CN107973559B - Preparation method and application of porous geopolymer microspheres - Google Patents
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Abstract
The invention discloses a preparation method of porous geopolymer microspheres, which adopts a dispersion suspension solidification method to prepare the porous geopolymer microspheres. Compared with the prior art, the invention realizes low-temperature solidification and one-step molding granulation without high-temperature calcination and solidification and addition of other additives. Meanwhile, the invention also realizes the mass use of the solid wastes, and has the advantages of wide raw material source, low cost, simple process and no toxicity or pollution in the whole process. In addition, the porous geopolymer microspheres prepared by the method have high efficiency, and the balling degree exceeds 90 percent; the particle size is adjustable, and the pore diameter is uniformly distributed; the pore volume is large and controllable, and the specific surface area of the microsphere reaches 110m2And/g, can be directly used for a packed column of column separation. Tests show that the porous geopolymer microsphere has a good heavy metal adsorption effect, can be used as a heavy metal adsorbent, and has a wide application prospect in the aspect of removing heavy metals and radioactive elements in water.
Description
Technical Field
The invention belongs to the technical field of adsorbent carriers, and particularly relates to a preparation method and application of porous geopolymer microspheres.
Background
The column separation method is an effective method for removing heavy metals and radioactive elements in water, partial adsorbing materials such as zeolite molecular sieves and activated carbon can be directly filled into columns, but organic solvents or inorganic adsorbing materials with small particle sizes can be used only by being carried on spherical particle carriers with proper particle sizes. At present, silica gel, polymer-based composite materials and macroporous silicon-based materials are developed and utilized, and the application range of a column separation method is widened. However, the production process is complex and the cost is high, which limits the industrial application.
The geopolymer is prepared by exciting aluminosilicate-containing raw materials (including natural products, artificially synthesized powder, industrial wastes and the like) at normal temperature or high temperature through acidic or alkaline substances4]And [ SiO ]4]Tetrahedral three-dimensional network inorganic gelling materials. Geopolymer phase comparisonOther inorganic polymers have the advantages of excellent performance, simple preparation process, low energy consumption, environmental friendliness and the like, and can be widely applied to the fields of building materials, nuclear waste treatment, casting, metallurgy, refractory materials, plastics and the like. At present, the porous inorganic microspheres prepared at home and abroad mainly adopt a high-temperature calcination method, and the preparation process is complicated and the cost is high.
Disclosure of Invention
The invention aims to provide a simple, cheap and environment-friendly preparation method and application of porous geopolymer microspheres.
In order to solve the technical problems, the invention adopts the following technical scheme:
the preparation method of the porous geopolymer microspheres adopts a dispersion suspension solidification method and specifically comprises the following operations: and mixing and stirring the powder with alkali-activated activity and an alkali solution uniformly to obtain mixed slurry, slowly adding the uniformly dispersed pore-forming agent aqueous solution into the mixed slurry, continuously stirring, finally dripping the uniformly stirred slurry into the high-speed dispersed hot dimethyl silicone oil, curing in an oven, pouring out the cured synthetic product from the dimethyl silicone oil, filtering and calcining to obtain the composite material.
The powder with alkali excitation activity is slag, steel slag, water granulated slag, fly ash, silicon micropowder, red mud, metakaolin and synthetic powder.
The alkaline solution is a solution of sodium water glass, potassium water glass, sodium hydroxide, potassium hydroxide, lithium hydroxide, strontium hydroxide, cesium hydroxide, carbonate, bicarbonate, sulfate, bisulfate, aluminate, and aluminosilicate.
The pore-forming agent is calcium carbonate, ammonium bicarbonate, sodium bicarbonate, polyethylene glycol, polymethyl methacrylate, polyvinyl chloride, polyvinyl alcohol, sodium alginate and polystyrene.
The preparation method of the porous geopolymer microspheres comprises the following steps:
(1) preparing slurry: mixing and stirring the powder with alkali-activated activity and an alkali solution uniformly to form mixed slurry, then slowly adding the uniformly dispersed pore-forming agent aqueous solution into the mixed slurry, and continuously stirring, wherein the stirring speed is 500-4000 revolutions per minute, and stirring for 1-5 minutes to form a uniform slurry;
(2) balling: dripping the uniform slurry obtained in the step (1) into high-speed dispersed hot dimethyl silicone oil;
(3) and (3) curing: putting the dimethyl silicone oil obtained in the step (2) and the obtained product into an oven for curing and solidification;
(4) and (3) filtering: performing vacuum filtration on the dimethyl silicone oil obtained in the step (3) and the obtained product to obtain geopolymer microspheres;
(5) and (3) calcining: and (4) calcining the geopolymer microspheres obtained in the step (4) in a muffle furnace to obtain the porous geopolymer microspheres.
In the step (1), the powder with alkali-activated activity is calculated by slag, the alkali solution is calculated by sodium silicate, the solvent is calculated by water, and the pore-forming agent is calculated by polymethyl methacrylate, wherein the mass ratio of the slag to the sodium silicate to the water to the polymethyl methacrylate is 1:0.1-0.7: 0-0.005.
The temperature of the hot dimethyl silicone oil in the step (2) is 40-150 ℃, and the stirring speed is 200-2000 r/min;
the temperature of the oven in the step (3) is 50-150 ℃, and the curing time is 5 minutes-48 hours;
the calcining temperature in the step (5) is 200-900 ℃, and the calcining time is 0.5-12 hours.
The porous geopolymer microspheres prepared above are used as adsorbents.
The porous geopolymer microspheres prepared by the method are used as heavy metal or radioactive element adsorbents.
The average particle size of the porous geopolymer microspheres is 5-500 microns, the porosity is 10-60%, and the specific surface area is 20-120m2/g。
Aiming at the problems of the existing porous inorganic microspheres and preparation thereof, the inventor establishes a preparation method of the porous geopolymer microspheres, adopts a dispersion suspension solidification method, and specifically comprises the following steps: mixing and stirring the powder with alkali-activated activity and an alkali solution uniformly to form a mixed slurry, and then slowly adding the uniformly dispersed pore-forming agent aqueous solutionAdding the mixture into the mixed slurry, continuously stirring, finally dripping the uniformly stirred slurry into the high-speed dispersed thermal dimethyl silicone oil, curing the mixture by using an oven, pouring out the cured synthetic product from the dimethyl silicone oil, filtering and calcining the product to obtain the high-performance composite material. Compared with the prior art, the invention realizes low-temperature solidification and one-step molding granulation without high-temperature calcination and solidification and addition of other additives. Meanwhile, the invention also realizes the mass use of the solid wastes, and has the advantages of wide raw material source, low cost, simple process and no toxicity or pollution in the whole process. In addition, the porous geopolymer microspheres prepared by the method have high efficiency, and the balling degree exceeds 90 percent; the particle size is adjustable, and the pore diameter is uniformly distributed; the pore volume is large and controllable, and the specific surface area of the microsphere reaches 110m2And/g, can be directly used for a packed column of column separation. Tests show that the porous geopolymer microsphere has good adsorption effect on heavy metals and radioactive elements, can be used as a heavy metal adsorbent, and has wide application prospect in the aspect of removing the heavy metals and the radioactive elements in water.
Drawings
Figure 1 is an optical microscope micrograph (50 x) of porous geopolymeric microspheres prepared using the preparation method of the present invention.
FIG. 2 is a scanning electron micrograph (1000 times) of porous geopolymer microspheres prepared using the preparation method of the present invention.
FIG. 3 is a scanning electron micrograph (2000 times) of porous geopolymer microspheres prepared using the preparation method of the present invention.
Detailed Description
Example 1
(1) Preparing slurry: mixing 30g of slag and 12g of liquid sodium silicate (modulus 2.5) and stirring uniformly to obtain mixed slurry, then slowly adding the uniformly dispersed pore-forming agent aqueous solution (3g of calcium carbonate and 5g of water) into the mixed slurry and stirring continuously, wherein the stirring speed is 500 revolutions per minute, and the stirring is carried out for 2 minutes, so that the system becomes uniform slurry;
(2) balling: dripping the uniform slurry obtained in the step (1) into high-speed dispersed hot dimethyl silicone oil, wherein the temperature is 50 ℃, and the stirring speed is 200 revolutions per minute;
(3) and (3) curing: putting the dimethyl silicone oil obtained in the step (2) and the obtained product into an oven for curing and solidifying, wherein the temperature is 60 ℃, and the curing and solidifying time is 1 hour;
(4) and (3) filtering: performing vacuum filtration on the dimethyl silicone oil obtained in the step (3) and the obtained product to obtain geopolymer microspheres;
(5) and (3) calcining: and (4) calcining the geopolymer microspheres obtained in the step (4) in a muffle furnace at 700 ℃ for 12 hours to obtain the porous geopolymer.
Through detection, the particle diameter of the microsphere is 5-300 mu m, and the pore volume is 0.1998cm3Per gram, specific surface area 35.36m2/g。
0.06g of the resulting porous geopolymer was weighed out in 100mL of Pb at a concentration of 150ppm2+The adsorbed amount was 268.7mg/g in 24 hours of solution.
Example 2
(1) Preparing slurry: mixing 20g of slag and 8.57g of liquid sodium silicate (modulus 1.5) and stirring uniformly to obtain mixed slurry, then slowly adding the uniformly dispersed pore-forming agent aqueous solution (10g of calcium carbonate +10g of water) into the mixed slurry and stirring continuously, wherein the stirring speed is 1000 revolutions per minute, and the stirring is carried out for 1 minute, so that the system becomes uniform slurry;
(2) balling: dripping the uniform slurry obtained in the step (1) into high-speed dispersed hot dimethyl silicone oil, wherein the temperature is 100 ℃, and the stirring speed is 500 revolutions per minute;
(3) and (3) curing: putting the dimethyl silicone oil obtained in the step (2) and the obtained product into an oven for curing and solidifying, wherein the temperature is 70 ℃, and the curing and solidifying time is 12 hours;
(4) and (3) filtering: performing vacuum filtration on the dimethyl silicone oil obtained in the step (3) and the obtained product to obtain geopolymer microspheres;
(5) and (3) calcining: and (4) calcining the geopolymer microspheres obtained in the step (4) in a muffle furnace at 500 ℃ for 12 hours to obtain the porous geopolymer.
Through detection, the particle diameter of the microsphere is 50-500 mu m, and the pore volume is 0.2498cm3Specific surface area 65.48 m/g2/g。
0.08g of the resulting porous geopolymer was weighed out in 100mL of Pb at a concentration of 300ppm2+The adsorbed amount was 301.5mg/g after 36 hours in solution.
Example 3
(1) Preparing slurry: mixing and stirring 20g of metakaolin, 10g of slag and 12g of sodium hydroxide solution (the concentration is 10 mol) uniformly to form mixed slurry, then slowly adding the uniformly dispersed pore-forming agent aqueous solution (2g of polymethyl methacrylate and 25g of water) into the mixed slurry, continuously stirring, uniformly mixing, wherein the stirring speed is 300 revolutions per minute, and stirring for 5 minutes to form uniform slurry in a system;
(2) balling: dripping the uniform slurry obtained in the step (1) into high-speed dispersed hot dimethyl silicone oil, wherein the temperature is 90 ℃, and the stirring speed is 700 revolutions per minute;
(3) and (3) curing: putting the dimethyl silicone oil obtained in the step (2) and the obtained product into an oven for curing and solidifying, wherein the temperature is 90 ℃, and the curing and solidifying time is 1 hour;
(4) and (3) filtering: performing vacuum filtration on the dimethyl silicone oil obtained in the step (3) and the obtained product to obtain geopolymer microspheres;
(5) and (3) calcining: and (4) calcining the geopolymer microspheres obtained in the step (4) in a muffle furnace at 800 ℃ for 12 hours to obtain the porous geopolymer.
The detection shows that the particle size of the microsphere is 10-300 mu m, and the pore volume is 0.1836cm3Specific surface area of 28.75 m/g2/g。
0.06g of the resulting porous geopolymer was weighed out in 30mL of Sr at a concentration of 50ppm2+The adsorbed amount was 30.65mg/g in the solution for 1 hour.
Example 4
(1) Preparing slurry: mixing 30g of metakaolin and 20g of sodium hydroxide solution (the concentration is 8 mol) uniformly to form mixed slurry, then slowly adding the uniformly dispersed pore-forming agent aqueous solution (10g of polymethyl methacrylate and 15g of water) into the mixed slurry, continuously stirring, uniformly mixing, wherein the stirring speed is 1200 revolutions per minute, and stirring for 1 minute to enable the system to form uniform slurry;
(2) balling: dripping the uniform slurry obtained in the step (1) into high-speed dispersed hot dimethyl silicone oil, wherein the temperature is 40 ℃, and the stirring speed is 200 revolutions per minute;
(3) and (3) curing: putting the dimethyl silicone oil obtained in the step (2) and the obtained product into an oven for curing and solidifying, wherein the temperature is 60 ℃, and the curing and solidifying time is 2 hours;
(4) and (3) filtering: performing vacuum filtration on the dimethyl silicone oil obtained in the step (3) and the obtained product to obtain geopolymer microspheres;
(5) and (3) calcining: and (4) calcining the geopolymer microspheres obtained in the step (4) in a muffle furnace at the temperature of 400 ℃ for 12 hours to obtain the porous geopolymer.
Through detection, the particle diameter of the microsphere is 20-400 mu m, and the pore volume is 0.2798cm3Specific surface area of 100.56 m/g2/g。
0.06g of the resulting porous geopolymer was weighed out in 30mL of Sr at a concentration of 150ppm2+The adsorbed amount was 50.54mg/g in the solution for 2 hours.
Claims (4)
1. A preparation method of porous geopolymer microspheres is characterized by comprising the following steps:
(1) preparing slurry: mixing and stirring the powder with alkali-activated activity and an alkali solution uniformly to form mixed slurry, then slowly adding the uniformly dispersed pore-forming agent aqueous solution into the mixed slurry, and continuously stirring, wherein the stirring speed is 500-4000 revolutions per minute, and stirring for 1-5 minutes to form a uniform slurry; the powder with alkali excitation activity is calculated by slag, an alkali solution is calculated by sodium silicate, a solvent is calculated by water, and a pore-forming agent is calculated by polymethyl methacrylate, wherein the mass ratio of the slag to the sodium silicate to the water to the polymethyl methacrylate is 1:0.1-1:0.1-0.7: 0-0.005;
(2) balling: dripping the uniform slurry obtained in the step (1) into high-speed dispersed hot dimethyl silicone oil; the temperature of the hot dimethyl silicone oil is 40-150 ℃, and the stirring speed is 200-2000 r/min;
(3) and (3) curing: putting the dimethyl silicone oil obtained in the step (2) and the obtained product into an oven for curing and solidification; the temperature of the oven is 50-150 ℃, and the curing time is 5 minutes-48 hours;
(4) and (3) filtering: performing vacuum filtration on the dimethyl silicone oil obtained in the step (3) and the obtained product to obtain geopolymer microspheres;
(5) and (3) calcining: calcining the geopolymer microspheres obtained in the step (4) in a muffle furnace to obtain porous geopolymer microspheres; the calcining temperature is 200-900 ℃ and the calcining time is 0.5-12 hours;
the powder with alkali excitation activity is slag, steel slag, water granulated slag, fly ash, wollastonite powder, silica micropowder, red mud, metakaolin and synthetic powder; the alkali solution is a solution of sodium water glass, potassium water glass, sodium hydroxide, potassium hydroxide, lithium hydroxide, strontium hydroxide, cesium hydroxide, carbonate, bicarbonate, sulfate, bisulfate, aluminate and aluminosilicate; the pore-forming agent is calcium carbonate, ammonium bicarbonate, sodium bicarbonate, polyethylene glycol, polymethyl methacrylate, polyvinyl chloride, polyvinyl alcohol, sodium alginate and polystyrene.
2. Porous geopolymeric microspheres made according to claim 1 for use as adsorbents.
3. The porous geopolymeric microspheres of claim 1 used as heavy metal or radioactive element adsorbents.
4. The adsorbent according to any one of claims 2 or 3, wherein: the average particle size of the porous geopolymer microspheres is 5-500 micrometers, the porosity is 10-60%, and the specific surface area is 20-120m2/g。
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