewage treatment and a preparation method thereof, and the sewage treatment membrane prepared by the invention has the advantages of small aperture, various adsorption channels and higher sewage adsorption efficiency. Chinese patent CN02112755.7 proposes a spherical porous light ceramsite produced by using industrial waste slag, steelmaking red mud and fly ash as main raw materials, clay as an adhesive, and a proper amount of pore-forming agent through high-temperature sintering and a manufacturing method thereof. The produced ceramsite is specially used for water treatment filter materials, and the performance index of the ceramsite meets the requirement of environmental water treatment. Although the above patent scheme solves the problems of single pore channel type, small specific surface area and low removal efficiency of pollutants in water to a certain extent, the problem that the adsorption efficiency and the reutilization of the complex polluted water body are still difficult to ensure due to the small pore diameter of the membrane material or the industrial waste residue ceramsite treated at high temperature, and the high temperature treatment has large burden on the environment and high energy consumption.
Disclosure of Invention
The invention aims to solve the technical problems and provides the preparation method of the porous light ceramsite which takes the phosphorus solid waste as the raw material, has the advantages of simple process, low energy consumption, high utilization rate of the phosphorus solid waste, low cost, environmental friendliness, high porosity of the prepared porous light ceramsite, and strong heavy metal adsorption effect and decontamination capability.
The technical scheme comprises the following steps:
step T1: placing the polydopamine modified expanded polystyrene microspheres in a tube furnace, controlling the temperature at 350-550 ℃ under the inert gas protection atmosphere, and keeping the temperature for 30 minutes-2 hours to obtain nitrogen-doped carbonized porous hollow spheres;
step T2: mixing and stirring 10 parts by weight of phosphorus solid waste powder, 1-2 parts by weight of gypsum excitant, 1-2 parts by weight of foaming agent, 5-10 parts by weight of cement clinker and 3-5 parts by weight of nitrogen-doped carbonized porous hollow spheres, granulating, and normally maintaining to obtain the porous light ceramsite.
In the step T2, the phosphorus solid waste powder is phosphogypsum powder with the particle size of less than 0.075 mm; the inert gas is nitrogen or argon.
In the T2, the gypsum excitant is one of alum, calcined alum, sodium sulfate and sodium oxalate, and the foaming agent is azo compounds, preferably one of azodicarbonamide, diisopropyl azodicarboxylate or diethyl azodicarboxylate.
The polydopamine modified foaming polystyrene microsphere is prepared by the following method:
step S1: crushing and sieving waste expanded polystyrene by a crusher to obtain waste expanded polystyrene particles with the particle size of 0.2-1 mu m;
step S2: adding 10 parts by weight of old expanded polystyrene particles into an alkaline solution, mechanically stirring for 6-12 hours, and filtering and washing to obtain pretreated old expanded polystyrene microspheres;
step S3: preparing a Tris-HCl buffer solution with the concentration of 0.05-2 g/L of dopamine, adding 10-15 parts by weight of old expanded polystyrene microspheres to uniformly disperse, mechanically stirring for 12-24 hours, standing, washing and drying to obtain the polydopamine modified expanded polystyrene microspheres.
In the step S2, the alkaline solution is one of a sodium hydroxide solution, ammonia water or water glass; the concentration of the alkaline solution is 0.1-0.5 mol/L, and the addition amount is 50-100 parts by weight.
In the step S3, the concentration of the Tris-HCl buffer solution is 0.01mol/L, and the pH value is 7.3 +/-0.1.
The waste expanded polystyrene has wide sources, and can be used as shockproof materials of mechanical equipment, household appliances, instruments, artware and other easily damaged valuables and packages of fast food.
The phosphorus solid waste powder is prepared by crushing phosphogypsum to 2-20 mm in a crusher, and then sending the crushed phosphogypsum into a ball mill for dry grinding until the crushed phosphogypsum can pass through a 0.075mm square-hole sieve.
In view of the problems in the background art, the inventor makes the following improvements: 1) two wastes are used, the expanded polystyrene microspheres modified by dopamine are prepared by taking waste expanded polystyrene as a raw material, then phosphorus solid waste powder is mixed to prepare the porous light ceramsite together, and the main materials of the prepared porous light ceramsite are all wastes except a small amount of excitant, foaming agent and cement clinker, so that the production cost is greatly reduced, the problems of resource waste and environmental pollution are solved, and the wastes are recycled; 2) waste expanded polystyrene has the characteristics of light weight, easy removal and low cost, in order to obtain the expanded polystyrene microsphere modified by dopamine, the inventor firstly crushes the waste expanded polystyrene, treats the surface with alkali so as to activate the surface of the waste expanded polystyrene, then further modifies the surface by utilizing the dopamine, and treats the surface at high temperature in a nitrogen atmosphere so as to realize the preparation of the nitrogen-doped carbonized porous hollow spheres, and the nitrogen-doped carbonized porous hollow spheres have better porosity and ion adsorption performance, and the porous light ceramsite prepared by using the nitrogen-doped carbonized porous hollow spheres as a raw material can improve the metal ion adsorption performance in the aspect of ceramsite; 3) the phosphorus solid waste powder is used for replacing other industrial solid wastes, and is preferably phosphogypsum, because the phosphogypsum contains calcium sulfate dihydrate, a large amount of porous structures can be realized through heat treatment on the basis of replacing the original materials, and the prepared porous light ceramsite has the performance of high porosity. Compared with 10 parts by weight of phosphorus solid waste powder, 3-5 parts by weight of nitrogen-doped carbonized porous hollow spheres are added, so that the preparation cost of the material is increased excessively, the final strength of the ceramsite is influenced, the adsorption effect of the material is weakened excessively, and the self weight of the ceramsite is increased.
Has the advantages that:
the preparation method is simple, high in waste utilization rate, low in cost and environment-friendly, and the prepared porous light ceramsite is high in porosity, strong in heavy metal adsorption effect and decontamination capability, can be used for water body purification, and has important value for environmental protection.
Detailed Description
Example 1
Step 1: the recycled waste expanded polystyrene is crushed for 2 hours by a crusher and sieved to obtain the waste expanded polystyrene particles (the average fineness is 1 mu m, and the appearance of the particles is approximately spherical).
Step 2: and (3) mechanically stirring 10 parts by weight of the crushed old expanded polystyrene in 50 parts by weight of a sodium hydroxide aqueous solution with the concentration of 0.1mol/L for 6 hours, and filtering and washing to obtain the pretreated old expanded polystyrene microspheres.
And step 3: dispersing 10 parts by weight of old expanded polystyrene microspheres in 20 parts by weight of Tris-HCl buffer solution of dopamine with the concentration of 0.05g/L, mechanically stirring, treating for 12 hours, standing, washing and drying to obtain the polydopamine modified old expanded polystyrene microspheres.
And 4, step 4: 10 parts by weight of polydopamine-modified waste foamed polystyrene microspheres are placed in a tube furnace, the nitrogen-doped carbonized porous hollow spheres are obtained under the protection of nitrogen in a small atmosphere, the temperature is controlled at 350 ℃, and the holding time is 0.5 hour.
Step 5: mixing and stirring 10 parts by weight of phosphorus solid waste powder, 1 part by weight of gypsum alum, 1 part by weight of azodicarbonamide, 5 parts by weight of cement clinker and 3 parts by weight of nitrogen-doped carbonized porous hollow balls, granulating, and normally maintaining to obtain the novel porous light ceramsite.
The performance test data of the novel porous light ceramsite prepared by the embodiment are shown in Table 1
Example 2
Step 1: same as example 1
Step 2: and (3) mechanically stirring 10 parts by weight of the crushed old expanded polystyrene in 100 parts by weight of an ammonia water solution with the concentration of 0.5mol/L for 12 hours, and filtering and washing to obtain the pretreated old expanded polystyrene microspheres.
And step 3: dispersing 15 parts by weight of old expanded polystyrene microspheres in 30 parts by weight of Tris-HCl buffer solution of dopamine with the concentration of 2g/L, mechanically stirring, treating for 24 hours, standing, washing and drying to obtain the waste expanded polystyrene microspheres modified by polydopamine.
And 4, step 4: 20 parts by weight of polydopamine modified waste foamed polystyrene microspheres are placed in a tube furnace, the nitrogen protection atmosphere is small, the temperature is controlled at 550 ℃, and the holding time is 2 hours, so that the nitrogen-doped carbonized porous hollow spheres are obtained.
Step 5: mixing and stirring 10 parts by weight of phosphorus solid waste powder, 2 parts by weight of gypsum sodium sulfate, 2 parts by weight of diisopropyl azodicarboxylate, 10 parts by weight of cement clinker and 5 parts by weight of nitrogen-doped carbonized porous hollow spheres, granulating, and normally maintaining to obtain the novel porous light ceramsite.
The performance test data of the novel porous light ceramsite prepared by the embodiment are shown in Table 1
Example 3
Step 1: same as example 1
Step 2: and (3) mechanically stirring 10 parts by weight of the crushed old expanded polystyrene in 75 parts by weight of a 0.3mol/L water glass solution for 6 hours, and filtering and washing to obtain the pretreated old expanded polystyrene microspheres.
And step 3: dispersing 12.5 parts by weight of old expanded polystyrene microspheres in 25 parts by weight of Tris-HCl buffer solution of dopamine with the concentration of 1.025g/L, mechanically stirring, treating for 24 hours, standing, washing and drying to obtain the polydopamine modified old expanded polystyrene microspheres.
And 4, step 4: placing 15 parts by weight of polydopamine-modified waste foamed polystyrene microspheres in a tube furnace, keeping the temperature at 350-550 ℃ for 2 hours in a nitrogen protection atmosphere, and obtaining the nitrogen-doped carbonized porous hollow spheres.
Step 5: mixing and stirring 10 parts by weight of phosphorus solid waste powder, 1.5 parts by weight of sodium oxalate, 1.5 parts by weight of diethyl azodicarboxylate, 7.5 parts by weight of cement clinker and 4 parts by weight of nitrogen-doped carbonized porous hollow spheres, granulating, and normally maintaining to obtain the novel porous light ceramsite.
The performance test data of the novel porous light ceramsite prepared by the embodiment are shown in Table 1
Example 4
Step 1: same as example 1
Step 2: 10 parts by weight of the old expanded polystyrene obtained after the crushing is mechanically stirred and treated for 6 hours in 75 parts by weight of sodium hydroxide aqueous solution with the concentration of 0.4mol/L, and the pretreated old expanded polystyrene microspheres are obtained through filtration and water washing.
And step 3: dispersing 10 parts by weight of old expanded polystyrene microspheres in 30 parts by weight of Tris-HCl buffer solution of dopamine with the concentration of 1.5g/L, mechanically stirring, treating for 12 hours, standing, washing and drying to obtain the polydopamine modified old expanded polystyrene microspheres.
And 4, step 4: 20 parts by weight of polydopamine modified waste foamed polystyrene microspheres are placed in a tube furnace, the nitrogen protection atmosphere is small, the temperature is controlled at 550 ℃, and the holding time is 2 hours, so that the nitrogen-doped carbonized porous hollow spheres are obtained.
Step 5: mixing and stirring 10 parts by weight of phosphorus solid waste powder, 2 parts by weight of gypsum sodium sulfate, 2 parts by weight of diethyl azodicarboxylate, 10 parts by weight of cement clinker and 5 parts by weight of nitrogen-doped carbonized porous hollow spheres, granulating, and normally maintaining to obtain the novel porous light ceramsite.
The performance test data of the novel porous light ceramsite prepared by the embodiment are shown in Table 1
Comparative example 1
Step 3 is omitted, and the old expanded polystyrene microspheres obtained in step 2 are used to replace the polydopamine-modified old expanded polystyrene microspheres in step 4, and the rest is the same as in example 1.
Comparative example 2
In step 5, alum and azodicarbonamide were not added, as in example 1.
TABLE 1
The data of the comparative example and the comparative example on sewage treatment show that the waste polyethylene foam microspheres subjected to alkali treatment and dopamine modification can be well carbonized, and can show excellent adsorption performance after ceramsite is prepared; the use of the exciting agent and the foaming agent is also an important part of the good adsorption performance and the regeneration performance of the surface of the ceramsite.
Claims (6)
1. A preparation method of porous light ceramsite by taking phosphorus solid waste as a raw material is characterized by comprising the following steps:
step T1: placing the polydopamine modified expanded polystyrene microspheres in a tube furnace, controlling the temperature at 350-550 ℃ under the inert gas protection atmosphere, and keeping the temperature for 30 minutes-2 hours to obtain nitrogen-doped carbonized porous hollow spheres;
step T2: mixing and stirring 10 parts by weight of phosphorus solid waste powder, 1-2 parts by weight of gypsum excitant, 1-2 parts by weight of foaming agent, 5-10 parts by weight of cement clinker and 3-5 parts by weight of nitrogen-doped carbonized porous hollow spheres, granulating, and normally maintaining to obtain the porous light ceramsite.
2. The method for preparing porous light-weight ceramsite from "phosphorus solid waste" as defined in claim 1, wherein in said step T1, said inert gas is nitrogen or argon; in the step T2, the phosphorus solid waste powder is phosphogypsum powder with the particle size smaller than 0.075 mm.
3. The method for preparing porous light-weight ceramsite according to claim 1, wherein said gypsum excitant is one of alum, calcined alum, sodium sulfate and sodium oxalate, and said foaming agent is one of azodicarbonamide, diisopropyl azodicarboxylate or diethyl azodicarboxylate, in T2.
4. The method for preparing the porous light-weight ceramsite taking the phosphorus solid waste as the raw material according to any one of claims 1 to 3, wherein the polydopamine modified expanded polystyrene microspheres are prepared by the following method:
step S1: crushing and sieving waste expanded polystyrene by a crusher to obtain waste expanded polystyrene particles with the particle size of 200 nm-1 mu m;
step S2: adding 10 parts by weight of old expanded polystyrene particles into an alkaline solution, mechanically stirring for 6-12 hours, and filtering and washing to obtain pretreated old expanded polystyrene microspheres;
step S3: preparing a Tris-HCl buffer solution with the concentration of 0.05-2 g/L of dopamine, adding 10-15 parts by weight of old expanded polystyrene microspheres to uniformly disperse, mechanically stirring for 12-24 hours, standing, washing and drying to obtain the polydopamine modified expanded polystyrene microspheres.
5. The method for preparing porous light-weight ceramsite of claim 4, wherein in step S2, said alkaline solution is one of sodium hydroxide solution, ammonia water or water glass; the concentration of the alkaline solution is 0.1-0.5 mol/L, and the addition amount is 50-100 parts by weight.
6. The method for preparing porous light-weight ceramsite of claim 4, wherein said Tris-HCl buffer solution has a concentration of 0.01mol/L and a pH of 7.3 + 0.1 in said step S3.
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| CN115124364A (en) * | 2022-07-04 | 2022-09-30 | 湖南工学院 | Light high-strength ceramsite based on solid waste and preparation method thereof |
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